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1070-150 Rev. B5 PQ

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1. ssssss A 3 A 4 AC Transport option affecting available current A 4 A 5 using AC board A 3 A 4 Alcatel pump illustration 4 24 C 2 maintenance 4 23 4 27 C 1 C 6 maintenance schedule C 2 Oll ecce taies 4 25 C 3 Altitude effects 1 8 Alumina activated chiecking eter C 5 C 6 maintenance schedule C 2 replacing oe ai a C 5 C 6 Analog outputs in illustration of Model 6000 ports A 2 linking parameters 2 9 3 10 A 5 Annulus See Cooling annulus Annulus port Tti ctlon iocus etie inen A 7 in illustration of Model 6000 ports A 2 Atmospheric control 3 6 3 7 Aux 2A fuse FUNGUO sess costes oett ee trt oe et aces A 8 in illustration of Model 6000 ports A 2 replacement values ssse A 23 Auxiliary expansion connections pinout tables ssssssssssss A 19 Auxiliary signal drives 4 17 B Bellows metal TUN ctlon ioc cete eddies 2 4 in illustration of probe components 2 4 Black Lemo connector function nee etie A 10 in illustration of probe head ports A 9 pinout table sssssssss A 13 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 Blue Lemo connector MUINCUON 4 ste eo
2. Immediately vent the room by opening windows and doors if there is an excessive helium release If there is any amount of liquid helium in the PPMS dewar use the procedures described here to transfer helium into the dewar If there is no liquid helium in the dewar you must use one of the warm dewar fill procedures in Appendix B to prevent blockages in the impedance tube To facilitate the liquid helium transfer we recommend that you review the process before you begin If you are unfamiliar with these transfers ask for help from someone who is familiar with the supply vessel 1 Bring the helium supply dewar close to the PPMS dewar 2 Verify that the proper adapters and extensions are installed on the helium transfer line see Figure 4 17 Important The extensions perform an essential function The input extension ensures that liquid can always enter the transfer line even as the level of liquid in the storage dewar changes A short extension is used on the output line to help reduce boil off from the transfer It is less cumbersome than the long one used for transfers into a warm dewar see Appendix B OUTPUT PPMS END INPUT SUPPLY END i OUTPUT ADAPTER SHORT OUTPUT INPUT ADAPTER i EXTENSION INPUT EXTENSION Figure 4 17 Helium transfer line arrangement with the short output extension used for helium transfers into a cold dewar Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4
3. WARNING Do not remove disable or otherwise tamper with the dewar rupture disk or the pressure relief valves Any type of modification can lead to dangerous operating conditions When liquid helium or nitrogen boils and expands in a sealed container such as the PPMS dewar it can cause large pressure buildups Explosions can occur if this pressure is not relieved The PPMS dewar and probe contain pressure relief valves and rupture disks to allow gaseous cryogens to escape before dangerous pressures are reached Figure 1 2 illustrates these safety features OPENS AT 10 PSIG OPENS AT 4 PSIG PRESSURE RELIEF VALVE D OPENS AT 1 PSIG F ira ee VU i a RUPTURE DISK PRESSURE RELIEF VALVES JRES BETWEEN OPEN AT 1 PSIG PSIG NITROGEN FILL PORT WITH PRESSURE RELIEF VALVE Figure 1 2 Pressure relief valves and rupture disk on PPMS dewar and probe head 1 4 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 1 Section 1 4 Introduction and System Setup Safety Precautions WARNING If a dewar ruptures or cryogenic materials spill vent the room immediately and evacuate all personnel Only perform cryogen transfers when you are in a well ventilated room Cryogens expand to hundreds of times their liquid volume when they boil which occurs well below room temperature A relatively small volume of liquid nitrogen or helium can
4. 8 At the liquid helium supply dewar set the valves and liquid access port a Vent the pressure by slightly opening the gas phase valve b Close the gas phase valve after the pressure has been reduced c Open the liquid access port This port is open only during the transfer d Close the primary relief valve This valve remains closed only during the transfer 9 At the PPMS dewar open one of the two helium fill ports on the probe head by pulling the entire fill port fixture straight up see Figure 4 19 10 Simultaneously insert a the output end of the transfer line into the PPMS dewar through the open helium fill port and b the input end of the transfer line into the liquid helium supply dewar through the liquid access port see Figures B 1 and B 2 Carefully lower both ends of the transfer line completely into the dewars and seat the adapters in their respective ports Gas will begin flowing from the output adapter Point the output adapter exhaust tube away from all hardware on top of the dewar The exhaust will get extremely cold and could damage some of the parts especially O rings and sealed valves CAUTION Point the output adapter exhaust tube away from all hardware on the dewar and probe head The extremely cold exhaust can damage parts especially O rings and sealed valves 12 Verify that each adapter on the transfer line is properly seated and is sealing the transfer line Quantum Design PPMS Hardw
5. C 6 PPMS Vacuum Pump Assembly Service Record Use this service record to help schedule and track servicing of the vacuum pump assembly see Sections 4 7 4 and C 2 C 5 We provide two blank sheets for your convenience Pump Assembly COMPONENT MANUFACTURER SERIAL NUMBER a SERVICE TYPE SERVICE DATE Change rotary vane pump oil Empty oil in oil mist filter Change oil mist filter cartridge Check activated alumina in foreline trap Change activated alumina in foreline trap Other explain COMMENTS Quantum Design PPMS Hardware Manuall 1070 150 Rev B5 C 7 February 2008 Section C 6 Appendix C PPMS Vacuum Pump Assembly Service Record Vacuum Pump Assembly Maintenances SERVICE TYPE SERVICE DATE Change rotary vane pump oil Empty oil in oil mist filter Change oil mist filter cartridge Change activated alumina in foreline trap Other explain mM HEN COMMENTS C 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 References Quantum Design 1995 Physical Property Measurement System Commands Manual 1996 Physical Property Measurement System Firmware Manual 1998 Physical Property Measurement System PPMS MultiVu Application User s Manual Quantum Design PPMS Hardware Manual 1070 150 Rev B5 References 1 February 2008 Index A A1 port See Analog outputs AC board idco hsc A 3 A 4 ACMS option affecting available current A 4 A 5 using AC board
6. Weekly or sooner depending on the amount of use check the amount of oil that has collected in the bell jar that surrounds the oil mist filter If the filter becomes too full oil can back up into the gas lines and plug the system Monthly or sooner depending on the amount of use check the oil level in the pump refill it to the full mark with the appropriate oil see Table 4 4 and check the status of the filter cartridge l 2 Quantum Design Open the front panel of the electronics cabinet Figure 4 20 illustrates the cabinet and pump Look at the oil level window on the front of the pump The oil level should be between the two outer markings see Figure 4 21 Table 4 4 gives the specific level for each pump If the pump needs more oil first check whether the oil needs to be changed While the cabinet is open compare the oil in the pump to clean oil a Ifthe pump oil is clean use the instructions in Section 4 7 3 2 to add oil b Ifthe pump oil is dirty use the instructions in Appendix C to drain the pump and replace the oil Check the amount of oil in the oil mist filter and container a Ifthe container is half full use the instructions in Section 4 7 3 2 to empty it unless you also need to change the filter cartridge In the latter case use the instructions in Appendix C b Ifthe filter cartridge looks like it is full of oil use the instructions in Appendix C to install a new one PPMS Hardware Manual 1
7. Chapter 3 Section 3 9 Theory of Operation Experimental Considerations When you mount a sample it is important to secure it with a method that will withstand the experimental extremes Be sure to determine the thermal magnetic and conductive properties of the bonding media before using it in an important experiment The temperature range of the PPMS is 1 9 400 K The magnetic field available depends on the magnet that is purchased with the system Other properties of the bonding media and of any electrical leads could also be important For example with thin film samples the leads and bonding media must not chemically react with the sample The sample puck is conductive so when you use it as a mounting technique verify that the electrical leads are isolated and individually insulated When using the sample puck you also need to consider how the sample might interact with it often samples must not be in electrical contact with the puck Note that thermal contact with the puck 1s still desired in the latter cases You can use a substance such as sapphire to electrically isolate resistive samples from the puck and still allow good thermal contact A thin layer of Kapton tape serves as a less expensive substitute For experiments that use other sample holders you should consider the relevant properties of the sample holder For example for DC magnetization measurements you can use a clear plastic drinking straw as a sample holder because the s
8. as sample holder 2 11 connections pinout table A 12 dimensions sees 2 11 3 12 inserting in sample chamber 4 12 4 14 removing connector PC board 4 10 4 11 removing from sample chamber 4 14 4 15 sample interface illustration 2 11 A 12 verifying electrical connections 2 13 4 11 4 12 Puck adjustment tool function once 2 12 2 13 illustration eeeeeeeeeeessss 4 18 USING a ict ee Dee e 4 18 Puck insertion puck extraction tool illustration 2 12 4 12 USING s eee ete 4 12 4 15 Puck wiring test station 2 13 4 11 Pump adding oil eer 4 23 4 27 as part of base hardware 1 2 checking activated alumina C 2 C 5 C 6 checking oil level 4 23 4 25 C 2 components illustration 2 11 4 24 connections block diagram A 1 foreline trap 4 18 4 24 C 2 C 5 C 6 function esesesssss 2 10 3 2 4 23 illustration 4 24 C 1 C 2 oc ERE 4 25 C 3 replacing oil seesese C 2 C 4 safety precautions esses 1 6 service periodici EE e e ound wand C 1 C 6 TOUTING cc cepa ceteri 4 18 4 23 4 27 versions sss 4 24 4 25 C 2 Pump por
9. 000 Oe before the persistence switch heater is turned off The field that 1s reported 1s calculated from the drop across the resistor The temperature coefficient of the calibration resistors in the Model 6700 is nominally 30 ppm C so variations in the temperature of the instrument might have very small effects on the reported field Notice that the field reported by the PPMS is only that due to the current through the magnet circuit the reported field value does not account for any background sources or remnant field in the magnet 3 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 3 Section 3 6 Theory of Operation Helium Level Metering After the persistence switch heater is turned off magnetic field relaxation or flux creep can still occur To minimize this effect the PPMS offers a specific magnet charging technique called Oscillate mode which is described in Section 3 5 3 52 Magnetic Field Approach Modes The PPMS uses Oscillate mode No Overshoot mode or Linear mode to approach a field set point In Oscillate mode the magnet controller allows the magnet to overshoot or undershoot the field set point by about 30 if possible and then narrows in on the set point in an oscillatory fashion under shooting or overshooting the set point by 30 on each iteration Oscillate mode can undesirably affect samples that show field hysteresis behavior Oscillate mode is best used to help eliminate field relaxa
10. 3 e ern e Ee d ie needed 4 3 Helium levels relative to probe and 9 T magnet sess 4 5 Opening the Send GPIB Command utility in MultiVu eese 4 7 Using the Send GPIB Command dialog to verify control mode 4 7 Switching from pot fill mode to CLTC sss 4 8 Verifying that CLTC is the low temperature control mode ssesss 4 8 Checking the low temperature control mode using the Mon6000 dialog 4 9 Switching low temperature control modes using the Mon6000 dialog 4 9 Sample mounted on PUCK eee erre iet na etie t boe eiTe ia nas 4 11 Intermediate sample leads sese 4 11 Checking for proper electrical connection of the sample sss 4 12 Handle of puck insertion puck extraction tool disengaged and engaged 4 12 Inserting the puck into the cylinder of puck insertion tool ssuss 4 12 Custom adapter for making connections to the sample leads 4 16 P ck adjustmenf tool iei tne ertet eee dee eei I E Hehe a 4 18 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Figure 4 16 Figure 4 17 Figure 4 18 Figure 4 19 Figure 4 20 Figure 4 21 Figure 4 22 Figure A 1 Figure A 2 Figure A 3 Figure A 4 Figure A 5 Figure A 6 Figure A 7 Figure A 8 Figure A 9 Figu
11. 4 2 2 1 Power Loss eov ret ed e ee Re Hr et rhe pee ern e ee e ER ee 4 2 4 22 2 Power Off Sequere eret citi ene dette deste into re dne e RE eee deseen CERERI De 4 3 4 2 2 3 Power Om Sequence eu eire edet ere erede eek E eee eese terea 4 4 42 3 Shutdown MOdSe center tet ee ie EEEE EEE 4 4 4 2 4 Monitoring the Helium Level esee enne ener 4 5 vi PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Contents Table of Contents 4 2 4 1 Helium Levels Using a Magnet sssssesssseseeeeereeenenee nennen nnns 4 5 4 2 4 2 Helium Levels Not Using a Magnet ssssssseseeeeeeeenenenne eene enne 4 5 4 2 5 Monitoring the Nitrogen Level sess 4 6 4 3 Setting the Low Temperature Control Mode ssssessesseeeeeeeeeeeenenennn 4 6 2 31 y MULE VU 4t eter e TP E BEER ERR OSEE LIENS 4 7 4 3 1 1 Verify Option and Control Mode sse ener 4 7 4 3 1 2 Change Low Temperature Control Mode sese 4 8 4 22 MORHODUO scien etaient pisei auti ebd idle a paso mal dott fel uu ive ua pid 4 9 4 4 Sample Mounting irt pete donee eei epatis leeqeerie edoceri d e eiie 4 10 4 4 1 Guidelines for Mounting Samples sess enne 4 10 4 4 2 Mounting a Sample on a Sample Puck ssssssssssssseeeereeenrenenenne 4 10 4 5 Sample Puck Installation and Removal essere eene 4 12 4 5 L Installing a Sample Puck etr tde
12. At the liquid nitrogen supply dewar close the liquid supply valve on the nitrogen supply line when the exhaust turns to liquid this indicates that the jacket is full It will take about 1 hour to fill the jacket of a warm dewar because most of the liquid nitrogen will evaporate until the jacket walls have cooled At the PPMS dewar remove the liquid nitrogen transfer adapter and re install the nitrogen fill port fittings a Put on your protective gear so that you do not receive serious burns from the extremely cold fitting supply line and transfer adapter b Remove the liquid nitrogen transfer adapter by turning the brass fitting counter clockwise and lifting the transfer adapter out of the dewar In the event that the fitting and adapter are frozen together you can use a warm air blower to accelerate the thawing process Otherwise you must wait until the parts thaw enough to be separated c Close both nitrogen fill ports by reinstalling the brass fittings and turning the large brass fittings clockwise PPMS Hardware Manual 1070 150 Rev B5 B 9 February 2008 Section B 3 Appendix B Warm Fill Nitrogen Jacketed Dewars Filling Warm Dewars CAUTION Always re install the fill port fittings and or O rings onto the nitrogen fill ports after you have transferred liquid nitrogen into the dewar These fittings prevent dangerous ice blockages in the fill ports d Periodically hold a wetted finger in front of the hose nipple on th
13. Re Install Pump isere raens tansi a eene nennen nennen nnns C 4 CS Servicing the Eoreline Trap tone edet inte C 5 C5 1 1 Prepare PPMS for ServiGe oit ier rete eet en eer dete oda S C 5 C 5 1 2 Remove Alumina Canister and Examine the Pellets sss C 5 C 5 1 3 Reassemble the Canister Trap and Pump sese C 6 C 6 PPMS Vacuum Pump Assembly Service Record sese C 7 IRE BEC Ed UR CUS etc c References 1 i TUIS Qa Index 1 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 ix February 2008 Contents Table of Figures Figures Figure 1 1 Figure 1 2 Figure 2 1 Figure 2 2 Figure 2 3 Figure 2 4 Figure 2 5 Figure 2 6 Figure 2 7 Figure 2 8 Figure 2 9 Figure 2 10 Figure 2 11 Figure 2 12 Figure 2 13 Figure 2 14 Figure 3 1 Figure 3 2 Figure 3 3 Figure 3 4 Figure 3 5 Figure 3 6 Figure 4 1 Figure 4 2 Figure 4 3 Figure 4 4 Figure 4 5 Figure 4 6 Figure 4 7 Figure 4 8 Figure 4 9 Figure 4 10 Figure 4 11 Figure 4 12 Figure 4 13 Figure 4 14 Figure 4 15 Components of the base PPMS and approximate dimensions measurements are rounded sse 1 2 Pressure relief valves and rupture disk on PPMS dewar and probe head 1 4 Top view and cross section of a standard dewar see 2 2 Top view and cross section of a nitrogen jacketed dew
14. VIG ovenans E E EEEO E RE B 1 B 2 Helium and Nitrogen Transfers into Warm Dewars ssessseeeeeeeneeneen nennen B 1 B 2 1 Nitrogen Jacketed Dewars ssssssseseseesee eene nennen nennen nnne B 2 B 2 2 Standard Dewarsc eate ieu serta oe dei rt He a rev Edad B 2 B 2 3 Material uni eer ODD BI ove QR S REI E REOR REC IEER vas B 2 B 3 Warm Fill Nitrogen Jacketed Dewars ssseeseeeeeeeeeeeee nennen nene ener enne B 3 viii PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Contents Table of Contents B 3 1 Simultaneous Nitrogen and Helium Transfer B 3 B 3 2 Sequential Nitrogen and Helium Transfers esses B 7 B 4 Warm Fill Standard Dewars sss eene enne nennen B 12 APPENDIX C Vacuum Pump Assembly Maintenance ecce esee ee eene ee enne en nne en setas seen sete tastes se tena seno C 1 C1 Introductionis Evo ee tero tibt et b e werte dr RS C 1 C 2 Vacuum Pump Assembly 5 2 6e ed e teet EN eee ior bce Euge iode i ode doe C 1 OHE PUMP Versiotis isa etie ee iE t cire e Ere dig ie RE IR Pique dides C 2 C 4 Changing the Pump Oil and Oil Mist Cartridge essessssssseseeeeeeeeneenee enn C 3 4 11 Prepare PPMS for Service ote ae nte tet eer eerta teda C 3 C412 Drain Pump Oll tete ettet ete En RR te Rente a Leto deed pe eot dgd C 4 C 4 1 3 Drain Replace Oil Mist Filter Cartridge essere C 4 C 4 1 4 Fill and
15. a magnet related question or encounter a problem when you are using a magnet contact Customer Service at Quantum Design Model 6700 Magnet Controller CAUTION Do not alter or remove the connection from the Model 6700 to the P7 Magnet port on the Model 6000 Altering or removing this connection could destroy the 24 V power supply in the Model 6000 and or Model 6700 and void the manufacture s warranty The Model 6700 Magnet Controller Figure 2 8 is a bipolar power supply that allows smoother ramping through zero 0 field than traditional one sided power supplies As is discussed in Section 3 5 the Model 6700 uses four different approach modes to control charging and discharging of the magnet MODEL 6700 MAGNET CONTROLLER Figure 2 8 Front panel of the Model 6700 Magnet Controller Quantum Design PPMS Hardware Manual 1070 150 Rev B5 2 9 February 2008 Section 2 8 Chapter 2 Electronics Cabinet Hardware 2 7 1 1 MODEL 6700 MAGNET CONTROLLER FRONT PANEL There are three LEDs on the front panel of the Model 6700 the Logic Power LED which is lit when the Model 6000 is powered on and the DC Enable and On Line LEDs which are lit whenever the system is deliberately charging or discharging the magnet 2 7 1 2 MODEL 6700 MAGNET CONTROLLER REAR PANEL The rear panel of the Model 6700 has a power switch that indirectly turns off the current to the magnet Never turn off the power to the Model 6700 w
16. adding gas sources gauges and pumps see Section 3 4 The complexity of the system allows several different ways to set up the same experiment The automated sequence feature of the PPMS lets you automate the entire measurement process Any function the Model 6000 can perform including controlling all PPMS hardware and recording measurement values can be accessed within a sequence file that runs automatically so you can perform an experiment without being present Try exploring this feature The Sequence Files section in the Physical Property Measurement System Commands Manual discusses measurement automation in detail The Physical Property Measurement System PPMS MultiVu Application User s Manual discusses how to use PPMS MultiVu sequence files and sequence commands PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 3 Section 3 8 Theory of Operation Example Measurement If the Model 6000 does not have the specifications necessary for your experiment you can still measure a sample in the PPMS by using your own instruments Appendix A lists the pinouts for the sample puck probe head Lemo connectors and Model 6000 D connector so that you can make the necessary electrical connections You can attach a current source and voltmeter to the sample to perform four wire resistivity measurements By attaching the sample leads to the sample in a slightly different configuration you can make Hall coefficient measur
17. and the liquid nitrogen A liquid nitrogen transfer adapter is included with all nitrogen jacketed dewars The transfer adapter Figure 2 2 is a short L shaped tube that fits on the end of most standard liquid nitrogen transfer lines and facilitates the liquid nitrogen fill procedure The standard nitrogen jacketed dewar has a 30 L liquid helium capacity and a 40 L liquid nitrogen capacity PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 2 Section 2 2 Hardware Dewar m 45 50 re 40 77 LIQUID NITROGEN 4X LIFTING LUGS FILL PORTS EVACUATION VALVE p 17 25 10 41 p 9 88 ID 4 215 00 4 ae LIQUID HELIUM RUPTURE DISC LIQUID NITROGEN NI FILL PORTS VACUUM k ACTIVATED CHARCOAL NITROGEN JACKET SUPERINSULATION LIQUID NITROGEN TRANSFER ADAPTER Figure 2 2 Top view and cross section of a nitrogen jacketed dewar and a side view of a liquid nitrogen transfer adapter dimensions are in inches 2 2 1 3 HIGH CAPACITY NITROGEN JACKETED DEWAR High capacity nitrogen jacketed dewars are used solely with systems that have a 7 T or 9 T longitudinal magnet Figure 2 3 illustrates a top view and a cross section of a high capacity nitrogen jacketed dewar which has a 87 L liquid helium capacity and a 48 L liquid nitrogen capacity ja B ERINSULATIO N A E ATID e 9 l A
18. and the potential drop can be known to a high degree of accuracy Ohm s law gives the resistance The user bridge board operates in several different modes to accommodate a variety of requirements and still allow a Quantum Design PPMS Hardware Manual 1070 150 Rev B5 3 11 February 2008 Section 3 9 Chapter 3 Experimental Considerations Theory of Operation 3 9 3 12 high degree of measurement sensitivity The resistance that the bridge board measures is reported in the Status Bridge screen on the front panel of the Model 6000 To perform different types of measurements different hardware is used but the basic premise of the system remains the same The sample sits within the thermally magnetically controlled environment of the sample space while electrical wiring to the base of the chamber allows connection to current sources voltmeters ammeters and the like The Model 6000 frequently contains all such necessary equipment You can manipulate various measurement parameters including the measured resistance applied current sample temperature applied magnetic field time select line status and so on These values can be placed into a data buffer in the Model 6000 linked to one of the Model 6000 analog outputs or uploaded into a data file on a personal computer The PPMS software can graph the data file as the data is recorded You can export data files to another format in order to use them with data manipulation applicatio
19. assembly consists of a U bolt a locking mechanism and a plate The plate fits just underneath the sample chamber access port which is located on the probe head see Figures 2 4 and 2 5 You typically will use the probe lifting assembly in conjunction with a hoist You can tie or pass a rope through both the U bolt and a fixture in the ceiling so that you can slowly raise and lower the probe When the probe lifting assembly is not being used remove it from the probe Section 4 7 4 explains how to use the probe lifting assembly Figure 2 6 Probe lifting assembly 2 6 Model 6000 PPMS Controller The Model 6000 PPMS Controller Figure 2 7 is an integrated user interface that houses the electronics and the gas control valves for the PPMS The Model 6000 contains the CPU board motherboard and system bridgeboard The CPU board is the system processor the motherboard controls system integration and the system bridgeboard supplies temperature readings Gas valves and gas lines inside the Model 6000 are used to control temperature Refer to Sections 2 6 1 1 and 2 6 1 2 and Appendix A for more information on the Model 6000 Refer to the Physical Property Measurement System Firmware Manual and the Physical Property Measurement System Commands Manual for practical information about using the Model 6000 CONTRAST KNOB _ MENU KEYS STATUS LEDS qe r POWER MODEL 6000 PHYSICAL PROPERTY MEASUREMENT SYSTEM Figure 2 7 Fron
20. displace all the air in a room during a spill Nitrogen and helium are colorless and odorless and the only symptoms of insufficient oxygen are dizziness and unconsciousness followed by death 1 4 2 Magnets WARNING All magnet safety precautions must take into account the strong three dimensional fields produced by the superconducting magnets People wearing a pacemaker or other electrical medical device must stay at least 16 5 ft 5 m from the PPMS dewar Ferromagnetic objects must be kept at least 16 5 ft 5 m from the PPMS dewar Magnetic fields must be at zero 0 before you disconnect the magnet controller from the probe head Helium levels must be at least 60 to use a magnet to full field Never disconnect a charged magnet from the magnet control electronics Model 6700 or Model 3120 and never disconnect any other system connections while a magnet is charged The superconducting PPMS magnets can trap magnetic flux so it would be possible to leave a charged magnet that is completely disconnected from the rest of the system Under such circumstances you have no means to discharge the magnet directly Several different cables have connections for magnet control In the event that you must disconnect the probe from the magnet controller verify that the magnet has been driven to zero field before you disconnect any cables with the exception of the sample chamber connection The sample cham
21. een A 11 in illustration of probe head ports A 9 pinout table sessssssssss A 16 BNC connector eeeeesss 2 8 A 5 C CLTC characteristics ssssssussss 3 5 description anisini 3 2 3 4 impedance ciens 2 5 3 3 selecting etes 3 5 4 6 4 10 USIMGs su cer Ee hd 4 6 4 10 Communication port connections pinout tables nemen A 14 A 15 Continuous Low Temperature Control See CLTC Cooling annulus function sin eds 2 5 3 2 illustration 2 4 3 3 3 6 Crossover temperature 3 2 Cryogens safety precautions 1 4 1 5 D Data files exporting and uploading 3 12 A 5 D6Wa L oe ge eee lees 2 1 2 3 as part of base hardware 1 2 electrical connections pinout table A 16 filling See Helium transfer Nitrogen transfer Warm dewar fill in illustration of gas and vacuum SYSTEM ura ce e Rees 3 6 ODtlOriS LL 1 3 2 1 2 3 safety features illustration 1 4 Dewar port T liction cese ce eie e e Pee ae A 8 in illustration of Model 6000 ports A 2 Differential pressure sensor function 3 6 Driven mode eee tees 3 8 Dual flow impedance See CLTC Index 1 February 2008 Index E Edwards pump illustration tr 4 24 C 2 maintenance 4 23 4 27 C 1 C 6 Olltrszstcis t e
22. gloves eye protection and covered shoes when you work with liquid nitrogen or any other cryogen Review Section 1 4 1 Cryogens before you transfer liquid nitrogen Always use a well ventilated room to perform this procedure 4 7 2 1 TRANSFERRING LIQUID NITROGEN If there is any liquid helium in the PPMS dewar you can use the procedures below to transfer liquid nitrogen into the nitrogen jacketed dewar However if the dewar contains no liquid helium you must use the warm dewar fill procedures in Appendix B The warm dewar fill procedures are designed to prevent blockages in the impedance tube To facilitate the liquid nitrogen transfer we recommend that you review the process before you begin If you are unfamiliar with these transfers ask for help from someone who is familiar with the supply vessel 1 Atthe PPMS dewar prepare for the liquid nitrogen transfer a Remove the brass fittings from one of the two liquid nitrogen fill ports by turning the larger fitting counter clockwise until it comes off the dewar This prevents the O ring from freezing b Open the other nitrogen fill port by turning the larger brass fitting counter clockwise to loosen it and then removing the small insert plug when it is loose see Figure 4 16 DI NITROGEN FILL PORT Figure 4 16 Preparing for a liquid nitrogen transfer 2 Screw the liquid nitrogen transfer adapter on
23. helium by cooling the system before you perform the helium transfer To do this you fill the liquid nitrogen jacket and then let the system sit for 48 hours before you transfer in the liquid helium Important When you transfer nitrogen and helium separately you must maintain a continuous flow of helium through the impedance tube so that ice does not form within the tube The procedures below will ensure a continuous helium flow The procedures for a sequential transfer are not difficult but involve many steps To facilitate a trouble free transfer we recommend that you review the entire set of instructions before you begin As noted in Section B 2 3 Materials you will be working with transfer lines and valves for three dewars the PPMS dewar a liquid nitrogen supply dewar and a liquid helium supply dewar and a helium gas cylinder The transfer setup is shown below in Figure B 5 the liquid nitrogen dewar is not shown The entire process will be easier if there are two people Quantum Design PPMS Hardware Manual 1070 150 Rev B5 B 7 February 2008 Section B 3 Appendix B Warm Fill Nitrogen Jacketed Dewars Filling Warm Dewars TRANSFER LINE on ADAPTERS LONG OUTPUT EXTENSION INPUT EXTENSION NITROGEN LIQUID FIL PORT OPEN DU B RIM T B Pea i GAS PHASE VALVI TRANS nee E uL m y 7 A DIRECT VENT SAFETY VALVE OR ANSFER ONLY REAR EVACUATION gt PM
24. into a warm dewar helium into a warm standard dewar no nitrogen jacket o Section B 3 explains how to transfer helium and nitrogen into warm nitrogen jacketed dewars B 2 Helium and Nitrogen Transfers into Warm Dewars WARNING Always wear protective clothing including thermal gloves eye protection and covered shoes when you work with liquid nitrogen liquid helium or any other cryogen Review Section 1 4 1 Cryogens before you transfer liquid nitrogen o Always use a well ventilated room to perform these procedures Immediately vent the room by opening windows and doors if there is an excessive helium release The procedures in this appendix explain how to fill a warm dewar which refers to situations in which the PPMS dewar has never been filled with helium or the dewar has been unused for an extended period of time and is dry If there is any liquid helium in the dewar use the routine transfer procedures described in Sections 4 7 2 These warm dewar fill procedures include safeguards to prevent frozen contaminants from blocking the impedance tube such a blockage would disable temperature control in the PPMS To use these procedures you must have installed the probe in the dewar and connected the system pumping lines and electrical lines as shown in Figure A 1 The magnet and user bridge Quantum Design PPMS Hardware Manual 1070 150 Rev B5 B 1 February 2008 Section B 2 Appendi
25. leads connected the leads will allow any current in the magnet to safely drain away Also leave the blue Lemo connected to the system Important Do not disconnect the blue Lemo or the magnet leads while the power is off When the power to the Model 6000 is cycled off and back on the Model 6000 retains certain parameters including all information stored in the sequence file and data buffer the field in the magnet and most of the user configuration parameters To support the nonvolatile RAM the Model 6000 has a lithium battery that lasts about 10 years 4 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 2 System Operation General Guidelines When there is a power loss the software will automatically place the PPMS in Shutdown standby mode but the PPMS will lose the settings for any measurements e g temperature field that are in process at the time of the outage Further the system will stop sending output to any motor Other types of information that will not be retained or restored include commands that are being executed when the power is lost as well as any direct output from the Model 6000 such as analog outputs which return to 0 V If a power outage occurs when you are using a sequence to perform measurements the sequence will stop running When the power comes back on you will need to reset the measurement parameters and restart the measurement When the power to one or more c
26. magnet based on a system with a 9 T longitudinal magnet ITEM EFFECT FIELD APPROXIMATE RADIAL REQUIRED DISTANCE FROM THE Oe DEWAR Electron microscope Disturbance 1 85 0 in LL 216 cm Color and monochrome computer monitors Disturbance 1 5 50 0 59 8 in CRT type unshielded 127 152 cm Credit cards bank cards etc Erasure 10 40 2 in 102 cm Watches and micromechanical devices Disturbance 10 40 2 in 102 cm Pacemaker lowest known field Disturbance 17 33 1 in 84 cm Magnetic tapes Erasure 20 31 1 in 79 cm Transformers and amplifiers Saturation 50 22 8 in 58 cm Floppy disks Erasure 350 11 8 in 30 cm The magnetic fields are three dimensional so their effects will extend above and below the magnet as well as around it Quantum Design PPMS Hardware Manual 1070 150 Rev B5 1 7 February 2008 Section 1 5 Chapter 1 Environmental Considerations and PPMS Setup Introduction and System Setup 1 5 2 Physical Dimensions When you are deciding where you will locate the PPMS consider the constraints below as well as the dewar and cabinet dimensions which are listed in Table 1 2 Note that these measurements are approximate o Empty space is needed around the PPMS to allow regular transfers of helium and nitrogen and for a transfer vessel usually a large portable dewar which must be brought near the PPMS dewar o Vertical clearance of a
27. many different needs For example you can monitor the channels of the user bridge from the Model 6000 analog outputs or front panel or from the personal computer Appendix A lists all Model 6000 inputs and outputs and explains the uses and capabilities of each port so that you can customize the system The voltages of the four Model 6000 analog outputs can be linked to 30 different sources with desired gain settings These analog outputs allow use of an oscilloscope chart recorder or similar instrument The Link BNC to Parameter section in the Physical Property Measurement System Commands Manual explains how you configure the analog outputs The Model 6000 provides three 24 V auxiliary drives relays a low current 15 V power source two different types of digital TTL level inputs two 10 V to 10 V analog inputs the Model 6000 can digitize and three optically isolated 5 V external select lines TTL level outputs Model 6000 units that have a user bridge board also have access to two current drivers that provide up to 1 A or 20 W of power whichever limit 1s reached first You can configure each input and output The Model 6000 also provides two communication ports IEEE 488 and RS 232 a motor output that includes connections for a 0 24 V actuator index and limit switch and a configurable pressure gauge input Besides electrically configuring the system as necessary you can also configure the gas and vacuum lines as required
28. of Operation Magnetic Field Control All other system plumbing is used for atmospheric control Under normal operation the flush valve opens the sample chamber to the pump The vent valve allows helium gas into the sample chamber during venting and purging procedures A purging procedure vents the sample chamber with clean gas and pumps it out through the flush valve and then repeats the same process two more times When the chamber is sealed both the vent valve and flush valve are closed The vent and flush valves are never open at the same time The system s solid state silicon pressure sensor is located on the sample space line within the Model 6000 between the vent valve and flush valve as shown in Figure 3 3 Gas Line Configuration The standard PPMS configuration does not provide a high or ultra high vacuum environment It keeps the sample chamber at a few torr with gaseous helium vapor supplied by the dewar However the gas lines can be configured in several different ways For example you can substitute some other clean gas for the helium that vents the sample chamber and provides the several torr of pressure that maintains thermal uniformity within the sample space The alternate gas source should be connected to the Sample Vent Up port that is on the rear of the Model 6000 When you use an alternate gas source you should blank off the Gas Source port which provides helium from the dewar so that the differential pressure sensor w
29. of the gray Lemo cable You can confine the wiring for this adapter to a box We highly recommend using a breakout box which provides an easily configured reusable method of changing sample connections It will keep the process flexible and isolate each wire in the gray Lemo cable allowing contact to each wire individually Such a box would have a female 25 pin D connector DB 25 and input and output connections to the leads as necessary for example 12 banana plug connectors 6 BNC connectors other D connectors or a bread board MALE DB 25 TO P USER BRIDGE MALE DB 25 CONNECTOR CUSTOM FEMALE DB 25 DELIVERED WITH SYSTEM CONNECTOR BNC CONNECTOR TO CUSTOM EQUIPMENT ANOTHER MALE DB 25 CONNECTOR TO PB AUXILLIARY OR OTHER Figure 4 14 Custom adapter for making connections to the sample leads 4 16 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 6 System Operation System Customization 4 6 2 Using Other Electronic Devices The Model 6000 is designed to facilitate use with many other electronic instruments It has an input for an external pressure gauge and an output to an external motor Its four analog output BNC connectors monitor a variety of system signals The P8 Auxiliary port contains two signal inputs to an analog to digital converter in order to digitize and record external signals The P User Bridge port pr
30. on the Send and Read button In the Response area the utility will report two numbers e g 0 1 as shown in Figure 4 4 The first number indicates the active temperature control mode and the second indicates if the CLTC option has been installed For example the first number in Figure 4 4 is 0 indicating that the system is using pot fill mode and the second number is 1 indicating that the CLTC option has been installed A 0 0 report would indicate that pot mode 1s being used but there is no CLTC option and a 1 1 report would indicate that low temperatures are being controlled by the CLTC option The status codes are summarized in Table 4 1 PPMS Hardware Manual 1070 150 Rev B5 4 7 February 2008 Section 4 3 Setting the Low Temperature Control Mode Table 4 1 Status codes for temperature control modes STATUS TEMPERATURE CLTC INSTALLED CODE CONTROL MODE 0 0 Pot fill No 0 1 Pot fill Yes 1 1 CLTC Yes 4 3 1 2 CHANGE LOW TEMPERATURE CONTROL MODE Chapter 4 System Operation To use MultiVu to change the low temperature control mode you will issue a command to shut down the PPMS along with a number specific to the control mode that you want to be activated The shutdown commands are summarized in Table 4 2 The example below uses the commands that activate CLTC x Send shutdown 2 Device type the following 1 Inthe Send text box Command sans N
31. probe back to Quantum Design for modification option installation or repair 4 2 2 Powering the System Off and On Generally the power to the PPMS hardware should be left on including the power to the Model 6000 Model 6700 and vacuum pump to maintain system safeguards as explained in Section 4 2 2 1 In the event you must turn off the power to the system or any component use the sequence in Section 4 2 2 2 Turn on the system or component as soon as possible using the sequence in Section 4 2 2 3 Important Before you turn off the power to the Model 6000 verify that the system is in Shutdown mode with the magnet in Persistent mode and the Field at zero 0 Oe Also leave the magnet leads and blue Lemo attached to the system If there is an unplanned power outage we recommend that you turn off the power to all components and the main system breaker in that sequence then pull the power plug from the wall Leave the magnet leads and blue Lemo attached to the system When the power returns turn on the system by using the sequence in Section 4 2 2 3 You do not need to turn off the system if it will be idle but you can conserve helium by putting it in Shutdown standby mode Section 4 2 3 Important Shutdown mode does not turn off the system it reduces the use of helium while allowing the Model 6000 to monitor the status of the system 4 2 2 1 POWER LOSS During a power loss or when you power off the system leave the magnet
32. sample chamber through the flush valve in the Model 6000 When the flush valve is open the sample chamber is open to this port Under normal circumstances this port is directly connected by a short hose to the System Vacuum port which is internally connected to the Pump port and consequently to the vacuum pump A 3 17 Sample Space Port The Sample Space port connects the sample space to the vent valve the flush valve and the gas lines in the Model 6000 The 1 4 inch stainless steel hose connects the Sample Space port to the QC quick connect fitting on the probe head A 3 18 Sample Vent Up Port The Sample Vent Up port accesses the sample space through the vent valve in the Model 6000 Under normal circumstances a small hose directly connects the Sample Vent Up port to the Gas Source port providing helium gas from the dewar boil off for venting and purging the sample chamber If you want to vent and purge the chamber with another gas simply disconnect this hose and connect an alternate gas source to the Sample Vent Up port In this case the Gas Source port must be plugged Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 7 February 2008 Section A 3 Appendix A Model 6000 Rear Panel Ports Connections Ports and Pinouts A 3 19 Gas Source Port The Gas Source port connects internally to the dewar port to provide a helium gas source for sample chamber venting and purging A short hose usuall
33. screen displays the status of the user bridge channels Use the CTRL gt gt 3 Immediate Operations gt gt 06 Bridge menu to control each bridge channel To record the current and resistance of each channel use the CTRL gt gt 3 Immediate Operations gt gt 11 Measure command The user bridge board also provides access to two additional current drivers of the Model 6000 These drivers which provide up to 1 A or 20 W of current whichever current limit is reached first can be monitored with the Status System Cont screen To monitor them use the CTRL A 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 3 Connections Ports and Pinouts Model 6000 Rear Panel Ports gt gt 3 Immediate Operations gt gt 08 DrvOut menu To record the current and power through each driver channel use the CTRL gt gt 3 Immediate Operations gt gt 11 Measure command A 3 20 P2 System Bridge Port The P2 System Bridge port accesses 1 the two heater drivers for the heaters on the sample chamber and 2 the PPMS system bridge board that monitors the three system thermometers The P2 port connects to the black ringed Lemo connector on the probe head The system bridge board is identical to the optional user bridge board but is required for system thermometry You cannot access three of the four system bridge channels You can access the fourth channel but it is reserved for some PPMS options tha
34. the low temperature control mode that is currently active then you will issue the command to switch to the other mode 4 3 1 1 VERIFY OPTION AND CONTROL MODE In MultiVu you will use the Send GPIB Commands dialog to verify the mode that is being used I 2 Quantum Design Select Utilities gt gt Send GPIB Commands from the MultiVu dropdown menus Figure 4 3 ly PPS Multivu Simulation Mode 15 x File View Sample Sequence Measure Graph Instrument Utilities Help mmm m e a n m e Activate Option Dieu eloj Hale Ed 2 Gonfigure Option Log PPMS Data Error Handling Event Log Sigma Log PPMS Data Helium Fill Status Calculator EverCool k Figure 4 3 Opening the Send GPIB Command utility in MultiVu The Send GPIB Commands dialog will open as shown in Figure 4 4 Send GPIB Commands x Send fot x Device Jis Command None C CRLF C LF Custom Terminator Response 011 a Result No error Bytes 4 Send Send and Read Close Figure 4 4 Using the Send GPIB Command dialog to verify control mode In the Send GPIB Commands dialog note the Send text box at the top of the dialog the Response area in the middle of the dialog and the Send and Read button at the bottom of the dialog You will use these sections to verify the temperature control mode In the text box next to Send type the following clt just as is shown in Figure 4 4 Then click
35. 0 Activate an option 4 2 3 Shutdown Mode Shutdown also known as standby mode does not turn off the system but it does help conserve helium resources while allowing the Model 6000 to monitor the status of the system Place the PPMS in Shutdown mode whenever it will be idle and you want to conserve helium When the temperature control hardware is in Shutdown mode the software adjusts the flow control valve to maintain approximately 100 cc min of flow through the cooling annulus turns off the system heaters and lowers the power to the impedance heater Note that with these adjustments the PPMS does not remain at a steady temperature Important The magnet must be in Persistent mode and the Field must be at zero 0 Oe before you place the system in Shutdown mode see Step 1 in Section 4 2 2 2 When you initiate the Shutdown mode the software automatically places temperature control in standby mode and seals the sample chamber These settings will be displayed in the front panel of the Model 6000 and in the Status bar at the bottom of the MultiVu window e To put the system in Shutdown mode using the Model 6000 select CTRL gt gt Interactive Control gt gt 8 Shutdown Mode e To put the system in Shutdown mode using MultiVu select Instrument gt gt Shutdown from the dropdown menus at the top of the MultiVu window To end Shutdown mode set a new temperature in MultiVu select Instrument gt gt Temperature 4 4 PPMS Ha
36. 070 150 Rev B5 4 25 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation 4 7 3 2 ADDING OIL AND DRAINING THE OIL MIST CONTAINER WARNING Put the system in shutdown mode and disconnect but leave seated the two metal pumping lines before you service the pump or related components If there are leaks into the sample chamber and cooling annulus ice can form and cause serious system malfunctions Prepare the PPMS for Pump Service 1 Place the PPMS in Shutdown mode in MultiVu select Instrument gt gt Shutdown When you place the system in shutdown mode it automatically seals the sample chamber turns off the heaters and restricts the flow control valve Disconnect but leave seated the two metal pumping lines that come from the probe head When the pumping lines are disconnected in this way the sample chamber and cooling annulus are sealed at the probe head Leaving the rest of the system components turned on turn off the pump according to the instructions below If the pump has been in operation you might need to let it cool before you work on it a Early PPMS units without a toggle switch on the pump unplug the pump to turn it off Do not turn off the switch on the power strip this strip powers other system equipment in addition to the pump b Recent PPMS units with a toggle switch on the back of the pump turn off the toggle switch Open the c
37. 1 7 lVD6S dieta ten bcp rtt dta 1 3 2 6 Magnet current port A 18 Magnet Reset option sssss A 8 Magnetic field control approach modes ssssssssess 3 8 description en 3 7 3 8 Magnetic field relaxation minimizing 3 8 Maintenance 4 18 4 28 C 1 C 6 foin coa e ecrit C 7 C 8 Q rings ina iiti treten edo 4 28 periodic pump ssssss C 1 C 6 FOULING so isc oer a 4 18 4 28 helium transfer cold dewar 4 21 4 23 nitrogen transfer cold dewar 4 19 4 20 puck adjustment sesesssssss 4 18 pump service oaeee 4 23 4 27 schedule pump 4 23 4 24 C 2 Measurement automating See Sequences considerations 3 12 3 13 4 10 example 25 15 299 9 araen aa 3 11 3 12 cp 1 1 3 11 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 Index Measurement options accessing option boards A 3 measurements with 3 11 3 12 sample mounting techniques 3 11 3 12 3 13 4 10 4 12 sealing sample chamber 2 6 USNO i eA oor he ke ce uL I oe s 1 1 Metal hose connectors niger A 10 in illustration of ports on probe head A 9 Model 6000 PPMS Controller as part of base hardware 1 2 automating system operation CM UEREUR
38. 1 8 2 2 helium cool down filling a warm dewar EA E B 1 B 3 B 12 B 14 Ilijstratiori a RR 2 2 OPON ou iei erem 1 3 2 1 routine helium transfer refilling a cold dewal s scudo t 4 21 4 23 Standby mode See Shutdown mode Stepper motor connecting to system A 6 Syst 5A fuse functions oi tr RR A 8 in illustration of Model 6000 ports A 2 replacement values A 23 System bridge board description sssssssssssssess A 3 electrical connections pinout table A 13 System Vacuum port function sss A 7 in illustration of Model 6000 ports A 2 T TCM connector description eeessssssssss A 10 in illustration of probe head ports A 9 pinout table sssssssessss A 18 Temperature control approach modes sssssssssess 3 6 components illustration 3 3 description sssssssssss 3 2 3 6 in Shutdown mode sssss 4 4 modes eode trn I ERETRAE 3 2 3 6 setting low temperature control 4 6 4 10 Temperature range ieee 1 1 Test cutout See Puck adjustment tool Top plate assembly as part of base hardware 1 2 descriptions spaa e a aeaea 2 6 Osrngs ick metere RR 2 6 4 28 Top plate baffle assembly 2 6 3 2 U Ultra fitting fulictiOn et tret ree t E A 10 in illustration of probe h
39. 20 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 5 Connections Ports and Pinouts Pinout Tables A 5 10 Expansion Connections Motor The P10 Motor port is on the Model 6000 P 10 Motor port Figure A 13 Motor expansion connections Table A 10 Expansion connections motor P10 MOTOR D FUNCTION CONNECTOR Pos Phi P Pos Pha Pos Ph3 s Aia 9 Sime Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 21 February 2008 Section A 5 Appendix A Pinout Tables Connections Ports and Pinouts A 5 11 Expansion Connections External The P11 External port is on the Model 6000 P11 External port Figure A 14 External expansion connections Table A 11 Expansion connections external P11 EXTERNAL FUNCTION D CONNECTOR pt Seectt C L Select 1 E Select 2 C Select 2 E Select 3 C Busy 1 In Hold Busy 2 In User 8 Selt3 E A 22 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 6 Connections Ports and Pinouts Replacement Fuse Values A 6 Replacement Fuse Values Tables A 12 and A 13 list the manufacturers recommended replacement fuse values The Quantum Design stock number for each fuse is shown in the far right column of each table Table A 12 Replacement fuse values for 100 120 VAC systems HARDWARE PORT FUSE VALUE AND SIZE QUANTUM DESIGN
40. 21 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation 3 Atthe liquid helium supply dewar perform in sequence the steps below using Figure 4 18 for reference a Vent the pressure from the supply dewar by slightly opening the gas phase valve b After the pressure has been reduced close the gas phase valve c Open the liquid access port This port is open only during the transfer d Close the primary relief valve on the supply dewar This valve remains closed only during the transfer procedures TRANSFER LINE A ADAPTERS w AY a At INPUT SHORT OUTPUT EXTENSION EXTENSION NITROGEN s LIQUID ACCESS PORT TOP FILL POR OPEN DURING TRANSFER ONLY Sca Janik SEED BRIMARY RELIC VALVE PRESSURE GAUGE REAR CLOSED DURING CAS PHASE VALVE TRANSFER ONLY 75 DIRECT VENT SAFETY VALVE EVACUATION 3 DEWAR VALYE LIQUID HELIUM HELIUM GAS SUPPLY DEWAR CYLINDER Figure 4 18 Arrangement for refilling a cold nitrogen jacketed dewar with liquid helium Note the short output extension on the transfer line 4 Using rubber or plastic tubing connect a helium gas cylinder to the gas phase port on the liquid helium supply dewar as shown in Figure 4 18 5 At the PPMS dewar open one of the two helium fill ports on the probe head by pulling the entire fixture straight up see Figure 4 19 B 5 6 Slowly lower
41. 3 1 Temperature Control Modes sess enne en 3 2 3 3 1 1 High Temperature Control ssssssssesseeeeeeee ener 3 4 3 3 1 2 Continuous Low Temperature Control seen nennen 3 4 3 3 1 3 Pot Fill Mode Temperature Control sssesssssseeeeeeeeeeen nennen 3 4 3 3 1 4 Selecting the Low Temperature Control Mode sess 3 5 3 3 2 Temperature Approach Modes ccccccccssecsseceseceeceseceecseeceeeeeeaeeeseeeseecseecseecsaeenseenaeens 3 6 3 4 Atmospheric Control esi tiet edet e tt sept le e Eee Sede rt d il aede Eo do tease duas 3 6 3 5 Magnetic Field Control in ce tette tret c te peeled Forte lon Aaa 3 7 3 54 Controls Mecharistins nae tre ERE UE Et SO e ERU IRSE CLUSTER 3 8 3 5 2 Magnetic Field Approach Modes esses enn enne enne 3 9 3 6 Helium Level Metering esses ener enne erret eren trennen nennen nennen nnne 3 9 3 7 Model 6000 Flexibility essere enne ener erre enne 3 10 3 8 Example Meas remernit 5 0o enemies enr n tm EOS 3 11 3 9 Experimental Considerations ssessssssssssseeseee eene enne enne nnne nennen nnne 3 12 CHAPTER 4 System OPE rat en T E 4 1 Ale UG ER 4 1 4 2 General Guidelines x dec ed rer ve Cree a e e a peds 4 1 4 2 1 Handling the Probe ccecccccscesecesecesscseecseeeeeceeeeeeeseeeseeeseecsaecsaecnsecaeceseeeaeenesseeeeeetens 4 4 2 20 Powering the System Off and On eene enne 4 2
42. 3 10 3 11 3 12 battery xe eR IDEM IT RUN 4 2 connections block diagram A 1 customizable features 3 10 3 12 4 16 4 17 A 2 A 8 data buffer ane a i 3 12 flow control valve 3 2 3 4 3 5 3 6 4 4 A 7 front panel illustration 2 8 PUNCO serre Ert Peor test 2 8 2 9 A 2 TUSes sr eben e eden e Peg A 8 A 23 ports description coim A 2 A 8 illustration eee A 2 pinout tables A 12 A 17 A 19 A 22 power receptacle ssessessss A 8 safety precautions ssssssss 1 6 shutting off power sssssess 4 2 Model 6500 PPMS Option Controller A 11 Model 6700 Magnet Controller See also Magnet Red Lemo connector connections block diagram A 1 front panel illustration 2 9 function uie tees 2 9 2 10 3 7 safety precautions sssssssss 1 6 Model 7100 AC Transport Controller A 11 Motor expansion connections pinout table sssssssssss A 21 N Negative temperature coefficient thermometer See NTC thermometer Nitrogen fill port illustration 1 4 2 3 4 19 on nitrogen jacketed dewar 2 2 4 19 B 5 B 8 opening illustration 4 19 B 5 B 8 OMN ttp eben 4 19 4 20 Index 3 February 2008 Index Nit
43. 6 Using rubber or plastic tubing connect a helium gas cylinder to the gas phase port on the liquid helium supply dewar 7 At the PPMS dewar open one of the two helium fill ports on the probe head by pulling the entire fill port fixture straight up see Figure 4 19 8 At the liquid helium supply dewar open the liquid access port This port remains open only during the transfer 9 Simultaneously insert a the output end of the transfer line into the PPMS dewar through the open helium fill port and b the input end of the transfer line into the liquid helium supply dewar through the liquid access port see Figure B 8 10 Carefully lower both ends of the transfer line completely into the dewars and seat the adapters in their respective ports Gas will begin flowing from the output adapter Point the output adapter exhaust tube away from all hardware on top of the dewar The exhaust will get extremely cold and could damage some of the parts especially O rings and sealed valves CAUTION Point the output adapter exhaust tube away from all hardware on the dewar and probe head The extremely cold exhaust can damage parts especially O rings and sealed valves 11 Verify that each adapter on the transfer line is properly seated and sealing the transfer line 12 Raise the input side of the transfer line about 1 cm 1 2 in off the bottom of the supply dewar so that it does not collect ice or other debris that might have settled on th
44. 9 February 2008 Section 4 4 Chapter 4 Sample Mounting System Operation 4 4 4 4 1 4 4 2 4 10 5 Youcan verify that you have changed to pot fill mode by typing c1t again in the Command to Send panel The Response Received panel should display 0 1 if the system has changed to pot fill mode successfully 6 To activate CLTC type shutdown 2 in the Command to Send panel Sample Mounting Several broad considerations affect the sample mounting technique you will use no matter what type of sample holder you choose including a sample puck and a plastic straw These considerations are the temperature range of the experiment and the electrical and magnetic properties of the elements in the mounting arrangement Guidelines for Mounting Samples The sample mounting method that you use must withstand the temperature range of the experiment Not all glues and tapes stick well at low temperatures Furthermore differential thermal expansion between elements of your arrangement could prevent it from functioning as you intended The sample puck is conductive so electrical leads will be shorted together if they contact the puck anywhere other than at the solder pads Often samples must be electrically isolated from the puck so that the only electrical path is through the sample Other sample holders such as the PPMS rotators are made from dielectric material and do not short the signals when a sample contacts them directly If
45. B 6 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 3 Filling Warm Dewars Warm Fill Nitrogen Jacketed Dewars 4 Atthe PPMS dewar close the helium fill port on the probe head by reinserting the relief valve 5 Atthe liquid helium supply dewar close the valve on the liquid access port 6 Atthe PPMS dewar perform in sequence the steps below a Puton your protective gear This gear is necessary to prevent serious burns from the extremely cold fitting supply line and transfer adapter b Remove the liquid nitrogen transfer adapter by turning the brass fitting counter clockwise and lifting the transfer adapter out of the dewar In the event that the fitting and adapter are frozen together you can use a warm air blower to accelerate the thawing process Otherwise you must wait until the parts thaw enough to be separated c Close both nitrogen fill ports by reinstalling the brass fittings and turning the large brass fittings clockwise CAUTION Always re install the fill port fittings and or O rings onto the nitrogen fill ports after you have transferred liquid nitrogen into the dewar These fittings prevent dangerous ice blockages in the fill ports 7 The liquid helium transfer is now complete The helium level meter will turn itself off when you exit the Fill Dewar screen or if the fill time exceeds 30 minutes B 3 2 Sequential Nitrogen and Helium Transfers You can conserve liquid
46. Design PPMS Hardware Manual 1070 150 Rev B5 v February 2008 Contents Table of Contents 2S BrobezLafting Assernibly etie et eere ded tier rem ete een 2 8 2 6 Model 6000 PPMS Controller eese eren enne nre nennen enne 2 8 2 60 11 Model 6000 Front Panel ostasi ee etre cete eet cote tenete ge ladansestezeces 2 8 2 6 1 2 Model 6000 Rear P nel 2 rr eder a e eer ER ERR pe Ea ERE RENE Phe 2 9 2 7 Optional Magnet Controller sessi nennen nnns 2 9 2 7 1 Model 6700 Magnet Controller eese 2 9 2 7 1 1 Model 6700 Magnet Controller Front Panel 2 10 2 7 1 2 Model 6700 Magnet Controller Rear Panel essen 2 10 2 7 2 Model 3120 Magnet Power Supply sess 2 10 2 84 Electronics Cabinetza 5 e aeta e E B Seta es 2 10 2 9 Vacuum Da o P o coe ER RE E PERIERE INE ER PERF the taba ehe coe e ERE Puede 2 11 2 10 Sample Puck and Assorted Tools esses nnne 2 11 2 101 Puck3Insertion OO eot eer retten ahaa irt a enden qp ee e ae 2 12 210 2 Puck Adjustment TOON aine gero ehe eee ree re test ds 2 12 2 10 3 Puck Wiring Test Station eene enne ener entren nennen 2 13 CHAPTER 3 Theory of acit ehm o Mr 3 1 Sed Introductions 5o it eR ORG ERE RR RH e EBENE Pe EN UBER dede 3 1 3 2 PPMS System Block Diagram nene enne n nn ee nennen nennen 3 1 3 3 Temperature Control repe rrt e er et erepti ae ee The e ee repe Rees 3 2 3
47. Fill Status dialog in MultiVu select Utilities gt gt Helium Fill or through the Model 6000 select CTRL gt gt 1 Interactive Control gt gt 0 Fill Dewar 8 At the liquid nitrogen supply dewar close the liquid supply valve when the exhaust turns to liquid this indicates that the nitrogen jacket is full It will take about 1 hour to fill the jacket of a warm dewar because most of the liquid nitrogen will evaporate until the jacket walls have cooled Note The dewar belly will take slightly longer to fill than the nitrogen jacket because helium has a lower boiling point than nitrogen The helium level reading will be negative until the helium in the dewar has reached the base of the helium level meter 9 When the helium level reads 30 40 the impedance tube will no longer be exposed You can then set a system temperature so that the PPMS will be ready to use when the transfer procedures have been completed CAUTION Let the liquid helium level reading reach 30 40 before you change the PPMS set point temperature Shut Off and Disassembly 1 When the liquid helium level reaches 97 100 in the PPMS dewar after about 1 hour close the regulator at the helium gas cylinder to stop the transfer 2 Atthe liquid helium supply dewar reset the valves a Close the gas phase valve b Open the primary relief valve 3 Remove the helium transfer line and adapters from the liquid helium supply dewar and the PPMS dewar
48. IX A Connections Ports and Pinouts A 1 Introduction This appendix contains the following information o Section A 2 illustrates the connections o Section A 5 contains pinout tables for all between the system hardware electrical ports components o Section A illustrates and describes the o Section A 6 lists the recommended ports on the rear panel of the Model replacement fuse values 6000 o Section A 4 illustrates and describes the ports on the rear of the PPMS probe head A 2 System Connections The proper connections between the probe head Model 6000 Model 6700 and pump are shown in Figure A 1 Use the figure as a guide when you connect the components eliminate reference to Model 6700 in the figure below Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 1 February 2008 Section A 3 Appendix A Model 6000 Rear Panel Ports Connections Ports and Pinouts Figure A 1 Connections for PPMS hardware solid lines identify electrical connections and dashed lines identify gas vacuum lines Electrical connections to the probe have color coded Lemo connectors at the probe end Three separate pumping lines are attached to the probe a smaller metal hose that attaches to the sample chamber a larger metal hose that connects to the cooling annulus and a small white polypropylene hose that connects to the dewar Figure A 1 does not illustrate connection of a personal com
49. LVE 2 LIQUID NITROGE N FILI S RUPTURE DIS A Cod X LIFTINC LUGS L KET Nacrat CHARCOAL LIQUID HEL Figure 2 3 Top view and cross section of a high capacity nitrogen jacketed dewar dimensions are in inches Quantum Design PPMS Hardware Manual 1070 150 Rev B5 2 3 February 2008 Section 2 3 Probe 2 3 Chapter 2 Hardware Probe The probe Figure 2 4 is immersed in the liquid helium bath inside the dewar A sophisticated device with delicate components the probe incorporates the basic temperature control hardware the superconducting magnet the helium level meter the gas lines the sample puck connectors and various electrical connections You can prevent damage to the probe by following the probe handling instructions in Section 4 2 1 The probe is composed of several concentric stainless steel tubes and other important elements Its outer layer isolates the sample chamber from the liquid helium bath Two concentric tubes separated by a sealed evacuated region prevent heat exchange between the sample chamber and the helium bath The vacuum space between the outer and inner vacuum tubes contains reflective superinsulation to minimize radiative power loss into the helium bath An aluminum heat shield in the vacuum region directs heat to the neck of the dewar where there is no liquid helium A metal bellows at the bottom of the probe prevents it from being damaged by differential thermal expansion between the outer vacuum t
50. QuantumDesign n a d NT Physical Property Measurement System Hardware Manual Part Number 1070 150 B5 Quantum Design 6325 Lusk Boulevard San Diego CA 92121 USA Technical support 858 481 4400 800 289 6996 Fax 858 481 7410 Sixth edition of manual completed February 2008 Trademarks All product and company names appearing in this manual are trademarks or registered trademarks of their respective holders U S Patents 4 791 788 Method for Obtaining Improved Temperature Regulation When Using Liquid Helium Cooling 4 848 093 Apparatus and Method for Regulating Temperature in a Cryogenic Test Chamber 5 311 125 Magnetic Property Characterization System Employing a Single Sensing Coil Arrangement to Measure AC Susceptibility and DC Moment of a Sample patent licensed from Lakeshore 5 647 228 Apparatus and Method for Regulating Temperature in Cryogenic Test Chamber 5 798 641 Torque Magnetometer Utilizing Integrated Piezoresistive Levers Foreign Patents U K 9713380 5 Apparatus and Method for Regulating Temperature in Cryogenic Test Chamber Safety Instructions are inside Refer servicing to hazard replace fuses only with same type qualified personnel and rating of fuses for selected line voltage j No operator serviceable parts For continued protection against fire Observe the following safety guidelines when you use your system To avoid damaging the system verify that the system power req
51. S DEWAR VALVE LIQUID HELIUM HELIUM GAS SUPPLY DEWAR CYLINDER Figure B 5 Arrangement for sequential transfer of nitrogen and helium into warm nitrogen jacketed dewar with the supply line for liquid nitrogen indicated at left of figure nitrogen cylinder is not shown Set Up 1 Verify that the system pump and the Model 6000 are turned on and operating properly If either the pump or the Model 6000 is on but appears to be malfunctioning contact a Quantum Design representative 2 Using rubber or plastic tubing connect a helium backfill adapter to a helium gas cylinder as shown in Figure B 6 The helium backfill adapter 1s a fixture that fits into one of the helium fill ports on the probe head The helium gas cylinder provides the helium backfill during the liquid nitrogen transfer and during the dewar cool down period 3 Openone ofthe two helium fill ports on the probe head by pulling the relief valve straight up as shown in Figure 4 19 4 Insert the helium backfill adapter into the helium fill port Verify that the adapter fits snugly a 4 NITROGEN FILL PORT HELIUM GAS CYLINDER PPMS DEWAR i Figure B 7 Preparing for a liquid nitrogen Figure B 6 Inserting a helium backfill adapter transfer 5 At the PPMS dewar prepare for the liquid nitrogen transfer a Remove the brass fittings from one of the two liquid nitrogen fill p
52. STOCK NUMBER Model 6000 Pwr Entry Module 2A 5 x 20 mm Delayed Acting FD2A 20MM Sys 5 A 1 in Fast Acting F35 Aux 2 A 1 in Fast Acting F2 0A Quench Heater 63 A 5 x 20 mm Delayed FD 63A 20MM Acting 50 A Magnetic Power Pwr Entry Module 5 A 5 x 20 mm Slow Blow F5 20MMSB Supply 100 A Magnetic Power Pwr Entry Module 10 A 5 x 20 mm Slow Blow F10 20MMSB Supply ACMS Pwr Entry Module 1 A 250 V 20 mm Delayed FD1A 20MM Acting EP C LL Pwr Entry Module 1 A 250 V 20 mm Delayed FD1A 20MM Acting Option Controller Pwr Entry Module 1A 5 x 20 mm Fast Acting F1 20MM High Vacuum Cntr Pwr Entry 3 15 A 5 x 20 mm Slow Blow FD3 15A 20MM Table A 13 Replacement fuse values for 200 240 VAC systems HARDWARE PORT FUSE VALUE AND SIZE QUANTUM DESIGN STOCK NUMBER Model 6000 Pwr Entry Module 1 A 5 x 20 mm Delayed Acting FD1A 20MM Sys 5 A 1 in Fast Acting F35 Aux 2 A 1 in Fast Acting F2 0A Quench Heater 63 A 5 x 20 mm Delayed FD 63A 20MM Acting 50 A Magnetic Power Pwr Entry Module 2 5 A 5 x 20 mm Slow Blow FD2 5 20MMSB Supply 100 A Magnetic Power Pwr Entry Module 5 A 5 x 20 mm Slow Blow FD5 20MMSB E ACMS FDOSA CSA Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 23 February 2008 A PP EN DIX B Filling Warm Dewars B 1 Introduction This appendix contains the following information o Section B 2 presents an overview ofhelium o Section B 4 explains how to transfer and nitrogen transfers
53. TENSION Figure B 1 Helium transfer line arrangement B 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 3 Filling Warm Dewars Warm Fill Nitrogen Jacketed Dewars o A liquid helium supply dewar for filling the dewar 100 liters except systems with magnets 14 T and above which need 200 liters o A helium gas cylinder standard size to pressurize the liquid helium supply dewar or to provide a helium backfill For systems with an EverCool dewar this cylinder is in addition to the helium gas supply cylinder that 1s used to replenish the system o A liquid nitrogen supply dewar nitrogen jacketed dewars only about 80 liters o A liquid nitrogen transfer adapter included with the nitrogen jacketed dewars o A liquid nitrogen supply line included with the nitrogen jacketed dewars o Anoptional warm air blower for removing hardware nitrogen jacketed dewars only o Rags to wipe up liquids such as condensed water from the air Important If you do not have a Quantum Design helium transfer kit your hardware might differ from the hardware described in this appendix B 3 Warm Fill Nitrogen Jacketed Dewars WARNING Always wear protective clothing including thermal gloves eye protection and covered shoes when you work with liquid helium or any other cryogen Review Section 1 4 1 Cryogens before you transfer liquid helium B 3 1 Simultaneou
54. To do so remove the screw from the bottom of the puck The base of the puck is slotted so that the two components fit together properly when reattached ce Nj ES Figure 4 9 Sample mounted on puck Figure 4 10 Intermediate sample leads Verify that the leads all pass through the notches on the edge of the puck as shown in Figure 4 9 Note that if the leads extend past the outer rim of the puck it will be easy to damage them with the puck insertion tool during puck insertion Also you should use insulated electrical leads because the puck is conductive In some cases it can prove useful to create an intermediate set of leads that contact the solder pads but stop short of the sample as illustrated in Figure 4 10 You can then treat the sample and another set of leads for example in an oven or coating chamber while isolating the puck from the treatment When you have completed preparation of the sample and leads you can secure them to the puck and attach the sample leads to the intermediate leads To prevent electrical signals from being shorted you must separate the sample and the conductive puck by a substance that has high resistivity compared to the sample In many cases this substance can be a piece of tape Take the phase characteristics of the insulating material into consideration because the material will not perform correctly if it conducts or superconducts in the temperature range for your exper
55. WAR VALVE LIQUID HELIUM HELIUM GAS SUPPLY DEWAR CYLINDER Figure B 2 Arrangement for the simultaneous transfer of nitrogen and helium into a warm nitrogen jacketed dewar The supply line for liquid nitrogen is indicated at the left of the figure nitrogen cylinder is not shown Set Up 1 Verify that the system pump and the Model 6000 are turned on and operating properly If either the pump or the Model 6000 is turned off turn it on If either the pump or the Model 6000 is on but appears to be malfunctioning contact a Quantum Design representative Using the Model 6000 or the MultiVu x Temperature dialog shown in Figure B 3 r Status Instrument gt gt Temperature set the temperature Tep K to 5 K the rate to 10 K min and the approach mode to fast settle State Unknown r Control By setting the temperature to 5 K you open the flow control valve and ensure the maximum flow Set Point 5 00 K through the impedance tube Maximum flow is Rate 10 00 K min necessary to flush out the impedance and keep Mode faeces contaminants from freezing inside it while it cools to cryogenic temperatures The temperature will not actually drop to 5 K because there is no liquid helium in the dewar Figure B 3 Temperature dialog At the PPMS dewar prepare to attach the transfer and Settings for helium transier hoses a Remove the brass fittings from one of the two liquid nitrogen fill ports by turning th
56. a system temperature so that the PPMS will be ready to use when the transfer procedures have been completed CAUTION Let the liquid helium level reading reach 30 40 before you change the PPMS temperature Set point Shut Off and Disassembly 1 When the helium level reaches 97 100 after about 1 hour close the regulator of the helium gas cylinder to stop the transfer 2 Atthe liquid helium supply dewar reset the valves a Close the gas phase valve b Open the primary relief valve 3 Remove the transfer line and adapters from the liquid helium supply dewar and the PPMS dewar 4 Atthe PPMS dewar close the helium fill port on the probe head by reinserting the relief valve 5 Atthe liquid helium supply dewar close the liquid access port The liquid helium transfer is now complete The helium level meter will turn itself off when you exit the Fill Dewar screen or if the fill time exceeds 30 minutes Quantum Design PPMS Hardware Manual 1070 150 Rev B5 B 11 February 2008 Section B 4 Appendix B Warm Fill Standard Dewars Filling Warm Dewars B 4 Warm Fill Standard Dewars WARNING Always wear protective clothing including thermal gloves eye protection and covered shoes when you work with liquid helium or any other cryogen Review Section 1 4 1 Cryogens before you transfer liquid helium Always use a well ventilated room to perform this procedure Immediately vent the room by op
57. also Puck insertion puck extraction tool illustration sss 2 12 4 12 USING iz eere etiatn Meets 4 12 4 15 Sample mounting attached leads illustration 4 11 bonding media s 3 13 4 10 for four terminal resistance measurement 3 11 3 12 intermediate leads creating 4 11 isolating sample leads 3 11 3 13 methods 3 12 3 13 4 10 4 12 solder pads 2 12 3 11 4 10 verifying electrical connections 2 13 4 11 4 12 Sample puck See Puck Sample puck connector 2 5 2 12 2 13 A 11 Sample Pump Out port function 5e iet pan A 7 in illustration of Model 6000 ports A 2 Sample Size a a a aa 3 12 Sample space port functione ncc enhn A 7 in illustration of Model 6000 ports A 2 Sample Vent Up port See also Gas Source port function eB A 7 in illustration of Model 6000 ports A 2 Sample wiring test station 2 13 4 11 Index 5 February 2008 Index Sequences automating system operation M C ERE 3 10 3 12 Service centers ssuusss 1 9 1 10 Setup environmental factors affecting 1 7 1 9 Shutdown mode 4 2 4 3 4 4 Standard dewar Capacity c niet PR 2 2 description aeaa a aaa 2 2 dimensions eeeeee
58. ample chamber is constructed of copper in order to provide a region of uniform temperature The very base of the sample chamber contains a 12 pin connector that contacts the bottom of an installed sample puck Two thermometers and a heater are immediately below the sample puck connector Their proximity to the copper sample puck and mating connector helps them maintain close thermal contact with the puck and sample during experiments The wiring for the sample puck connections heaters and thermometers runs up the outside of the sample chamber to the probe head The pins from the sample puck connector are wired to the pins on the gray ringed Lemo connector on the probe head Appendix A has a list of pinouts for the sample puck sample puck connector and gray Lemo connector The region between the sample chamber and the inner vacuum tube is referred to as the cooling annulus Helium is pulled through the impedance tube into the cooling annulus so that it can warm and cool the sample chamber evenly Impedance Assembly The impedance assembly enables and disables the flow of helium into the cooling annulus from the dewar The assembly consists of a narrow tube the impedance a heater that warms the impedance and a thermometer that indicates when the impedance is warm When the impedance is warm a bubble forms inside the tube blocking the flow of liquid helium Then when the impedance heater is off the liquid helium cools the impedance tube and flow
59. an be used as low current power sources For example the 15 V and 15 V outputs can be used to power operational amplifiers The 15 V and 15 V lines draw directly on the Model 6000 power supply so it is important that these leads are never shorted Up to 200 mA of total current is available from the 15 V and 15 V lines when the ACMS and AC Transport options are not installed or active However this current is shared with the AC board When the AC board is driving relatively large alternating currents for the ACMS or AC Transport option the current that 1s available at these outputs drops to 10 mA A 3 8 3 TWO SENSE LINES The P8 Auxiliary port has two sense lines that are essentially digital on off inputs that operate at TTL levels 5 V inactive 0 V shorted active To record the status of each sense line use the CTRL gt gt 3 Immediate Operations gt gt 11 Measure gt gt DigIn command The Model 6000 does not control based on the status of the sense lines The sense inputs can be used during an experiment for example simply to indicate when a certain instrument in the system is operating A 4 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 3 Connections Ports and Pinouts Model 6000 Rear Panel Ports A 3 8 TWO ANALOG SIGNAL INPUTS The P8 Auxiliary port has analog signal inputs 10 V to 10 V that can be digitized and recorded by the Model 6000 The M
60. ar sss 2 3 Top view and cross section of a high capacity nitrogen jacketed dewar dimensions are in inches sss 2 3 Major components of the PPMS probe ssessssssssseseeeene eene 2 4 Cross section of top plate assembly 2 7 Probe lifting assembly sese nre nnns 2 8 Front panel of Model 6000 PPMS Controller sess 2 8 Front panel of the Model 6700 Magnet Controller eee 2 9 PPMS electr nics cabinet s oro eet etes rai ae erbe eet e RES ER 2 10 An oil mist direct drive pump used to control pressure and temperature in the PPMS sss eee 2 11 Top and bottom views of a sample puck sssessssseeeeeeee 2 11 Sample insertion tool with lever in engaged position c ccesccesseeseeteeteetteeteees 2 12 Puck adjustment 100 occ t hte tr ER ete dad ne Eee ei eo igo 2 13 Puck wiring test station sess eene enne enne nnne 2 13 PPMS block diagram ssesesssseeseeseeeeeeen eene nene 3 Cross sections of the PPMS probe and its temperature control components 3 3 Gas and vacuum control in the PPMS esses 3 6 Changing the field in the magnet sesssssssseseeeeeeeeneen enne 3 8 Schematic of helium level meter eese rennen 3 10 Leads attached for four terminal resistance measurement ssssssssss 3 11 PPMS Field dialog 5 1
61. ardware See also Model 6000 PPMS Controller Model 6700 Magnet Controller Probe Puck connections block diagram A 1 description ss niot e 2 1 2 13 dewar 1 2 1 3 1 4 2 1 2 3 3 6 A 2 A 8 A 16 magnet 1 1 1 3 1 5 1 7 2 4 2 6 3 7 3 8 A 17 A 18 OVOtVIOW c idee ets cre aaa e 1 2 1 3 Heat Capacity option ssssssse 1 1 Helium back fill adapter SEDE B 5 B 6 B 7 Helium fill port Tinto eode eh rte A 9 I StratiOri zs etos eret deret s 4 22 Helium level meter description 3 9 Helium level monitoring 4 5 4 6 Helium transfer cool down warm dewar nitrogen jacketed dewar B 1 B 11 standard dewar B 1 B 3 B 12 B 14 illustration B 4 B 8 B 12 line arrangement illustration 4 17 B 2 materials eeeeesssseesee B 2 B 3 routine cold dewar 4 21 4 23 Helium transfer Kit cccccccceeeseseeeeeeeeees B 3 High capacity nitrogen jacketed dewar See also Nitrogen jacketed dewar capacity 25 eser dete iis 2 3 dimensions eeeeeeee 1 8 2 3 illustration iii si ania sii 2 3 OpPllON nie e Ri Le 1 3 2 1 High temperature control mode 3 2 3 4 High Vacuum option sssesss 3 7 Hose nipple UNGUON cC A 10 in illustration of prob
62. are Manual 1070 150 Rev B5 B 5 February 2008 Section B 3 Appendix B Warm Fill Nitrogen Jacketed Dewars Filling Warm Dewars 13 Raise the input side of the transfer line about 1 cm 1 2 in off the bottom of the supply dewar so that it does not collect ice or other debris that might have settled on the bottom 14 Using rubber or plastic tubing connect a helium gas cylinder to the gas phase port on the liquid helium supply dewar Transfer At the liquid helium supply dewar open the gas phase valve 2 Atthe helium gas cylinder open the regulator and adjust the pressure to approximately 7 kPa 1 psi This pressurizes the supply dewar and maintains positive flow from the supply dewar to the PPMS dewar 3 Keep the dewar pressurized this way for 2 minutes before you perform Step 4 4 Use the Chamber dialog in MultiVu select Instrument gt gt Chamber gt gt Purge Seal or the Model 6000 CTRL gt gt 1 Interactive Control gt gt 2 Purge amp Seal to remove air from the sample chamber 5 At the liquid nitrogen supply dewar open the liquid supply valve Exhaust should begin coming from the second nitrogen fill port on the PPMS dewar 6 At the PPMS dewar visually monitor the exhaust from the second nitrogen fill port during the entire fill process Do not leave the PPMS unattended during this step and always stand at least 0 5 m 1 5 ft from the exhaust plume 7 Monitor the helium transfer with the Liquid Helium
63. are listed below For more detailed information about each command refer to the Physical Property Measurement System Commands Manual CTRL gt gt 1 Interactive Control gt gt 6 Move to Index CTRL gt gt 1 Interactive Control gt gt 7 Move CTRL gt gt 3 Immediate Operations gt gt 03 Move CTRL gt gt 3 Immediate Operations gt gt 07 DigSet CTRL gt gt 3 Immediate Operations gt gt 11 Measure CONFIG gt gt 6 Hardware gt gt 3 Position Configuration A 3 12 P11 External Port The P11 External port has three optically isolated outputs and two digital input busy lines that can help synchronize PPMS activity with other instruments The select line outputs provide TTL levels A nominal 10 k resistor must be used on the collector with the emitter tied to ground The select line outputs can be controlled by using the ExtSet command within a sequence or by using the CTRL gt gt 3 Immediate Operations gt gt 09 ExtSet menu When the select lines are activated the symbols S1 S2 and S3 appear in the Status System Cont digital status line You must provide the busy input lines with 5 V When the busy lines sense the 5 V difference between this voltage and the input line the channel is in a released state When the input line is also at 5 V the input lead shorted to the 5 V lead the channel enters a hold state There are two busy lines a user line and a hold line The hold state of each l
64. at least 298 K to prevent cryopumping of air into the chamber If the temperature is below 298 K set it to 298 K and wait for the chamber to reach room temperature CAUTION Always bring the sample chamber to room temperature before you open it to the atmosphere This will prevent condensation and cryopumping of air constituents inside the chamber which can cause probe malfunctions such as blocked valves and loss of temperature control 2 Verify that the field in the magnet is less than 1 tesla If the field is greater than that set it to less than 1 tesla and wait for the magnet to reach the set point PPMS Hardware Manual 1070 150 Rev B5 February 2008 Quantum Design Chapter 4 Section 4 5 System Operation Sample Puck Installation and Removal CAUTION Do not place the puck extraction insertion tool or any other object into the sample chamber when high fields are in the magnet as the force on the extraction tool could overwhelm you and cause you to damage the equipment 3 Ventthe sample chamber with clean dry gas to help keep the sample chamber free of contaminants in the air To vent the chamber you can use the Model 6000 menu CTRL gt gt 1 Interactive Control gt gt 5 Vent Continuous or you can use the PPMS software Instrument gt gt Chamber gt gt Vent Cont 4 Open the hinge clamp and remove the KF blank flange from the sample chamber access port see Figure 2 5 If the blank flange is di
65. be lifting assembly port but above the pressure relief valve Figure A 3 4 Use the pin on the end of the chain to close the locking mechanism of the lifting assembly You must close the locking mechanism before you lift the probe 5 Attach the probe lifting assembly to a hoist or a pulley if necessary to lift or lower the probe 6 When you have finished raising or lowering the probe remove the assembly Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 27 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation 4 7 5 Inspecting O Rings You can increase the reliability and lifetime of the PPMS by maintaining the O rings so they are always in good condition The regularly accessible O rings are on the top plate assembly and on the helium and nitrogen fill port fixtures You also might see other O rings when you perform maintenance and servicing All O rings in the system should be clean and they should be lubricated with silicon vacuum grease To ensure that the O rings remain in prime condition adopt the following habits o f you see an O ring visually inspect it o fan O ring appears dirty clean it with a clean lint free cloth e g a Kimwipe o If an O ring is dry apply silicon vacuum grease to it o fan O ring is cracked replace it o fan O ring is leaking contact Quantum Design 4 28 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 A PP E ND
66. ber connection that is the cable from the gray Lemo connector that is on the PPMS probe head is the only cable that you can safely disconnect while the magnet is charged You must leave all other connections intact The safety guidelines given here are generalized to a 9 T longitudinal magnet Verify that any person wearing a pacemaker or other electrical or mechanical medical device stays at least 16 5 ft 5 m from the PPMS dewar This distance applies to people located in adjacent rooms and on floors above and below the equipment because the magnets produce three At the current time August 2004 5 m should be a large enough distance to protect wearers of metallic implants or medical devices from most magnetic fields produced by Quantum Design magnets However the safe distance from newer magnets in development could be greater Hence personnel who work with and around the superconducting magnets should review thoroughly documentation for new equipment Quantum Design PPMS Hardware Manual 1070 150 Rev B5 1 5 February 2008 Section 1 4 Chapter 1 SafetyPrecautions Introduction and System Setup 1 4 3 1 6 dimensional fields The magnetic fields produced by the PPMS can be dangerous or fatal to anyone who is wearing a pacemaker or other electrical medical device This information should be posted in the laboratory where the PPMS is operated and adjacent areas so that people wearing such devices are aware of the prese
67. bles Connections Ports and Pinouts A 5 5 Dewar Connections The blue Lemo connector is on the probe head The P6 Dewar port is on the Model 6000 a Blue Lemo connector b P6 Dewar port Figure A 8 Dewar connections a Blue Lemo connector b P6 Dewar port Table A 5 Dewar connections BLUE LEMO P6 DEWAR FUNCTION CONNECTOR D CONNECTOR A 16 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 5 Connections Ports and Pinouts Pinout Tables A 5 6 Magnet Connections Model 6700 to Model 6000 The M1 connector is on the Model 6700 The P7 Magnet port is on the Model 6000 a M1 b P7 Magnet port o w d Qd O wq qw o o o o oo o Figure A 9 Magnet connections a M1 b P7 Magnet port Table A 6 Magnet connections Model 6700 to Model 6000 M1 D P7 MAGNET FUNCTION CONNECTOR D CONNECTOR Digital Gnd Data Out Sys Sync Reset Return 15 V 24 V Magnet V Shield Clock Magnet Sel Data In 15 V 15 V Return 24 V Magnet V Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 17 February 2008 Section A 5 Appendix A Pinout Tables Connections Ports and Pinouts A 5 7 Magnet Connections Probe to Controller The magnet connector is on the probe head Recent systems use a TCM connector and earlier systems use a red Lemo The magnet current port is on the Model 6700 a 1 TCM 100 A top plate feedthro
68. bout 6 ft 1 8 m is needed above the dewar so that you can easily insert and extract the probe These dimensions are suitable for inserting and removing the probe for all configurations of the PPMS dewar including the VSM and systems that have a 14 T magnet which requires a crane o Vertical clearance of about 3 3 ft 1 m is needed above the dewar for the sample insertion tool and the helium transfer line Table 1 2 Approximate physical dimensions of the PPMS dewars and the electronics cabinet HARDWARE PHYSICAL DIMENSIONS Standard dewar no 45 in high x 19 in diameter nitrogen jacket 114 cm high x 48 cm diameter Nitrogen jacketed dewar 46 in high x 21 in diameter 116 cm high x 53 cm diameter High capacity nitrogen 46 in high x 28 in diameter jacketed dewar 116 cm high x 71 cm diameter EverCool dewar 45 in high x 22 in diameter w o cold head 114 cm high x 55 cm diameter Electronics cabinet 22 in wide x 24 in deep x 45 in high 56 cm wide x 61 cm deep x 114 cm high The inch to cm equivalences are approximate because both measures were rounded after inches had been converted to centimeters 1 5 3 Local Altitude and Humidity The altitude and humidity of the laboratory can affect the performance of the PPMS The PPMS is designed to operate at altitudes below about 6000 ft 1829 m You can operate the PPMS at altitudes of 6000 ft 1829 m an
69. covered in Section 4 7 3 and Appendix C Figure 2 10 An oil mist direct drive pump used to control pressure and temperature in the PPMS Sample Puck and Assorted Tools The sample puck Figure 2 11 is a unique modular component that gives the PPMS great flexibility The puck holds the sample for many experiments that use the base PPMS platform and that do not require motion of the sample Some options such as the AC Measurement System ACMS option and the horizontal rotator options do not use the sample puck SOLDER PAD SAMPLE INTERFACE BOTTOM VIEW Figure 2 11 Top and bottom views of a sample puck Quantum Design PPMS Hardware Manual 1070 150 Rev B5 2 11 February 2008 Section 2 10 Chapter 2 Sample Puck and Assorted Tools Hardware The puck is a 0 91 in 2 3 cm diameter disk that is constructed of oxygen free high conductivity copper that maintains high thermal uniformity It has been gold plated to prevent oxidation The system thermometers and heaters are located directly beneath the installed puck so temperature control is intimately related to the temperature of the sample Options that use other sample mounting techniques often have an additional thermometer located near the sample The base of the puck contains 12 solder pads through which electrical leads establish contact with the sample you supply these leads These solder pads are hard wired to a set of 12 pins on
70. ct iet otibus Me ceto ET 4 25 C 3 Electrical connection between puck and sample verifying 2 13 4 11 Electrical safety ssssss 1 3 1 6 Electronics cabinet as part of base hardware 1 2 dimensions 1 2 1 8 2 10 TUI COT iit tti cci aar ceti 2 10 illustration odit 2 10 4 23 safety precautions ssssss 1 6 Expansion connections pinout tables ROREM A 19 A 22 F Fast Settle temperature approach mode 3 6 Finger contractor 2 12 2 13 4 18 Finger spreader 2 12 2 13 4 18 Flow control valve function 3 6 Flush valve normal behavior 3 7 FIUXCEGOD aet edet i s 3 8 Fuses replacement values A 23 G Gas lines configuring nre caters 3 7 illustration eet acne eet 3 6 modifying soei inanin ieee 4 17 Gas Source port function See also Sample Vent Up port A 8 in illustration of Model 6000 ports A 2 when to plug sesesesss 3 7 A 8 GPIB instrument interfacing with Model 6000 3 11 A 3 Gray Lemo connector TUNCUON e Ie A 11 in illustration of probe head ports A 9 pinout table seesssssssss A 12 Gray Lemo connector cable 4 9 A 11 Index 2 PPMS Hardware Manual 1070 150 Rev B5 H H
71. d above but it is not an optimal environment To control the sample temperature in the PPMS at temperatures that are below the boiling point of helium the pressure difference between the inside and outside of the dewar must be monitored If you are at a high altitude where atmospheric pressure drops significantly below 760 torr 1 atm you might notice some problems with temperature control or some sluggishness during low temperature operation gt A room with a ceiling about 10 ft 3 m high should provide enough vertical clearance to insert and remove the probe depending on your setup These dimensions are correct as of August 2004 1 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 1 Section 1 6 Introduction and System Setup Contacting Quantum Design The PPMS is best suited for dry environments and it should be operated with the humidity less than 90 Ice naturally forms when water in the air condenses and then freezes on cold surfaces and serious system problems can be caused when even the smallest piece of ice forms inside the PPMS As humidity increases it is easier for water to enter the system Eventually this will cause temperature control problems The PPMS does not have an airlock chamber so the sample chamber should be warmed to room temperature and vented continuously with a clean dry gas whenever the chamber is opened to the atmosphere The system is designed so that you can warm and ven
72. dware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 3 Filling Warm Dewars Warm Fill Nitrogen Jacketed Dewars CAUTION Point the output adapter exhaust tube away from all hardware on the dewar and probe head The extremely cold exhaust can damage parts especially O rings and sealed valves 10 Verify that each adapter on the transfer line is properly seated and is sealing the transfer line 11 Raise the input side of the transfer line about 1 cm 1 2 in off the bottom of the supply dewar so that it does not collect ice or other debris that might have settled on the bottom 12 At the liquid helium supply dewar prepare for the transfer a Connect the helium gas cylinder to the gas phase port b Open the gas phase valve 13 At the helium gas cylinder open the regulator and adjust the pressure to approximately 7 kPa 1 psi 14 Monitor the helium transfer with the Liquid Helium Fill Status dialog in MultiVu select Utilities gt gt Helium Fill or through the Model 6000 select CTRL gt gt 1 Interactive Control gt gt 0 Fill Dewar The helium level reading will be negative until the helium in the dewar has reached the base of the helium level meter Note The dewar belly will take slightly longer to fill than the jacket because helium has a lower boiling point than nitrogen 15 When the helium level meter reads 30 4096 the impedance tube will no longer be exposed You can then set
73. e large fitting counter clockwise until it comes off the dewar This prevents the O ring from freezing b Open the other nitrogen fill port by turning the large brass fitting counter clockwise to loosen it and then removing the small insert plug when it is loose see Figure B 4 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 3 Filling Warm Dewars Warm Fill Nitrogen Jacketed Dewars NITROGEN FILL PORT Figure B 4 Preparing for a liquid nitrogen transfer 4 Screw the liquid nitrogen transfer adapter onto the end of the liquid nitrogen supply line 5 At the PPMS dewar insert the small end of the liquid nitrogen transfer adapter into the open liquid nitrogen fill port and turn the brass fitting clockwise to secure the adapter in place Do not begin transferring nitrogen yet leave the nitrogen supply line closed 6 Bring the liquid helium supply dewar close to the PPMS dewar 7 Verify that the proper adapters and extensions are installed on the helium transfer line see Figure B 1 Note that the long extensions perform an essential function The extension on the input line ensures that liquid can always enter the transfer line even as the liquid level in the dewar changes The extension on the output line forces liquid helium all the way to the bottom of the PPMS dewar so that escaping cold gas will cool all the system components before it leaves the dewar
74. e or the Model 6000 set the temperature to 5 K the rate to 10 K min and the approach mode to fast settle By setting the temperature to 5 K you open the flow control valve and ensure the maximum flow through the impedance tube Maximum flow is necessary to flush out the impedance and keep contaminants from freezing inside it while it cools to cryogenic temperatures Note B 12 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 4 Filling Warm Dewars Warm Fill Standard Dewars that the temperature will not actually drop to 5 K because there is no liquid helium in the dewar 3 Bring the liquid helium supply dewar close to the PPMS dewar 4 Verify that the proper adapters and extensions are installed on the helium transfer line see Figure B 1 Note that the extensions perform an essential function The long extension on the input line ensures that liquid can always enter the transfer line even as the liquid level in the storage dewar changes The long extension on the output line forces liquid helium all the way to the bottom of the PPMS dewar so that escaping cold gas will cool all the system components before it leaves the dewar 5 Atthe liquid helium supply dewar set the valves a Vent the pressure by slightly opening the gas phase valve b Close the gas phase valve after the pressure has been reduced c Close the primary relief valve This valve remains closed only during the transfer
75. e A 2 System bridge connections BLACK P2 SYSTEM SYSTEM BRIDGE BOARD LEMO BRIDGE D FUNCTION CONNECTOR CONNECTO R Cur Driver Ch3 Block Heater Cur Driver Ch4 Neck Heater Cur Driver Ch4 Neck Heater 12 Channel tv 6 7 Channel 21 4 8 Chamel2V ff Channel 4 t P Channel 4 5 Channel 4 V Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 13 February 2008 Section A 5 Pinout Tables A 5 3 Communication Port Connections GPIB The P4 IEEE488 port is on the Model 6000 P4 IEEE488 port GPIB hhh Th Tn Tn nnn 7 GNE r DU mw o GN o a ONDE a GENUS GENS ONE GUN UND ZLAELZD ZL LAN i C o 32 l l2 Figure A 6 GPIB communication port connections Table A 3 Communication port connections GPIB P4 IEEE488 GPIB FUNCTION CONNECTOR DIO1 DIO2 A 14 PPMS Hardware Manual 1070 150 Rev B5 February 2008 Appendix A Connections Ports and Pinouts Quantum Design Appendix A Section A 5 Connections Ports and Pinouts Pinout Tables A 5 4 Communication Port Connections RS 232 The P5 RS232 port is on the Model 6000 P5 RS232 port Figure A 7 RS 232 communication port connections Table A 4 Communication port connections RS 232 P5 RS232 RS 232 FUNCTION CONNECTOR XE TXD DSR p x Lc a NENNEN Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 15 February 2008 Section A 5 Appendix A Pinout Ta
76. e bottom Transfer 1 At the liquid helium supply dewar open the gas phase valve 2 At the helium gas cylinder open the regulator and adjust the pressure to approximately 7 kPa 1 psi 3 Keep the dewar pressurized this way for 2 minutes before you proceed 4 Use the Chamber dialog in MultiVu select Instrument gt gt Chamber gt gt Purge Seal or the Model 6000 commands CTRL gt gt 1 Interactive Control gt gt 2 Purge amp Seal to remove air from the sample chamber 5 Monitor the helium transfer with the Liquid Helium Fill Status dialog in MultiVu select Utilities gt gt Helium Fill or through the Model 6000 select CTRL gt gt 1 Interactive Quantum Design PPMS Hardware Manual 1070 150 Rev B5 B 13 February 2008 Section B 4 Appendix B Warm Fill Standard Dewars Filling Warm Dewars Control gt gt 0 Fill Dewar The helium level reading will be negative until the helium in the dewar has reached the base of the helium level meter 6 When the helium level reads 30 4095 the impedance tube will no longer be exposed You can then set a system temperature so that the PPMS will be ready to use when the transfer procedures have been completed CAUTION Let the liquid helium level reading reach 30 40 before you change the PPMS set point temperature Shut Off and Disassembly 1 When the helium level reaches 97 100 close the regulator at the helium gas cylinder to stop the transfer It takes ap
77. e head ports A 9 Humidity effects sss 1 8 I Impedance assembly 2 5 Impedance heater f nctlon 5 AGA ER 2 5 in illustration of probe components 2 4 Impedance thermometer f nctlon cenae PIE 2 5 in illustration of probe components 2 4 Impedance tube 2 5 3 2 3 6 function inr PPP 2 5 in illustration of probe components 2 4 preventing blockage of B 1 B 4 B 7 Quantum Design February 2008 L Lemo connectors 4 9 A 9 A 13 A 16 A 18 Linear field approach mode 3 9 Liquid nitrogen transfer adapter FUNCION 4 eiii ere a i dea 2 2 Illi S tration uci ct ces 2 3 UE 4 19 4 20 B 5 B 9 Low temperature control modes 3 2 3 4 3 5 4 6 4 10 M M1 connector seeseeeen A 17 Magnet See also Model 6700 Magnet Controller charging usarioan aein 3 7 3 8 description eror i edan 2 6 discharging sees 3 7 3 8 effect on equipment 1 5 1 7 electrical connections pinout tables A 17 A 18 field center in illustration of probe components 2 4 location aote nete aes 2 6 field FANGS usc eie Rene 1 1 longitudinal illustration 2 4 MOJES sc een Iph ext 2 6 3 6 3 7 safety precautions 1 3 1 5
78. e input line ensures that liquid can always enter the transfer line even as the liquid level in the storage dewar changes The long extension on the output line forces liquid helium to the bottom of the PPMS dewar so that escaping cold gas will cool all the system components before it leaves the dewar 5 Atthe liquid helium supply dewar set the valves and liquid access port a Vent the pressure by slightly opening the gas phase valve b After the pressure has been vented close the gas phase valve c Open the liquid access port This port is open only during the transfer d Close the primary relief valve This valve remains closed only during the transfer procedure At the helium backfill cylinder close the regulator 7 At the liquid helium supply dewar insert the input end of the transfer line into the liquid access port see Figures B 1 and B 5 8 At the PPMS dewar remove the helium backfill adapter from the helium fill port on the probe head Then quickly insert the output end of the transfer line into the PPMS dewar through the open helium fill port 9 Carefully lower both ends of the transfer line completely into the dewars and seat the adapters in their respective ports When gas begins to flow from the output adapter point the output adapter exhaust tube away from all hardware on top of the dewar The exhaust will be extremely cold and it could damage some of the parts especially O rings and sealed valves B 10 PPMS Har
79. e low temperature control mode Note that you need to press the lt Enter gt key after you enter each command into the Mon6000 dialog 1 Open the Mon6000 dialog a Locate the Tools subdirectory of the ODPPMS directory the ODPPMS directory might be on your C drive b Locate the file named Mon6000 exe and double click on it to open it 2 When the Mon6000 dialog opens Figure 4 7 you will see separate text entry panels titled Command To Send and Response Received Mon6000 for Win32 File Acquisition Search About Command To Send Auto 1 sec Response Received Ce Eee Cid Figure 4 7 Checking the low temperature control mode using the Mon6000 dialog 3 Enter your temperature mode verification command i e clt into the Command To Send panel and press the Enter key As shown in Figure 4 7 the Response Received panel will then display the active low temperature regime You can see that the CLTC option is installed and it is being used because the Response Received panel displays 1 1 just as it would in MultiVu 4 To shut down the PPMS and activate pot fill mode enter the shutdown command shutdown 1 as is shown in Figure 4 8 and press the Enter key 7 Mon6000 for Win32 File Acquisition Search About Command To Send Auto 1 sec Response Received SS Se E E Figure 4 8 Switching low temperature control modes using the Mon6000 dialog Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4
80. e pressure gauges can be permanently damaged if they are connected improperly Always verify that any electrical connections to the PPMS are solid and properly grounded 4 6 3 Modifying the Gas and Vacuum System If you plan to modify the gas and vacuum lines in the PPMS first read Chapters 2 and 3 Sections 3 3 and 3 4 Be especially careful that you understand how the PPMS functions because your alterations can easily affect temperature control When you make your changes verify that any new plumbing connections are solid and have good seals Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 17 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation 4 7 Routine Maintenance Procedures This section describes routine maintenance procedures that you should perform regularly Less frequently performed procedures are discussed in Appendix B or Appendix C Regular maintenance procedures include adjusting the puck transferring nitrogen and helium into a cold dewar which you typically perform several times a week basic servicing of the vacuum pump assembly which you should perform throughout the year and O ring inspections which you should perform whenever you see an O ring in the PPMS The less frequently performed procedures include transferring liquid nitrogen and helium into a warm dewar Appendix B and performing major pump assembly services Appendix C Appendix C also contains a maintenance sch
81. e probe head Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 3 February 2008 Section A 3 Appendix A Model 6000 Rear Panel Ports Connections Ports and Pinouts A 3 7 P7 Magnet Port The P7 Magnet port connects the Model 6000 to the M1 port on the Model 6700 A 3 8 P8 Auxiliary Port The P8 Auxiliary port offers several auxiliary outputs and inputs Table A 8 lists the specific pinouts for the P8 Auxiliary port A 3 8 4 THREE 0 V 24 V AUXILIARY SIGNAL DRIVES The P8 Auxiliary port has three 0 V 24 V auxiliary signal drives that act as relays 24 V is considered the asserted state The auxiliary signal drives might be used for example to open and close valves in the system The total current available to these three drives the motor actuator and motor phase leads is 2 A The auxiliary signal drives are controlled from the CTRL gt gt 3 Immediate Operations gt gt 07 DigSet menu via GPIB or serial port input or from within a sequence The asserted state of auxiliary signal drives 1 and 2 is represented in the Status System Cont screen by the A1 and A2 digital status codes These status symbols are for digital inputs and outputs Do not confuse them with the analog inputs or analog outputs called A1 and A2 on the Model 6000 rear panel A 3 8 2 CONSTANT 15 V AND 15 V OUTPUTS The P8 Auxiliary port has constant 15 V and 15 V outputs that c
82. e probe head to verify that the helium backfill cylinder is still providing helium to the dewar 5 Leave the system standing for 48 hours with a full nitrogen Jacket and an active helium backfill cylinder Important To avoid excessive helium loss you should allow 48 hours for the dewar and probe to cool before you begin to transfer liquid helium Helium Transfer 1 Verify that the system pump and the Model 6000 are turned on and operating properly If either the pump or the Model 6000 is turned off turn it on If either the pump or the Model 6000 is on but appears to be malfunctioning contact a Quantum Design representative 2 Using the Model 6000 or the MultiVu Temperature dialog shown in Figure B 3 Instrument gt gt Temperature set the temperature to 5 K the rate to 10 K min and the approach mode to fast settle By setting the temperature to 5 K you open the flow control valve and ensure the maximum flow through the impedance tube Maximum flow is necessary to flush out the impedance and keep contaminants from freezing inside it while it cools to cryogenic temperatures The temperature will not actually drop to 5 K because there is no liquid helium in the dewar 3 Bring the liquid helium supply dewar close to the PPMS dewar Verify that the proper adapters and extensions are installed on the helium transfer line see Figures B 1 and B 5 Note that the long extensions perform an essential function The long extension on th
83. ead ports A 9 Ultra Low Field option 1 1 A 8 Index 6 PPMS Hardware Manual 1070 150 Rev B5 User bridge board 3 10 3 12 V Vacuum lines illustration c oer etna 3 6 modings adierei i ea 4 17 Vacuum pump See Pump Vacuum TUDES mocna en tatia 2 4 Varian pump illustration mennun ai 4 24 C 2 o Medo 4 25 C 3 SEIVICE i anini 4 23 4 27 C 1 C 6 Vent valve normal behavior 3 7 W Warm dewar fill filling an empty dewar comparison of methods B 2 B 3 nitrogen jacketed dewar sequential nitrogen and helium transfer assesses B 7 B 11 simultaneous nitrogen and helium transfer eeu aaia eiei B 3 B 7 standard dewar B 12 B 14 when to use eee 4 19 4 21 B 1 Quantum Design February 2008
84. ecautions ssssssss 1 6 uploading data sseesess 3 12 Physical Property Measurement System See PPMS Pinout tables a n A 12 A 22 Platinum resistance thermometer 3 2 Plumbing See Atmospheric control Ports illustration eeeeess A 2 A 9 on Model 6000 4 17 A 2 A 8 pinout tables sssssse A 12 A 22 probe head ots A 9 A 11 Index 4 PPMS Hardware Manual 1070 150 Rev B5 Pot fill mode See also Low temperature control modes characteristics eese 3 5 description seeesese 3 2 3 4 3 5 selecting sssssss 3 5 4 6 4 10 USING con rre zie e ee rr d Rs 4 6 4 10 POWet Off uu e cette etes 4 2 4 4 PPMS See also Hardware automating ss 3 10 3 11 3 12 block diagram seeeeee 3 1 customizing 1 1 3 10 3 12 4 11 4 17 A 2 A 8 A 11 dimensions ce eeeecececeee eee eeeeeeeeees 1 2 1 8 hardware overview 1 2 1 3 maintenance periodic eret e aee C 1 C 6 FOULING orf ooi Itidem 4 18 4 28 measurements 1 1 3 11 3 12 operating guidelines 4 1 4 10 OVOIVIOW i oie elias cec d ec eS 1 1 DOMS Wie hee 4 10 4 17 A 1 A 11 power loss ssseseeeeeee 4 2 4 3 safety precaut
85. edule and a form for tracking equipment service 4 7 1 Puck Adjustment You will need to adjust the sample puck whenever it fits loosely into the bottom of the chamber or after you have inserted it into the sample chamber approximately 10 times Figure 4 15 displays the components of the puck adjustment tool and the steps below explain how to use it 1 Place the puck on the finger spreader see Figure 4 15 FINGER TEST CUTOUT Te ACE A ee itty FINGER nd IND 4 p CYLINDER 1 LINDER 2 Figure 4 15 Puck adjustment tool 2 Remove the puck from the finger spreader 3 Place the puck inside the finger contractor 4 Press straight down on the puck and continue pressing until the puck is pressed completely into the finger contractor When the entire chuck is in the contractor the contractor evenly applies force to the outside of the fingers pushing them inward The contractor pushes the fingers regardless of external wear or variations on the puck so that they obtain their optimal location 5 Remove the puck from the finger contractor 6 Place the puck inside the test cutout Verify that the puck fits easily but snugly in the test cutout 4 18 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 7 System Operation Routine Maintenance Procedures 4 7 2 Refilling a Cold Dewar WARNING Always wear protective clothing including thermal
86. ements You can use other instruments to measure other sample characteristics You can even interface GPIB capable instruments with the Model 6000 and a PC in order to facilitate automated data collection from other instruments With some planning you can set up the PPMS to automatically perform all types of different experiments If you have questions about how to customize the PPMS to fit your specific application contact a Quantum Design representative Quantum Design offers a variety of options designed specifically to help meet the needs of your experiments 3 8 Example Measurement The PPMS can be configured for four terminal resistance Hall effect magneto resistance critical current critical field critical temperature DC magnetization AC susceptibility heat capacity and thermal conductivity measurements to name some of its more common uses Quantum Design is continually developing PPMS options that standardize frequently made measurements making them easier to perform and more accurate You use each option in conjunction with the PPMS in a different manner One of the most common measurements made with the PPMS is resistivity Quantum Design offers more than one resistivity option for the PPMS This section describes a resistance measurement to illustrate how you can use the PPMS To perform four terminal resistance measurements you mount a sample on a puck and attach four leads to the Figure 3 6 Leads attached for samp
87. emperature is reported with a typical accuracy of 0 5 Temperature can be varied with full sweep capability and slew rates from 0 01 K min up to 12 K min Temperature stability is lt 0 2 for temperatures lt 10 K and lt 0 02 for temperatures gt 10 K Please familiarize yourself with the information in this manual which is designed to help you operate and maintain the basic PPMS platform It is important that you understand the basic PPMS platform before you perform PPMS experiments or use PPMS options For information about PPMS MultiVu which is the Windows based software application that controls operation of the PPMS and its options refer to the Physical Property Measurement System PPMS MultiVu Application User s Manual Quantum Design PPMS Hardware Manual 1070 150 Rev B5 1 1 February 2008 Section 1 3 Chapter 1 Overview of System Hardware Introduction and System Setup 1 3 Overview of System Hardware Figure 1 1 illustrates a base PPMS and the approximate dimensions of each component Note that the actual dimensions and layout of your PPMS will reflect the system that you purchase e g options type of dewar and your laboratory Dimensions of the electronics cabinet and the various dewars are listed in Table 1 2 The base system includes the following hardware components which are described in Chapter 2 o dewar o Model 6000 PPMS Controller o probe o vacuum pump o top plate assembly o pumping lines o probe lift
88. ened sss C 1 Versions of the PPMS vacuum pump ssessesseeeeeeeeeenneenne eene C 2 PPMS Hardware Manual 1070 150 Rev B5 xi February 2008 Contents Table of Tables Tables Table 1 1 Table 1 2 Table 3 1 Table 4 1 Table 4 2 Table 4 3 Table 4 4 Table A 1 Table A 2 Table A 3 Table A 4 Table A 5 Table A 6 Table A 7 Table A 8 Table A 9 Table A 10 Table A 11 Table A 12 Table A 13 Table C 1 Table C 2 xii Possible effects of the PPMS magnet based on a system with a 9 T longitudinal magnet sss 1 7 Approximate physical dimensions of the PPMS dewars and the electronics cabinet seeessseseesseeeeeereneeen trennen 1 8 Characteristics of low temperature control modes ses 3 5 Status codes for temperature control modes sssssssseseeeeeee 4 8 Commands to shut down the PPMS and set the temperature control modes 4 9 Status codes for the Model 6000 digital inputs and outputs ssssssse 4 17 Types of vacuum pumps used on the PPMS and their characteristics 4 25 Sample co nriectlons icu eet te ete Pee eerte eee rein A 12 System bridge connections esssssseseseeeeeeeeee nennen enne en A 13 Communication port connections GPIB seen A 14 Communication port connections RS 232 sssssssssseseeeeeeeeen A 15 DP
89. ening windows and doors if there is an excessive helium release The procedures for a filling a warm standard non nitrogen jacketed dewar with liquid helium are not difficult but involve many steps Quantum Design staff strongly recommend that you read the entire set of procedures before beginning the transfer As noted in Section B 2 3 Materials you will be working with transfer lines and valves for two dewars the PPMS dewar and a liquid helium supply dewar and a helium gas supply cylinder The transfer setup is shown below in Figure B 8 Your preparation will facilitate the process which also will be smoother if there are two people TRANSFER LINE oa ADAPTERS INPUT LONG OUTPUT EXTENSION EXTENSION LIQUID ACCESS PORT TOP OPEN DURING TRANSFER ONLY PRIMARY RELIEF VALVE PRESSURE GAUGE REAR SED DURING CAS PHASE VALVE TRANS SER ONLY V DIRECT VENT SAFETY VALVE EVACUATION PPMS DEWAR VALME LIQUID HELIUM HELIUM GAS SUPPLY DEWAR CYLINDER Figure B 8 Liquid helium transfer arrangement for transferring helium into a warm non jacketed dewar Set Up 1 Verify that the system pump and the Model 6000 are turned on and operating properly If either the pump or the Model 6000 is on but appears to be malfunctioning contact a Quantum Design representative 2 Using the MultiVu Temperature dialog shown in Figure B 3 Instrument gt gt Temperatur
90. er the top plate a centering ring O ring and hinge clamp the top plate baffle assembly and a threaded adapter The top plate is a KF blank flange that closes the sample chamber access port A centering ring with an O ring around its diameter fits between the blank flange and the access port in order to seal the sample chamber A hinge clamp holds the blank flange on top of the access port The top plate baffle assembly is a set of baffles on a light G 10 rod that is attached to the bottom of the blank flange The baffles confine thermal gradients to specific regions of the sample chamber aiding thermal control so that the system can achieve temperatures as low as 1 9 K A small threaded adapter at the end of the baffle rod allows you to attach other components to the rod Note that some PPMS options seal the sample chamber differently and do not use the components shown in Figure 2 5 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 2 Hardware Quantum Design Section 2 4 Top Plate Assembly HINGE CLAMP KF BLANK FLANGE SS ISG SESS CENTERING RING WITH O RING SAMPLE CHAMBER ACCESS PORT TOP PLATE BAFFLE ASSEMBLY Figure 2 5 Cross section of top plate assembly PPMS Hardware Manual 1070 150 Rev B5 2 7 February 2008 Section 2 6 Chapter 2 Model 6000 PPMS Controller Hardware 2 9 Probe Lifting Assembly The probe lifting assembly Figure 2 6 is used to install and remove the probe The
91. er Service at Quantum Design if you have questions about the other dewars If you have any questions about this issue please contact Customer Service at Quantum Design Quantum Design PPMS Hardware Manual 1070 150 Rev B5 2 1 February 2008 Section 2 2 Dewar 4X LIFTING LUGS EVACUATION VALVE 2 2 Chapter 2 Hardware 2 2 1 1 STANDARD DEWAR Figure 2 1 illustrates a top view and a cross section of a standard dewar The standard dewar contains a set of heat shields around the neck of the helium container and does not have a nitrogen jacket Otherwise it is similar to but slightly smaller than the nitrogen jacketed dewar Standard dewars have a 30 L liquid helium capacity 5X VAPOR SHIELDS LIQUID HELIUM ACTIVATED CHARCOAL RUPTURE DISC SUPERINSULATION Figure 2 1 Top view and cross section of a standard dewar illustrating construction of dewars without a nitrogen jacket dimensions are in inches 22 1 2 NITROGEN JACKETED DEWAR Nitrogen jacketed dewars Figure 2 2 consume significantly less liquid helium than dewars without nitrogen jackets Two liquid nitrogen fill ports give the top of the nitrogen jacketed dewar a distinctive appearance The operating efficiency of nitrogen jacketed dewars is partly due to a layer of liquid nitrogen sandwiched between the superinsulation and the liquid helium which further insulates the helium bath as does the vacuum in the region between the liquid helium
92. ere is a leak in the vacuum space Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 1 February 2008 Section 4 2 Chapter 4 General Guidelines System Operation Handle the probe with care it is an intricate delicate and expensive piece of equipment Always use the plate just below the probe head Figure 2 4 to support the probe The long tubes that run between the probe head and the magnet end of the probe are part of the equipment they are not structural supports they cannot support the full weight of the probe and they are easily damaged Always provide support at both the magnet end and the probe head when you lay the probe in a horizontal position It is important to work slowly and carefully when you lower a probe into or lift a probe out of a full or partially full dewar To facilitate this process Quantum Design includes a probe lifting assembly with the system see Section 4 7 4 By gradually lowering the probe into the dewar you decrease the unnecessary helium boil off caused by a warm probe It also can avoid serious damage to the equipment that could occur if a part of the probe froze or boiled because of unexpected circumstances such as a leak In addition you can watch for unusual behavior such as condensation or gas escaping from relief valves when you slowly move a probe in and out of liquid helium Keep the original packing crate and padding for the probe so that you can use it in the event you ship the
93. erify that it is properly seated inside into the cylinder of puck insertion tool the hollow cylinder of the puck insertion tool The puck should rotate smoothly The P150 sample wiring test station is also referred to as the puck wiring test station The name of this tool varies by context it might be called the puck insertion tool the puck extraction tool or the sample holder tool 4 12 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 5 System Operation Sample Puck Installation and Removal 4 Engage the puck insertion tool by flipping down the black switch located on top of the tool or by releasing the switch if it is fully depressed so that the switch lies flat across the handle see Figure 4 13 The tool should now be gripping the outer rim of the puck 5 Verify that the puck remains properly seated in the hollow cylinder of the puck insertion tool The puck must be level and it must not rotate otherwise it could come loose in the sample chamber or bend the pins at the bottom of the sample chamber If the puck lodges in the sample chamber you might have to disassemble the probe to remove it CAUTION The puck insertion tool and puck will be inserted into the sample chamber Verify that the puck is level within the cylinder of the puck insertion tool and firmly attached to the tool so that it cannot fall into the sample chamber Also hold the tool so that the bottom is level
94. ew r Connections nte vci te ae e aat E EE TA A N PUES EE Led ae A 16 Magnet connections Model 6700 to Model 6000 sse A 17 Magnet connections probe to controller esses A 18 Expansion connections auxiliary eene A 19 Expansion connections pressure gauge sse ener A 20 Expansion connections motor esee nennen A 21 Expansion connections external esses ener A 22 Replacement fuse values for 100 120 VAC systems eene A 23 Replacement fuse values for 200 240 VAC systems sese A 23 Maintenance schedule for PPMS rotary vane pumps esses C 2 Characteristics of vacuum pumps used on the PPMS sssssseeeee C 3 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 P R EF A C E Contents and Conventions P 1 P 2 P 3 Introduction This preface contains the following information o Section P 2 discusses the overall scope of Section P 4 illustrates and describes the manual conventions that appear in the manual o Section P 3 briefly summarizes the contents of the manual Scope of the Manual This manual contains the information that you will need to use the Physical Property Measurement System PPMS including materials on its basic functionality and the hardware that is unique to it This manual does not cover the PPMS MultiVu software which is the Windows based application that ru
95. ff the toggle switch PPMS Hardware Manuall 1070 150 Rev B5 C 3 February 2008 Section C 4 Appendix C Changing the Pump Oil and Oil Mist Cartridge Vacuum Pump Assembly Maintenance 4 Open the console cabinet and hold your hand near the pump If the pump is uncomfortably warm let it cool before you proceed to the next section C 4 1 2 DRAIN PUMP OIL 1 Ifthe system has an Alcatel pump remove the black faceplate that frames the oil level window Figure C 2 2 Remove the oil fill cap on the top of the pump Save the O ring 3 Slide the pump forward out of the cabinet so the oil will be able to drain into a container 4 Place an empty container capacity at least one liter under the drain plug on the front of the pump 5 Remove the drain plug and allow the oil to drain completely lifting the rear of the pump if necessary to empty it 6 Reinstall the drain plug C 4 1 3 DRAIN REPLACE OIL MIST FILTER CARTRIDGE Unscrew the bell jar of the oil mist filter which is mounted on the inside wall of the electronics cabinet 2 Pour the oil into the used oil container 3 Examine the filter cartridge If the filter cartridge is not saturated with oil go to Step 4 of this section If the filter cartridge is saturated with oil you must replace it contact Quantum Design if you need a replacement a Unscrew the oil mist filter cartridge b Lubricate and install the new O ring supplied with the cartridge on the
96. fficult to move due to low internal pressure do not force it Allow the pressure within the chamber to match the external pressure before you open the sample chamber to atmosphere 5 Remove the O ring from the sample chamber access port 6 Disengage the puck insertion tool by flipping up the black switch located on top of the tool or by fully depressing the switch see Figure 4 12 7 Gently lower the puck insertion tool cylinder end first into the sample chamber until the tool touches the bottom of the chamber 8 Engage the puck insertion tool by flipping down the black switch located on top of the tool or by releasing the switch 1f it is fully depressed so that the switch lies flat across the tool s handle see Figure 4 12 9 Gently raise the insertion tool out of the sample chamber You should feel some initial resistance as you pull the puck out of its seat 10 Verify that the sample puck is in the insertion tool If it is not return to Step 6 If it is disengage the lever and let the puck fall safely into your hand Do not drop the puck Now you can insert another puck install a PPMS option into the sample chamber or close the sample chamber 4 5 3 Closing an Empty Sample Chamber Use the procedures below to close the sample chamber when it does not have a sample installed Place the O ring and KF blank flange over the sample chamber access port see Figure 2 5 2 Place the flange clamp in position around the top
97. filter c Lubricate and install the new seal supplied with the cartridge for the bell jar d Screw on the new filter cartridge 4 Screw the bell jar back into place C 4 1 4 FILL AND RE INSTALL PUMP 1 Fill the pump with oil to the top mark of the oil level window do not overfill 2 Reinstall the oil fill cap 3 Ifthe system has an Alcatel pump replace the faceplate that frames the oil level window Figure C 2 4 Slide the pump back into the electronics cabinet 5 Turn the pump on and wait one minute so that the metal pumping lines can be evacuated Verify that the pumping lines are seated in their connectors but not pressed in completely 6 Reconnect the two metal pumping lines to the probe head 7 Purge and seal the sample chamber 8 Close the front door of the electronics cabinet 9 The oil change procedure is now complete Please dispose of the used oil properly C 4 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix C Section C 5 Vacuum Pump Assembly Maintenance Servicing the Foreline Trap C 5 Servicing the Foreline Trap The foreline trap acts as the inlet filter for the pump The filtering component is activated alumina which needs to be checked twice a year WARNING Put the system in Shutdown mode and disconnect the two metal pumping lines before you service the pump or related components Any leaks into the sample chamber and cooling annulus can produce ice a
98. g helps keep the sample chamber free of contaminants from the air To vent the chamber you can use the Model 6000 menu CTRL gt gt 1 Interactive Control gt gt 5 Vent Continuous or you can use the PPMS MultiVu application software Instrument gt gt Chamber gt gt Vent Cont Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 13 February 2008 Section 4 5 Sample Puck Installation and Removal 4 5 2 4 14 10 11 12 T3 14 15 16 17 18 Chapter 4 System Operation Open the hinge clamp and remove the KF blank flange from the sample chamber access port see Figure 2 5 If the blank flange is difficult to move because the internal pressure is low do not force it Allow the pressure within the chamber to match the external pressure before you open the sample chamber to atmosphere Remove the O ring from the sample chamber access port Gently lower the puck insertion tool into the sample chamber with the puck end first Stop when the sample puck touches the puck connectors at the bottom of the chamber Do not force the puck down farther after it touches the connectors Slowly rotate the puck insertion tool until the key on the puck drops into the indexing notch When the puck drops into the notch you will feel it lock into position Gently push down on the puck insertion tool in order to engage the puck interface and to make solid electrical contact between the interface and the p
99. hamber see Figure 3 2 where it heats the sample to the desired temperature and warms the vapor in the cooling annulus thus uniformly warming the entire sample space Thermal gradients in the sample space are further minimized by a neck heater which is wrapped around the sample chamber and located just above the sample space and near the neck thermometer The flow control valve and the block and neck heaters use the sample temperature and neck temperature as feedback to obtain rapid thermal control Maximum warming and cooling rates are around 6 K min 3 3 1 2 CONTINUOUS LOW TEMPERATURE CONTROL The system uses the Continuous Low Temperature Control CLTC option to regulate temperatures below about 4 2 K by drawing cold helium gas through the carefully tuned CLTC flow impedance that restricts the gas flow Flow through the primary impedance is completely turned off and the helium gas is drawn from the CLTC impedance through the annulus to cool the sample space The system heaters warm the gas and the sample space directly CLTC mode includes a precooling phase that begins when the temperature in the sample space is about 11 K The precooling minimizes thermal gradients in the sample chamber so that the unit can indefinitely maintain temperatures below 4 2 K and ensures that the temperature of the chamber smoothly transitions through 4 2 K The precooling method uses aggressive feedback on multiple parameters This might cause a temporary loss of
100. he temperature set point slowly from only one direction so it does not overshoot or undershoot the set point Thermal equilibrium takes considerably longer to achieve in No Overshoot mode 3 4 Atmospheric Control The PPMS vacuum and gas lines accommodate thermal control and atmospheric control of the sample chamber Figure 3 3 illustrates the vacuum and gas lines SUPERINSULATION LIQUID NITROGEN VACUUM MODEL 6000 REAR PANEL See LIQUID HELIUM COOLING ANNULUS Hn I SAMPLE SPACE v UL I IMPEDANCE ASSEMBLY Figure 3 3 Gas and vacuum control in the PPMS TO COOLING ANNULUS TO SAMPLE SPACE zl TO DEWAR REMOVABLE HOSES O dNAd 3ldWvS WANSVA WALSAS dNNd OL dN LN3A JIdNYS FLOW METER L ae E e FLOW CONTROL N VALVE VENT FLUSH SOLID STATE SILICON VALVE VALVE PRESSURE SENSOR Z DIFFERENTIAL PRESSURE SENSOR The flow control valve and the differential pressure sensor are part of the PPMS temperature control system The flow control valve which is between the pump and cooling annulus adjusts the rate at which helium vapor is drawn across the sample chamber The differential pressure sensor which is between the annulus and dewar monitors the pressure difference between the annulus and dewar in order to facilitate filling the annulus with helium for low temperature operation 3 6 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 3 Section 3 5 Theory
101. helium fill ports is fitted with a 1 psi pressure relief valve to allow pressure to be released before dangerous levels are reached Do not tamper with these pressure relief valves Sample Chamber Access Port The sample chamber access port is used to move samples in and out of the sample chamber A blank flange with an O ring seal normally covers the sample chamber access port A hinge clamp which is provided with the system holds the blank flange on the top of the port Some PPMS options have hardware that attaches to the flange Sample Chamber Pressure Relief Valve The sample chamber pressure relief valve prevents the buildup of dangerous pressures within the sample chamber The valve extends from the back of the sample chamber access port Do not tamper with this pressure relief valve PPMS Hardware Manual 1070 150 Rev B5 February 2008 A 9 Section A 4 Appendix A Probe Head Ports Connections Ports and Pinouts A 4 4 Smaller Metal Hose Connector The smaller 1 4 inch metal hose connector attaches to the Sample Space gas port on the rear of the Model 6000 The 1 4 inch metal hose connector allows sample space venting and evacuation A 4 5 Larger Metal Hose Connector The larger 3 8 inch metal hose connector attaches to the Annulus gas port on the rear of the Model 6000 The 3 8 inch metal hose connector allows the pump to pull helium through the impedance tube and annulus A 4 6 Hose Nipple The hose nipple d
102. hile the magnet is ramping CAUTION Never turn off the power to the Model 6700 while the magnet is ramping 2 7 2 Model 3120 Magnet Power Supply See Model 3120 Magnet Power Supply user s manual for more information 2 8 Electronics Cabinet The electronics cabinet Figure 2 9 holds the Model 6000 and Model 6700 if present the vacuum pump and a power strip It also has room for the additional hardware and electronics needed with some PPMS options Refer to Section 1 4 3 for electrical specifications for the cabinet MODEL 6000 MODEL 6700 FRONT PANEL I 56er EE Figure 2 9 PPMS electronics cabinet 2 10 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 2 Hardware 2 9 2 10 Section 2 10 Sample Puck and Assorted Tools Vacuum Pump A direct drive pump operates continuously to control pressure in the sample chamber and to aid thermal control Valves in the Model 6000 regulate the vacuum and the gas flow rates Figure 2 10 shows one of the models of pumps used in the PPMS The pump is installed in the bottom of the electronics cabinet It should have an oil mist filter attached to its exhaust line and a foreline trap on its input to protect the system from contamination The oil mist filter is located on an inside wall of the electronics cabinet The vacuum pump must be maintained to ensure optimal performance of your PPMS Pump operation and maintenance are
103. ill still work Additional plumbing and gauges can also be inserted between the pump and flush valve If a high or ultra high vacuum is required in the sample space you can insert an alternate type of vacuum pump into the system near the probe head where larger throughputs can be achieved The efficiency of sample space temperature control can be adversely affected by changing the pressure of gas within the sample chamber However rather than thermal control through heat exchange some experiments require an adiabatic environment e g heat capacity Quantum Design offers a High Vacuum option for the PPMS for precisely such requirements 3 5 Magnetic Field Control WARNING The helium level must be above the superconducting magnet a helium level of about 6096 to take the magnet to full field There is high potential for damage such as an uncontrolled magnet quench when the superconducting magnet is not completely covered by helium See Sections 1 4 2 and 4 2 4 for more information Figure 3 4 illustrates how the current through the magnet coil is changed to charge or discharge the magnet The essential process is as follows 1 The Model 6700 Magnet or Model 3120 Controller matches the current in the magnet 2 Asmall portion of the superconducting magnet wire the persistence switch is heated by another resistive wire 3 The heated persistence switch becomes non superconducting which switches the magnet contro
104. iment The thermal conductivity of an insulator also might be important depending on the nature of the experiment It is often important that the sample and puck are in good thermal contact which ensures that the temperature of the system thermometer accurately represents the temperature of the sample If the sample is in poor thermal contact with the puck heat conduction will occur through the leads and through helium gas which is significantly slower than through the puck The surface of the puck can be machined to the desired geometric characteristics To do this you first remove the screw from the bottom of the puck and take off the connector PC board so that it will not be damaged during machine work Work carefully so that you do not alter the edge of the puck where the key and the groove for the puck insertion tool are located Also you can remove the connector PC board from the bottom of the puck before you perform other puck treatments such as heat treatment If you want to verify proper electrical connection of the sample before you insert the puck into the sample chamber you can use a digital voltmeter or similar instrument after you have mounted the sample Using Figure 4 11 as an example gently contact the gold plated receptacles on the bottom of the puck with the meter probes Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 11 February 2008 Section 4 5 Chapter 4 Sample Puck Installation and Removal System Operatio
105. ine is indicated in the Status System Cont screen by UR and HL on the digital input status line respectively You can also use the CTRL gt gt 3 Immediate Operations gt gt 11 Measure command to read the status Furthermore when you use the sync command within a sequence the hold state of the hold line pauses sequence execution This function applies only to the hold line not the user line A 6 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 3 Connections Ports and Pinouts Model 6000 Rear Panel Ports A 3 13 Annulus Port The Annulus port connects the annulus to the flow control valve in the Model 6000 The longer 3 8 inch stainless steel hose connects the Annulus port to the QC quick connect fitting on the probe head A 3 14 Pump Port The Pump port connects the Model 6000 gas lines to the vacuum pump that pumps on the sample chamber and the annulus The shorter 3 8 inch stainless steel hose attaches to the Pump port A 3 15 System Vacuum Port The System Vacuum port provides direct access to the system pump allowing the connection of other gas and vacuum lines and devices between the vacuum pump and flush valve Under normal circumstances a short hose connects the Sample Pump Out port to the System Vacuum port allowing the pump to pump directly on the sample space A 3 16 Sample Pump Out Port The Sample Pump Out port accesses the
106. ing assembly o connection cables o electronics cabinet o power cords i 3 1m PROBE EXTRACTION HEIGHT 19 DIAMETER 48cm 22 a i Cg 56cm al lt 61cm Figure 1 1 Components of the base PPMS and approximate dimensions measurements are rounded 1 2 7 The inch to cm equivalences are approximate because both measures were rounded after inches had been converted to centimeters 1 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 1 Section 1 4 Introduction and System Setup Safety Precautions Most systems also include a personal computer a sample puck kit and a helium transfer kit You can order other options to expand the capabilities of the base system including a magnet and either the Model 6700 Magnet Controller or the Model 3120 Magnet Power Supply The PPMS can be equipped with a 1 T 7 T 9 T 14 T or 16 T longitudinal magnet or a 7 T transverse magnet With the exception of 14 T and 16 T longitudinal systems and 7 T transverse systems PPMS units can operate with one of three different types of dewars the standard nitrogen jacketed or high capacity nitrogen jacketed dewar Two nitrogen fill ports located on top of the nitrogen jacketed dewar distinguish it from the standard non nitrogen jacketed dewar Figure 1 2 illustrates the nitrogen fill ports and Figures 2 1 2 3 illustrate these three dewars A li
107. ion 4 7 2 1 explains how to transfer liquid nitrogen into a cold PPMS dewar To determine if nitrogen remains in the jacket look for ice on one of the pressure relief valves You can check the nitrogen level by dipping a clean frosted metal rod into the jacket through one of the nitrogen fill ports To frost the rod dip it in liquid nitrogen then expose it to room temperature air 4 3 Setting the Low Temperature Control Mode The Quantum Design PPMS offers two unique modes for controlling low temperatures in the sample chamber Continuous Low Temperature Control CLTC and pot fill these modes are explained in Chapter 3 Since January 1998 the PPMS has included both modes with CLTC shipped as the default Earlier model PPMS systems included only the pot fill mode but owners of such systems can purchase the CLTC option If your PPMS has the capability for both low temperature control modes you can change from CLTC to pot fill mode or vice versa by using the MultiVu Utilities dropdown menu or the Mon6000 utility which is often located in C N ODPPMS Tools Here we include instructions for using both utilities To determine if you have the CLTC option follow the MultiVu instructions in Section 4 3 1 1 through Step 3 4 6 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 System Operation Section 4 3 Setting the Low Temperature Control Mode 4 3 1 MultiVu As explained below you will first verify
108. ions 1 3 1 7 setup and environmental factors s isbers the douse aaacaatniea lob lebe EES TETE 1 7 1 8 shutting Off power ssss 4 2 4 4 PPMS MultiVu ssss 3 10 3 12 Pressure gauge external expansion connections pinout table A 20 providing power ssssesee A 5 Probe See also Magnet Temperature control as part of base hardware 1 2 COMPONENMS ccecececeeececeeeeeteeeeeees 2 3 2 6 description ien eei 2 3 extraction height illustration 1 2 handling instructions 4 1 4 2 4 27 head See Probe head lowering into dewar 4 1 4 2 4 27 removing from dewar 4 1 4 2 4 27 Probe head connections block diagram A 1 description eeeeeeee 2 5 A 9 ports description 1 oie trei A 9 A 11 illustration sss A 1 A 2 A 9 pinout tables A 12 A 13 A 16 A 18 pressure relief valves illustration 1 4 A 9 Probe lifting assembly as part of base hardware 1 2 T ri ctionis acci t t ded 2 8 NET 4 27 Protective cap fnt ia sett ette 2 4 2 5 in illustration of probe components 2 4 Quantum Design February 2008 Puck See also Sample mounting adjusting tension 4 18 adjustment tool 2 12 2 13 4 18
109. le An example is shown in Figure 3 6 you can use four terminal resistance other geometrical arrangements of the leads measurement Solder each lead to an appropriate solder pad on the base of the puck This allows the hardware to make electrical contact with the sample In the Model P400 Resistivity option the hardware that makes electrical contact with the sample is the user bridge board in the Model 6000 and the solder pads you use are 3 4 5 and 6 see Appendix A To perform simultaneous measurements on another sample the other sample would be mounted to the same puck and its leads would be soldered to pads 7 8 9 and 10 Take care that you electrically isolate each sample and each sample lead The puck is conductive so the leads must be insulated and samples must be mounted with an electric but not thermal insulator underneath them Most PPMS options also allow you to use special pucks that have labeled solder pads prewired to the surface of the puck for easier sample mounting Some options such as the ACMS option or the Horizontal or Vertical Rotator option use different sample holders You will insert the puck into the sample chamber by using the procedures explained in Section 4 5 During the measurement the hardware will pass a current through the sample via two leads using the other two leads to measure the electric potential drop across the sample Because the input impedance of the voltmeter is very high both the current
110. lerta one eue A 7 A314 Pump POrt z Lei etait uderintenteiiet E eie eus A 7 A 3 15 System Vacuum Port cccssccssccssesscsssccsscccsscecsonsecsescessecceseuscsssaessesccenseeseuseseenaeseeceess A 7 A 3 16 Sample Pump Out Port sssini 3 e tecti t pie tee oe CEU Ee er deer dee UR ide A 7 A3 T7 Sample Space Port ae eee e tte eee tede jas Ne dag e due A 7 A318 Sample V ent Up Dort nere ctn o t er e E A 7 A319 Gas Source Port eunte pene e ee ed ge inated A 8 A320 Dewar Port eget ette TU ER Feeder adeo teta aa ep eere oae nice canes A 8 I 3 2 1 Syst SA FUSE seis nid eee ett n e e E ot vb A ER HER ERE wet rage eco A 8 Ix 3 22 AUX 2 Ac FUSE odo ieu iie e iate Y deste re e Aa E t dae ro LEER e LER OE sues A 8 A323 Quench Heater FUSE Leere eet erede E aree Yee kn vvv NN eR REN cus beans WS ERES UNE A 8 A324 Power Receptacles ca os ete ee e Irt REA e eive deque a A 8 AA Probe Head Ports undae tette etiem p epp ERES UR A 9 ADT Helium Fill Ports a tec eed veste a toa oe a Pct tota ieu dte A 9 A 4 2 Sample Chamber Access Port ener ener nns A 9 A 4 3 Sample Chamber Pressure Relief Valve esses A 9 A 4 4 Smaller Metal Hose Connector ccccccccesccesscessceeeceeeceeeeeeseeeseeescecsaecsaecaeseeeseeeeeeenses A 10 A 4 5 Larger Metal Hose Connector eene enne A 10 4 6 Hose Nipple feck E et Sees deett Reed cotra edet Lee edu ve Epp pe dbs ente cv A 10 AA Ultra Extting nee omn etn Ter co p logus A 10 A 4 8 Magnet C
111. ller into the previously closed superconducting circuit 4 The magnet controller drives the magnet to the current that is necessary for the new field Quantum Design PPMS Hardware Manual 1070 150 Rev B5 3 7 February 2008 Section 3 5 Chapter 3 Magnetic Field Control Theory of Operation MAGNET J PERSISTENT iL H H 4 SWITCH T o MAGNET PERSISTENT AACN MAGNET PERSISTENT MAG SWITC gt JER MAGN SWITC H H VITCH s H Ha ITCH acier J PERSISTENT S SWITCH T H H PERSISTENT SWITCH r M AGNET MAGNET PERSISTENT El H H MAGNET H H Figure 3 4 Changing the field in the magnet To change the field in the magnet from Ho a to H f the magnet power supply first matches the magnet current b Then the persistent switch heater is turned on c switching the power supply into the circuit The current is driven to the new value d and the persistent switch heater is turned off e The persistence switch heater is generally turned off after the field set point is reached allowing the entire magnet to superconduct again The magnet 1s in Persistent mode when the persistence switch is superconducting In Persistent mode the current in the magnet does not dissipate so the power supply current can be turned off The magnet can also be operated in Driven mode which retains the current source in the magnet circuit in order to drive the c
112. ly o Section 2 5 describes the probe lifting o Section 2 10 describes the sample puck assembly and the puck tools o Section 2 6 describes the Model 6000 PPMS Controller Dewar The dewar contains the liquid helium bath in which the probe is immersed Primarily constructed of aluminum the outer layer of the dewar has reflective superinsulation to help minimize helium consumption The outer layer is evacuated through a valve on the top of the dewar Figures 2 1 2 2 and 2 3 this evacuation valve must not be modified or altered The dewar regions that are evacuated contain activated charcoal on cold surfaces to aid cryopumping Most PPMS units can operate with one of three different types of dewars the standard dewar Figure 2 1 the nitrogen jacketed dewar Figure 2 2 or the high capacity nitrogen jacketed dewar Figure 2 3 The exceptions include EverCool units and systems that have a 14 T or 16 T longitudinal magnet or a 7 T transverse magnet Instructions for filling warm or empty dewars with nitrogen and helium are given in Appendix B and instructions for refilling cold dewars with nitrogen and helium are given in Sections 4 7 2 Note Due to physical constraints EverCool systems and systems with a 14 T or 16 T longitudinal magnet or a 7 T transverse magnet have special dewars that are not discussed in this manual For more information about EverCool dewars refer to the PPMS EverCool Dewar Option User s Manual Contact Custom
113. m Connections eene enne entente ente nennen nnne nenne nene irren nennen A 1 A 3 Model 6000 Rear Panel Ports ecccesesssesscesesseeeeceseesecaeeeneseceaeeaeeeeceaecaeeeneeaecaaeeaeereeaeeatees A 2 A 37 TP T User Bridge Port 5e neret RR BERHEMDIEEIS A 2 33 2 P2 System Bridge Pott oneen ie tene nre eode nivem etat ped eios A 3 A33 IP3 Option Portu ante eT RAT Te REN Pa dete ES Enn ta A 3 A 3A IBIESIBEBASS POF booeuitasii aoreet Dare a E trou e tanned atere vaste iu PU ars A 3 A SS c PS RS252 POM util Gute cederent R E ae e otetlepa pp diu in ida bat UIS A 3 A360 PG Dewar Dort usas E A MO DHEPIIU eise Ups A 3 Ab PIM aaNet Portae D RR EE PR TNI NOSetuss A 4 A38 PS Auxiliary Portu abeat tdt etie A E R E AA AE EO A 4 A 3 8 1 Three 0 V 24 V Auxiliary Signal Drives sse A 4 A 3 8 2 Constant 15 V and 15 V Outputs nnne A 4 3 8 3 TWO SENSE EINES uci te a rH RET E pou squesa thie ne eget etie bine A 4 A 3 8 4 Two Analog Signal Inputs sees A 5 A389 PO Pressure Bottin be dee et o teer Satan e Feet nose edis A 5 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 vii February 2008 Contents Table of Contents A300 1 2 83 dnd A4 OIG oe ceteeti Dare ebeedet b eir rebate etie A 5 ALS TL IOPTO MOtOr POE en repre tei teile ette ete oe re e aee ERES A 6 A3 122P 11 HExtemal Port ioi efte bt epi ales elas ue Hehe ives virtues A 6 53 13 Amn lus POrt ee oet od ent aer tec cb ades iie t cpu a
114. m Design PPMS Hardware Manual 1070 150 Rev B5 A 5 February 2008 Section A 3 Appendix A Model 6000 Rear Panel Ports Connections Ports and Pinouts A311 P10 Motor Port If the system includes options that use a Quantum Design sample transport or rotator motor the motor is connected to the P10 Motor port If a sample transport or rotator motor is not installed then the P10 Motor port can be used to drive a small 12 V external stepper motor A 0 24 V actuator identical to the auxiliary digital signal drives in the P8 Auxiliary port is included in the P10 Motor port When this actuator is active the Status System Cont screen displays the AC digital status code The total current available to the motor actuator motor phase leads and three auxiliary signal drives is 2 A The P10 Motor port also includes a TTL level index switch and limit switch leads in addition to the four phase leads and actuator leads Index and limit switches should normally be wired closed When these circuits are broken the Status System Cont screen displays the LM and NX digital status codes to indicate that the limit and index switches are active This occurs whenever a motor is not connected to the Model 6000 or whenever an index or limit switch is tripped You can use the Status System screen to monitor the motor position Commands pertinent to the motor configuration position control and position measurement
115. manner that is not specified by Quantum Design the protection afforded by the equipment could be impaired Quantum Design PPMS Hardware Manual 1070 150 Rev B5 1 3 February 2008 Section 1 4 Chapter 1 SafetyPrecautions Introduction and System Setup 1 4 1 Cryogens WARNING Always wear protective clothing and ensure that the room has good ventilation when you work with cryogenic materials such as liquid helium and liquid nitrogen This will protect you against cryogenic material hazards 1 they can expand explosively when exposed to room temperature 2 they can cause serious burns Always wear protective clothing including thermal gloves eye protection and covered shoes when you work with liquid helium liquid nitrogen or other cryogens Avoid loose clothing or loose fitting gloves that could collect cryogenic liquids next to the skin The extreme cold of liquid and gaseous cryogens can cause serious burns and has the potential to cause loss of limbs Surfaces that have been exposed to these cryogens are extremely cold and should not be allowed to contact skin Work with cryogenic materials in well ventilated areas only In the event a helium container ruptures or there is a helium spill vent the room immediately and evacuate all personnel In a poorly ventilated area helium can displace the air leading to asphyxiation Because helium rises well vented rooms with high ceilings are generally safest
116. mist filter that cleans the exhaust FRONT PANEL Figure C 1 PPMS electronics cabinet with front panel opened Quantum Design PPMS Hardware Manual 1070 150 Rev B5 C 1 February 2008 Section C 3 Appendix C Pump Versions Vacuum Pump Assembly Maintenance For optimal performance of your system the pump oil mist filter and foreline trap require regular maintenance as shown in Table C 1 Instructions for more major types of service are provided here while instructions for basic services e g adding oil to the pump are in Chapter 4 Table C 1 Maintenance schedule for PPMS rotary vane pumps COMPONENT SERVICE FREQUENCY Pump Check oil level Check monthly sooner with heavy use Add oil When reaches lower part of oil level window Change oil When dirty when vacuum is unsatisfactory or yearly Oil mist filter Dump oil Check monthly and dump when half full or Sooner Change cartridge When saturated with oil Foreline trap Check activated alumina Twice a year Change activated alumina When discolored and yellowish C 3 Pump Versions The PPMS is generally equipped with one of three pumps an Alcatel pump an Edwards pump or a Varian pump Since 1997 all systems have used CE compliant Edwards or Varian pumps Figure C 2 shows the three pumps and Table C 2 lists some basic characteristics of each For detailed information about your pump refer to the separate vacuum pump manual that was su
117. mmersed in liquid helium is resistive the resistance of the wire 1s directly proportional to the amount of liquid helium required to fill the tank The value that the PPMS reports is a percentage of full For example 100 indicates the dewar is full 75 indicates the dewar is three quarters full and so on The helium level meter does not extend all the way to the bottom of the dewar so 0 does not mean the dewar is dry only that the meter is completely exposed When the helium level meter is completely exposed the impedance tube intake of the probe is not immersed in liquid helium and temperature control will be lost or inhibited Heat is generated by the metering process so the helium level meter is usually not on continuously but the helium level is automatically checked on an hourly basis You should monitor the helium continuously only during helium transfers For more information about continuous monitoring refer to the Helium Level section in the Physical Property Measurement System Commands Manual Quantum Design PPMS Hardware Manual 1070 150 Rev B5 3 9 February 2008 Section 3 7 Chapter 3 Model 6000 Flexibility Theory of Operation 3 7 3 10 LIQUID HELIUM LEVEL 100 R Rc Figure 3 5 Schematic of helium level meter Model 6000 Flexibility The electrical inputs and outputs on the Model 6000 allow the PPMS to accommodate a wide range of experiments and to be configured to fit
118. n Figure 4 11 Checking for proper electrical connection of the sample You can use this technique to check for undesired shorts poor connections and so on or you can insert the puck into a P150 sample wiring test station and use the numbered banana jacks for the same purpose Notice that the puck plugs into a plastic ring in the test station so any shorts to ground can only be measured by directly contacting the puck itself However when the puck is plugged into the sample chamber it contacts metal and is truly grounded To ensure the validity of your data verify that there are no shorts to the surface of the puck 4 5 Sample Puck Installation and Removal 4 5 1 Installing a Sample Puck After you have mounted the sample on the puck and soldered the leads to the appropriate solder pads you can insert the puck into the sample chamber by using the instructions below 1 Disengage the puck insertion puck extraction tool by flipping up the black switch located on top of the tool or by fully depressing the switch as shown in Figure 4 12 Figure 4 12 Handle of puck insertion puck extraction tool disengaged and engaged 2 Insert the puck with the sample facing upward into the hollow cylinder at the bottom of the puck insertion tool The sample will be inside the cylinder and the connectors and solder pads will be outside the cylinder see Figure 4 13 Figure 4 13 Inserting the puck 3 Rotate the puck to v
119. n solid thermal contact with the 12 pin connector located at the bottom of the sample chamber The puck adjustment tool consists of two metal cylinders In Figure 2 13 Cylinder 1 is the finger spreader Cylinder 2 is the finger contractor and the test cutout The finger spreader and the finger contractor adjust the tension of the chuck fingers The test cutout which has the same dimensions as the cutout in the heater block tests how well the chuck fingers will contact the heater block The puck insertion tool is also called the puck extraction tool or sample insertion tool depending on context 2 12 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 2 Section 2 10 Hardware Sample Puck and Assorted Tools FINGER CONTRACTOR FINGER SPREADER CYLINDER 1 CYLINDER 2 Figure 2 13 Puck adjustment tool You will use the puck adjustment tool after you have inserted the sample puck into the sample chamber approximately 10 times or whenever the puck fits loosely into the bottom of the chamber Instructions for using the puck adjustment tool are given in Section 4 7 1 2 10 3 Puck Wiring Test Station The puck wiring test station Figure 2 14 is used to verify the contact between a sample and puck The test station contains three sets of contacts all wired in series a Lemo connector identical to the sample chamber connector on the probe head a puck connector and 12 banana jacks PPMS measurement o
120. n t rete e UD SINE M ate teu Nro cni ah ie Prin 1 4 1 4 2 Magnets ite eret ee decente e a a Ve ve NR Tree Np UPPER ge cv S 1 5 1 43 Electricity tiia nee e Ee EE dea EST EQUES EPOR SENE AERE OON eS ds 1 6 1 5 Environmental Considerations and PPMS Setup sssssssssssssseseeeeeenenenee 1 7 1 5 1 Magnetic Field Considerations sssssesesseeeeeeeeeeen eene 1 7 125 2 Physical Dimensionss eet ette E ee tee er Ha To ees Eee tid 1 8 1 5 3 Local Altitude and Humidity esses enne 1 8 1 6 Contacting Quantum Design tnr tee ee to e n ge Re a dn 1 9 CHAPTER 2 RAN WAL esr M 2 1 2 1 Introduction iren e ER ART e ERREUR ETEREH TA ce 2 1 PNE DTP 2 1 22 TA Standard De wat ves ere irit eter ier p aree e Aeg 2 2 2 2 1 2 Nitrogen Jacketed Dewat ccecccesscssssssseeescessecssecsseceseceseceseceseeseeeseneceaeesseeeseeeaeesaes 2 2 2 2 1 3 High Capacity Nitrogen Jacketed Dewar sse 2 3 2 3 SRT OWS ic eerte oret nta DER EE oo HERE ses teet v RE P ERR ER RR 2 4 2 31 Sample Chamber 5n eei tete sone eme meret e Led restera ea detis e ge ee ine e dine 2 5 2 3 2 Impedance Assembly ener teeth caus eek tee teer eerte debeas 2 5 2 3 3 Baftled Rods eret b teer em ERE ea dete en 2 5 2 3 4 Probe Head eta ie S gt traer cett pe te TET s Fede 2 5 2 35 Optional Magnet 5n se mr e eee o ot ere tret e ot tts 2 6 24 Top Plate Assembly tette tee UI QT IE e ELIO BE LI d ide 2 6 Quantum
121. n the picture reference to Model 6700 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 3 1 February 2008 Section 3 3 Chapter 3 Temperature Control Theory of Operation 3 3 Temperature Control Figure 3 2 shows cross sections of the PPMS probe including the components that control temperature The outer layer of the probe is an evacuated region filled with reflective superinsulation This layer is between the liquid helium bath and cooling annulus where it minimizes thermal exchange between the sample chamber and the 4 2 K liquid helium bath It contains an aluminum heat shield that directs heat to the neck of the probe rather than into the helium bath where it would increase the rate of helium consumption Without this evacuated region temperature control would be difficult or impossible and helium consumption would be significantly higher The cooling annulus is the active region of temperature control The continuously pumping vacuum pump draws helium from the dewar through the impedance tube and into the cooling annulus The helium vapor flows through the annulus at rates that are controlled by a flow control valve in the Model 6000 PPMS Controller The sample chamber is also usually kept at a pressure of a few torr with helium gas so that the walls of the sample space can maintain thermal contact with the sample The sample chamber has a top plate baffle assembly that helps isolate the sample space at the bottom of the chamber fr
122. n the rear of the Model 6000 The black Lemo connector contains connections to the three system thermometers and the two sample chamber heaters A 4 10 Blue Lemo Connector The blue ringed Lemo connector attaches to the P6 Dewar port on the rear of the Model 6000 The blue Lemo connector contains connections to the helium level meter impedance thermometer impedance heater and magnet persistence switch A 4 11 Gray Lemo Connector The gray ringed Lemo connector contains connections to the sample puck connectors on the bottom of the sample chamber The gray Lemo connector might connect to one of several ports It might connect to the P1 User Bridge port for four wire resistance measurements to the P3 Option port for use with PPMS options such as the ACMS option or to other PPMS controllers such as the Model 7100 AC Transport Controller or the Model 6500 PPMS Option Controller You can access pins on the P1 User Bridge port for connection to instruments other than the Model 6000 A list of pinouts is in Section A 5 A 5 Pinout Tables The following tables detail the pinouts for the electrical ports in the PPMS including ports on the Model 6000 probe head and sample puck None of these tables includes pinout information for the P3 Option port on the Model 6000 Refer to the appropriate option manual for the pinout information regarding this port Note The diagrams that accompany the tables illustrate hardware
123. n you design an experiment One of the first constraints to consider is the size of the sample The diameter of the sample puck is 2 3 cm with a set of notches around its perimeter in which the electrical leads seat The maximum sample height is 5 0 cm While the superconducting PPMS magnets have a high field homogeneity the uniformity of the field over the sample is greater for small samples Similarly although the PPMS provides very precise temperature control the effect of thermal gradients on the sample is less for small samples Recall that temperature control in the PPMS is usually based on the temperature of the sample puck Settling times before the sample is at the same temperature as the puck also could be longer for large samples The PPMS is ideally suited for measurements of bulk solid samples and thin film samples Powdered aqueous and liquid samples can be accommodated with a variety of techniques but you should use caution with such techniques because the PPMS is very difficult to clean in the event such a sample is lost within it The use of sealed sample holders requires additional caution because they tend to burst when the sample chamber is evacuated Before introducing a sealed sample holder into the PPMS you should verify that it will not break when it is subjected to an external pressure of only a few torr as it will be inside the PPMS sample chamber PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008
124. nce January 1998 PPMS systems have included the high temperature regime and both low temperature regimes with CLTC shipped as the default mode Before that time the PPMS included only the high temperature regime and pot fill mode but owners of such systems can add the CLTC option as a purchased upgrade 3 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 3 Theory of Operation FOOLING ANNI SAMPLE CHAMBE mr o m Section 3 3 Temperature Control Quantum Design CLT IMPEDANC MANIFOLD Figure 3 2 Cross sections of the PPMS probe and its temperature control components PPMS Hardware Manual 1070 150 Rev B5 February 2008 Section 3 3 Chapter 3 Temperature Control Theory of Operation 3 3 1 1 HIGH TEMPERATURE CONTROL At temperatures above about 4 2 K the system cools the sample space by drawing cold helium vapor at a variable rate through the impedance tube into the cooling annulus and across the outside of the sample chamber Even when the sample space is not being cooled the system maintains a helium flow of about 100 cc min through the cooling annulus A block heater is mounted at the base of the sample c
125. nce of large magnetic fields Important The automated control system can turn on the magnet while the system is unattended Furthermore the three dimensional magnetic field of the PPMS will penetrate nearby walls the ceiling and the floor Therefore your safety considerations should include such adjacent spaces Also note that transverse magnets produce substantially stronger fields around the dewar than longitudinal magnets do e The superconducting magnets supplied with PPMS units all produce strong fields that are not completely confined to the system unless it has some type of magnetic shielding For example PPMS superconducting magnets can disturb computer monitors affect electron microscopes erase credit cards attract ferromagnetic tools and so on Table 1 1 summarizes some of these effects Quantum Design recommends that you measure the magnetic field around the PPMS and draw a line showing where the measured field drops below 5 G It is your responsibility to determine the location of this line because it varies from system to system This line is typically about 3 10 ft 1 3 m from the edge of the dewar Do not bring heavy ferromagnetic objects such as gas cylinders and large tools within this region when the magnet is charged Gas cylinders in the laboratory should be secured to the walls and only informed personnel should be allowed to use large tools in the presence of the PPMS It is possible to cause injury to
126. nce the last change Check the oil mist cartridge at the same time as the pump oil levels and change it when it is full of oil Use the same oil type that was provided with the equipment see Table C 2 WARNING Put the system in Shutdown mode and disconnect the two metal pumping lines before you service the pump or related components If there are leaks into the sample chamber and cooling annulus ice can form and cause serious system malfunctions C 4 1 1 PREPARE PPMS FOR SERVICE 1 Place the PPMS in Shutdown mode in MultiVu select Instrument gt gt Shutdown When you place the system in Shutdown mode the software automatically seals the sample chamber turns off the heaters and restricts the flow control valve 2 Disconnect but leave seated the two metal pumping lines that come from the probe head When the pumping lines are disconnected the sample chamber and cooling annulus are sealed at the probe head 3 Leaving the rest of the system components turned on turn off the pump according to the instructions below If the pump has been in operation you might need to let it cool before you begin to work on it a b Quantum Design Early PPMS units without a toggle switch on the pump unplug the pump to turn it off Do not turn off the switch on the power strip this strip powers other system equipment in addition to the pump Recent PPMS units with a toggle switch on the back of the pump turn o
127. nd serious system malfunctions C 5 1 1 PREPARE PPMS FOR SERVICE l 2 Open the front panel of the electronics cabinet Figure C 1 Place the PPMS in shutdown mode in MultiVu select Instrument gt gt Shutdown When you place the system in shutdown mode the software automatically seals the sample chamber turns off the heaters and restricts the flow control valve Disconnect but leave seated the two metal pumping lines from the probe head This seals the sample chamber and cooling annulus at the probe head Leaving the rest of the system components turned on turn off the pump according to the instructions below If the pump has been in operation you might need to let it cool before you work on it a Early PPMS units without a toggle switch on the pump unplug the pump to turn it off Do not turn off the switch on the power strip this strip powers other system equipment in addition to the pump b Recent PPMS units with a toggle switch on the back of the pump turn off the toggle switch Open the console cabinet and hold your hand near the pump If the pump is uncomfortably warm let it cool before you proceed to the next section C 5 1 2 REMOVE ALUMINA CANISTER AND EXAMINE THE PELLETS 1 Quantum Design Carefully unscrew the cap on the front of the foreline trap see Figure C 2 Note that there is a spring located on the shaft inside the canister Remove the activated alumina canister Hold the ca
128. ner The power receptacle contains two fuses for the controller power supply Replace these fuses only with equivalent 2 A time delay fuses 120 VAC power environments or with equivalent A time delay fuses in 220 VAC power environments as noted on the back panel You can use a screwdriver or other flat instrument to pry open the door covering these fuses Verify that the power setting which is visible through a window in the door is correct for the power being used A 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Connections Ports and Pinouts A 4 Section A 4 Probe Head Ports Probe Head Ports The ports on the rear of the PPMS probe head connect the probe hardware to the Model 6000 and Model 6700 Bhan Sot HELIUM FILL PORTS WITH SAMPLE CHAMBER 1 PSI PRESSURE RELIEF VALVES 3 PRESSURE RELIEF VALVE SAMPLE CHAMBER SMALLER METAL HOSE ACCESS PORT SAMPLE SPACE LARGER METAL HOSE COOLING ANNULUS MAGNET CONNECTO LUE LEMO CONNECTOR DEWAI BLACK LEMO CONNECTOR P2 SYSTEM BRIDGE REY LEMO CONNECTOR SER BRIDGE P3 OPTION 4 HOSE NIPPLE WITH 4 ULTRA FITTING 5 PSI PRESSURE RELIEF VALVE EWAR GAS LINE A 4 1 A 4 2 A 4 3 Quantum Design Figure A 3 Ports on rear of PPMS probe head Helium Fill Ports You open the helium fill ports by pulling the relief valves straight up thus allowing access directly into the helium dewar for regular dewar fills Each of the two
129. nister by the bottom not the edges and remove the items listed below in order from the top of the canister The bottom will fall out and spill the activated alumina if you hold the canister by the edges long spring wing nut washer lid washer short spring mmo ao FB grille PPMS Hardware Manuall 1070 150 Rev B5 C 5 February 2008 Section C 5 Appendix C Servicing the Foreline Trap Vacuum Pump Assembly Maintenance 4 Examine the activated alumina pellets If they are discolored and yellowish replace them with fresh pellets If you need replacement material contact Quantum Design C 5 1 5 REASSEMBLE THE CANISTER TRAP AND PUMP 1 To reassemble the activated alumina canister install the items in the order listed below a reversal of the removal procedures a grille b short spring c washer d lid e washer f wingnut long spring 2 Insert the activated alumina canister into the foreline trap with the spring facing the opened end of the trap 3 Screw the cap back onto the front of the foreline trap 4 Turnon the pump and wait one minute so that the metal pumping lines can be evacuated 5 Reconnect the two metal pumping lines to the probe head 6 Purge and seal the sample chamber 7 Close the front door of the electronics cabinet C 6 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix C Section C 6 Vacuum Pump Assembly Maintenance PPMS Vacuum Pump Assembly Service Record
130. ns ccccesccessceseceeseeseeeeeeeeseeeseeeseeeeeeaeees A 15 Dewar connections a Blue Lemo connector b P6 Dewar port ss A 16 Magnet connections a M1 b P7 Magnet port sse A 17 Magnet connections a 1 TCM connector or a 2 Red Lemo connector and b Magnet controller A 18 Auxiliary expansion connections eesseseseeeeee eene A 19 Pressure gauge expansion connections ccececeesseesceeseesecsseceseceseceeeeeeeeeeeeeneenaes A 20 Motor expansion connections 00 ccccccccsseesseceseceecesseceseceseceseceeeseeceeeeeeseeeseeeaeesaes A 21 External expansion CONNECTIONS cccccsceesseesecseeeeseceseceseceseceeeseeeeeaeeeseeeseeeaeeaaes A 22 Helium transfer line arrangement eene B 2 Arrangement for the simultaneous transfer of nitrogen and helium into a warm nitrogen jacketed dewar sse B 4 Temperature dialog and settings for helium transfer sess B 4 Preparing for a liquid nitrogen transfer essen B 5 Arrangement for sequential transfer of nitrogen and helium into warm nitrogen jacketed dewar ccccesccesseeesceesceeseeeeeeeeeseecssecneeneeeseenes B 8 Inserting a helium backfill adapter B 8 Preparing for a liquid nitrogen transfer sse B 8 Liquid helium transfer arrangement for transferring helium into a warm non jacketed dewar sess B 12 PPMS electronics cabinet with front panel op
131. ns such as spreadsheets or professional graphing programs If you are using the PPMS as a temperature and field control platform you can measure sample resistance as a function of temperature and magnetic field Entire resistance curves can be plotted and the critical temperature can be determined for superconducting samples For the example given above you could set the PPMS to measure the sample resistance at 20 different temperatures and then increase the applied magnetic field by 0 25 T and repeat the resistance measurements at all 20 temperatures This type of measurement can be facilitated by using sequences When you use a sequence file the PPMS becomes fully automated It can automatically perform temperature changes field changes applied current changes and resistance measurements It can automatically control all PPMS hardware and thus place the system in Shutdown mode when the experiment is complete The Model 6000 can control numerous other operations Refer to the Physical Property Measurement System Commands Manual and the Physical Property Measurement System PPMS MultiVu Application User s Manual for further information regarding sequence commands The main point of illustration here is that the above resistance experiment can be performed entirely automatically You can automate other experiments in a similar manner Experimental Considerations Although the PPMS is extremely flexible you must consider certain limitations whe
132. ns the PPMS For detailed information about PPMS MultiVu refer to the Physical Property Measurement System PPMS MultiVu Application User s Manual The PPMS has a variety of measurement options as well as alternate set ups so some of the manual materials might not be relevant to your equipment For example this manual explains how to use nitrogen jacketed PPMS dewars If your PPMS uses a standard dewar 1 e one without a nitrogen jacket you can ignore instructions that concern only liquid nitrogen Also this manual includes material about systems that have a magnet If your system does not include a magnet you can ignore those sections All other PPMS functions are identical for systems with or without magnets Contents of the Manual o Chapter 1 introduces the PPMS including safety considerations and system setup and explains how to contact Quantum Design o Chapter 2 describes and illustrates the main PPMS hardware components o Chapter 3 describes how the PPMS operates and gives an example of a measurement Quantum Design PPMS Hardware Manual 1070 150 Rev B5 xiii February 2008 Section P 4 Conventions in the Manual P 4 xiv Preface Contents and Conventions o Chapter 4 explains how to use and customize the PPMS and describes routine maintenance procedures such as refilling a cold dewar with helium o X Appendix A describes and illustrates the PPMS electrical ports o A Appendix B explains how to transfer heli
133. o reete eee ret Pear i TER eg 4 12 4 5 2 Removing a Sample Puck sees enne eene entren enne 4 14 4 5 3 Closing an Empty Sample Chamber sse enne 4 15 4 6 System Customization s ni eene enne enr ern en nee nnne nes 4 16 4 6 1 Making Alternate Connections to the Sample Leads esses 4 16 4 6 2 Using Other Electronic Devices eeeseseeeeeeeeeene ener erret 4 17 4 6 3 Modifying the Gas and Vacuum System sess 4 17 4 7 Routine Maintenance Procedures sse eene ener enne nns 4 18 4 7 Ll Puck Adjustment 55 ra e n nte EVE PORE NN dS IESUS 4 18 4 7 2 Refilling a Cold Dewar 5 e orate ette edt ee da ertet tt ee IRR te 4 19 4 7 2 1 Transferring Liquid Nitrogen nnne 4 19 4 7 2 2 Transferring Liquid Helium seesesssseeeeeneeer enne enne 4 21 4 7 3 Servicing the Vacuum Pump Assembly sese 4 23 4 7 3 1 Checking the Oil in the Pump eene 4 25 4 7 3 2 Adding Oil and Draining the Oil Mist Container esssssseeeee 4 26 4 7 4 Using the Probe Lifting Assembly ssssssesseseeeeeeeeeneenneen nennen 4 27 4 7 5 Anspecting O RIDg3 a eed er e ee er det y e eere dct Te re fee 4 28 APPENDIX A Connections Ports and PinoUts ecce ecce esee ee esee eene eene esee ness senses sese sese sese eese e eese e A 1 AJ Introduction ue eret ten tee er t RE ti e lr ie etie aee eee pe Net A 1 A 2 Syste
134. odel 6000 records the two analog inputs at a rate of approximately 2 Hz To measure the signal from each of these inputs use the CTRL gt gt 3 Immediate Operations gt gt 11 Measure gt gt Sig1 or Sig2 The signal can be manipulated like any other data signal that is placed into data files graphed with PPMS software linked to the analog outputs and so on The status of these signal inputs can be observed in the Status System Cont screen when it has been enabled with the CONFIG gt gt 5 Software gt gt 1 User Preferences menu A 3 9 P9 Pressure Port The P9 Pressure port provides power to and a signal from an external pressure gauge such as a Pirani or Baratron gauge The pinouts can be configured to match specific models of gauges For more information refer to Table A 9 and the manual for the gauge of interest or contact a Quantum Design representative for more information about how to configure the pinouts for a gauge To see the port configuration use the CONFIG gt gt 6 Hardware gt gt 4 Pressure Sensor menu When this menu displays a selection other than internal all system pressure information is rerouted to obtain information from the indicated gauge or none at all rather than from the internal solid state silicon pressure sensor of the Model 6000 The pressure shown in the Status System screen reflects this pressure information To record the pressure reading use the CTRL gt gt 3 Immediate Ope
135. oes not need to connect to anything The hose nipple can let you access the helium in the dewar so that you can observe the helium boil off rate This gas line however passes through a 1 3 psi pressure relief valve first so the dewar should not be pressurized with this port You can attach a helium recovery unit to this port A 4 7 X Ultra Fitting The 1 4 inch Ultra fitting should be connected to the Dewar port on the rear of the Model 6000 with a 1 4 inch white polypropylene hose This line allows the Model 6000 to monitor the pressure differential between the dewar and the annulus during low temperature operations Additionally this line provides helium from the dewar boil off for venting the sample space A 4 8 Magnet Connector TCM or Red Lemo Connector The TCM connector earlier model systems have a red ringed Lemo connector attaches to the two large color coded terminals on the rear of the Model 6700 The red or blue banded cable connects to the blue terminal on the Model 6700 and the black unbanded cable connects to the black terminal These connectors are illustrated in Section A 5 7 Important Verify that the magnet polarity 1s correct by using Table A 7 A 10 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Section A 5 Connections Ports and Pinouts Pinout Tables A 4 9 Black Lemo Connector The black ringed Lemo connector attaches to the P2 System Bridge port o
136. of the sample chamber access port 3 Latch the clamp 4 Purge and seal the sample chamber by using the Model 6000 menu CTRL gt gt 1 Interactive Control gt gt 2 Purge and Seal or MultiVu Instrument gt gt Chamber gt gt Purge Seal See Footnote 1 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 15 February 2008 Section 4 6 Chapter 4 System Customization System Operation 4 6 System Customization The PPMS is designed to be flexible and meet a variety of needs so it accommodates customization Before you begin any modifications please read all applicable portions of the manual so that you understand how the components function and how your alterations could affect the system Contact Quantum Design if you have questions about altering the system Some common issues are addressed below 4 6 1 Making Alternate Connections to the Sample Leads If the Model 6000 does not provide the function you need you can make electrical contact to the sample from other instruments by connecting an adapter to the gray Lemo connector cable The pinouts are mapped for this purpose in Appendix A CAUTION Always use an adapter to access the leads in the gray Lemo connector cable the cable that connects the probe head to the Model 6000 Use of an adapter ensures that you will be able to use the cable with other applications Figure 4 14 illustrates how to use an adapter to make connections at the D connector end
137. om the heat radiated by room temperature components at the top This baffle assembly is required for the sample space to reach the lowest attainable temperatures Sample temperature 1s monitored by a platinum resistance thermometer and a negative temperature coefficient NTC thermometer that are mounted directly beneath the electrical connectors for the sample puck The platinum thermometer reads temperatures ranging between approximately 80 K and 400 K the NTC thermometer reads temperatures ranging between approximately 1 9 and 100 K A weighted average of the two thermometer readings is used in the crossover region between 80 K and 100 K Another NTC thermometer which 1s not shown in Figure 3 2 is mounted just above the sample space to monitor the temperature gradients in the chamber 3 3 1 Temperature Control Modes The PPMS offers three unique operational regimes for controlling temperature in the sample space one for high temperatures and two for low temperatures The high temperature regime is used for temperatures above the liquid helium boiling point 4 2 K at 1 atm which is the so called crossover temperature The low temperature regimes Continuous Low Temperature Control CLTC and pot fill mode are used to regulate temperatures below the crossover temperature Each low temperature regime can be used to lower the sample space temperature to about 1 9 K but their characteristics and advantages differ as shown in Table 3 1 Si
138. omponents is turned off the system cannot effectively monitor its own status For example the Model 6000 assumes that all other components are present and functioning even if a component has been powered off If you turn off the power to the Model 6000 for several hours while the flow control valve is open the pump will stay on filling the cooling annulus with liquid helium As a result the system will require an unusually long time to warm to above 4 2 K when you turn on the Model 6000 We recommend that you use the sequence below to turn off the PPMS and that you always place the PPMS in Shutdown mode before you turn it off these procedures will help bring the system to a stable helium conserving state x 4 2 2 2 POWER OFF SEQUENCE Status 1 Ifthe magnetic field is not in Persistent mode and at Field 1327460 Qe zero 0 Oe reset it according to the sequence below State Persistent Select Instrument gt gt Field Figure 4 1 ENT M Control In the Field dialog box set the Mode to do Set Point De Persistent and the Set Point to zero 0 Oe Rate 100 0 De sec c Click on the Set button Approach unes d Leave the dialog box open so that you can Mode Persistent v monitor the field until it is within 1000 Oe of zero do not continue until the field is within 1000 Oe Close of zero e Inthe Field dialog box click on the Close button Figure 4 1 PPMS Field dialog 2 Bringthe system
139. one C CRAF CLF f Custom shutdown 2 Terminator Response just as is shown in Figure 4 5 2 Click on the Send and Result Bytes Im Read button Sand Send and Read Close Figure 4 5 Switching from pot fill mode to CLTC 3 To verify which temperature mode the system has activated type clt and click on the Send and Read button again Figure 4 6 4 If the system has switched to CLTC the Response area should now display 1 1 Figure 4 6 Send GPIB Commands x Send fot Device jis Command None Co CRVLF Cuir C Custom f Terminator Response Result No error Bytes 4 Send f Close Figure 4 6 Verifying that CLTC is the low temperature control mode 4 8 PPMS Hardware Manual 1070 150 Rev B5 February 2008 Quantum Design Chapter 4 Section 4 3 System Operation Setting the Low Temperature Control Mode Table 4 2 Commands to shut down the PPMS and set the temperature control modes COMMAND ACTION shutdown 0 Shut down the PPMS but do not change the temperature control mode shutdown 1 Shut down the PPMS and set the temperature control mode to pot fill shutdown 2 Shut down the PPMS and set the temperature control mode to CLTC 4 3 2 Mon6000 The Mon6000 dialog is set up somewhat differently than the Send GPIB Commands dialog in MultiVu but you will use the same commands that you use with MultiVu Table 4 1 to verify or change th
140. onnector TCM or Red Lemo Connector sse A 10 4 9 Black Lemo Connector ci creta e e eed decades etes A 11 A4 T0 Blue Eemo Gonnector erint er e rie e rte Deere ue etie EEr A 11 AAMT Gray Eemo Connector tet eet eee cts Fa tee tee tv bee eee ae LEE ERE RES A 11 A S Pinout Tables anie re titt aer etti te rer Te eo c epe eap Ene dee Teen t deeds A 11 A 5 1l Sample Connections tania e gehe viet dU d A RRO A 12 A 5 2 System Bridge Connections ccccesccescesscsesceeseeeseeeseeeseeeseecsaecsaecesecesecnseeeeeeseeeeeneeeaes A 13 A 5 3 Communication Port Connections GPIB sseesseeeeeeeeeenne A 14 A 5 4 Communication Port Connections RS 232 sse A 15 ASS Dewar Connections dedos iste et e Leas Ba eoe ee ev pede toos Pee been RENE da A 16 A 5 6 Magnet Connections Model 6700 to Model 6000 sse A 17 A 5 7 Magnet Connections Probe to Controller sse A 18 A 5 8 Expansion Connections Auxiliary sess A 19 A 5 9 Expansion Connections Pressure Gauge ccssccesscesscessceseceeeceeeeeeseeeeeeeseeeseeeeeesaes A 20 A 5 10 Expansion Connections Motor c cccccesssesseesseessecssecssecnseceseceseeseeseeeseeeseneeeseeeaeenaes A 21 A 5 11 Expansion Connections External esses A 22 A 6 Replacement Fuse Values eene nennen a AI A 23 APPENDIX B Bing Warm DO Wars eer DR B 1 Bel IntroductiQny 5o ttti ERN ot ea van NUTS IRR
141. onsole cabinet and hold your hand near the pump If the pump is uncomfortably warm let it sit until it has cooled before proceeding to the next section Fill the Pump 1 3 4 5 6 If the pump parts are difficult to access slide the pump forward out of the electronics cabinet If the system has an Alcatel pump Figure 4 21 remove the black faceplate that frames the oil level window Remove the oil fill cap on the top of the pump see Table 4 4 Save the O ring Fill the pump with oil to the top mark of the oil level window do not overfill Reinsert the O ring and oil fill cap If the system has an Alcatel pump replace the faceplate that frames the oil level window Drain the Oil Mist Filter l 2 3 4 26 Hold a container under the bottom of the bell jar and unscrew the plug When the oil has drained pour the oil into a used oil container Screw the plug back into the bell jar PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 7 System Operation Routine Maintenance Procedures CAUTION Check the level of oil in the oil mist filter at least once a week If the filter becomes too full oil can back up into the gas lines and plug the system Prepare the PPMS for Use 1 Slide the pump back into the electronics cabinet 2 Turn the pump on and wait one minute so that the metal pumping lines can be evacuated Verify that the pumping lines are seated in their connecto
142. orts by turning the large fitting counter clockwise until it comes off the dewar see Figure B 7 This will prevent the O ring from freezing b Open the other nitrogen fill port by turning the large brass fitting counter clockwise to loosen it and then removing the small insert plug when it is loose B 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix B Section B 3 Filling Warm Dewars Warm Fill Nitrogen Jacketed Dewars 10 11 Screw the liquid nitrogen transfer adapter onto the end of the nitrogen supply line At the PPMS dewar insert the small end of the liquid nitrogen transfer adapter into the open liquid nitrogen fill port and turn the brass fitting clockwise to secure the adapter in place Using the Model 6000 or the MultiVu Temperature dialog shown in Figure B 3 Instrument gt gt Temperature set the temperature to 5 K the rate to 10 K min and the approach mode to fast settle By setting the temperature to 5 K you open the flow control valve to ensure the maximum flow through the impedance tube Maximum flow is necessary to flush out the impedance and keep contaminants from freezing inside it while it cools to cryogenic temperatures The temperature will not actually drop to 5 K because there is no liquid helium in the dewar At the helium gas cylinder prepare it to act as a backfill a Open the regulator to allow helium gas into the dewar and through the impedance tube b Adj
143. ovides access to two current drivers and the P8 Auxiliary port contains 15 V and 15 V low power current sources Several digital inputs and outputs are in various locations on the Model 6000 See Appendix A for detailed information about these capabilities You also can use the Model 6000 front panel to monitor additional equipment that uses the Model 6000 digital input and output lines The state of each digital input and output 1s displayed in the Digital status line at the bottom of the Status System Cont screen The status codes are summarized in Table 4 3 Table 4 3 Status codes for the Model 6000 digital inputs and outputs STATUS LINE AND STATE TYPE OF LINE LOCATION CODE HL Hold Line Active Low Busy Input P 11 External UR User Line Active Low Busy Input P 11 External A1 Auxiliary Drive 1 Active 24 V Auxiliary Output P 8 Auxiliary A2 Auxiliary Drive 2 Active 24 V Auxiliary Output P 8 Auxiliary LM Limit Switch Active 5 V Motor Input P 10 Motor NX Index Switch Active 5 V Motor Input P 10 Motor S1 Select Line 1 Active Select Output P 11 External 2 Select Line 2 Active Select Output P 11 External 3 Select Line 3 Active Select Output P 11 External AC Actuator Activated 24 V Actuator P 10 Motor Appendix A contains the information that is necessary for correctly interfacing other electronic devices with the PPMS For example som
144. pan tkb att ne jp Web _ http www qd japan com Service for Japan Korea Quantum Design Korea Kyungbin Building Fourth Floor 517 18 Dogok dong Kangnam gu Seoul 135 270 Korea Tel 82 2 2057 2710 Fax 82 2 2057 2712 Web http www qdkorea com Service for Korea People s Republic of China Oxford Instruments Beijing Office Room 714 Office Tower 3 Henderson Center No 18 Jianguomennei Ave Dongcheng District Beijing 100005 P R China Tel 8610 6518 8160 8161 8162 Fax 8610 6518 8155 Email lambert oxford instruments com cn Web _ http www oxford instruments com cn Service for People s Republic of China Taiwan Omega Scientific Taiwan Ltd 5F 1 No 415 Sec 4 Hsin Yi Road Taipei Taiwan R O C Tel 886 2 8780 5228 Fax 886 2 8780 5225 Email lonson lin omega cana com tw Service for Taiwan Hong Kong Singapore PPMS Hardware Manual 1070 150 Rev B5 February 2008 Chapter 1 Introduction and System Setup Quantum Design C H APT ER 2 Hardware 2 1 2 2 Introduction This chapter contains the following information o Section 2 2 describes the dewar including o Section 2 7 describes the optional Model its functions and the three main types 6700 Magnet Controller o Section 2 3 describes the probe and its main Section 2 8 describes the electronics components cabinet o Section 2 4 describes the top plate o Section 2 9 describes the vacuum pump assemb
145. personnel and damage to PPMS equipment by allowing heavy objects to be attracted to the PPMS Keep the helium level above the superconducting magnet There is high potential for damage such as an uncontrolled magnet quench when the superconducting magnet is not completely covered by helium See Sections 3 5 and 4 2 4 for more information Electricity WARNING The PPMS console personal computer and vacuum pump are all powered by standard 120 VAC or 240 VAC power lines These voltages are potentially lethal so you should exercise appropriate care before opening any of the electronics units including turning off the equipment and disconnecting it from its power source Turn off and unplug all electronic equipment before removing any of its covers Keep electrical cords in good working condition and replace frayed and damaged cords Keep liquids away from the workstations Safe operation of the PPMS requires the appropriate electrical power input The input power requirements for the PPMS are the following o 50 60 Hz 100 120 VAC at 15 A o 50 60 Hz 200 240 VAC at 10 A PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 1 Section 1 5 Introduction and System Setup Environmental Considerations and PPMS Setup 1 5 1 5 1 Environmental Considerations and PPMS Setup You must consider a number of environmental constraints when you install the PPMS in a laboratory incl
146. ports not connectors at the end of the cables Quantum Design PPMS Hardware Manual 1070 150 Rev B5 A 11 February 2008 Section A 5 Appendix A Pinout Tables Connections Ports and Pinouts A 5 1 Sample Connections The sample connector is at the bottom of the sample chamber The gray Lemo connector is on the probe head Pins 1 and 2 on the gray Lemo connector are connected to wires that extend into the annulus These wires are not used for any function but they provide a site for system expansion The P1 User Bridge D connector is on the Model 6000 a Sample puck b Gray Lemo c P1 User bridge port connector BOTTOM VIEW Figure A 4 Sample connections a Sample puck b Gray Lemo connector c P1 User bridge port Table A 1 Sample connections SAMPLE GRAY LEMO P1 USER USER BRIDGE BOARD CONNECTO CONNECTO BRIDGE D FUNCTION CONNECTOR A 12 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Connections Ports and Pinouts Section A 5 Pinout Tables A 5 2 System Bridge Connections The black Lemo connector is on the probe head The P2 System Bridge D connector is on the Model 6000 a Black Lemo connector b P2 System bridge port jl a 44 2 K 9 o o ZO ON OOOOO0O0O0O0O0O00C 1D Ois 252423222120191817161514 AO Figure A 5 System bridge connections a Black Lemo connector b P2 System bridge port Tabl
147. pplied with the system Forline Oil 1 i Trap Forline T Len Trap Forline Trap Oil Level Window Oil Level Window L Alcatel rotary vane pump Edwards rotary vane pump Varian rotary vane pump Leybold rotary vane pump Figure C 2 Versions of the PPMS vacuum pump C 2 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix C Section C 4 Vacuum Pump Assembly Maintenance Changing the Pump Oil and Oil Mist Cartridge Table C 2 Characteristics of vacuum pumps used on the PPMS MANUFACTURER COMPONENT Alcatel Edwards Varian Leybold Color Orange and black Gray Ivory and gray Gray with Side car Alcatel 100 Direct Edwards Supergrade Varian General Purpose Leybold HE 200 Oil Type Drive Mechanical A oil Mechanical Pump Fluid Vacuum Pump Fluid Between upper and Between max and Between arrows best at Between upper and Cil Level lower markings best min 1 2 or more lower markings best at 1 2 or more at 1 2 or more Oil fill cap Top foremost cap Top front right Top front left Top Center Drain plug Lower plug Bottom right Bottom front center Bottom right C 4 Changing the Pump Oil and Oil Mist Cartridge The pump oil must be changed once a year unless it 1s dirty compare it to clean oil or the pump is not producing a satisfactory vacuum In the latter cases you should immediately change the oil even if it has been less than a year si
148. proximately 1 hour to fill the dewar 2 Atthe liquid helium supply dewar reset the valves a Close the gas phase valve b Open the primary relief valve 3 Remove the transfer line and adapters from the PPMS dewar and the liquid helium supply dewar 4 Atthe PPMS dewar close the helium fill port on the probe head by reinserting the relief valve 5 Atthe liquid helium supply dewar close the liquid access port The liquid helium transfer is now complete The helium level meter will turn itself off when you exit the Fill Dewar screen or if the fill time exceeds 30 minutes B 14 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 A PP E NDIX C Vacuum Pump Assembly Maintenance C 1 Introduction This appendix contains the following information o Section C 2 provides an overview of the o Section C 5 has instructions for changing vacuum pump assembly and its maintenance the activated alumina in the foreline trap requirements o Section C 3 describes the three types of o Section C 6 is a maintenance record vacuum pumps provided with the PPMS o Section C 4 has instructions for changing the oil and the oil mist filter cartridge in the rotary vane pump C 2 Vacuum Pump Assembly The vacuum pump assembly is located inside the electronics cabinet see Figure C 1 It includes a rotary vane pump that uses oil to help pull the vacuum a foreline trap with activated alumina to filter the intake air and an oil
149. ptions e g Heat Capacity come with templates that allow you to label the banana plug functions when the standard cabling is being used for an option PUCK CONNECTOR BANANA JACK LEMO CONNECTOR TOP VIEW Figure 2 14 Puck wiring test station The puck wiring test station is also referred to as the P150 sample wiring test station Quantum Design PPMS Hardware Manual 1070 150 Rev B5 2 13 February 2008 C H APTER 3 Theory of Operation 3 1 Introduction This chapter contains the following information o Section 3 2 illustrates the main PPMS o Section 3 6 describes the helium level subsystems and their interactions meter and monitoring helium levels O Section 3 3 describes temperature control o Section 3 7 describes features of the and operational regimes Model 6000 that can be customized o Section 3 4 describes atmospheric control o Section 3 8 presents an example of a and gas line configuration measurement o Section 3 5 describes magnetic field o Section 3 9 describes variables to control consider during a measurement 3 2 PPMS System Block Diagram Figure 3 1 illustrates how the temperature control gas flow control magnetic field control and helium level metering subsystems are incorporated in the PPMS REAR PANEL PROBE HEAD EU d Pd Seton CONTROLLER WAK RUB __ HEATERS es E fag eee i MOI 700 ra 670 ET CONTROLLER RS232 IEEE 488 Figure 3 1 PPMS block diagram eliminate i
150. pump Edwards rotary vane pump Varian rotary vane pump Leybold rotary vane pump Figure 4 21 Vacuum rotary vane pumps used with the PPMS Table 4 4 lists the characteristics of each pump and Sections 4 7 3 1 4 7 3 2 explain how to check the oil level in the pump and oil mist containers Appendix C contains the instructions for changing the oil and oil mist filter cartridge and for servicing the foreline trap For detailed information about your pump refer to the separate vacuum pump manual that comes with the system 4 24 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 System Operation Section 4 7 Routine Maintenance Procedures Table 4 4 Types of vacuum pumps used on the PPMS and their characteristics Pump MANUFACTURER CHARACTERISTIC Alcatel Edwards Varian Leybold Color Orange and black Gray Ivory and gray Gray with Side car Alcatel 100 Direct Edwards Varian General Leybold HE 200 Oil Type Drive Mechanical Supergrade A oil Purpose Mechanical Vacuum Pump Fluid Pump Fluid Between upper and Between max Between arrows best Between upper Oil L l lower markings best and min at 1 2 or more and lower i Eeve at 1 2 or more markings best at 1 2 or more Oil fill cap Top foremost cap Top front right Top front left Top Center Drain plug Lower plug Bottom right Bottom front center Bottom right 4 7 3 1 CHECKING THE OIL IN THE PUMP
151. puter to the system which is through the PA IEEEA88 GPIB port on the rear of the Model 6000 see Section A 3 4 A 3 Model 6000 Rear Panel Ports Figure A 2 illustrates the rear panel of the Model 6000 The upper half contains electrical connections The lower half houses the system fuses and connections to the gas lines for temperature and pressure control Some ports provide access to standard PPMS hardware and others allow custom configuration P3 OPTION P4 IEEE488 P1 USER BRIDGE P2 SYSTEM BRIDGE Oo ucc ae nea 5 P6 DEWAR P7 MAGNET P8 AUXILIARY P9 PRESSURE P10 MOTOR P11 EXTERNAL qa uan OX doro um ANALOG OUTPUTS OO sys SAMPLE HEATER ANNULUS PUMP ACUU M T VENT UP SYST SA AUX 2A O O SAMPLE SPACE SOURC DEWAR Og o O o 2A 120 VAC 1A 220 VAC Figure A 2 Ports on rear panel of Model 6000 A 3 1 P1 User Bridge Port If the system includes the Resistivity option the P1 User Bridge port accesses the additional bridge board that 1s in the Model 6000 The P1 User Bridge port usually connects to the gray ringed Lemo connector on the probe head and thus connects the user bridge board to the installed sample The optional resistance bridge board provides channels for four separate four wire resistance measurements In some models the small round port next to the P1 User Bridge port provides parallel access to the fourth of these channels The Model 6000 Status Bridge
152. quid nitrogen transfer adapter is included with all nitrogen jacketed dewars The probe is the component that is inserted into the dewar If the system has a longitudinal magnet the magnet is attached to the probe as illustrated in Figure 2 4 Any system with a magnet also includes the Model 6700 Magnet Controller or the Model 3120 Magnet Power Supply Please save the original packing crates for your system so that you can ship components back to Quantum Design for installation of an option upgrading or repair 1 4 Safety Precautions WARNING The PPMS superconducting magnets produce extremely strong three dimensional magnetic fields that can be dangerous and the PPMS uses cryogenic liquids for temperature control Critical PPMS related safety precautions include those for using superconducting magnets for using cryogenic materials liquids and gases and for using electrical equipment as is reviewed below Above all Quantum Design and its staff ask that you use standard safe laboratory procedures Use common sense Pay attention to the system s state and your surroundings Ifthe behavior of the system appears unusual something might be wrong with it If so take appropriate action Supervise inexperienced users and train them in general electrical safety procedures The PPMS has safety features to prevent accidents from causing injury or serious equipment damage f you use the equipment in a
153. quid indicating that the jacket 1s full The fill time will depend on the amount that was in the jacket when you started and how fast you perform the transfer For example jackets that are refilled twice a week take about 15 minutes to refill 7 At the PPMS dewar perform in sequence the steps below a Remove the liquid nitrogen transfer adapter turn the brass fitting counter clockwise and lift the transfer adapter out of the dewar In the event that the fitting and adapter are frozen together you can use a warm air blower to accelerate the thawing process Otherwise you must wait until the parts thaw enough to be separated b Close both nitrogen fill ports re install the brass fittings and turn the large brass fittings clockwise CAUTION Always re install the fill port fittings and or O rings onto the nitrogen fill ports after you have transferred liquid nitrogen into the dewar These fittings prevent dangerous ice blockages in the fill ports 4 20 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 7 System Operation Routine Maintenance Procedures 4 7 2 2 TRANSFERRING LIQUID HELIUM WARNING o Always wear protective clothing including thermal gloves eye protection and covered shoes when you work with liquid helium or any other cryogen Review Section 1 4 1 Cryogens before you transfer liquid helium o Always use a well ventilated room to perform this procedure
154. r with the Liquid Helium Fill Status dialog in MultiVu select Utilities gt gt Helium Fill or the Model 6000 select CTRL gt gt 1 Interactive Control gt gt 0 Fill Dewar When the helium level reads 85 100 close the regulator at the helium gas cylinder At the liquid helium supply dewar reset the valves a Close the gas phase valve b Open the primary relief valve Remove the transfer line and adapters from the liquid helium supply dewar and the PPMS dewar At the PPMS dewar close the helium fill port on the probe head by reinserting the relief valve At the liquid helium supply dewar close the liquid access port see Figure 4 18 The liquid helium transfer is now complete The helium level meter will turn itself off when you exit the Fill Dewar screen or if the fill time exceeds 30 minutes 4 7 3 Servicing the Vacuum Pump Assembly To help ensure that your equipment is in working condition when you want to perform measurements it is essential that you regularly maintain the PPMS vacuum pump assembly A rota pull ry vane pump which is located inside the electronics cabinet Figure 4 20 uses oil to help the vacuum Oil mist 1s naturally expelled from the pump exhaust and collected by an oil mist filter installed on the inside wall of the electronics cabinet Air to the pump is filtered through the foreline trap Maintenance Schedule The require regular maintenance using the procedures in Sec
155. rations gt gt 11 Measure gt gt More command Up to 200 mA of total current is available from the 15 V and 15 V lines when the ACMS and AC Transport options are not installed or active However this current is shared with the AC board When the AC board is driving relatively large alternating currents for the ACMS or AC Transport options the current that 1s available at these outputs drops to 10 mA A 3 10 Al A2 A3 and A4 Ports The Al A2 A3 and A4 ports are the analog outputs These four BNC connectors can be linked to any of about 30 different PPMS parameters such as temperature magnetic field user bridge board resistance or motor position This allows 10 V to 10 V feedback to other instruments or connection to chart recorders oscilloscopes and so on The A1 output is also connected in parallel to the signal channel 1 connector on the front panel of the Model 6000 When you link parameters to the analog outputs you must specify a value for both 0 V and 10 V so that the appropriate gain and offset are used Each channel has an output impedance of 100 Q You can use the CTRL gt gt 3 Immediate Operations gt gt 12 Link menu to link the channels to measurable parameters You can also use the CTRL gt gt 3 Immediate Operations gt gt 10 SigOut menu to configure the analog outputs to supply constant voltages The Status System Cont screen displays the status of each analog output Quantu
156. rdware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 2 System Operation General Guidelines 4 2 4 Monitoring the Helium Level Er The helium level in the dewar must be regularly PR O 3E monitored especially if you are using magnets the helium level must be above about 60 to charge magnets to high fields If you do not have or are not using a magnet you can let the helium level drop to approximately 30 before refilling the dewar as explained below Section 4 7 2 2 has instructions for refilling a cold PPMS dewar with liquid helium In many cases you can safely transfer helium into the PPMS dewar while a sequence is running Do a T not add helium to the dewar if you are ramping the NET magnet or if the temperature is below 5 K H 4 2 4 1 HELIUM LEVELS USING A MAGNET Figure 4 2 Helium levels relative to probe and 9 T magnet The PPMS is not like a car although you can drive a car until the fuel gauge reads nearly empty the PPMS could be seriously damaged if you operate the magnet when it is not immersed in liquid helium When a charged superconducting magnet is not completely immersed in liquid helium there could be an uncontrolled magnet quench warming the magnet so that it loses its superconducting properties and gives off large amounts of energy in the form of resistive heat Figure 4 2 shows approximate helium levels
157. re A 10 Figure A 11 Figure A 12 Figure A 13 Figure A 14 Figure B 1 Figure B 2 Figure B 3 Figure B 4 Figure B 5 Figure B 6 Figure B 7 Figure B 8 Figure C 1 Figure C 2 Quantum Design Contents Table of Figures Preparing for a liquid nitrogen transfer seen 4 19 Helium transfer line arrangement with the short output extension used for helium transfers into a cold dewar sss 4 2 Arrangement for refilling a cold nitrogen jacketed dewar with liquid helium ete donde an I ro e Eee 4 22 Opening a helium fill port on the head of a PPMS probe standard dewar shown esssssseeeeeeeene 4 22 Electronics cabinet with front panel open 4 23 Vacuum rotary vane pumps used with the PPMS sssssssssseeeeeee 4 24 Probe hf ng assembly 5 in eren rr tereti np ei poe retra 4 27 Connections for PPMS hardware sss ener A 1 Ports on rear panel of Model 6000 sss ene A 2 Ports on rear of PPMS probe head 0 cccccccsccessceseceeeeeeeeeeneesseeeseeeseecnsecnaeenseenseenes A 9 Sample connections a Sample puck b Gray Lemo connector Pl User bridge port 3 ae nta Ee RE DE EAR Ee Ie dod A 12 System bridge connections a Black Lemo connector b P2 System bridge Porteira ee ee AE a EET EE ER A 13 GPIB communication port connections esssessesseeeeeeeen eene enne A 14 RS 232 communication port connectio
158. relative to a 9 T PPMS magnet the exact location of the top of the magnet varies from magnet to magnet To ensure that the magnet remains immersed you should perform a helium transfer whenever the helium level meter reads below about 60 As explained in the next section the helium level does not change at a consistent rate In the event you plan to let the helium level drop below 60 verify that the magnet does not have a persistent field WARNING Keep the helium level above the superconducting magnet a helium level of 60 There is high potential for damage such as an uncontrolled magnet quench when the superconducting magnet is not completely covered by helium See Sections 1 4 2 and 3 5 for further information 4 2 4 2 HELIUM LEVELS NOT USING A MAGNET When you are not using a magnet during measurements we recommend that you begin carefully monitoring the helium level when it reaches 30 Maintaining the helium level at 30 or above will help prevent serious temperature control problems see below Although typical static helium boil off rates are usually less than 5 7 liters per day the actual rate of PPMS helium consumption varies depending on ambient conditions and how the system is being used For example when the helium level reaches 30 it begins decreasing faster than when it is above 30 the shape of the dewar interior and the nature of the helium level meter mean that the absolute boil off rate does no
159. rogen jacketed dewar capacity ives nice tg ee ds 2 2 2 3 description ssssssssss 2 2 2 3 dimensions eesss 1 8 2 2 2 3 helium transfer cool down warm dewar B 1 B 11 routine cold dewar 4 21 4 23 illustration esses 2 3 4 22 nitrogen transfer cool down warm dewar B 1 B 11 routine cold dewar 4 19 4 20 0 0 1101 a PPE rtc te e dns 1 3 2 1 Nitrogen level monitoring 4 6 Nitrogen transfer cool down filling jacket of a warm dewar B 1 B 11 illustration 4 19 B 2 B 4 B 8 materials e Hee B 2 B 3 routine refilling jacket of a cold dewar 4 19 4 20 No Overshoot field approach mode 3 9 No Overshoot temperature approach Imode ea med re RM 3 6 NTC thermometer sssssssssss 3 2 O Oil pump See also Pump 4 25 C 3 O rings INSPECTING ssssssss 4 28 Oscillate field approach mode 3 8 P Pacemaker effect of magnets on 1 5 1 7 Parameters manipulating for measurement sssssss 3 11 Persistence switch 2 6 3 7 3 8 Persistent mode sss 2 6 3 7 Personal computer connecting to P5 RS232 port A 3 safety pr
160. rs For cooling the For example a rapid change from room temperature to 2 K will cause wild temperature oscillations for some time while a slow change might require little to no precooling The length of time is impossible to estimate because it depends on the equipment and the experimental situation but the minimum will probably be 3 4 hours 3 4 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 3 Theory of Operation Section 3 3 Temperature Control system opens the flow control valve which decreases the pressure above the liquid helium thereby lowering the boiling point of the helium The temperature of the liquid helium in the annulus drops accordingly For warming the system closes the valve slightly allowing the pressure in the annulus to increase and subsequently raising the boiling point of the helium The heaters are used for short time periods to accelerate the warming process In the event you reset the temperature from below 4 2 K to above 4 2 K it will take about 45 minutes to empty the cooling annulus During this time the system cannot control temperature in the sample space 3 3 1 4 SELECTING THE LOW TEMPERATURE CONTROL MODE CLTC is the default mode of low temperature control in the PPMS but you can use the mode that best meets your experimental needs Table 3 1 summarizes the general characteristics and advantages of each mode Low temperature control modes are changed by
161. rs but not pressed in completely Reconnect the two metal pumping lines to the probe head Purge and seal the sample chamber Close the front door of the electronics cabinet Oe mou The procedures are now complete Please dispose of any used oil properly 4 7 4 Using the Probe Lifting Assembly WARNING Always remove and insert the probe very slowly raise it about one inch per minute The probe could explode violently if it is removed from the dewar rapidly and there is a leak in the vacuum space You must use specific techniques to handle the probe because it is fragile and easily damaged Quantum Design provides a probe lifting assembly Figure 4 22 to help you move the probe in and out of the dewar To prevent damage to the probe when it is out of the dewar please use the probe handling guidelines described in Section 4 2 1 The steps below explain how to use the probe lifting assembly We recommend that you review the procedures before you begin referring to Section A 4 and Figures 2 5 4 19 and A 3 if necessary 1 Open the helium fill ports on the probe head by pulling the relief valves straight up Figure 4 19 2 Remove the hinge clamp from the sample chamber access port Figures 2 5 and A 3 3 From the front of the probe the side with the Quantum Design logo slide the probe lifting assembly onto the probe head so that the lifting assembly is underneath the sample chamber access Figure 4 22 Pro
162. s Nitrogen and Helium Transfer You can save time by filling the nitrogen jacket and helium dewar belly simultaneously Note that more helium will boil away during a simultaneous transfer than during a sequential transfer Section B 3 2 but a sequential transfer includes an 48 hours waiting period that is not needed for a simultaneous transfer The procedures for a simultaneous transfer are not difficult but involve many steps To facilitate a trouble free transfer we recommend that you review the entire set of instructions before you begin As noted in Section B 2 3 Materials you will be working with transfer lines and valves for three dewars the PPMS dewar a liquid nitrogen supply dewar and a liquid helium supply dewar as well as a helium gas supply cylinder The transfer setup is shown below in Figure B 2 the liquid nitrogen dewar is not shown The entire process will be easier if there are two people Quantum Design PPMS Hardware Manual 1070 150 Rev B5 B 3 February 2008 Section B 3 Appendix B Warm Fill Nitrogen Jacketed Dewars Filling Warm Dewars TRANSFER LINE c A ADAPTERS LONG OUTPUT Ni EXTENSION i INPUT EXTENSION NITROGEN he LIQUID ACCESS PORT TOP FILL PORT OPEN DURING TRANSFER ONLY PRIMARY RELIEF VALVE PRESSURE GAUGE CREAR CLOSED DURING GAS PHASE VALVE TRANSFER ONLY DIRECT SAFETY VALVE EVACUATION S DE
163. s into the cooling annulus where it either vaporizes or fills the annulus depending on the pressure inside the annulus The cap at the bottom of the probe protects the impedance tube Newer probes those manufactured since January 1998 are enabled for the Continuous Low Temperature Control CLTC option they have a carefully tuned second impedance in parallel with the primary impedance Owners of earlier model probes can purchase the CLTC option by contacting Quantum Design See Sections 3 3 and 4 3 for more information on temperature control modes Baffled Rods The rods that run the length of the probe contain electrical connections to the magnet and impedance assembly One of the rods contains the helium level meter Several baffles provide support for the rods The rods are delicate and cannot support the full weight of the probe Probe Head The top part of the probe that protrudes out of the dewar is referred to as the probe head The probe head contains the two helium fill ports and all the connection ports for attaching gas vacuum and electrical lines from the Model 6000 PPMS Controller Most of the ports and connections are on the back of the probe head Figures 2 4 and A 3 illustrate the probe head and Appendix A discusses the ports and connections The probe head includes the access port into the sample chamber A blank flange covers the access port unless certain PPMS options have been installed Quantum Design PPMS Hard
164. set off in this manner to signal electrical hazards that could result in bodily harm or loss of life PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 C H AP T E R Introduction and System Setup 1 1 1 2 Introduction This chapter contains the following information o Section 1 2 presents an overview of the o Section 1 5 describes environmental function of the PPMS factors to consider in setting up the system o Section 1 3 presents an overview of the o Section 1 6 explains how to contact PPMS hardware Quantum Design s service centers o Section 1 4 covers important safety guidelines Overview of the PPMS The Physical Property Measurement System PPMS provides a flexible automated workstation that can perform a variety of experiments requiring precise thermal control You can use the PPMS to execute magnetic electro transport or thermo electric measurements or you can modify the system in order to perform your own laboratory experiment The unique open architecture of the PPMS allows you to fully configure the basic PPMS platform or to use the PPMS with different PPMS measurement options such as the AC Measurement System option Heat Capacity option or Ultra Low Field option All PPMS options like the PPMS platform are fully automated Control of the PPMS sample environment includes magnetic fields up to 16 T depending on the magnet purchased and a 1 9 400 K temperature range T
165. t f nCtlon Le eet ees A 7 in illustration of Model 6000 ports A 2 Purging sample chamber description 3 7 Q Quantum Design contacting 1 9 1 10 Quench Heater fuse TUNICUONT 2 ii iin ia e a bue ids A 8 in illustration of Model 6000 ports A 2 replacement values s A 23 R Red Lemo connector descriptlORi 2 iiit het three A 10 in illustration of probe head ports A 9 pinouttable 2 cie tette Eden A 18 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 Index Resistivity option example measurement 3 11 3 12 function of user bridge Dodd mee 3 11 3 12 A 2 Rods baffled description 2 5 in illustration of probe components 2 4 Rotary vane pump See Pump S Sample hysteretic approach modes 3 4 3 6 3 9 inserting in sample chamber 4 12 4 14 mounting on puck See Sample mounting optimal types sssssse 3 12 removing from sample chamber 4 14 4 15 Sample chamber See also Temperature control Description GloSIDg i ee ciara aes ee 4 15 description 35d 2 5 in illustration of probe components 2 4 Sample chamber access port and top plate assembly 2 6 2 7 function 12a ciet euet te ee ees A 9 Sample chamber pressure relief valve A 9 Sample holders 3 12 3 13 Sample insertion tool See
166. t panel of Model 6000 PPMS Controller 2 6 1 1 MODEL 6000 FRONT PANEL Figure 2 7 illustrates the front panel of the Model 6000 which has a power button a display screen a contrast knob a number pad and a signal output BNC connector as well as menu keys arrow keys and two status LEDs The status LEDs light up during remote control of the system and when an error is logged into the data file 2 8 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 2 Hardware 2 7 2 7 1 Section 2 7 Optional Magnet Controller The signal output comes from an internal digital to analog converter The signal output can be linked to any one of about 30 system parameters including temperature field position excitation current and resistance The output has a 10 V to 10 V range and values for the linked parameter must be specified for both 0 V and 10 V This analog output is linked in parallel to the A1 analog output port on the Model 6000 rear panel 2 6 1 2 MODEL 6000 REAR PANEL The rear panel of the Model 6000 has ports for all system connections including necessary PPMS connections connections to optional Quantum Design hardware and auxiliary connections that accommodate interfacing with other devices Appendix A discusses these ports in more detail Optional Magnet Controller A PPMS with a magnet will also include a magnet controller either the Model 6700 or the Model 3120 If you ever have
167. t require their own thermometer If you plan to use the PPMS for resistance measurements Quantum Design recommends using one of the PPMS resistivity options because the base PPMS is not configured for easy access to the fourth system bridge channel A 3 3 P3 Option Port The P3 Option port accesses boards that are installed with certain PPMS options For example the AC Measurement System option and the AC Transport option use the AC board which is installed behind the P3 Option port For details about this port refer to the appropriate option manual or contact your Quantum Design representative A 3 4 P4 IEEEASS Port The P4 IEEE488 port is the GPIB communications port for the Model 6000 The GPIB provides a standardized method of communication for all types of electronic instruments Multiple GPIB capable instruments can be connected in parallel Use the CONFIG gt gt 3 IEEE 488 Setup menu to configure the GPIB A 3 5 PS RS232 Port The P5 RS232 port provides an RS 232 interface to the Model 6000 Personal computers or other devices with standard RS 232 ports can be connected to this port Use the CONFIG gt gt 2 Serial Port Setup menu to configure the P5 RS232 port A 3 6 P6 Dewar Port The P6 Dewar port connects the Model 6000 to the helium level sensor the impedance heater and the superconducting magnet persistence switch heater The P6 Dewar port connects to the blue ringed Lemo connector on th
168. t the sample chamber by pushing a few buttons 1 6 Contacting Quantum Design If you have questions or problems related to your QD equipment please contact your local QD service representative at one of the offices listed below When you call please be able to give the representative a full description of the problem including the circumstances involved and the recent history of your system United States Quantum Design World Headquarters 6325 Lusk Boulevard San Diego CA 92121 Tel 1 858 481 4400 1 800 289 6996 Fax 1 858 481 7410 Email service qdusa com Web _ http www qdusa com Service for Canada Mexico the U S and other countries not listed below Europe L O T Gmbh amp Co KG Im Tiefen See 58 D 64293 Darmstadt Germany Tel 49 6151 880631 Fax 49 6151 896667 Email qgd euroservice a lot oriel de Web _ http www lot oriel com Service for Austria Belgium Crete Croatia Czech Republic Denmark England Finland France Germany Greece Hungary Ireland Israel Italy Luxembourg Netherlands Norway Poland Portugal Russia Slovakia Slovenia Spain Sweden Switzerland Turkey and Yugoslavia Quantum Design PPMS Hardware Manual 1070 150 Rev B5 1 9 February 2008 Section 1 6 Contacting Quantum Design 1 10 Japan Quantum Design Japan Sanpo Ikebukuro Building Annex 4 32 8 Ikebukuro Toshima ku Tokyo 171 0014 Japan Tel 81 3 5954 8570 Fax 81 3 5954 6570 Email gdja
169. t translate into a constant percentage drop in the helium level meter Levels appear to drop faster when the dewar is full or almost empty because the helium container is narrower at the top and bottom Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 5 February 2008 Section 4 3 Chapter 4 Setting the Low Temperature Control Mode System Operation Carefully consider helium consumption rates before you start a long experiment especially when the PPMS will be running an unsupervised automated sequence If you are not using a magnet during measurements you can maintain temperature control with helium levels as low as 12 Below about 12 the helium bath no longer covers the impedance tube and the system quickly loses the ability to control temperature Further contaminants can enter the impedance and create a blockage which will cause additional problems Because changes are so unpredictable by the time the helium level reaches 129 it is difficult to accurately monitor low helium levels For these reasons we recommend maintaining the helium level around 30 at all times except for prolonged idle periods 4 2 5 Monitoring the Nitrogen Level The nitrogen in nitrogen jacketed dewars serves a less crucial purpose than the helium so it could boil away almost completely without any repercussions other than more rapid consumption of helium However to keep the helium well insulated you should fill nitrogen jackets about twice a week Sect
170. temperature control reflecting processes that prevent liquid helium from collecting in the annulus while the neck is cooled However the duration of each precooling process is heavily dependent on the thermal history of the system 3 3 1 3 POT FILL MODE TEMPERATURE CONTROL In pot fill mode the system initiates a pot fill at about 4 2 K when it fills the cooling annulus with a controlled amount of liquid helium and manipulates the boiling point of the helium The liquid helium is drawn through the primary impedance tube with the impedance heater off The fill procedure is regulated by the pressure difference between the cooling annulus and the dewar When the annulus is almost full which takes about 45 minutes the impedance heater is turned on warming the impedance tube until the helium pressure inside the tube prevents liquid helium from entering either end This state is commonly called on the pot The system can use pot fill mode to maintain temperatures of about 1 9 K for hours The liquid helium bath around the sample space provides a uniform stable thermal environment However it can be difficult to maintain a temperature very close to the boiling point of the liquid helium because the control mechanisms in the high temperature and pot fill modes are so different When the system is on the pot it controls temperature increases and decreases by opening and closing the flow control valve in the Model 6000 and by using the heate
171. the base of the puck When you install the puck the 12 pins connect to the sample puck connectors located on the bottom of the sample chamber and then ultimately to the pins of the gray ringed Lemo connector on the probe head The puck is keyed to ensure that the electrical connectors align properly The last solder pad counting clockwise is square instead of round You will use this solder pad as a reference point to help you wire sample leads to the proper solder pads Refer to Section 4 4 for sample mounting instructions Each PPMS option includes several pucks so you can mount different samples on different pucks You also can configure each puck for a different type of experiment 2 10 1 Puck Insertion Tool The puck insertion tool is a long rod used for installing the puck in the sample space The lever of the puck insertion tool is engaged when it is lying flat across the handle as is shown in Figure 2 12 When the lever is engaged the tool grips the puck by a groove in its outer rim eneas BR RRR RR MOINDRE Figure 2 12 Sample insertion tool with lever in engaged position The puck insertion procedure is described in Section 4 5 The procedure is easy and requires only a few seconds after you have warmed the sample chamber to room temperature 2 10 2 Puck Adjustment Tool The puck adjustment tool Figure 2 13 is used to adjust the tension in the fingers of the puck so that the fingers maintai
172. the PPMS will be used as a magnetometer knowing the magnetic moment of the sample holder is also important To determine its effect on the sample measurement measure the magnetic moment of the sample holder without a sample In general samples must be securely mounted to the sample holder so that their position will remain constant or known in some cases Secure mounting also is important to help prevent losing samples inside the sample chamber it usually requires great effort to retrieve lost samples and to clean the chamber Mounting a Sample on a Sample Puck There are many methods to secure a sample to a puck Leads are frequently soldered or welded to samples but the type of wires used and the method of contact vary by application In addition tapes conductive epoxies greases glues and paints can be used Conductive pads can be coated onto semiconducting thin film samples Each method can have an array of thermal electrical magnetic and reactive properties If you will be using a puck as the sample holder first consult Appendix A or the appropriate option manual to determine the proper solder pads to use for electrical contact Also plan the geometrical arrangement of the leads PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 Section 4 4 System Operation Sample Mounting It will be easier to solder leads to the solder pads 1f you remove the connector PC board from the bottom of the puck
173. the input end of the transfer line into the supply dewar Tighten the adapters that seal the transfer line to the liquid access port Continue lowering the input end until an exhaust plume appears Nx p at the output end l B 7 Insert the adapter at the output end of the transfer line into the PPMS dewar through the helium fill port refer back to Figure 4 18 Push the transfer line completely into the dewar Gas will begin flowing from the output adapter Point the output adapter exhaust tube away from the evacuation valve and the rest of the dewar top The exhaust will be so cold it can freeze and damage parts such as O rings and sealed valves Figure 4 19 Opening a helium fill port on the head of a PPMS probe standard dewar shown 4 22 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Chapter 4 System Operation Section 4 7 Routine Maintenance Procedures CAUTION Point the output adapter exhaust tube away from all hardware on the dewar and probe head The extremely cold exhaust can damage parts especially O rings and sealed valves 10 11 12 13 14 15 16 17 Verify that each adapter on the transfer line is properly seated so that it seals the transfer line At the liquid helium supply dewar open the gas phase valve At the helium gas cylinder open the regulator to start transferring helium into the PPMS dewar Monitor the helium transfe
174. tion When charging to zero field the Oscillate mode should be used to keep the remnant field in the magnet as small as possible In No Overshoot mode the magnet is charged to 70 of the difference between the field set point and the present field and then the magnet slowly approaches the set point from only one direction in continuous 70 increments until the magnet is close enough to the set point to drive directly to it without overshooting it The charging direction is never reversed when No Overshoot mode is used but field relaxation can occur That is after the magnet enters Persistent mode the actual field in the magnet can change slightly from the reported field You should use No Overshoot mode with field hysteretic samples Linear mode is the quickest charging mode Linear mode fine tunes the field after an initial attempt at charging the magnet directly to the field set point Both field overshooting and field relaxation are possible in Linear mode Important When you set measurement parameters do not confuse the No Overshoot temperature approach mode with the No Overshoot magnet charging approach mode 3 6 Helium Level Metering The helium level meter is inside one of the rods running the length of the probe The meter is thus outside the sample chamber and vacuum tubes The helium level meter is a long superconducting wire configured for a four wire resistance measurement Because the portion of superconductor that is not i
175. tions 4 7 3 1 and 4 7 3 2 Quantum Design pump oil level oil mist filter and foreline trap At least once a month check the oil level in the pump and and oil mist filter and add oil as TENIS appropriate At least once a week check the amount of oil that has collected around the oil mist filter and empty as Figure 4 20 Electronics cabinet and necessary Check the oil levels more frequently if the rotary vane pump pump is heavily used PPMS Hardware Manual 1070 150 Rev B5 4 23 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation e Once a year the pump and the oil mist filter cartridge need a complete service as explained in Appendix C e Twice a year use the instructions in Appendix C to clean the foreline trap which acts as the inlet filter for the pump Appendix C also contains a maintenance record so that you can track when service was last performed CAUTION Check the level of oil in the oil mist filter at least once a week If the filter becomes too full oil can back up into the gas lines and plug the system Pump Versions Since 1997 all PPMS units have used CE compliant Edwards or Varian pumps before that time the PPMS was equipped with an Alcatel pump see Figure 4 21 Forline Trap ES To 1 Qil Mist Forline Filter Forline Oil Level a l Window Oil Level Window Oil Level Window i Alcatel rotary vane
176. to a stable state by putting it in Shutdown mode e To use the Model 6000 select CTRL gt gt Interactive Control gt gt 8 Shutdown Mode e To use MultiVu select Instrument gt gt Shutdown from the dropdown menus at the top of the MultiVu window 3 Deactivate any active option Utilities gt gt Activate Option 4 Exitthe MultiVu program and turn off the power to the computer 5 Disconnect the annulus line the large pumping line at the probe head Open the annulus connection enough to stop the flow but leave it seated in the connector 6 Turn off the power to the individual PPMS components including the vacuum pump 7 Turn off the main breaker on the back of the PPMS cabinet 8 Unplug the PPMS plug from the power source Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 3 February 2008 Section 4 2 Chapter 4 General Guidelines System Operation 4 2 2 3 POWER ON SEQUENCE Plug in the PPMS power cord Turn on the main breaker on the back of the PPMS cabinet Turn on the power to the computer Turn on the power to the individual PPMS components including the vacuum pump Start MultiVu Set the temperature to 5 K Instrument gt gt Temperature When you set the temperature to 5 K the equipment automatically opens the valves and starts pumping out the lines DN cas oue ibat ors 7 Wait five minutes for the system to stabilize 8 Reconnect the annulus line at the probe head 9 Setanew temperature 1
177. to the end of the nitrogen supply line 3 Atthe PPMS dewar insert the small end of the liquid nitrogen transfer adapter into the open liquid nitrogen fill port and turn the brass fitting clockwise to secure the adapter in place Figure 4 16 Quantum Design PPMS Hardware Manual 1070 150 Rev B5 4 19 February 2008 Section 4 7 Chapter 4 Routine Maintenance Procedures System Operation 4 Atthe liquid nitrogen supply dewar slowly turn the liquid supply valve until it is about 50 open Exhaust should begin coming out of the second nitrogen fill port on the PPMS dewar Do not open the liquid supply valve more than 50 a fully opened valve can produce violent spillovers of exhaust that are extremely hazardous and difficult to avoid WARNING Always open the liquid supply valve slowly and only open it about 5096 Although the transfer is fast when the valve is completely open such transfers are extremely hazardous 5 Atthe PPMS dewar visually monitor the exhaust from the second nitrogen fill port during the entire fill process While you are monitoring the exhaust put on your protective gear This gear is necessary to prevent serious burns from the extremely cold fitting supply line and transfer adapter Do not leave the PPMS unattended during this step and always stand at least 0 5 m 1 5 ft from the exhaust plume 6 Atthe liquid nitrogen supply dewar close the liquid supply valve when the exhaust turns to li
178. traw fits within the sample chamber Is easy to use with option hardware is not conductive and has very low magnetic susceptibility Quantum Design PPMS Hardware Manual 1070 150 Rev B5 3 13 February 2008 C HAPTER 4 System Operation 4 1 4 2 Introduction This chapter contains the following information o Section 4 2 presents general guidelines o Section 4 5 explains how to install a puck for using the PPMS into the sample chamber and how to remove it o Section 4 3 describes how to change the o Section 4 6 describes some of the ways the low temperature control mode pot fill or PPMS can be customized CLTC Oo Section 4 4 discusses sample mounting o Section 4 7 describes routine maintenance procedures procedures such as refilling a cold dewar and checking the oil in the vacuum pump General Guidelines The PPMS is a precision laboratory instrument that is designed to be robust and adaptable However it is complex and some parts are fragile This section provides guidelines for the appropriate use and maintenance of the system and its critical components You can help prevent damage to the system and ensure that it provides optimal measurements by reviewing this material and following the guidelines 4 2 1 Handling the Probe WARNING Always remove the probe from the dewar very slowly raise it about one inch per minute The probe could explode violently if you rapidly pull it from the dewar when th
179. ube and the heat shield A cap at the bottom of the probe protects the bellows The protective cap is not sealed and liquid helium flows freely into it Major components of the probe are the sample chamber impedance assembly optional magnet baffled rods and probe head which are discussed in the following sections PPI PRC SAMPLE SPACE COOLING ANNULUS E 23 SL 3 INS ATION go e SUPER INSULATION 270 amp VACUUM HEAD 19 ACUUM OO 7 4 SAMPLE CHAMBER M le ER CENTER OF MAGNETIC FIELD HEA SHIELD N NO 4 El BOTTOM OF SAMPLE CHAMBER WITH SAMPLE PUCK CONTACTS BAFFLES aA m MAGNET arr i THERMOMETERS AND HEATERS 24 E IMPEDANCE A HEATER AND 4 A MAGNETI T THERMOMETER d ZIZ A ANASON 1 N ER PROTECTIVE CAP Em z gt OPEN TO HELIUM IMPEDANCE d A TUBE aD v C X i BELLOWS HELIUM LEVEL METER 2 4 Figure 2 4 Major components of the PPMS probe PPMS Hardware Manual 1070 150 Rev B5 February 2008 Quantum Design Chapter 2 Hardware 2 3 1 2 3 2 2 3 3 2 3 4 Section 2 3 Probe Sample Chamber The sample chamber is inside the two vacuum tubes The lower 3 9 in 10 cm of the s
180. uck Disengage the puck insertion tool and then raise the tool several centimeters Be alert for resistance when you raise the insertion tool Resistance can indicate that the puck has caught in the tool as you began lifting it out so you will need to remove the puck and again try to insert it Remove the puck insertion tool from the sample chamber Place the O ring over the sample chamber access port and place the KF blank flange on it Place the flange clamp in position around the top of the sample chamber access port and then latch the clamp Purge and seal the sample chamber To purge and seal the chamber you can use the Model 6000 menu CTRL gt gt 1 Interactive Control gt gt 2 Purge and Seal or MultiVu Instrument gt gt Chamber gt gt Purge Seal The system is now prepared for you to conduct experiments To determine your next steps refer to the appropriate option manual After you have performed a measurement and verified the operations of the instrument you might find it useful to write a sequence that automates the measurement as explained in the PAysical Property Measurement System Commands Manual and the Physical Property Measurement System PPMS MultiVu Application User s Manual Removing a Sample Puck The procedures for removing the puck from the sample chamber are essentially the reverse of the installation procedure 1 Verify that the sample chamber is at or above 298 K The temperature must be
181. uding the effects of magnetic fields generated by the superconducting magnet the physical dimensions of the equipment vertical clearance above the dewar and the local altitude and humidity The PPMS is intended for indoor use at altitudes less than about 6000 ft 1829 m If you will be operating the system at altitudes above our specifications please discuss it with your Quantum Design representative The PPMS should be operated in an ambient temperature between 5 C and 40 C with a maximum relative humidity of 80 at 40 C Important The electrical safety features of the PPMS might be impaired if it is operated outside these environmental considerations Magnetic Field Considerations Before you install the PPMS consider how the three dimensional field generated by the superconducting magnet will affect nearby people and objects For example measuring out from a 9 T longitudinal magnet at full field we obtained the surrounding radial distances at which various field strengths occur These results are shown in Table 1 1 according to their effects on people and objects including those located above and below the magnet This list is not comprehensive so you should consider all the equipment in your laboratory that might be affected by magnetic fields Also remember that a PPMS with a stronger magnet e g 14 T or 16 T will produce effects at significantly smaller distances than those listed Table 1 1 Possible effects of the PPMS
182. ugh connector a 2 Red Lemo connector 4f b Magnet controller BLACK BLUE Figure A 10 Magnet connections a 1 TCM 100 A Top plate feedthrough connector or a 2 Red Lemo connector and b Magnet controller Table A 7 Magnet connections probe to controller MAGNET CONNECTION iio MAGNET CURRENT FUNCTION ae 31 Mag red or blue banded cable 2 Mag black cable TCM NEN A Top plate Mag blue banded cable Current e 2 Mag black cabe black cable Current A 18 PPMS Hardware Manual 1070 150 Rev B5 Quantum Design February 2008 Appendix A Connections Ports and Pinouts A 5 8 Expansion Connections Auxiliary The P8 Auxiliary port is on the Model 6000 P8 Auxiliary port Figure A 11 Auxiliary expansion connections Table A 8 Expansion connections auxiliary P8 AUXILIARY FUNCTION pD CONNECTOR Hi Vac Solenoid 13 Shield Quantum Design PPMS Hardware Manual 1070 150 Rev B5 February 2008 Section A 5 Pinout Tables A 19 Section A 5 Appendix A Pinout Tables Connections Ports and Pinouts A 5 9 Expansion Connections Pressure Gauge The P9 Pressure port is on the Model 6000 P9 Pressure port 4 Figure A 12 Pressure gauge expansion connections Table A 9 Expansion connections pressure gauge P9 PRESSURE GAUGE AND D FUNCTION CONNECTOR Baratron Sig Baratron Rtn A
183. uirements match the alternating current AC power available at your location If the system has not been configured for the correct power available at your location contact your local service representative before you proceed with the system installation To prevent electrical shock verify that the equipment is properly grounded with three wire grounded plugs To prevent electrical shock unplug the system before you install it adjust it or service it Do not spill food or liquids on the system or its cables Refer to the section titled Safety Precautions before you install or operate this system Direct contact with cryogenic liquids materials recently removed from cryogenic liquids or exposure to the boil off gas can freeze skin or eyes almost instantly causing serious injuries similar to frostbite or burns Wear protective gear including clothing insulated gloves and safety eye protection when you handle cryogenic liquids Transfer liquid helium only in areas that have adequate ventilation and a supply of fresh air Helium gas can displace the air in a confined space or room resulting in asphyxiation dizziness unconsciousness or death Keep this system away from radiators and heat sources Provide adequate ventilation to allow for cooling around the cabinet and computer equipment Refer to the manuals for the supplied computer and monitor for additional safety warnings and notices before you operate the system Reg
184. ulatory Information o o This apparatus has been tested to the requirements of the EMC Directive 89 336 EEC This apparatus is defined as ISM Group 1 Class A and B equipment per EN 50011 1991 industrial and light industrial environment limits of radio frequency emission This apparatus has been tested to the requirement of the Low Voltage Directive 73 23 EEC See the EU Declaration of Conformity for additional regulatory information regarding your PPMS Quantum Design PPMS Hardware Manual 1070 150 Rev B5 iii February 2008 C ON TE N T S Table of Contents PREFACE Contents and Conventions C M xiii P Introduction ede nee ert etis tree thee ease bddeessl Seulsastestnevousbed xiii P2 Scope of the Manual 4e etie eei t ttt d ices Bde evel ss auteni iere xiii P 3 Contents of the Manual enne entren enn en nennen reser ener nennen xiii P 4 Conventions in the Manual ssssssssesseeee eene ener entren nennen nennen nennen nnne xiv CHAPTER 1 Introduction and System Setup sce ccccccosscsessieccenssedesdescrssocnsssevtucdessassossasootecssencssssasacenasdeeneass 1 1 1 1 Introductionis Re De ee eer d RR ei eec pes v eee 1 1 1 2 Overview ol the PPMS itr id ehe tei POR ERE Ee D ESTIS EE RSURE pacawech ERE A PENNE ese 04d 1 1 1 3 Overview of System Hardware ssssssssseseseeeeee nennen eene entrent entren nn 1 2 1 4 Safety Precautions icc mter ep e E e e Pe ui e Reed 1 3 EAT CTyOPODS tie
185. um and nitrogen to fill warm empty standard dewars and nitrogen jacketed dewars o A Appendix C provides maintenance instructions for the vacuum pump assembly Conventions in the Manual File menu File gt gt Open STATUS dat lt Enter gt lt Alt Enter gt Important Note Bold text identifies the names of menus dialogs options buttons and panels used in the PPMS MultiVu software The gt gt symbol indicates that you select multiple nested software options Bold text and all capital letters distinguish the names of keys located on the front panel of the Model 6000 PPMS Controller The Courier font indicates file and directory names and computer code Angle brackets distinguish the names of keys located on the PC keyboard A plus sign connecting the names of two or more keys indicates keys that you press simultaneously Text is set off in this manner to signal essential information that is directly related to the completion of a task Text is set off in this manner to signal supplementary information about the current task the information may primarily apply in special circumstances CAUTION Text is set off in this manner to signal conditions that could result in loss of information or damage to equipment WARNING Text is set off in this manner to signal conditions that could result in bodily harm loss of life or irreparable damage to equipment WARNING Text is
186. urrent Field changes can be made more quickly in Driven mode but the resulting field is much noisier 3 5 1 Control Mechanisms For each PPMS the field in the sample space is a known function of the current in the magnet Systems are individually calibrated to their own field to current ratio To ensure that the proper field exists in the magnet during magnet charging and discharging the current from the power supply is passed through one of two calibrated resistors magnet controller before the persistence switch heater is turned off The two resistors are for high power and low power operation and the appropriate resistor is used for each current The voltage drop across the resistor is directly proportional to the current in the magnet and thus proportional to the field within the sample space The field is calculated from this potential drop and if the field is not within a certain range of the field set point the magnet current is adjusted accordingly until the field 1s within the acceptable range For 7 T and 9 T longitudinal magnets the field must be within about 1 5 Oe of the set point for set points above about 9500 Oe For set points below 9500 Oe the field must be within about 0 15 Oe of the set point before the persistence switch heater is turned off For 14 T magnets the field must be within about 3 Oe of the set point for set points above about 15 000 Oe and the field must be within about 3 Oe of the set point for set points below 15
187. using the MultiVu software application or the Mon 6000 utility as explained in Chapter 4 System Operation For more information on MultiVu and the Mon 6000 utility see the Physical Property Measurement MultiVu Application User s Manual and the Physical Property Measurement System Firmware Manual respectively Note Because the two control modes are so different sometimes you can use pot fill mode to cool the chamber when CLTC mode is not bringing temperatures below 4 2 K Rather than stopping the experiment to investigate the cooling problem you can switch to pot fill mode and attempt to bring the unit to your target temperature If the unit cools successfully when you use pot fill you might be able to complete the experiment before you fix the cooling problem Table 3 1 Characteristics of low temperature control modes CONTROL METHOD CTLC CHARACTERISTICS Begins a precooling phase at about 10 K Reaches low temperatures without collecting liquid helium around the sample space ADVANTAGES Transitions through 4 2 K helium boiling point smoothly Attains stable temperatures at and near 4 2 K helium boiling point Increases temperature quickly and smoothly DISADVANTAGES Control of temperature might be temporarily lost at beginning of precooling phase depending on thermal history Control of temperature is relatively less stable than with pot fill mode Pot fill mode Takes o
188. ust the regulator on the helium backfill cylinder so that gaseous helium is expelled from the 1 3 psi relief valve the hose nipple on the back of the probe head and from the 1 psi relief valve on the closed helium fill port c Keep the dewar pressurized this way for 2 minutes before you proceed Use the Chamber dialog in MultiVu select Instrument gt gt Chamber gt gt Purge Seal or the Model 6000 CTRL gt gt 1 Interactive Control gt gt 2 Purge amp Seal to remove air from the sample chamber At the helium backfill cylinder adjust the regulator so that helium is expelled from only the hose nipple Place a wetted finger in front of the hose nipple to verify that helium is exiting there Nitrogen Transfer 1 Quantum Design At the liquid nitrogen supply dewar open the valve on the nitrogen supply line Exhaust should begin coming from the second nitrogen fill port on the PPMS dewar At the PPMS dewar visually monitor the exhaust from the second nitrogen fill port during the entire fill process Do not leave the PPMS unattended during this step and always stand at least 0 5 m 1 5 ft from the exhaust plume Important Periodically check the flow from the helium backfill cylinder by placing a wetted finger in front of the hose nipple on the probe head If helium is not being released from the 1 3 psi relief valve behind this fixture increase the flow of helium by adjusting the regulator of the helium gas cylinder
189. ver temperature control at about 4 2 K Fills cooling annulus with liquid helium and manipulates boiling point of helium Maintains extremely uniform thermal environment for the sample space Maintains a very quiet thermal environment for the sample space Provides best absolute temperature accuracy and stability below 4 2 K helium boiling point Loses temperature control when transitioning through 4 2 K helium boiling point Control of temperature at and near 4 2 K helium boiling point is relatively less stable than with CTLC mode CLTC cooling problems are most often from frozen contaminants blocking one of the impedance tubes To clear the tube you must remove the entire PPMS probe from the liquid helium dewar Quantum Design PPMS Hardware Manual 1070 150 Rev B5 February 2008 3 5 Section 3 4 Chapter 3 Atmospheric Control Theory of Operation 3 3 2 Temperature Approach Modes You can set the PPMS to approach a temperature set point with the Fast Settle mode or the No Overshoot mode Fast Settle mode changes the temperature very rapidly but it can undesirably affect samples that show temperature hysteresis behavior In Fast Settle mode the temperature control hardware first overshoots or under shoots the temperature set point in order to help overcome thermal gradients in the sample chamber then the hardware backtracks to the set point In No Overshoot mode the PPMS approaches t
190. ware Manual 1070 150 Rev B5 2 5 February 2008 Section 2 4 Chapter 2 Top Plate Assembly Hardware 2 3 5 Optional Magnet 2 4 2 6 The PPMS can be purchased with a 1 T 7 T 9 T 14 T or 16 T longitudinal magnet or a 7 T transverse magnet The magnet is a superconducting solenoid composed of a niobium titanium alloy embedded in copper It is on the outside of the probe so it is always immersed in liquid helium The magnet coil constitutes a closed superconducting circuit The persistence switch is a small heater on the magnet wire that drives a section of the magnet non superconducting The persistence switch allows the magnet controller either the Model 6700 or the Model 3120 to be switched into the magnet circuit so that the magnetic field can be changed When the heater is turned off the entire magnet can superconduct which eliminates the need for a current source during constant field operation This state is referred to as the Persistent mode of the magnet Section 3 5 discusses magnetic field control in more detail For 1 T 7 T 9 T 14 T and 16 T longitudinal magnets the magnetic field is centered 2 1 in 5 4 cm above the surface of an installed sample puck but the field uniformity varies The 7 T transverse magnets are shipped with the center of the field 1 6 in 4 0 cm above the surface of an installed puck Top Plate Assembly The top plate assembly Figure 2 5 consists of the components that seal the sample chamb
191. when you insert it into the sample chamber If the puck lodges in the sample chamber you might have to disassemble the probe to remove it 6 Verify that the temperature of the sample chamber is at or above 298 K The temperature must be at least 298 K when the chamber 1s opened to the atmosphere to prevent cryopumping air into the chamber If the temperature of the chamber is below 298 K set it to 298 K and wait until it reaches room temperature You can set the temperature by using the CTRL gt gt 3 Immediate Operations gt gt 1 Temp menu in the Model 6000 by using the shortcut in the MultiVu Status bar or by using MultiVu CAUTION Always bring the sample chamber to room temperature before you open it to the atmosphere This will prevent condensation and cryopumping of air constituents inside the chamber which can cause probe malfunctions such as blocked valves and loss of temperature control 7 Verify that the field in the magnet is less than 1 tesla If the field is greater than that set the field to less than 1 tesla and wait for the magnet to reach the set point select Instrument gt gt Field to open the MultiVu Field dialog box CAUTION Do not place the puck insertion tool or any other object into the sample chamber when there are high fields in the magnet as the force on the insertion tool could overwhelm you and cause you to damage the equipment 8 Ventthe sample chamber with clean dry gas Ventin
192. x B Helium and Nitrogen Transfers into Warm Dewars Filling Warm Dewars board connections are not necessary to perform a dewar fill but they are needed to use the system fully If you are not experienced at transferring liquid helium ask for help from someone who is familiar with the liquid helium supply vessel At the least read over these instructions to familiarize yourself with the process and materials before you begin the helium transfer B 2 1 Nitrogen Jacketed Dewars There are two methods for refilling a warm nitrogen jacketed dewar The quickest method involves a simultaneous transfer of liquid nitrogen and liquid helium Section B 3 1 The other method minimizes helium loss during the transfer by using a sequential transfer of liquid nitrogen and liquid helium Section B 3 2 The sequential procedure requires a continuous flow of helium gas through the probe impedance tube during the liquid nitrogen transfer and for a subsequent 48 hours cooling period B 2 2 Standard Dewars To fill a warm standard dewar no nitrogen jacket use the instructions in Section B 4 B 2 3 Materials o Rubber or plastic tubing 1 2 m o A helium backfill adapter sequential transfer only o A helium transfer line with input extension and long output extension an output adapter and an input adapter see Figure B 1 OUTPUT PPMS END INPUT SUPPLY END OUTPUT ADAPTER 4 i T INPUT ADAPTER LONG OUTPUT INPUT EXTENSION EX
193. y connects the Gas Source port to the Sample Vent Up port directing helium from the dewar into the sample space through the vent valve in the Model 6000 If you use an alternate gas source the Gas Source port must be plugged A 3 20 Dewar Port The polypropylene tubing provided with the system connects the Dewar port to the small Ultra fitting on the probe head This connection to the dewar serves two purposes 1 It provides a gas source for venting and purging the sample chamber and 2 it allows monitoring of the pressure differential across the impedance assembly This second function is necessary to allow proper low temperature operation and control so it is important to keep this line connected even when an alternate gas source is used for venting the sample chamber A 3 21 Syst 5A Fuse The Syst 5A fuse is the fuse for the system heater and stepper motor power supply Replace the fuse only with an equivalent 5 A 250 V time delay fuse A 3 22 Aux 2A Fuse The Aux 2A fuse protects the auxiliary relays and external motor ports Replace the fuse only with an equivalent 2 A 3 AG fuse A 3 23 Quench Heater Fuse The Quench Heater fuse is required to operate the Magnet Reset option used by the Ultra Low Field option Replace the fuse only with an equivalent 630 mA 280 V time delay fuse A 3 24 Power Receptacle The power cord connection for the Model 6000 is at the rear in the lower right cor

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