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DynaCool Manual

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1. cc cccesesseeeseeeeeeeceeeeeeeeeeaaaaeeeeeees C 1 Figure C 2 44 pin d Shell pin and socket layout ccscccccccccccceceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeess C 2 viii PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Contents Table of Tables Table 5 1 Maintenance procedures required for the DynaCool system sssssssosooeeeneesssssssssssssseeereresssssssssssses 5 8 Table C i Sample Puck Connections erus aeia cies OE eaten ensan Waac cen E AEEA C 2 Table C2 JQP 9 Temperature Control Connections sree a a E REENEN C 3 TEC JOP Cryostat Lemperature Conio rnc tect wei neate aires a ais C 4 Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 1X November 201 1 P R E FACE Contents Conventions and Safety P 1 P 2 P 3 Overview The preface describes the scope of the manual the conventions used and most importantly safety guidelines Scope of the Manual This manual discusses the Quantum Design PPMS DynaCool instrument It contains information about basic functionality describes the system hardware and the control software Most DynaCool systems include measurement options that you use for performing sample measurements This manual discusses how measurement options interface with DynaCool but does not cover any details about specific options Be sure to read the separate measurement option user manuals All DynaCool systems include a cryo
2. Change the plot axes by selecting Graph gt Data Selection or right click in an open graph window and select Data Selection The axes may be assigned any label for which data exists in the data file Up to four vertical axes may be displayed on separate plots in the same graph window but all plots in the graph window must share the same horizontal x axis When auto scaling is selected for all axes the plot axes will be rescaled each time new data is written to the data file so that all data is displayed This helps optimize data viewing as data is being collected Quickly auto scale the axes by right clicking in the graph window and selecting Auto Scale All Plots Use the gt gt button to add custom axis labels and to change the axis scaling multiplier by factors of 10 e Use the Filter button to plot only records with data that falls within a specified range For example specify a range for moment standard error to hide data with a large standard error i e noisy data The OK button applies the changes to the graph window and closes the Data Selection dialog The Apply button applies the changes to the graph window without closing the dialog The Cancel button closes the Data Selection dialog without making any changes to the graph window Select one X axis and Specify the data to Click to apply additional up to four Y axes plot on each axis label
3. Magnet Controller Press the reset button on the magnet controller to reset it You can access this button by removing the front panel of the pump cabinet see Section 2 13 Chamber Vacuum Gauge Power cycle the CAN Module Bay to reset the chamber vacuum gauge MAGNET SIGNAL DISTRIBUTION This panel also contains a magnet signal patch These three connectors merge separate signals paths from the magnet controller and optional low field controller into a single cable going to the magnet in the cryostat Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 5 November 2011 Section 2 2 Chapter 2 System Hardware Components Hardware OAR Pump Cabinet and Computer gas handling hoses annulus return chamber case helium bottle Figure 2 5 Front view of Pump Cabinet The pump cabinet Figure 2 5 serves as both a workstation and also a container for the following components Circulation Pump This is a sealed scroll pump that is used for circulating helium past the sample chamber for cooling the sample The outlet of the pump flows at relatively high pressure 500 to 800 Torr to the cryostat where it is cooled and partially liquefied before passing through a flow impedance and into the annulus surrounding the sample chamber It is then pumped at lower pressure 5 to 50 Torr back to the inlet of the pump This scroll pump requires regular maintenance at approximately 6 months intervals Refer to Chapter 5 for
4. PPMS DynaCool User s Manual 1307 110 Rev AO November 2011 Quantum Design Chapter 1 Getting Started Section 1 5 Installing and Removing Samples Rotate the puck to verify that it is properly seated inside the hollow cylinder The puck should rotate smoothly Engage the sample 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 tool s handle The tool should now grip the outer rim of the puck Verify that the puck remains properly seated in the hollow cylinder The puck must be level and should not rotate easily Gently pull on the puck to verify that the tool holds it securely WARNING An unlevel puck can get stuck in the sample chamber and can damage the pins at the bottom of the chamber Before inserting the puck into the chamber you must verify that the puck is level within the cylinder of the sample insertion tool Verify that the sample chamber is at or above 298 K The temperature must be at least 298 K to prevent condensation of water or cryopumping of air into the chamber If the temperature is below 298 K set it to 298 K and wait for the chamber to warm up Use MultiVu to set the temperature click on the temperature display in the status bar In the temperature dialog enter 298 K 20 K min and select Fast Settle mode Press the Set button An installation wizard in measurement option softw
5. Figure 2 2 shows the back of the cryostat where the connections are made to the high pressure 200 to 300 psi helium lines from the cryocooler compressor assembly The hoses are double sealing Aeroquip type Note that the small connector corresponds to the high pressure flow from the compressor and the large connector is the lower pressure return Also shown in the figure is the moisture wick This wick is a synthetic cloth extending from the base of the inner vacuum vessel to a region outside the magnetic shield Itis designed to wick excess condensed moisture from the case of the vacuum vessel In humid climates water can condense on the inner vacuum vessel when the vessel is automatically vented with air during an automated warm up procedure see Section 3 2 8 2 Under normal operation conditions there should be no moisture present either inside the magnetic shield or visible at the moisture wick Zee CAN Module Bay gray Lemo connector sample chamber wring temperature control module module bay for option electronics empty slots for additional CAN modules for options Figure 2 3 CAN Module Bay and sample puck wiring port gray Lemo Figure 2 3 shows the top of the CAN module bay It is attached to the cryostat shield near the gray Lemo connector The gray Lemo connector is the main electrical connection to the sample chamber Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 3 November 2011 Sect
6. Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 17 November 2011 Section 3 5 Chapter 3 Graphing Data Files Software Then specify the path and file name for the template file Specify Graph Files gph in the Save as type box to save the template as a graph file Be sure the file name you specify matches the data file you want the graph applied to in this case To apply a template to a data file select Graph gt Apply Template or right click the graph view and select Apply Template Then locate the template or graph file you want to use Graph gt Restore Graph applies the settings from the graph file to the graph window This will undo any settings changed since last time the graph file was saved Graph gt Default Graph sets the axes to defaults that are specified in the data file when the file is created For measurement options the default setting usually displays the data you are most likely to look at e g Sample Heat Capacity vs Temperature for the Heat Capacity Option 3 5 4 Exporting Data Files Many spreadsheet programs can read the standard dat files DynaCool MultiVu generates They have a comma delimited format but the files contain additional header information and may contain diagnostic data that complicates your data analysis or communication with collaborators To export data files or subsets of the data in a data file do the following E
7. Appendix B Section B 2 Diagnostic Software Background Log B 2 2 B 2 3 B 3 Temp K 25 00045 Field Oe 0 736537 Chamber Pres Tor 1 852165 Temp Status 1 Field Status 4 Chamber State Cryostat Status Fi Sample Them ID 643 Control Therm 1D 643 Figure B 2 Standard Items Tab Diagnostic Items The diagnostic items tab contains detailed information about the instrument state that is useful for troubleshooting Problems with temperature control magnetic field control and the cryostat control can all be diagnosed using data in this tab Advanced Items Advanced Items are all configurable data items A large amount of raw instrument data is available for logging when required Data can be logged from any CAN node on the bus Configuration of these data items 1s accomplished with a map qmap file which is usually supplied by a Quantum Design representative The map file is loaded using the Select Map File button and the resulting browse dialog Background Log Any time MultiVu is running it records diagnostic data to a background log file The file C QDDynaCool MultiVu BRLog dat is a normal MultiVu data file that can be viewed like any other data file The background log file is limited in size to 20 MB When this limit is reached the file is copied to BRLog_bu dat and a new BRLog dat file is created Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO B 3 November 2011 Section B 4
8. IOM IOK Stable Purged and seated SrgieMeanurenert Measurement Paaneters Avaragrg The ek f Sequence ide SmKseme 4107 Oe Holing Rela Seq none Cot 30100 K Set 1K Oe Purged none 2000K nin Fast Senie 310000 0e sec Urea 4 VSM Measurement Figure 3 9 VSM Option s Control Centers Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 9 November 2011 Section 3 4 Sequences 3 4 3 4 1 3 10 Chapter 3 Software Sequences Operation of DynaCool is automated using sequences Sequences are simple computer programs instructing the instrument to carry out a number of operations in a predetermined order Simple looping is Supported in sequences but branching is not Operations typically found in a sequence file include changing the sample temperature changing the magnetic field and measuring some property of the sample depending on which measurement option is active Additionally commands may be placed in sequences to log diagnostic data record a comment in the data file begin recording data to a new data file generate a message on the computer screen and even run another sequence MultiVu is also used to run pause lock and abort sequences on DynaCool and to view the status of sequences as they run Editing Sequences Create a new sequence file by clicking New Sequence D or selecting the menu item File gt New Sequence Open an existing sequence file for editing
9. Set Field Sets the instrument s magnetic field Specify the field the charging rate and the approach O Linear Controller will drive directly to the field and attempt to maintain the specified charging rate as closely as possible Oscillate Controller will intentionally overshoot the set point by 70 of the field change at the desired rate and will then oscillate into the set point field in smaller and smaller overshooting steps This is intended to eliminate flux motion in the superconducting magnet windings yielding a very stable magnetic field and reduced remanence Notice that sequence execution continues with the next command in the sequence as soon as the field is set not when the field set point is achieved To wait for a stable magnetic field before executing the next command use the Wait command Set Temperature Sets the sample temperature Specify the temperature the rate and the mode O Fast Settle Controller will drive directly to the temperature and attempt to maintain the specified rate as closely as possible until the set point is reached A small amount of temperature overshoot can occur in this mode No Overshoot Controller will drive to each set point at the desired rate until it 1s close to the set point and will then slow the rate to avoid temperature overshoot This is intended for use with highly temperature hysteretic samples Notice that sequence execution continues with the next command i
10. an additional heater on the cryopump is discussed in section 4 5 Thermometers First stage thermometer monitors the temperature of the main radiation shield This temperature appears in the Cryostat Monitor as Shield and in MultiVu Log Data as Ist Stage Temp K Reads 45 K when the system is cold e Second stage thermometer monitors the temperature of the 4 K Plate This temperature appears in the Cryostat Monitor as 4K Plate and in MultiVu Log Data as 2nd Stage Temp K Reads 4 2 K when the system is cold e Magnet thermometer monitors the temperature of the magnet This temperature appears in the Cryostat Monitor as Magnet and in MultiVu Log Data as Magnet K In addition the MultiVu status bar displays the magnet temperature below the cryostat status Typically reads lt 0 1 K warmer than the second stage thermometer when the system is cold and magnet is not charging It may read much warmer during magnet charging Heaters First stage heater applies heat to the main radiation shield This heater power appears in MultiVu Log Data as Ist Stage Power W Second stage heater applies heat to the 4 K Plate This heater power appears next to the 4K Plate temperature in the Cryostat Monitor and in MultiVu Log Data as 2nd Stage Power W When the system is cold the first stage heater is off and the second stage heater is used to control the second stage thermomete
11. but you perform the measurement using electronics and software not provided by Quantum Design The techniques described below give you the ability to set and read temperature magnetic field and chamber state in order to automate this type of measurement In all cases you control DynaCool by sending commands to MultiVu You do not send commands directly to DynaCool hardware because operation of the hardware is orchestrated by software services on the computer see Sections 3 1 and 3 6 MultiVu provides an interface to send commands to these services see Figure 3 1 The sections describing techniques to control DynaCool are Section D 2 describes how you use WinWrap Visual Basic Scripting to control DynaCool and third party instruments e Section D 3 describes how you use National Instruments LabVIEW to control DynaCool Section D 4 describes how you use Microsoft Object Linking and Embedding to control DynaCool If you have questions about any of these techniques email apps qdusa com WinWrap Visual Basic Scripting in MultiVu WinWrap is a Visual Basic Scripting development environment integrated into MultiVu WinWrap uses the Visual Basic for Applications scripting language You open the WinWrap environment using the MultiVu menu item Sequence gt Advanced gt Edit Macro For more details about using WinWrap read Application Note 1070 209 Getting Started with Visual Basic Scripting in MultiVu available on t
12. flowing into the system when the KF flange is removed This is normal The next startup operation will evacuate and purge the loop automatically c Remove the pump exhaust filter assembly from the pump exhaust port by unscrewing the VCO nut The pump exhaust port is located on the side of the pump housing facing the rear of the system cabinet The correct VCO nut to loosen is shown as item 8 in Figure 5 3 d Remove the 4 1 4 20 nuts holding the SH110 in place and remove the pump from the cabinet 3 Replace the tip seals a With the pump on a bench follow the instruction provided for removing the old tip seals and installing the new ones Make a note of the hours the pump has been running There is a chronometer located near the power inlet It is useful to log when the tip seals are replaced to predict when future tip seal replacement will be necessary 4 Clean out the particulate filter The particulate filter is part of the pump exhaust filter assembly removed from the pump exhaust see Figure 5 3 a Remove the two hex socket screws from the filter top item 1 b Pull the filter bottom off item 2 while the filter assembly is in the upright position to avoid spilling the tip seal dust c Empty out the filter bottom and wipe clean You can use some Isopropyl alcohol if needed to wipe the trap clean d Examine the radial o ring on the trap top and make sure it is clean and free of defects If needed replace this o ring with
13. solid red indicates power from USB but no communications to PC solid green indicates power and communications to PC DATA rapid green flashing indicates low speed communications on CAN bus rapid red indicates higher speed communications In addition to the CAN network connectors located inside each of the CAN bays in the top of the module bay there are five additional 9 pin D sub connectors for connecting CAN devices Four are located on the back as shown in Figure 2 4 One is located on the front panel of the module bay see Figure 2 1 Two of these connectors on the back panel are dedicated to the DynaCool system one for communications to the top plate electronics and the other for the cabinet electronics Each of the 9 pin D sub connectors can provide regulated power 24 V for external CAN devices Fuses for this DC power are located on the module bay back panel as shown in Figure 2 4 Note that while some CAN devices like the cryostat top plate electronics use this power other devices like the pump cabinet have their own independent regulated power supply The CAN reset button is also located on the back panel as shown in Figure 2 4 Pressing this button recessed will cause all devices that listen for QD CAN reset to reboot The following devices do not listen to QD CAN reset and therefore must be reset separately Cryostat Controller Press the reset button on the back of the Pump Cabinet to reset the cryostat controller
14. Appendix B Event and Error Logging Diagnostic Software In case a problem occurs when you are not running Log Data the problem might be diagnosed using the background log Quantum Design personnel may ask you for this file if you report a problem with your instrument B 4 Event and Error Logging Three types of text based event and error logs exist on the DynaCool computer Quantum Design Service may ask you for these files to help diagnose problems with your instrument B 4 1 MultiVu Event Log The event log is a text file C QDDynaCool MultiVu Event log containing diagnostic messages generated by the instrument recorded with time stamps The file is arranged chronologically with the most recent events at the end of the file The event log is limited to 10 MB in size When this limit is reached the file is copied to Event log bak and a new Event log is created Events that require your immediate attention are displayed in dialogs by MultiVu These events are also recorded in the event log along with less important events B 4 2 Temperature Magnet and Cryostat Service Logs The Temperature Magnet and Cryostat Services all record details of their operation in a joint log file Like the event log this file is arranged chronologically with the most recent information at the end of the file The service logs are at C QDDynaCool System QdWapiLog_pg txt where is a number from 1 to 10 The system starts recording information in fil
15. CFE Flow SCCM Also a rough measure of the circulation pump outlet flow is reported as Pump Flow uncal SCCM When the chamber temperature is stable the main flow is selected to provide adequate cooling bias for the thermometer heater feedback loop Typically the main flow is a few hundred sccm when the chamber is stable and the annulus pressure is lt 10 Torr When the chamber temperature is ramping down quickly gt 5 10 K minute the main flow is typically set to its maximum value of 5000 sccm and the annulus pressure is 50 Torr due to the high flow through the circulation pump When combined with low temperature mode discussed in the next section DynaCool typically achieves cooling from 300 K to 1 9 K in lt 40 minutes When the chamber temperature is ramping down more slowly the main flow is set to intermediate values as required for the requested ramp rate When the chamber temperature is ramping up the main flow is set to a low value typically 150 sccm 4 3 2 3 LOW TEMPERATURE FLOW In order to circulate helium the circulation loop is configured as described in the previous section The low temperature flow system provides about 1000 sccm of 1 7 K helium gas to cool the sample chamber when it is below about 10 K In this mode the main flow is set to zero and 4 2 K liquid from the bucket is expanded through the capillary flow impedance The inlet of the impedance is at bucket pressure about one atmosphere and th
16. DynaCool great flexibility For many measurement options the puck is a sample holder that provides both thermal and electrical connections to the bottom of the sample chamber The Electrical Transport Option ETO is a good example of a measurement option that uses a puck in this way Other options such as the Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 11 November 2011 Section 2 3 Chapter 2 Measurement System Hardware Hardware Vibrating Sample Magnetometer VSM option use a specialized version of the puck that integrates portions of the measurement instrumentation directly in the puck assembly 5 0 cm MAXIMUM SAMPLE HEIGHT SOCKET 4 0 cm MAGNETIC FIELD CENTER SOLDER PAD SAMPLE INTERFACE BOTTOM VIEW Figure 2 10 Top and bottom views of a sample puck All the different measurement pucks have a common connector configuration for plugging into the sample chamber The puck is a 2 3 cm 0 91 inch diameter disk constructed of high conductivity copper for maintaining high thermal uniformity The puck is gold plated to prevent oxidation and in the simple configuration shown in the figure provides a surface on which samples can be mounted with good thermal contact When the puck is installed in the sample chamber the system block is mounted in the sample chamber block directly beneath the installed puck providing intimate thermal contact between sample and thermometer Measurement op
17. L Other explain COMMENTS 5 10 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Section 5 9 Maintenance and Servicing Required Maintenance Log Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 11 November 2011 Section 5 9 Chapter 5 Required Maintenance Log Maintenance and Servicing Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS 5 12 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Section 5 9 Maintenance and Servicing Required Maintenance Log Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 13 November 2011 Section 5 9 Chapter 5 Required Maintenance Log Maintenance and Servicing Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS 5 14 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapte
18. Main Menu Bar FILE File menu contains commands for opening closing and printing sequence files and data files for saving sequence files graph files and graph template files for generating new sequence files and for exporting data files to alternate formats EDIT Edit menu contains commands to edit sequence files It is not shown unless a sequence window is selected VIEW View menu allows you to show and hide the various components of the MultiVu graphical user interface and to open different types of data file windows graph view table view record view raw data view SAMPLE Sample menu helps you install remove and locate samples and enter sample properties that are recorded in the data file This menu is populated only when a measurement option is active SEQUENCE Sequence menu contains commands to control the execution of sequences and to access the underlying script for advanced sequence editing MEASURE Measure menu contains commands to control measurements executed by measurement options This menu is populated only when a measurement option is active GRAPH Graph menu helps you manipulate the appearance of data file graph windows INSTRUMENT Instrument menu contains commands to control the temperature magnetic field and atmosphere state of the sample chamber and to put the instrument into shutdown mode when unused UTILITIES Utilities menu contains commands to activate and configure measurement opti
19. Purging and sealing the sample chamber performs four cycles of pumping out most of the chamber gas and then filling it up with vent gas Finally the chamber is pumped down to a pressure that is appropriate for experiments that require exchange gas about 10 Torr Normally you purge and seal the chamber at room temperature after installing a sample in order to clean out atmospheric contaminants introduced while the chamber was open Vent and Seal Venting and sealing the sample chamber fills the chamber with helium vent gas and then seals the chamber This operation is useful when you want to conserve vent gas because vent gas will not flow out of the vent gas supply bottle once the vent valve is closed You can use this operation before opening up the sample chamber at room temperature in order to change samples PPMS DynaCool User s Manual 1307 110 Rev AO 4 15 November 2011 Section 4 6 Chapter 4 Case Vacuum System Theory of Operation Pump Continuous This operation uses the chamber case pump to evacuate the sample chamber The flush and chamber isolation valves remain open and the pump remains on indefinitely Vent Continuous This operation also known as flooding fills the chamber with helium vent gas and does not seal the chamber Because the flow of vent gas is continuous this operation minimizes the amount of air that enters the chamber Be careful not to leave the system in this state for too long because doing so will em
20. The cryogenic sample chamber wiring running from near the sample chamber access port see Figure 2 1 down the outer wall along the length of the sample chamber to the block at the bottom of the sample chamber The vacuum tight electrical feedthrough at the bottom of the sample chamber The puck connector which plugs into the opposite side of the vacuum tight feedthrough at the bottom of the chamber See Appendix C for a pin out diagram of the puck wiring 2 3 8 CAN Modules Measurement electronics are contained within modular electronic housings commonly called CAN modules A typical CAN module is shown in Figure 2 15 Connections to measurement hardware are made on the front panel which is shown in the figure 2 16 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Section 2 3 Chapter 2 Hardware Measurement System Hardware s E i d d Oo Q s FA v DO 7 jjoe 7 e ites wa wow t Figure 2 15 Typical CAN module with Front panel right The 9 pin QD CAN D shell connector on the bottom panel Figure 2 16 of the modules connects to power CAN and synchronization lines in the module bay described in Section 2 2 2 GUIDE HOLE QD CAN CONNECTOR ADDRESS SELECTOR Figure 2 16 Rear panel of a typical CAN module CAN modules communicate with PC other system components e g chamber vacuum gauge and each other via the CAN system network Section 2 2 2 2 describes this in more deta
21. Theory of Operation Cryostat Control System 4 2 1 Pulse tube cryocooler The pulse tube cryocooler provides all of the cooling necessary for operation of PPMS DynaCool No liquid cryogens are required The pulse tube cryocooler has two cooling stages The first stage typically runs at 45 K while the second stage typically runs at 4 2 K The components cooled by the two stages are listed below These components are discussed in more detail later in this chapter Cooled by First Stage Main radiation shield Annulus radiation shield First stage of cryopump Electrical wiring heat loads coming from room temperature Mechanical support heat loads coming from room temperature Cooled by Second Stage 4 K plate Superconducting magnet Helium gas and liquid for sample chamber cooling e Second stage of cryopump Electrical wiring heat loads coming from first stage temperature e Mechanical support heat loads coming from first stage temperature Unlike many cryocooled systems the pulse tube cryocooler in DynaCool is not mounted in vacuum and is not coupled to any cryostat components via solid links Instead the cryocooler resides in helium gas in a cryogenic tank usually called the bucket The main radiation shield is cooled by conduction through a small gas gap to the first stage of the cryocooler and other first stage components are cooled by solid contact to the main radiation shield The 4 K Plate is cooled by contact with approxim
22. a programmed sequence or script The PPMS DynaCool comes equipped with either a 9 T or 14 T conduction cooled superconducting switch less magnet system This system includes a hybrid digital analog magnet controller designed for precise quiet control of the magnetic field The bipolar design also allows smooth continuous ramping through zero field Magnet control software monitors the temperature of the magnet and cryostat at 3 locations to ensure proper operation of the magnet system and avoid time consuming quenches The PPMS DynaCool has a built in magnetic shield For a system with a 9 T magnet this shield maintains the 5 gauss line lt 30 cm the surface of the cryostat cabinet allowing the system to be installed closer to other sensitive instruments for better lab space utilization 1 3 How to use this Manual This user manual is organized from front to back with broad review of features in the front and in depth description of details toward the back If you are familiar with PPMS type systems the first chapter may be all you need to get started with measurements However all users should read the first 3 chapters of this manual for proper working knowledge of the basic system features Chapter 4 contains an in depth description of the theory of operation Chapter 5 covers routine maintenance and servicing procedures 1 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 1 Section 1 4 Getting Start
23. and allows you to use one LabVIEW station with different instruments For more information about this technique consult the Application Note 1070 210 Interfacing LabVIEW Programs with Quantum Design Instruments available on the Quantum Design website http www qdusa com Quantum Design s support of LabVIEW is limited to the VIs controlling the Quantum Design instrument Quantum Design does not provide LabVIEW software itself or support controlling third party instruments using LabVIEW Many third party instrument providers supply LabVIEW VIs to allow you control their instruments from LabVIEW See the National Instruments website for information about LabVIEW http www ni com labview Object Linking and Embedding ActiveX MultiVu acts as an Object Linking and Embedding OLE server so it can be controlled from any program or programming language that can act as an OLE client Examples include Microsoft Excel all Microsoft Visual Studio languages such Visual Basic C and C as well as Embarcadero Delphi formerly known as Borland Delphi If you are a capable programmer and want to control third party instruments from your programming language of choice you may want to use this technique This technique is for advanced users only and Quantum Design does not support any of the third party development environments that you would use to implement an OLE client Note that the techniques described in the above sections us
24. b Gray Lemo connector BOTTOM VIEW Figure C 1 Sample connections a Sample puck b Gray Lemo connector Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO C 1 November 2011 Section C 3 Temperature Control C 3 Appendix C Pin out and Interconnect Diagrams Table C 1 Sample Puck Connections SAMPLE LEMO PUCK CONNECTOR Ce a a ee a a i a 7 JQP 8 SAMPLE D SHELL TYPICAL CONNECTOR FUNCTION 7 z2 10 z i 2 7 Z z 5 Temperature Control JQP 9 This connector is located under the cosmetic cryostat covers at the top of the sample chamber on the left side when facing DynaCool from the front The spare thermometer and heater are not connected The Serial Com connections are used to read thermometer calibration data and other configuration information from the sample chamber p N OUA aAa E a a i ee o E AR E a E EEA a a A ase wl A A S A PON DN LN IN FN LON FON ON LO EN FS pI NE fae EN igi GO Pe RN PR A Cl K 2 S KAKEKEH7HE HS MIO Da 2K SHI4H1 S i CSHIZHISHIZHITHIOKS HBH 7THEKSR4HSGHZEH 1 A EA i od a tN A ia a BEET N G Na GY SN na I Bn NS Nie CE BES NS A a a AMPA a A a EN lie A a ey Oh A TA SO ON E E a E E N E a e a e a H OH J SHO Z H HI QHD L ZOH SHO RY O BH RHI ALH Bu UO WOO OS 7 f LETHE HOOK POLIO MRO HEHE HS BS Ae a Aa a ae Be Aras Ue CEA ae zH ZAMS SHS Alicea 2K OA THA DMA B44 AAA IHA OKZ HBH Z TZ BBE GAYS UZ ONG D t A E
25. below to change the helium gas supply cylinder 1 Close the needle valve Use two 3 4 1inch box wrenches or two adjustable crescent wrenches to disconnect the helium gas transfer hose from the supply cylinder at the double sealing connector shown in Figure 5 1 Use one wrench to hold the male fitting on the regulator fitting stationary while using the other wrench to loosen the female fitting Only open the double sealing connection leave all the other joints sealed Do not change the setting on the regulator Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 1 November 2011 Section 5 2 Chapter 5 Changing the Helium Gas Supply Chamber Maintenance and Servicing bottle Valve cylinder fitting WE CGA 580 set pressure to 19 psi leak check using soapy hold stationary water here loosen here we needle helium supply hose Figure 5 1 Helium gas supply cylinder and regulator 2 Close the bottle valve and remove the regulator from the empty cylinder and connect it to the new cylinder Make sure the cylinder fitting is tight and that the sealing surfaces of the fitting are clean and undamaged 3 With the needle valve still closed open the bottle valve on the new cylinder and leak check the cylinder fitting using soapy water Because a typical cylinder of gas will remain in service for an extended period it is important to make sure the fittings are leak tight Even small leaks a
26. bottle and regulator This port provides helium gas for sample chamber venting and purging operations It also provides gas for charging the helium circulation loop Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 November 2011 Section 2 2 Chapter 2 System Hardware Components Hardware 2 2 3 2 BACK PANEL AND CABINET BAYS F Fi vad computer r breakers magnet power A module bay amp computer supply bay a magnet 12 amp l 4 magnet 10 amp amp cabinet A s main q magnet leads pump amp gas handling bay AC main power inlet to cryostat to module bay Figure 2 6 Back view of Pump Cabinet Figure 2 6 shows the back of the cabinet and the various connections The open bay at the top contains the PC AC power 240 VAC is provided to the PC monitor and other peripherals using the four IEC C13 female connectors in the side of the computer bay The computer is mounted to a metal sliding drawer assembly To access connectors on the backside of the computer it may be necessary to remove the screws holding this drawer assembly onto the black plastic rails that are attached to the floor of the computer bay Alternatively remove the front panel from the cabinet to access the rear of the computer Below the open computer bay is the covered magnet controller bay The power supply gets AC power and CAN network connectivity from connectors in the side of the bay The magnet
27. by clicking Open Sequence B or selecting the menu item File gt Open gt Sequence You will be prompted to locate the file you want to open The top of the sequence window shows the sequence file name An asterisk symbol after the file name means the sequence has changed since last time the file was saved Sequences must be saved before you run them Save a sequence file by clicking Save Sequence El or selecting the menu item File Save If not already assigned you will be prompted for a location and file name Add a command to the selected sequence by double clicking the command in the sequence command bar The new command is inserted above the highlighted command in the selected sequence window You will first be presented with a pop up window to fill in command specific information Then a summary of the command will appear in the sequence window More detail about each available sequence command is found at the end of this section Remove and reorganize sequence commands by highlighting them in the sequence window and using the Cut Copy Paste Delete and Undo commands in the Edit menu Disable commands in a sequence file without deleting them using Edit gt Disable Enable a disabled command with Edit gt Enable Figure 3 9 A disabled command will be skipped during sequence execution Disabled commands are preceded by an exclamation mark symbo
28. current leads and magnet signal cable pass through the side notch on bay cover on the left of Figure 2 6 The easiest way to gain access to the power supply bay is by removing the panel on the front side of the cabinet rather than the rear panel Below the magnet controller bay is the main AC power distribution panel with the main power inlet and breaker along with 4 sub system breakers From left to right the sub system breakers are MODULE BAY AND COMPUTER This 10 Amp breaker switches the power to the outlets in the computer bay and also the AC power line supplying the module bay Do not use this breaker to turn off the power to the module bay since you will lose power to the computer Instead use the power switch on the back of the module bay for this see Figure 2 4 MAG PWR 12 A This 12 Amp breaker switches power to the large IEC C19 connector below the magnet controller bay This is usually used only for 14 T DynaCool systems MAG PWR 10 A This 10 A breaker switches power to the IEC C13 connector inside the magnet controller bay This is usually used for 9 T DynaCool systems 2 8 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Section 2 2 Hardware System Hardware Components CABINET This 10 A breaker switches the power to the pumps and gas handling instruments inside the pump amp gas handling bay in the bottom of the cabinet It also switches power to the control electronics
29. eg RN A A I TY ge y E E at RN ee r oe ge SG a N f Male Pin Female Socket Figure C 2 44 pin D Shell pin and socket layout PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Appendix C Pin out and Interconnect Diagrams Quantum Design Table C 2 JQP 9 Temperature Control Connections 1 Block Thermometer I 5 Beamon 2 secon ve PIN FUNCTION 1 PPMS DynaCool User s Manual 1307 110 Rev AO November 2011 Section C 3 Temperature Control C 3 Section C 4 Appendix C Cryostat Temperature Control JQP 7 Pin out and Interconnect Diagrams C 4 Cryostat Temperature Control JQP 7 This connector is located under the cryostat cosmetic covers on the top plate of the cryostat to the left of the sample chamber when facing DynaCool from the front The Serial Com connections are used to read thermometer calibration data magnet configuration data and other cryostat configuration information See Figure C 2 for connector diagrams Table C 3 JQP 7Cryostat Temperature Control Weare Torone C 4 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 A P P EN DIX D Using Third party Instruments D 1 D 2 Overview This chapter describes three ways to interface with DynaCool when using third party instruments You use one of these techniques when you want to use DynaCool to control temperature magnetic field and chamber atmosphere
30. helium cycle for the pulse tube cooler in the cryostat Itis connected to the cryostat by the two high pressure helium hoses and the cold head power cable Itis connected to the pump cabinet by a serial cable Start and stop operations are controlled remotely over the serial cable and so it is not necessary to have direct access to the compressor except for maintenance or service This makes it possible to locate the compressor remotely up to 100 feet away in a location that has access to cooling water and 3 phase power This can also provide a degree of sound isolation between the laboratory space and the relatively noisy compressor The DynaCool system is designed to operate continuously between compressor maintenance cycles which should be regularly scheduled for every 20 000 operating hours A timer is located on the front of the compressor to help you track when you will need to schedule equipment maintenance It is important to adhere to the maintenance schedule and to facilitate this we have provided a maintenance log in Chapter 5 WARNING The cryocooler system can be seriously damaged if the required servicing is not performed Other system components also should be serviced at the same time as the compressor Only qualified Quantum Design service personnel should perform maintenance work on the cryocooler Contact your Quantum Design service representative to schedule maintenance on the cryocooler Please refer to the Cryomech
31. is described in section 4 6 The second stage components at 4 2 K are protected from room temperature thermal radiation by the main radiation shield Room temperature radiation is absorbed by the main radiation shield and the resulting heat load is conducted through the shield and then to the first stage of the pulse tube cryocooler The radiation heat load on the main radiation shield is reduced by wrapping it in reflective multi layer insulation The sample chamber and cooling annulus that surrounds it vary in temperature from lt 1 8 K to 400 K Because the cooling annulus is inside the bore of the superconducting magnet it would present a very large radiation heat load on the magnet when the chamber is at 400 K In order to prevent this the annulus radiation shield surrounds the cooling annulus without touching either the annulus or superconducting magnet bore The annulus radiation shield is connected to the main radiation shield Thermal radiation from the cooling annulus that shines on the annulus radiation shield is conducted up the annulus shield to the main shield and from there to the first stage of the pulse tube cryocooler This maintains the annulus radiation shield at low enough temperature lt 100 K that it does not present a significant radiation heat load to the magnet bore Monitoring and control In order to monitor and control the cryostat DynaCool includes three cryostat thermometers and two cryostat heaters
32. is difficult to move due to low pressure in the chamber 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 PPMS DynaCool User s Manual 1307 110 Rev AO 1 7 November 2011 Section 1 5 Chapter 1 Installing and Removing Samples Getting Started 11 Gently lower the sample insertion tool into the sample chamber puck end first until the sample puck touches the puck connector at the bottom of the chamber Do not force the puck down farther once it touches the connector 12 Rotate the sample insertion tool slowly until the key on the puck drops into the indexing notch When the puck drops into the notch you feel the puck lock into position 13 Gently push down on the sample insertion tool in order to engage the puck interface and to make solid electrical contact between the interface and the puck WARNING Do not use excessive force when engaging the puck interface The need for excessive force may indicate a problem such as a misaligned puck If you push hard you may bend the pins at the bottom of the sample chamber 14 Disengage the sample insertion tool and then raise the tool several centimeters Be sure there is no resistance when you raise the insertion tool Resistance indicates the puck may have gotten caught in the tool as you began lifting it out and you may thus need to remove th
33. loop fill at room temperature or with circulation during the condense operation The DynaCool sample chamber resides inside the annulus tube as shown in Figure 4 1 The space between the sample chamber and annulus tube is called the cooling annulus When the circulation loop is set to Circulating helium flows up the cooling annulus in order to cool the sample chamber and provide a bias of cooling power for temperature control The cooling helium flow is driven by the pressure difference between the cooling annulus and the bucket The cooling annulus is maintained at moderate vacuum by the circulation pump The bucket is maintained near 1 atmosphere by controlling the 4 K plate at 4 2 K as discussed in section 4 2 3 The exhausted helium from the circulation pump is returned to the bucket where it is cooled by the cryocooler and reused for sample chamber cooling Two cooling flow modes are available in DynaCool main flow through the counter flow heat exchanger and low temperature flow through the impedance In addition the circulation loop has 4 6 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Section 4 3 Theory of Operation Chamber Temperature Control System special modes that allow it to be charged with clean helium during system startup All of these modes are discussed below 4 3 2 1 LOOP PURGE DURING SYSTEM STARTUP During system startup the circulation loop is purged with clean helium
34. maintenance the front and side panels of the cabinet can be removed Most of the panels are held on using ball studs These can be removed by simply pulling the panel outward For safety reasons some panels require remove of screws These screws are clearly exposed on the relevant panel surfaces WARNING You should not operate the cabinet for more than a few minutes at a time with panels removed since the panels are critical for proper air cooling of all the components in the cabinet 2 2 3 1 GAS HANDLING CONNECTIONS The right side of the cabinet see Figure 2 5 contains a bulkhead connector for 4 stainless flexible hoses with face sealing VCO style fittings These hoses are as follows Annulus Pumping Line This large hose goes to the inlet of the Circulation Pump in the cabinet and carries the return flow of the circulation loop that cools the sample chamber Return Line This hose sends the circulating helium from the circulation pump back to the cryostat to complete the helium circulation Chamber Case Line This hose connects the chamber case pump and manifold in the cabinet with the sample chamber and manifold in the cryostat Under normal operating conditions this line enables venting pumping and purging of the sample chamber During system startup and other maintenance operations this line is also used to purge and evacuate the cryostat vacuum case Helium Bottle Line This hose is connected to the Helium gas supply
35. see Figure 3 7 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 3 Software Section 3 2 MultiVu 3 2 8 1 STATUS INFORMATION The right panel of the monitor shows information about the internal workings of the cryostat system Refer to Chapter 4 for a description of the cryostat architecture and theory of operation Cryostat State Machine Status The display box at the top of the status panel in Figure 3 8 shows the current cryostat state or mode example Cold Cryostat This is a slightly more detailed version of the status shown in the Cryostat and Cryocooler panel in Figure 3 7 The normal operational state when cold is Cold Cryostat however during warm up startup or other operations the cryostat state machine will pass through many other states Cryocooler Shows the status of the cryocooler system indicating compressor running or not running as well as compressor errors Magnet Shows the temperature of the magnet as well as the magnet state machine status 4 K Plate Shows the temperature of the 4 K plate as well as the second stage heater power required to maintain a constant temperature at the 4 K plate Shield Shows the temperature of the radiation shield that is anchored to the first stage of the cooler Loop Shows the circulation loop pressure as measured at the outlet of the circulation pump This pressure corresponds to the vapor pressure of th
36. supply in cabinet Figure 2 4 CAN Module Bay back panel The module bay gets 240 VAC main power from the Cabinet This is used for the 24 volts regulated power supply which provides power for the CAN module bay One spare 240 VAC outlet is provided on both the front and back panels of the module bay These are for connecting external options that require AC power Turning off the power to the Module bay using the power switch shown at lower right in Figure 2 will turn off power to the modules in the bay and the top plate electronics chamber vacuum gauge and cryostat utility controller located on the cryostat top plate under the cryostat cover It will also turn off the power to any optional devices that get their power directly from one of the CAN connectors on the module bay 2 4 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Hardware Section 2 2 System Hardware Components 2 2 2 2 CAN NETWORK CONTROLLER AND DISTRIBUTION 2 2 2 3 The module bay also contains the CAN network controller This is a device enabling communications between the PC and all of the devices on the CAN network The back panel of the module bay Figure 2 4 shows the CAN network controller and associated connections A USB cable from the computer provides power and communications to the network controller A pair of indicator lights above the USB connector can indicate the status of the CAN network controller PWR
37. that the system has gone into the Recover Cooling event and is currently attempting to recover cooling power from a magnet over temperature event This recovery state 1s meant to prevent a magnet quench by providing enhanced cooling power to the magnet to allow it to fully discharge This recovery state should exit automatically when magnet charging is safe again If the system fails to automatically recover cooling you can use this operation to regain control of the cryostat Instrument Utility Tools Under the menu item Utilities gt Tools gt you access utility programs that may be used for maintenance operations For example there is a Version utility that will report all the current DynaCool software version numbers for troubleshooting or upgrading There is also a CryoMon program which shows a diagram representation of the DynaCool cryogenics and gas handling system along with live sensor readings PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Software Section 3 3 Measurement Options 3 3 Measurement Options Most measurements in DynaCool require the use of measurement option software You do not use a measurement option if you provide the measurement electronics but all measurements provided by Quantum Design require option software to be active For details on the process of setting up a measurement option see the relevant option manual In order to activate an opti
38. the replacement in the kit Apply a small amount of M grease to the new o ring prior to installation e Press the filter bottom back in place and tighten the two hex socket screws 5 Reinstall the pump into the System cabinet a Place the pump back on the 4 vibration mounts and secure with the lock washers and nuts you removed in step 2 b Re connect the pump inlet hose to the pump inlet Make sure the KF 25 o ring is clean before making the joint c Re connect the exhaust filter assembly to the pump exhaust Make sure the VCO o ring is clean before making this joint The VCO nut should be turned 1 8 of a turn past finger tight to make sure it does not come loose 5 4 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Section 5 5 Maintenance and Servicing Replacing Fuses and Resetting Breakers 5 4 SP 5 5 1 Inspecting and Maintaining O rings O rings require regular inspection and lubrication The only O ring that you regularly encounter in DynaCool is the one on the sample chamber KF flange Be sure to maintain this O ring as described below In addition if you service any other parts of the system be sure to inspect and lubricate O rings you encounter during servicing as well Whenever you see an O ring take the time to visually inspect it If it appears dirty clean it with a lint free cloth Replace O rings that are cracked If the O ring is dry apply a small amount of sili
39. 1 22 System Hard ware OMpPONe mts seen T NE 2 1 PPA CryGStal ASSO DIY ian A a a noneae une tauren ene atdaaes 2 2 22D CAN Mod le hs oe a a eae a rg te ede aed oD eal a tae et east 2 3 2 2 2 1 CAN Power Supply and Power Distribution s cccicccccccccenccssoccssavevsassorevieesenerna sciceccesavesiacaedsheveaeias 2 4 2222 AN INetwork Controller and Dist DUtOl tii ncssccnnccsetanisacsescuadss tensesnaasenadertivasedsmanadastusnngmateeandes 2 5 222 0 M gnet Sinal Dist DUM OM aese a O E 2 5 Z2 Pomp Capiniet and COMDT nat a A tacts 2 6 2254 Gas Hand hie C onnections sesei oe E E ET E E E 2 7 D232 Dack Panel and Cabinet Bayssac aa E 2 8 2 2 4 Cryocooler C OMPrES sor ASSeMmOly sca c dest corer a A daa neees 2 10 225 Helium Gas Bottle and Regulator iiss se coc an tees ce dea ae tends dec wevetentdus sce tues acdeaansi sd cent eee tcadtseedeceneass 2 11 2 3 Measurement System el at WALG coason a EE scancquannas EE AS 2 11 Zol Sample PUCK Seine e E T a aeus ce 2 11 Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO jii November 2011 Contents Table of Contents 2 3 2 PUTAS et roi POO dss as gs5e Saou satis saan tiys aspen asta a oa A 2 12 IA Ah Sample Chamber Access Port and Chamber Baffles 0 ccccccccccccsssssssseseseeeeeeeeeeeeeeeeeeaeaeeennees 2 13 2 3 4 CVOPDUDI aea EE E E eth dunaske cen vocncn hana ker teutt 2 14 25 Pack AGUS tite tt POON 6 sleet a haute alte ede cc ieee de hend sie tte erence a tate eateia st aeced 2 14 2
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41. 3 6 Puck Wirm Lest SUA Oli xccrassatetisccantbesentimas EE Ea 2 15 Zal EX Perinicne PUCK WATING ear E 2 16 2 3 8 CAN Modules cercon en AE dee Yendgyusestonaviayiadesdausiauedenieyecactunavtevicdestaauh ues ewenseeee 2 16 CHAPTER 3 SIARA D K ENEE E A E A E E A E E E E TEE E E 3 1 3 1 ODN SUVS Wr recat acta eee et teens mies ence ect eaten abreast em ice en eteetsec E 3 1 Diels MUMU enean a E ee E 3 2 3 2 1 Ment B ai reroror rana TNT TOO TE E T ONNA 3 3 3 2 2 TOOL BAT carana AA E E E sQenaseetantaadie 3 4 3 2 3 CONTO kt Grolal fol gereeemcnree rere eee eee Meroe rere A ete Hanae ters ent tier Sent ren eee areeeeereeeee 3 4 3 2 4 Scgucnce Command Barens N a a an a r a a a a chats 3 4 3 2 5 SAW Baisa N NE OE mw EI OE ec eu eco tee nenc O O 3 5 3 2 6 SEduenNee W Mdo W aee a A N 3 5 3 2 7 Data Windows Graph Record and Table View Sarsecinicasin ai a S a 3 6 3 2 8 Cryostat Montor DAOS are e a E E E E EE 3 6 ILOA SUSO Ooae oa eaa ON TENE EO TE 3 7 S202 LIV C OnToNT ASKS sara a a a ncaa wate cts tea ae rae aca 3 7 3 2 9 stament Uly TOO Soca rescaled taal cnet eee eal 3 8 3 3 IMIG ASUPCIMETIL ODU ONS erpe n A Sesslverior A savas T E EA 3 9 3 4 DS ELE T CS E A E ENEP E N E T OE EE NATE E E E E EEE O E EEE 3 10 3 4 1 Edino GUC IC e oh a E AE 3 10 3 4 2 Advanced SCPC E TON oaa a a A 3 11 3 4 3 Runnin a SCQUEICES aeeie p a T E E E E EO 3 11 3 4 4 Locking SEQUenCe Ex COU MON essare as tuestslacnet neni sdsuiai sh aobanian catenss Lioenseleddeacashtabasnonenels
42. 40 VAC power to the AC IEC C13 connectors on the front and rear panels In order to turn on this power push both sides of this breaker to the up position Shutting Down the DynaCool System If you will not be using the system for an extended period of time or you have to shut it down for maintenance such as power or water outages or scroll pump maintenance Section 5 2 2 follow the procedures in Section 3 3 8 2 Cryostat Control Tasks to Shutdown the system Once the system has shut itself down 8 16 hours you may turn off the power to the cabinet PPMS DynaCool User s Manual 1307 110 Rev AO 5 7 November 2011 Section 5 9 Chapter 5 Required Maintenance Log Maintenance and Servicing 5 7 Starting up a Cold DynaCool System For starting up the system see Section 3 2 8 2 Cryostat Control Tasks for the Startup procedure 5 8 Compressor Adsorber Replacement The adsorber in the compressor has to be replaced every 20 000 hours Please refer to the Routine Maintenance section in the supplied Cryomech manual for detailed instructions on this procedure WARNING The cryocooler system can be seriously damaged if the required servicing is not performed Other system components also should be serviced at the same time as the compressor Only qualified Quantum Design service personnel should perform maintenance work on the cryocooler Contact your Quantum Design service representative to schedule maintenance on the
43. CAN terminator dongle to JQQ 3 CAN OUT Figure 2 7 Attach cryostat valve and flow control cable to JQQ 6 Figure 2 7 Attach cryostat thermometer amp heater control cable to JQQ2 Figure 2 7 Attach USB cable in the tether to the rear facing port on the computer Attach the CAN network IN cable from the module bay to JQQ 4 Figure 2 7 Connect computer display and devices A 3 6 Mount and Connect the CAN Module Bay L E EN e 10 11 Quantum Design Remove the 4 thumb screws from side of the CAN module bay and carefully hang the bay on the mounting bracket on bracket at the right side of the cryostat The two shoulder screws on the CAN module bay will engage the notches in the cryostat mounting bracket Attach the grounding strap from the cryostat shield to the CAN module bay using the first of the four thumbscrews Use the upper rear tapped hole for this This thumbscrew also holds the module bay to the bracket Install the remaining three thumbscrews to secure the module bay At the back panel of the module bay attach the cable from the magnet power supply to JQR 6 Figure 2 4 Attach the CAN cable from the cabinet to JQR 1 Figure 2 4 Attach USB cable from the computer to JQ5 5 Figure 2 4 Attach the CAN cable from the cryostat to JQR 2 Figure 2 4 Secure the cables at the back of the module bay using the Velcro strap Connect the magnet cable from the cryostat to JQR 7 Figure 2 4 Connec
44. Measurement Commands HE Record 974 of HgSuperconductimity ws Field Name Field Value 1 Time Stamo seconds relativ 5090 351 Z Temperature K 3 5298352241516 3 Field De 99 9373474121094 B Phase Angle Ch deg fa Frequency Ch2 Hz Averaging Time Ch2 s sfa 10 JOC Curent Ch m 0 13 J Quadkeature Vokag e Che a Ganch Ch2 15d 2nd Hamoric Ch2 2 75 325 3 75 426 JE 3rd Harmonic Ch fv Temperature KK de Status Code Sequences Idle 246 47 KfStable i Seq lt none gt lt ne 10 00 K rranf Fast Settle i 2A ad Status Bar Sequence Window Data Window Data Window graph view record view Figure 3 2 MultiVu Main Window 3 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Software 3 2 1 Quantum Design Section 3 2 MultiVu The main MultiVu window is shown above This window displays essential status information about the instrument and allows control of the instrument with simple mouse click commands The tool bar control center sequence command bar and status bar may each be docked and un docked by double clicking any non control region or by dragging them around the main window They may also each be hidden using the View menu Menu Bar The Menu Bar contains menus for accessing all fundamental software features File Edit View Sample Sequence Measure Graph Instrument Utilities Window Help Figure 3 3
45. OL CONFIGURATIONS DynaCool provides a configurable temperature control platform to allow a measurement option to control on a thermometer close to the sample and or extend the temperature control range The following control configurations are available Base Configuration This configuration is used when no measurement option is active or when the measurement option provides no additional thermometers In this mode the Measurement Temperature Sample Temperature Control Temperature and Block Temperature all report the value of the block thermometer Measurement configurations that use this mode include Control Measurement Control Sample Measurement Configuration Thermometer Thermometer Thermometer Electro Transport or Resistivity 1 8 400 K User measurements Block Block Block with no additional Thermometer Thermometer Thermometer thermometer Block Block Block Thermometer Thermometer Thermometer Base Configuration with Measurement Option Thermometer This configuration is used when the measurement option provides a thermometer close to the sample that is used to measure the sample temperature but the control system does not use this thermometer In this mode the Sample Temperature Control Temperature and Block Temperature all report the value of the block thermometer The Measurement Temperature reports the value of the measurement option thermometer Measurement configurations that use this mode include Quantum Desi
46. Pump Cabinet and Cryostat ccccccccccccccccecceeeeseeeeeseeeeeeeeeeeeeeeeeeeaaaaeeeneees 1 1 Cryostat monitor status panel showing Cold CryOStat ccccccccccccccecceceeeeeseesseseeeeeceeeeeeeeeaeaaeeeensees 1 4 Example OL AUC eaae aE sc es esa seb AAEE la bdeds ines EAE O acces Useueaats 1 5 Operat onor puck 11SemiOn OG lhccsscetei tans a e a 1 6 Puck insertion tool Connecnne 10 puck iio wees eat alee ated bets teehee eee 1 6 PRONE VIEW Ol Cly Osta E E E E E A T ates dautwanacantasart E A AE 2 2 Back Dase UL Cly OSlAL erenn E E A a 2 3 CAN Module Bay and sample puck wiring port gray Lemo ssseseeeeeeessssssssssssssseerrerssssssssssssse 2 3 CAN Module Bay Dack pane leargas stat gter steeds atalansataatnanetiinatos ucatdes 2 4 FONE VIEW OL Pump C ADIL css Pucdieashutoutans sieve tttnctiewentuedioa e tocdidiweutaa taudenscewaenceeuertuade 2 6 Back Wiew Ol PUMP CaDINel st tars cowstat sbasdei sed AE R E E E T e del boa uaakemoauraanes 2 8 Connectors to the Cryostat Controller electronics on the back of the Pump Cabinet 2 9 Henum Compressor siti street ot le ce Rita ices ec eel aed en Si oleate al ene Clean alRekit cee Sone 2 10 Helin Cas DOLE will FeO UIALON certea oon ae r A E vend 2 11 Top and bottom views of a sample DUCK see wesc ecisdascucenerccsessay eyes ese eats ieee ae saesat eee seat see 2 12 Puck Insertion Tool with Level in Engaged Position cccccccccccccccecssssssseeseeeeeeceeeeeeeeeeeeaeeasaaeeee
47. Quantum Design Physical Property Measurement System DynaCool User s Manual Part Number 1307 110 AO Quantum Design 6325 Lusk Boulevard San Diego CA 92121 3733 USA Technical support 858 481 4400 800 289 6996 Fax 858 481 7410 First edition of manual completed November 2011 Trademarks Two tau model is a trademark of Quantum Design Other product and company names appearing in this manual are trademarks or registered trademarks of their respective holders U S Patents 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 5 798 641 Torque Magnetometer Utilizing Integrated Piezoresistive Levers Other Patents Pending C ONTENTS Table of Contents PREFACE Contents Conventions and Safety eseseseesosesesessercsoseseseseoeoscsesesesrororoseseseseoroseroseseseororesoseseseororeseseses xi P 1 VEIN IOW aaie E OE E E dts iieeeunuaadeecenanuaneendnetenes xi P2 SCOPE OLNE Mamia ber se sanndie ac ead aetaletaaionoetes aasavo tiesneetabare seansens eas banedeeaa mateentaneeet xi Ro Conventions mine Minaka a a a dea dameatel uate eeadeacmetv nee vasemean uauens teed xi P 4 Safety Guidelines and Regulatory Information 20 0 0 ccccccccccssssseeseeseeeeceeeeeeeeeeeaaaaasessessseseeeeeeeeeeeeeeaaaas xii CHAPTER 1 Getin Sarte aasisss case dspasuctnccaveneseanavetvsaciened
48. Records specified diagnostic data to a data file at a specified rate No size limit is imposed on the data file generated so the data file can get extremely large and difficult or slow to process See Appendix B for more information on logging diagnostic data Sigma Log Data Records specified diagnostic data to a data file at a specified rate This command is similar to the Log Data command except that it allows you to record statistics such as a running average and standard deviation for each data item in each data record It may generate large data files with large header sections See Appendix B for more information on logging diagnostic data Measurement Option Commands If a measurement option is active an additional branch will be present populated with sequence measurement commands See the appropriate option manual for instructions on how to use these commands Graphing Data Files The graph view is the default for viewing data files Any data file with one or more data records may be opened in a graph view The appearance of graph views may be manipulated extensively to aid data analysis Open a data file to graph by clicking Open Data File by selecting File gt Open gt Datafile or on the control center click View to open the current data file PPMS DynaCool User s Manual 1307 110 Rev AO 3 15 November 2011 Section 3 5 Chapter 3 Graphing Data Files Software 3 5 1 Data Selection and Plot Axes
49. Rev AO 2 13 November 2011 Section 2 3 Chapter 2 Measurement System Hardware Hardware Before setting a temperature below 295 K you should always be sure that the sample chamber is sealed and contains only clean gas Normally you do this by executing a purge and seal operation after sealing the KF flange at room temperature Failure to do so can cause contaminants to freeze inside the sample chamber causing problems with many experiments Measurement options provide sample installation wizards that perform chamber operations at the appropriate times when installing samples WARNING Be sure to properly seal the sample chamber KF flange before setting temperatures below 295 K Failure to do so will cause ice to build up in the chamber a condition that is hazardous and may damage the DynaCool sample chamber due to excessive pressures resulting from an ice plug Even a small leak can cause ice to build up SO be sure to keep the KF flange surfaces clean and to not damage the O ring used to seal the flange 2 3 4 Cryopump The cryopump is used to achieve high vacuum in the sample chamber typically lt 10 Torr This is necessary for options like Heat Capacity and VSM Oven to provide thermal isolation between the sample and the chamber The cryopump is permanently mounted in the cryostat vacuum case and is controlled automatically by the system software Cryopumping is achieved by exposing the sample chamber volume to a multi stage cry
50. Sample Temperature reports the value of the extended range control thermometer The Control Temperature is either the Block Temperature or an additional option thermometer The Measurement Temperature reports the value of the measurement option thermometer Measurement configurations that use this mode include Measurement Control Sample Measurement Control Configuration Thermometer Thermometer Thermometer Therm ID Dilution Block Refrigerator Platform 643 Thermometer Sample Thermometer Thermometer Heat Capacity with Dilution Refrigerator Block Thermometer or Helium 3 Heat e apacity Helium 3 Sample Mattom 643 or 655 655 with Helium 3 Thermometer Sample Thermometer Thermometer The Helium 3 Refrigerator sets the block thermometer as the control thermometer in low temperature control modes and sets the Helium 3 sample thermometer as the control thermometer in high temperature control modes Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 11 November 2011 Section 4 4 Chapter 4 Magnetic Field Control System Theory of Operation 4 4 Magnetic Field Control System The magnetic field control system consists of the superconducting magnet and leads the magnet controller software and the magnet shield 4 4 1 Magnet and Leads The magnetic field in DynaCool is generated by a superconducting solenoid mounted in the cryostat vacuum space The magnet generates a vertical magnetic field Typical currents at ma
51. To do this the gas handling system is first configured so that the circulation pump evacuates the entire circulation loop and the outlet of the circulation pump is exhausted to the room circulation pump on bypass valve open circulation exhaust valve exhausting and helium fill valve closed Then the circulation loop is charged with clean helium from the supply bottle circulation pump off bypass valve open circulation exhaust valve circulating and helium fill valve open These steps are performed three times during the startup operation in order to ensure a clean charge of helium in the circulation loop 4 3 2 2 MAIN FLOW In order to circulate helium for chamber cooling the circulation loop is configured with the circulation pump turned on the bypass valve closed the circulation exhaust valve set to circulation and the helium fill valve closed The main flow system provides up to 5000 standard cc minute sccm of 4 2 K helium gas to cool the sample chamber Main flow starts as 4 2 K helium gas in the bucket The gas then flows up the counter flow heat exchanger CFE through the mass flow controller back down the CFE through connecting tubing and into the cooling annulus The flow then runs through the annulus pumping line to the circulation pump then through the return gas line back to the bucket The mass flow controller controls the main flow rate from 0 to 5000 sccm The flow read back value is reported in MultiVu Log Data as
52. User Manual for additional information about this compressor 2 10 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Section 2 3 Hardware Measurement System Hardware 22 Helium Gas Bottle and Regulator replace when cylinder pressure less than 300 psi set pressure Y to 15 psi Figure 2 9 Helium gas bottle with regulator The DynaCool system uses a helium gas supply cylinder and a bottle mounted pressure regulator to provide helium gas for charging the circulation loop and for venting and purging the sample chamber The gas cylinder and regulator should be connected to the system at all times Additional precision pressure regulators are located in the pump cabinet to provide further pressure reduction and regulation for the both the circulation loop and sample chamber Helium gas consumption depends on your use of the system A cool down will require approximately 500 liters STP of helium to charge the circulation loop A typical purge or vent operation will use less than 10 liters A full standard size gas cylinder contains about 8000 liters STP The regulated pressure gauge on left should be set to approximately 15 psi Replace the helium cylinder when the cylinder pressure gauge on right falls below about 300 psi See Section 5 2 for replacement instructions 2 3 Measurement System Hardware 2 3 1 Sample Pucks The sample puck Figure 2 10 is a unique modular component that gives PPMS
53. Utilities gt Sigma Log Data contains very similar capabilities to the log data command except that you may log the statistics average and standard deviation of each data item as well This generates data files that are significantly larger and more tedious to navigate than the standard log data command The average values recorded with this command may be a simple average of all new data or a running average of the last several data items in which case each average may be calculated with some of the same data as the previous data record The following three sections describe the data available on the tabs of both the Log Data and Sigma Log Data dialogs B 2 1 Standard Items The standard items tab contains information that is mostly available in the MultiVu status bar The status of the chamber gas temperature magnetic field and cryostat are recorded in the file as integers The log data window displays the meaning of these status codes in real time but this text is not included in the log data files Use Utilities gt Status Calculator to decode status codes The Query button will decode the current state of the instrument The ID numbers of the sample and control thermometers are also shown on this tab These numbers tell you which thermometers are in use for special option temperature control modes See Section 4 3 4 for details B 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011
54. amber Get the current chamber state Here are some resources for learning about how to use the available OLE methods Quantum Design Example WinWrap macros and associated documentation Example WinWrap macros are available on the Quantum Design website http www qdusa com in a link next to Application Note 1070 209 Getting Started with Visual Basic Scripting in MultiVu You can learn how to use the OLE interface by examining these example macros Also included with the macros is the file MultiVu_OLE_Dictionary pdf that contains descriptions of the OLE methods Example WinWrap macros Example WinWrap macros are available on the Quantum Design website http www qdusa com in a link next to Application Note 1070 209 Getting Started with Visual Basic Scripting in MultiVu In these macros look at calls of the form MultiVu Method arguments to learn how to use MultiVu OLE methods View the type library If your development environment includes a type library viewer you can view method signatures in the type library C QDDynacool Dynacool tlb PPMS DynaCool User s Manual 1307 110 Rev AO D 3 November 2011
55. amber is cold enough for the system to enter low temperature mode as described in section 4 3 2 3 4 3 2 Helium Flow and Circulation Loop The Circulation Loop provides cooling helium flow to the DynaCool sample chamber As shown in Figure 4 1 the circulation loop is made up of the cooling annulus annulus pumping line circulation pump bypass and circulation exhaust valves return gas line bucket counter flow heat exchanger mass flow controller impedance and connecting tubes in the cryostat The circulation loop has four common operating modes Circulating In this mode the circulation pump is running the bypass valve is closed the circulate exhaust valve is set to circulate and the fill valve is closed This is the mode used for normal temperature control Pumping In this mode the circulation pump is running the bypass valve is open the circulate exhaust valve is set to exhaust and the fill valve is closed These settings enable the circulation pump to evacuate the entire circulation loop and exhaust its contents to the room Sealed In this mode the circulation pump is off the bypass valve is open the circulate exhaust valve is set to circulate and the fill valve is closed This state is used while the system is cooling down and when it is shut down Venting In this mode the fill valve is open venting helium into the circulation loop This operation can be performed without circulation during the loop purge and
56. are may set the temperature for you WARNING Do not open the sample chamber if it is below room temperature Doing so may condense water and air in the sample chamber Such contaminants may form a plug in the chamber resulting in dangerous and damaging over pressure condition on warming Verify that the magnetic field is less than 1 T 10 000 Oe If the magnetic field is greater than 1 T set zero field and wait for the field to stabilize before continuing Use MultiVu to set the field click on the field display in the status bar In the field dialog set 0 Oe 200 Oe sec and select Linear approach Press the set key WARNING If you place the sample insertion tool into the sample chamber when the magnet is at high field the insertion tool will be strongly pulled into the sample chamber The force may overwhelm you and cause damage to the instrument 10 Quantum Design Vent the sample chamber with helium Use MultiVu click on the chamber atmosphere display in the status bar this display shows the pressure and chamber state Press the Vent Cont button in order to vent the chamber continuously Do not leave the chamber in this state for longer than necessary because doing so wastes vent gas from the bottle you supply An installation wizard may vent the chamber for you Open the hinge clamp and remove the KF blank flange and attached baffle set if present from the sample chamber access port If the blank flange
57. ately 150 cc of liquid helium in the bottom of the bucket Other second stage components are cooled by solid contact to the 4 K Plate Heat loads from second stage components cause small amounts of liquid helium to evaporate from the bottom of the bucket The evaporated helium then condenses on the second stage of the cryocooler and falls back onto the 4 K Plate creating a classic thermosiphon 4 2 2 Thermal Isolation Like any cryostat PPMS DynaCool contains components at different temperatures DynaCool contains components ranging from room temperature to lt 1 8 K when the sample chamber is at its minimum temperature Maintaining these temperature differences requires thermal isolation between cryostat components as described below Mechanical supports are engineered to provide mechanically robust linkages with minimal heat leak between different temperatures Materials with low thermal conductivity are chosen for this reason Also heat loads from room temperature are intercepted by the main radiation shield cooled by the cryocooler first stage to prevent excessive heat load on the 4 K Plate Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 3 November 2011 Section 4 2 Chapter 4 Cryostat Control System Theory of Operation 4 2 3 4 4 Components that are not in mechanical contact are isolated from each other by the cryostat case vacuum preventing heat transfer via gas conduction and convection The Case Vacuum System
58. ceeseaaeaeeassseeeeeees 3 13 Graph Data Selection Dialog on graph right click to Data Selection ccccceseeeeeeeeeeeeeeeeeees 3 16 PIOEapP ear ane OO Oe serseri nears eavtaanwotaiea nhs eases th ed bio nd vianash Meeaa A E 3 17 1 4 016 A512 Daliani a te reer er tenon Meera heer etree treo a henner etree etree mere ree 3 18 Dyhat ool Services Control Diallo Tesperit mastassanee ital atti bae a 3 19 The DynaCool Cryostat showing the components of the Cryostat Control System Chamber Temperature Control System and Magnetic Field Control System ccccccseeeeeeeeeeeeeeeeeaeeeeeeeeees 4 2 The DynaCool Cryostat showing components of the Chamber Atmosphere Control System and Case VA CUMIN SUC TI ite ppreacgerncgh a ccd bate asanaenodsoasetacens coun ge E nee yseteasneetee 4 14 Henum eas supply cy linder and Teo ul ator ssn nn R a Morne esata 5 2 Check valve assembly for purging air from the regulator of the helium gas supply cylinder 5 2 Pumpe MAUS Tfer ASS MIDI si u25 cccateals saostanc cuseia lak tewanieuen E E ancien hoowianeeshonnanie hamanorinerats 5 3 PPMS DynaCool User s Manual 1307 110 Rev AO vii November 2011 Contents Table of Figures Pigure Baty Data Lost ime Titer ace cise sacs raasei nance icon a E E B 2 Foure B 2 Standard ems Taberner ern E e EE E EE bouied Seuviau tin sn iudaneunie bene aguasercussiaeruiseans B 3 Figure C 1 Sample connections a Sample puck b Gray Lemo CONnNECCtOM
59. ch Refer to Figure 1 4 7 Gently lower the sample insertion tool into the sample chamber cylinder end first until the tool touches the bottom of the chamber 8 Engage the sample 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 tool s handle Refer to Figure 1 4 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 You may insert another puck install measurement option hardware into the sample chamber or close the sample chamber at this point To close the sample chamber you 1 place the O ring and KF blank flange over the sample chamber access port 2 place the flange clamp in position around the top of the chamber access port 3 latch the clamp and then 4 purge and seal the sample chamber 1 6 Configure Measurement Option and Perform Measurement Most measurements that you perform in DynaCool require the use of a measurement option such as Vibrating Sample Magnetometer or Heat Capacity Whenever you first start using an option or when you change from using one option to another follow the steps outlined below Consult the relevant measur
60. ch the MultiVu software D Verify that there are no red indicators in the status bar at the bottom of the MultiVu window If there are any messages indicating that a service is stopped then start the services by double clicking the DynaCool Services Control icon i in the lower right of the screen and pressing Start All Services from the DynaCool Services Window 2 Open the Cryostat Monitor from the Instrument gt Cryostat menu item and press the Startup button on the left and follow the brief instructions to begin the startup procedure Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 1 3 November 2011 Section 1 4 Chapter 1 Quick Start System Startup and Cool Down Getting Started 1 4 5 Wait for Cool Down After the startup procedure has been launched you can close the Cryostat Monitor window or leave it open to track the progress of the cool down A typical cool down time for a 9 T DynaCool is about 16 hours During this time the system performs several operation including Purge the cryostat vacuum space with air to flush out any residual helium gas e Evacuate the cryostat vacuum space Purge and fill the circulation loop with a clean charge of helium from the bottle Regenerate the chamber cryopump Start the cryocooler compressor and cool the system to its base temperature of about 4 K Condense 100 to 200 cc of liquid helium into the cooler reservoir Upon completion of the sta
61. ched the commands inside the scan field loop will be executed but the field will continue to ramp while they execute Scan Temperature Creates a program loop for executing repeated commands at user defined temperature increments All commands between the Scan Temperature line in the sequence and the End Scan line in the sequence will be repeated at each temperature specified by the scan temperature command Set the initial and final temperatures and the scale on which the spacing of the temperature steps should appear uniform linear 1 T log T Also set the total number of temperature steps For uniform linear spacing you may alternatively set the temperature increment Finally specify the rate and approach mode used by the temperature controller to achieve each set point PPMS DynaCool User s Manual 1307 110 Rev AO 3 13 November 2011 Section 3 4 Sequences 3 14 Chapter 3 Software Fast Controller will drive directly to each temperature and attempt to maintain the specified sweep rate as closely as possible until each set point is reached At each set point the temperature will stabilize until the commands within the loop are completed A small temperature overshoot can occur in this mode No Overshoot Controller will drive to each set point at the desired rate until it 1s close to the set point and will then slow the rate to avoid temperature overshoot At each set point the temperature will stabilize un
62. ck operates in a thermal isolation vacuum 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 2 14 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 2 Hardware 2 3 6 Quantum Design Section 2 3 Measurement System Hardware Finger Contractor Test Cutout FINGER SPREADER Cylinder 1 Cylinder 2 Figure 2 13 Puck Adjustment Tool Complete the following steps to use the puck adjustment tool L Place the puck on the finger spreader Refer to Figure 2 13 If there are two small screw heads on the bottom of the puck such as on a heat capacity puck be sure to align them with the cut outs on the spreader Press the puck downward and continue pressing until all the chuck fingers touch the base of the finger spreader When all the fingers touch the base of the spreader the spreader evenly applies radial force to the fingers pushing them outward and slightly beyond their optimal location Remove the puck from the finger spreader Place the puck inside the finger contractor Refer to Figure 2 13 Press straight down on the puck and continue pressing until you press the puck completely into the finger contractor When the entire puck is in the contractor the contractor evenly applies force to the outside of the fingers pushing them inward The contractor pushes th
63. condition one or more of these breakers may switch to the off position They may be switched back to the on position like a normal rocker switches The breakers on the back of the pump cabinet are e MODULE BAY AND COMPUTER This 10 Amp breaker switches the power to the outlets in the computer bay and also the AC power line supplying the module bay Do not use this breaker to turn off the power to the module bay since you will lose power to the computer Instead use the power switch on the back of the module bay for this see Figure 2 4 MAG PWR 12 A This 12 Amp breaker switches power to the large IEC C19 connector below the magnet controller bay This is usually used only for 14 T DynaCool systems Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 5 November 2011 Section 5 5 Chapter 5 Replacing Fuses and Resetting Breakers Maintenance and Servicing MAG PWR 10 A This 10 A breaker switches power to the IEC C13 connector inside the magnet controller bay This is usually used for 9 T DynaCool systems CABINET This 10 A breaker switches the power to the pumps and gas handling instruments inside the pump amp gas handling bay in the bottom of the cabinet It also switches power to the control electronics located in the side of the pump cabinet This breaker should be off when opening the side panel on the cabinet MAIN PWR This 30 Amp breaker switches power to all components of DynaCool except the compressor p
64. cone vacuum grease to it Apply only a thin film of grease to the O ring Do not apply so much grease that more than a film is visible Also inspect the metal surfaces that mate with the O ring and clean them if necessary Take care not to use sharp instruments on O rings or the mating surfaces as it could result in damage Keeping O ring seals in good working order prevents leaks that could cause malfunction or damage to the instrument Leaks at the sample chamber KF flange can cause the formation of an ice plug in the sample chamber which results in dangerous and damaging pressure during warming Be sure to maintain this often encountered O ring Replacing Fuses and Resetting Breakers The system has several user accessible fuses and breaker switches In case you encounter situations where a fuse blows or a breaker opens contact your Quantum Design service representative to investigate the root cause of the problem If you replace any blown fuses be sure to use only the values described here Use of other values creates electrical hazard and may damage your system This section does not discuss fuses and breakers in equipment supplied by other manufacturers such as the helium compressor and vacuum pump Refer to labels on such equipment and separate documentation for more information Pump Cabinet Power Input Breakers There are five breakers on the back of the pump cabinet all controlling 240 VAC power In the event of an over current
65. cooler system which consists of a cold head and a compressor manufactured by Cryomech Inc Be sure to read the Cryomech User Manual Conventions in the Manual This symbol signals specific caution or conditions that could result in system damage bodily harm or loss of life This symbol signals electrical hazards that could result in bodily harm or loss of life Used at all accessible 200 240 V power outlets Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO XI November 2011 Section P 4 Preface Safety Guidelines and Regulatory Information Contents Conventions and Safety This symbol signals information on fusing P 4 Safety Guidelines and Regulatory Information Before using this product please read the entire content of this manual and observe all instructions warnings and cautions These are provided to help you understand how to safely and properly use DynaCool Quantum Design Inc disclaims any liability for damage to the system or injury resulting from misuse or improper operation of the system Please contact your Quantum Design representative for any service issues This product is NOT user serviceable except for the operations that are described as performable by the user in Chapter 5 Observe the following safety guidelines when you use your system e Incase of emergency switch off the breaker on the back of the pump cabinet labeled MAIN PWR see Figure 2 6 and the main breaker on the com
66. cryocooler 5 9 Required Maintenance Log The following maintenance procedures should be performed regularly Some of the services must be performed by a qualified Quantum Design representative and you will need to schedule the maintenance visit with them The cryocooler system can be seriously damaged if it is not serviced properly The maintenance logs on the following pages facilitate keeping track of what service has been performed Make additional copies of the log pages as required Section 5 2 of this manual has instructions for services that you and other onsite personnel can perform Table 5 1 Maintenance procedures required for the DynaCool system Replace compressor adsorber 20 000 hours QD service personnel 2 years Scroll pump Replace tip seals As required see Site personnel pump manual 5 8 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Section 5 9 Maintenance and Servicing Required Maintenance Log Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 9 November 2011 Section 5 9 Chapter 5 Required Maintenance Log Maintenance and Servicing Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals
67. cuting repeated commands at user defined magnetic field increments All commands between the Scan Field line in the sequence and the End Scan line in the sequence will be repeated at each magnetic field specified by the scan field command Set the initial and final fields and the scale on which the field increments should appear uniform linear H2 H1 2 1 H log H Also set the total number of field steps For uniform linear spacing you may alternatively set the field increment Finally specify the rate and approach mode used by the magnet controller to achieve each set point o Linear Controller will drive directly to each field and attempt to maintain the specified charging rate as closely as possible until each set point is reached At each set point the field will stabilize until the commands within the loop are completed o Oscillate Controller will intentionally overshoot each set point by 70 of the total field change at the desired rate and will then oscillate into the set point field in smaller and smaller overshooting steps At each set point the field will stabilize until the commands within the loop are completed This is intended to eliminate flux motion in the superconducting magnet windings yielding a very stable magnetic field and reduced remanence o Sweep Controller will drive directly from the initial field to the final field without stopping Each time a field increment defined by the command is rea
68. d Shutdown This operation will shut down power to the system without any further operations Unlike the Shutdown this operation will not evacuate the circulation loop Use this operation as an emergency shutdown or prior to software or hardware maintenance if you plan to restart the system within 30 minutes Refresh Liquid This operation will burn off and condense liquid helium in the circulation loop It will take about 1 hour to complete Run this operation if you suspect that the helium level in the cryostat is abnormally low Abort This operation will abort the current startup operation and shut down power to the system Use this operation as an emergency shutdown to stop system startup After executing this abort you will have the option to choose Resume Startup to continue Resume Startup This operation will attempt to resume a system startup after a shutdown or abort of a previous startup operation The operations performed will depend on the progress of the previous aborted startup operation See Startup for a list of possible actions taken If the cryostat is cold this operation will not include purging and evacuating the cryostat case purging the circulation loop with helium or regenerating the cryopump To force a complete startup rather than resuming an existing one make sure the cryostat is warm 4 K Plate gt 270 K and use the Startup command instead Cancel Recovery The availability of this button indicates
69. determined that the pump is in need of maintenance Typical signs of worn tip seals include vibrations or unusually high annulus pressure when in low temperature mode The tip seals are the plastic sealing surfaces that create the seal between the stationary and moving scrolls Before beginning make sure you have all of the parts you need These are available in the DynaCool Tip Seal Replacement Kit Quantum Design part number 4307 041 You will also need a 9 64 hex socket key and an adjustable crescent wrench Figure 5 3 Pump exhaust filter assembly Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 3 November 2011 Section 5 3 Chapter 5 Replacing the Scroll Pump tip Seals Varian SH110 Scroll Pump Maintenance and Servicing 1 Warm up the DynaCool system a Press the warm up system button on the console and wait for the system to warm to room temperature This takes 8 16 hours b Shut down the computer and power down the system by switching off the main breaker switch located in the back of the cabinet 2 Remove the Scroll pump from the System Cabinet a Remove the lower front panel and lower right side panel of the System Cabinet by pulling the bottom out away from the cabinet and lowering the tabs out of the slots at the top b Unplug the power cord from the pump and remove the hose connected to the pump inlet at the top KF 25 flange Since the circulation system is under vacuum you will notice a lot of air
70. e the logger click Browse and specify a file name where the data will be saved You may specify a new file name or an existing log data file Be careful If you check the Overwrite Existing File box any existing data in the file will be deleted Also specify how often to log data records to the file Some problems are best diagnosed by very rapid data logging for a short period of time while others are best diagnosed with very long logs with infrequent data records A Quantum Design representative can usually help you determine the most appropriate logging interval to use when troubleshooting When you click View Data the specified data file will be opened in a graph view But no data will be present in the file until you select data items to log from the other three tabs Standard Items Diagnostic Items and Advanced Items and until you click Start begins the logging or Acquire Once records all of the checked data items one time only Once logging data will continue to be recorded to the file at the specified rate until you click Stop You may change the data items being logged while the logger is running A time stamp always accompanies each data record Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO B 1 November 2011 Section B 2 Appendix B Log Data Diagnostic Software second s 0 250 min max Figure B 1 Data Logging Interface The menu command
71. e OLE under the hood to communicate with MultiVu You establish an OLE connection with MultiVu in one of two ways PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Appendix D Section D 4 Using Third party Instruments Object Linking and Embedding Active X Early Binding With early binding the OLE client knows details of the OLE methods supplied by the MultiVu OLE server at compile time so you may get syntax checking and code completion for the OLE methods in your development environment To use early binding point your development environment at the type library C QDDynacool Dynacool tlb Late Binding With late binding the OLE client does not know details about the OLE methods supplied by MultiVu However late binding is more reliable than early binding in some programming environments and is typically less version dependent To use late binding refer to MultiVu using the Class ID QD MULTIVU DYNACOOL 1 Many OLE methods are available in MultiVu Most of these methods are for use by Quantum Design software only not end users Use only the following OLE methods SetTemperature Set the temperature rate and approach mode GetTemperature Read the present temperature and temperature status SetField Set the magnetic field rate approach mode and end mode GetField Get the present magnetic field and field status SetChamber Set the chamber state purge seal high vacuum etc GetCh
72. e fingers regardless of external wear or variations on the puck so that the fingers obtain their optimal location Remove the puck from the finger contractor Place the puck inside the test cutout Refer to Figure 2 13 Verify that the puck fits easily but snugly inside the test cutout Do not insert the puck into the sample chamber if it does not fit into the test cutout doing so could cause damage to the sample chamber Puck Wiring Test Station The puck wiring test station Figure 2 14 is used to verify the integrity of the wiring between a sample and puck or the wiring of any option hardware present on a puck The test station contains three sets of contacts all wired in parallel a Lemo connector identical to the sample chamber connector on the probe head a puck connector and 12 banana jacks DynaCool measurement options each come with a plastic overlay that can be placed over the banana jacks on the test station with convenient labels for each of the signals PPMS DynaCool User s Manual 1307 110 Rev AO 2 15 November 2011 Section 2 3 Chapter 2 Measurement System Hardware Hardware Lemo Connector Figure 2 14 Puck Wiring Test Station Z del Experiment Puck Wiring The experimental wiring in DynaCool consists of the following components The gray Lemo connector to the right of the cryostat cover see Figure 2 3 A cable under the cryostat cover running between the Lemo connector and the sample chamber
73. e is open during these operations in order to connect the chamber to the chamber case gas line 4 6 1 Case Vacuum Operation During Startup cooling down the cryostat the vacuum case is prepared as follows Vent the case to 600 Torr with air Pump the case down to 50 Torr Repeat the vent and pump cycle for a total of 3 cycles This procedure removes any residual helium from the vacuum case Helium is not removed by the charcoal sorbs until they achieve lt 15 K so helium in the vacuum space can prevent proper cooling 4 16 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Section 4 6 Theory of Operation Case Vacuum System Wait while other Startup operations occur Resume pumping on the vacuum case When the 1 and 2 Stage temperatures are both lt 250 K the case is sealed Typically the case pressure is lt 2 Torr at this point As the cool down commences the charcoal sorbs adsorb remaining gasses achieving the high vacuum condition required for normal cryostat operation Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 17 November 2011 cCc H APTER 5 Maintenance and Servicing 5 1 5 2 Overview This chapter describes the most common maintenance procedures needed to keep DynaCool running properly Also consult measurement option manuals for maintenance of option hardware Be sure to contact Quantum Design service if you ever have q
74. e liquid in the cryostat cooler chamber Also indicated is the status of the circulation loop as well as the state of the liquid in the cooler chamber This status normally will only change during startup and shutdown operations Case Shows the status of vacuum can Again this status will only change during startup and shutdown operations 3 2 8 2 CRYOSTAT CONTROL TASKS The buttons on the left of the Cryostat Monitor are for initiating various cryostat operations like startup and shutdown The buttons available at any given time will depend on the current cryostat state For example if the cryostat is in the Cold Cryostat state then the Startup task is not available When a button is clicked a description of the action to be performed is displayed along with OK and Cancel buttons displayed Here are the most commonly used tasks Quantum Design Startup This operation will perform a complete system startup This includes purging and evacuating the cryostat case purging the circulation loop with helium regenerating the cryopump cooling the magnet to operating temperature and preparing the circulation loop for temperature control A complete system startup will take between 12 and 36 hours to complete To resume a previously aborted startup you may use Resume Startup instead System Standby This will operate the cryostat in a reduced power standby mode In standby the cryocooler is turned on and off at reg
75. e number 1 and continues writing to this file until its size exceeds 10 MB or the computer is restarted At this point the system starts recording to file number 2 and so on After using file number 10 the system goes back to file number To determine which file is currently in use you find the one with the most recent modified date Typically Quantum Design Service will request all of these files if they are needed for problem diagnosis B 4 3 Option Log Files Options typically write information to dedicated log files See the appropriate option user manual for details Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO B 4 November 2011 A P P END IX C Pin out and Interconnect Diagrams C l Overview This appendix provides pin out and interconnection diagrams for DynaCool Refer to option manuals for pin outs of option hardware including option pucks and CAN modules C 2 Sample Puck Connections Gray Lemo and JQP 8 The sample connector which the puck mates with is located at the bottom of the sample chamber The sample gray Lemo connector is located on the right side of the cryostat enclosure above the CAN module bay The sample D shell connector is located under the cosmetic cryostat covers at the top of the sample chamber on the right side when facing DynaCool from the front The connections labeled Spare are not wired to anything but could be used to feed custom wires into the annulus a Sample puck
76. e outlet is at annulus pressure about 10 Torr As the helium undergoes expansion in the impedance some of it evaporates resulting in an impedance outlet flow that is a mixture of liquid and gas at about 1 7 K This mixture flows through connecting tubes to the bottom of the cooling annulus also known as the pot In low temperature mode a small amount of liquid helium accumulates in the bottom of the annulus In order to achieve stable temperature control with high cooling power DynaCool simultaneously controls Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 7 November 2011 Section 4 3 Chapter 4 Chamber Temperature Control System Theory of Operation the level of liquid in the bottom of the annulus and the flow rate of gas in the cooling annulus This control is achieved using a liquid level sensor in the cooling annulus a heater on the impedance and a heater on the pot These values are reported in MultiVu Log Data as Pot Liquid Level Impedance Power WY and Pot Power W DynaCool enters low temperature mode when cooling at 10 K Once in low temperature mode the system enters main flow mode when the temperature goes above 16 K In order to avoid excessive heat load conducted down the sample chamber DynaCool will not enter low temperature mode if the high neck temperature is above 220 K If the system reaches 10 K and the high neck temperature is gt 220 K then high main flow is maintained in orde
77. e puck and try inserting it again 15 Remove the sample insertion tool from the sample chamber 16 Check that the sample chamber access port KF flange blanking flange and O ring are clean Place the O ring over the port and replace the blank flange with attached baffle set 17 Place the flange clamp in position around the top of the sample chamber access port and then latch the clamp 18 Purge and seal the sample chamber using MultiVu click on the chamber atmosphere display in the status bar Press the Purge Seal button in order to purge and seal the sample chamber An installation wizard may do this for you The system is ready to begin an experiment You should refer to the appropriate measurement option manual to determine what to do next Once you perform a measurement and verify instrument operation you may want to write a sequence to automate the measurement See Section 3 4 for a discussion of sequences 1 5 3 Removing a Sample Puck The procedure for removing the puck from the sample chamber is essentially the reverse of the installation procedure Complete the following steps to remove the puck 1 Verify that the sample chamber is at or above 298 K The temperature must be at least 298 K to prevent condensation of water or cryopumping of air into the chamber If the temperature is below 298 K set it to 298 K and wait for the chamber to warm up An installation wizard in measurement option software will set the temperatu
78. e with air to remove any residual helium gas Purge circulation loop with helium and charge to gt atmosphere with helium gas Regenerate the cryopump Start the pulse tube cryocooler to cool the system from room temperature to operating temperature Wait for the 4K Plate to get cold enough to condense helium Meter helium gas into the bucket to condense about 150 cc in the bucket e Start 4K Plate temperature control helium circulation for sample chamber cooling and sample chamber temperature control DynaCool is ready to use The startup operation typically takes lt 16 hours for a system equipped with a 9 T magnet Chamber Temperature Control System This section describes how the chamber temperature is controlled and measured Figure 4 1 shows the major cryostat components described in this section Sample Chamber Thermometers and Heaters The DynaCool Temperature Control System controls the temperature of the isothermal region of the sample chamber The isothermal region is constructed of high conductivity copper in order to minimize thermal gradients providing a thermally uniform region for the sample environment The puck interface is located at the bottom of the isothermal region inside the sample chamber On the outside of the sample chamber the block thermometer is tightly coupled to the metal of the puck interface This ensures that the block thermometer is at the same temperature as the puck even when
79. ed Quick Start System Startup and Cool Down 14 Quick Start System Startup and Cool Down This section covers cooling down the cryostat from a completely warm state to normal operating temperature If your DynaCool system has not been fully installed in your lab please refer to Appendix A System Setup for instructions 1 4 1 Turn on Power to Electronics Make sure all the breakers on the back of the cabinet are turned on and the computer is booted up MultiVu should be running Make sure the breakers in the back of the cabinet are turned on The power light on the back of cabinet should be lit Make sure the power switch on the back of the CAN Module Bay is set to on The PWR indicator should be illuminated on the temperature control module in the CAN Module Bay Make sure the computer is on Observe that the PWR light from the USB based CAN Network transceiver is lit This is located in the back of the CAN module bay 1 4 2 Check Cooling Water and Power to Compressor Make sure the chilled cooling water is flowing through the compressor and that the circuit breaker is switched to the ON position DO NOT press the green start button 1 4 3 Check Helium Bottle Make sure the needle valve is open on the helium supply bottle and that the bottle pressure is at least 300 psi for a standard K size cylinder before proceeding 1 4 4 Launch Startup Procedure Follow the steps below to begin the cool down procedure 1 Laun
80. ement option manual for details about the measurement option you are using 1 If necessary uninstall any hardware from a measurement option previously in use Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 1 9 November 2011 Section 1 6 Chapter 1 Configure Measurement Option and Perform Measurement Getting Started a You always uninstall all option hardware from the sample chamber including pucks specialized baffle sets and hardware attached to the chamber KF flange e g VSM linear motor Be sure the chamber is at room temperature the magnetic field is zero and the chamber is venting continuously before attempting to remove any option hardware b Itis not necessary to uninstall CAN modules unless you need extra space in the module bay 2 Install hardware for the measurement option you are ready to use a For some options you install pucks specialized baffle sets and hardware attached to the sample chamber See the option manual for details In general you do not install samples including pucks with samples on them at this time b If necessary install any CAN module s needed for the option into the module bay The module s may already be installed from previous use of the option WARNING You must turn off the power to the module bay using the switch on the back of the bay see Chapter 2 whenever removing or installing CAN modules Hot plugging can destroy the module 3 Activate the opti
81. ent data collection Section 3 4 sequence editing and sequence execution Section 3 5 and graphing Section 3 6 In addition to these features MultiVu also contains instrument utilities diagnostics and error reporting The Temperature Magnet and Cryostat services run as Windows services in the background and their Operation is indicated by the icon located in the Windows tool tray in the lower right of the screen See Section 3 7 for more information The CAN Manager software provides CAN network communication services to all software on the PC including MultiVu and the control services The operation of CAN Manager is indicated by the icon JT TLF also located in the Windows tool tray in the lower right of the screen Double click or right click for more information 3 2 MultiVu Menu Bar ToolBar Control Center Sequence Command Bar loi DynaCool Mu Wu HgSupercond ctivity vs B 2 dat Fis View Sample Sequence Measu Dejn wo e S oil ala 2 Selected Sequence be Sequencel s q Sequence Commands Sequence 38Q Selected Ling e System Commands Scan gefip irom 1 6K to 400K at 12K man in 2 steps Untam Fast t For Temperature Delay 0 secs No Action Sequence Status Beep Sequence Ide g i Call Sequence ce Scnpt Chamber Operations Remark Scan Fisid Scan Temperature Scan Time End Sequence Lan rae oe Message et EnA lock Set iea Standby War
82. er 2011 Contents Table of Contents Aoa EOW Temperi POW setstoy a atsiniaussea sat aaiasto sara ane AA 4 7 4 3 3 Temperature Control Electronics and SOftware cccccccccccccssssssssssesseecececeeeeeeeeeaaaaeecseeeeeeeeeeeeseeeeeaaas 4 8 4 3 4 Temperature Valuesand COnMOULATIONS sotn r E e a r iow taventaatondeas 4 8 4 3 4 1 Temperature Values Reported in Software and Data Files 2 0 0 ccsssseeeessseeeeseeeceeeeeeeeeeeaaas 4 8 4 3 4 2 Temperature Control Configurations seeeeesssssssssssseeccereerssssssssssssecctrreesosssosssssssssseeeereeessssesss 4 9 Ad Masnec Fiod Control Syse esprai E EE E EEs 4 12 4 4 1 M snetand Leads anaa E E E E E 4 12 4 4 2 Masner C omiroller and SOWA ao EE E aces eee aes 4 12 4 4 3 Miene ue Shit ICING an naceadsatauiacudonentdiatinetuac ated daa imticsial aetatsna tena tins co tendssneuancas eaters dneittucantnidasselaneeddamad 4 13 4 4 4 Magnetic Field Accuracy Uniformity and Magnet Reset cccccccccccccccssssssseeseeeeeeeeceeeeeeeeeeeaaas 4 13 4 5 Chamber Atmosphere Conto Syste NT esia a i a a T a ait 4 13 4 5 1 Chamber Operations src onenn e EEE EE E TEA E REA 4 15 AsO MCAS NeACUUT o yS EM a ha ccc Re ce aa ate nel ce ete cue cana iet eet a 4 16 4 6 1 Case Vacuum Oper UO rita eas sects witha caste Senda essences bccn eta E caer ada eae 4 16 CHAPTER 5 Maintenance and SCE VA CUI Go 5555 5555 5055s ccs0s a sedeci ceca cd e E E a O E e 5 1 5 1 Ae ad oa pers Oe E A N N 5 1 5 2 Chanem the He lu
83. face are disabled Unlock the sequence by clicking Lock Sequence 8 again selecting the menu item Sequence gt Unlock or the Unlock button on the control center Then click the Unlock button on the popup dialog which displays the name and message of the person who locked sequence execution Sequence Commands The following sequence commands are present in DynaCool with no measurement option activated Additional measurement commands are available when using an option 3 4 5 1 SYSTEM COMMANDS Beep Causes the computer to make the Windows default beep sound PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 3 Software Quantum Design Section 3 4 Sequences Call Sequence Suspends execution of parent sequence file and begins execution of selected child sequence file or script file When execution of child sequence file or script is complete execution of parent sequence will continue with the next line Chamber Operations Changes the state of the sample chamber atmosphere Figure 3 1 See Section 4 5 1 for a description of chamber operations Chamber Status Control Pressure 11 8 Torr State Sealed Vent Seal Pump Cont Close Figure 3 11 Sample Chamber Atmosphere Control Center Remark Serves as a message comment or visual break for the user only Does nothing during sequence execution Scan Field Creates a program loop for exe
84. gn PPMS DynaCool User s Manual 1307 110 Rev AO 4 9 November 2011 Section 4 3 Chapter 4 Chamber Temperature Control System Theory of Operation Measurement Control Sample Measurement Control Configuration Thermometer Thermometer Thermometer Therm ID Heat Capacity Block Block Platform 643 643 1 8 400 K Thermometer Thermometer Thermometer Thermal Block Block Hot and Cold 643 643 Transport Thermometer Thermometer Thermometer Option Temperature Control Configuration This configuration is used by measurement options that provide a control thermometer near the sample and use the standard DynaCool temperature range 1 8 400 K In this mode the Measurement Temperature Sample Temperature and Control Temperature all report the value of the control thermometer provided by the option Measurement configurations that use this mode include Measurement Control Sample Measurement Control Configuration Thermometer Thermometer Thermometer Therm ID es aor Coil Coil Coil 1 8 400 K Thermometer Thermometer Thermometer Electro Transport or Resistivity Rotator Rotator Rotator with Horizontal Thermometer Thermometer Thermometer Rotator Torque Rotator Rotator Rotator TBD TBD Magnetometer Thermometer Thermometer Thermometer User E User User Depends on User User User with additional l Thermometer Thermometer Program choice choice control thermometer Extended Range Option Temperature Control This configuration is used by measuremen
85. gnetic Field Accuracy Uniformity and Magnet Reset DynaCool reports the magnetic field as the measured magnet current multiplied by a calibration factor determined at the factory for your magnet This factor is stored in the cryostat SROM The system does not take magnet relaxation or trapped flux into account For information on the resulting field remanence see your system specifications The uniform region of the magnetic field is centered 4 05 cm 1 6 inches above the top surface of standard sample puck The uniformity of the magnetic field depends on the magnet model so see your system specifications for more information about uniformity 4 5 Chamber Atmosphere Control System Many experiments carried out in DynaCool require control of the atmosphere present in the sample chamber Any experiment that involves low temperatures requires an atmosphere that will not freeze or condense on the sample and other experimental hardware Some experiments benefit from the thermal uniformity provided by exchange gas while others require thermal isolation provided by high vacuum DynaCool meets all of these needs with its chamber atmosphere control system In addition this system enables DynaCool to pump out prepare the cryostat vacuum case prior to system startup as described in section 4 6 Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 13 November 2011 Section 4 5 Chapter 4 Chamber Atmosphere Control System Theory of Operati
86. he Quantum Design website http www qdusa com Example WinWrap macros are also available on the website using a link next to the application note Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO D 1 November 2011 Section D 4 Appendix D Object Linking and Embedding Active X Using Third party Instruments D 3 D 4 D 2 Using WinWrap you control DynaCool using MultiVu commands You can control third party instruments using GPIB with simple MultiVu commands Note that no GPIB controller is provided with DynaCool so you need to provide one Quantum Design recommends using a USB GPIB controller from National Instruments for this purpose For advanced users controlling instruments that use other communication technologies is possible by making OLE or COM calls from WinWrap to external libraries National Instruments LabVIEW Quantum Design provides LabVIEW Virtual Instruments VIs for control of DynaCool from LabVIEW Using these VIs and the associated dll and server it is possible to control MultiVu from LabVIEW in two ways LabVIEW on the same computer as MultiVu This requires installation of LabVIEW on the MultiVu computer LabVIEW on a separate computer communicating with the MultiVu computer over a Local Area Network connection A server runs on the MultiVu computer in this configuration and you can use LabVIEW computers that you have already set up This configuration may save licensing costs
87. hese temperatures depends on the configuration of the temperature control system The following two sections describe these values and the different configurations of the DynaCool temperature control system 4 3 4 1 TEMPERATURE VALUES REPORTED IN SOFTWARE AND DATA FILES Block Temperature This value always reports the temperature read by the block thermometer which is mounted to the outside of the puck interface at the bottom of the sample chamber It is reported in MultiVu Log Data as Bock Temp KY Control Temperature This value reports the temperature that base DynaCool temperature software is controlling using the basic sample chamber temperature control in the range 1 8 400 K If you are not using an option which includes a control thermometer then the Control Temperature is the Block 4 8 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Section 4 3 Theory of Operation Chamber Temperature Control System Temperature Some options such as the Vibrating Sample Magnetometer include a control thermometer In this case the Control Temperature is the value from this thermometer e g the coil thermometer for Vibrating Sample Magnetometer This Control Temperature is reported in MultiVu Log Data as Control Temp K Also the Log Data item Control Therm ID reports an identification number for the control thermometer A value of 643 indicates the block thermometer Other values indica
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89. ided wrench for this 5 Connect the helium hose from the HIGH port on the compressor to the smaller of the two helium connections at the back of the cryostat Figure 2 2 Power up the System 1 Turn on the breakers on the compressor 2 Connect the cabinet power cord to wall power 3 Turn on main and sub system breakers on the back of the cabinet Figure 2 6 4 Turn on both the power switch and the spare breaker switch on the back of CAN module bay Figure 2 4 Attach Deck and Cryostat Cover i Re ae he ee After positioning the cryostat lower the feet into contact with the floor Locate mounting hardware for the deck Position deck on the feet of the cryostat Install mounting hardware on each of the feet Tighten securely Carefully install the cryostat cover onto the top of the cryostat PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 A P P EN DIX B Diagnostic Software B 1 B 2 Overview This appendix describes diagnostic software operations that help you troubleshoot problems with your DynaCool instrument Often you will use these features at the request of Quantum Design service personnel when you report a problem with the instrument Data that you collect using these procedures can be sent to Quantum Design service to speed the diagnosis of your problem Log Data The menu command Utilities gt Log Data is used to log diagnostic data for the instrument To us
90. il The base DynaCool system is configured with only a single CAN module in the module bay Temperature Control Module used for certain temperature control functions However most measurement options have at least one CAN module containing option specific instrumentation For a detailed description of specific CAN modules consult the relevant measurement option manual For instructions on insertion and removal of CAN modules see Section 2 2 2 1 Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 17 November 2011 C H A PTER 3 Software 3 1 Overview This chapter describes the MultiVu Windows software and also the background services running on the PC that manages the lower level temperature field and cryostat control functions Figure 3 1 shows the relationship between MultiVu and these other software components MultiVu Application Inmacool exe Temperature Service Magnet Service Cryostat Service MagqnetCtrliervice exe CryoCtrl ervice enxe InmacoolTempCtrl eryv ice_ exe CAN Network Manager QdCanSrvdsh exe Figure 3 1 Overview of software applications running on PC Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 1 November 2011 Section 3 2 Chapter 3 MultiVu Software MultiVu is the primary user interface that allows user control of the operation of DynaCool It combines in a single user interface the basic instrument control and status reporting Section 3 3 measurem
91. in the area 3 Connect the three flexible stainless hoses in the black tether from the cryostat to the VCO connections labeled annulus return and chamber case on the side of the cabinet See Figure 2 5 Tighten using wrench 1 8 turn past finger tight 4 Remove the front and rear panels on the bottom of the cabinet and inspect all the VCO fittings to make sure none of them have come loose during shipping A 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Appendix A System Setup Section A 3 Initial Installation A 3 4 Connect Magnet Controller at ee ae Pull the upper front cover off the upper section of the pump cabinet to expose the magnet controller At the back of the cabinet feed the magnet signal cable and the current leads through the back panel into the magnet controller bay See Figure 2 6 Attach the current leads to the magnet controller The blue tape marks the current lead that connects to the positive terminal on the controller Tighten the current leads securely using two wrenches Reattach the cover protecting the current lead terminals Connect the magnet signal cable to the JQB 1 Magnet Control connector on the magnet controller Replace the front cabinet cover A 3 5 Make Cabinet Connections Refer to Figure 2 6 and 2 7 for the following Sh ee ee IS Remove cables and hardware from the computer bay at the back of the cabinet Attach the
92. ing and scaling to axes O Select auto scaling for each Check for logarithmic axis or specify the min and axis scaling max value for each axis Graph Data Selection _MySample dat Mae Magnetic Field 0e yi T Moment emu A T Y2 l lv IM Std Err femu l v B l Vv NOTE Log scales show only positive valug Data Group Show Time In Minutes C Seconds Time Display Relative Absolutg Apply Cancel Click to limit plotted data based on certain data values Display time data as absolute time or Limit the data records plotted to the last relative to first data record in data file few records like a chart recorder or to a in minutes or seconds range of specified records Figure 3 12 Graph Data Selection Dialog on graph right click to Data Selection 3 16 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Section 3 5 Software Graphing Data Files 3 5 2 Plot Appearance Change the appearance of each plot by selecting Graph gt Appearance gt Plot 1 or Plot 2 etc or right click the plot you want to change and select Appearance Turn horizontal and vertical grid lines on and off with this dialog e Choose between markers on each data record lines between each data record or both markers and lines The lines shown can be limited to only those in the positive or negative x directions using the gt gt button Check Apply to A
93. ing this chapter For more information about how these components operate see Chapter 4 Theory of Operation 2 2 System Hardware Components The PPMS DynaCool consists of the following main components Cryostat Assembly CAN Module Bay Pump Cabinet and Computer Cryocooler Compressor Assembly Helium Gas Bottle and Regulator The following sections provide additional details on the main system components Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 1 November 2011 Section 2 2 Chapter 2 System Hardware Components Hardware 2 2 1 2 2 Cryostat Assembly sample chamber access port cryostat cover removable field display module bay for option electronics temperature display CAN network out and AC power for options lower part of magnetic shield deck Figure 2 1 Front view of cryostat Figure 2 1 shows the front of the cryostat with the CAN module bay attached to the side The cryostat assembly contains the cryogenic components of the system including the superconducting magnet sample chamber and pulse tube assembly for the cryocooler It also contains some gas handling valves and electronics The exterior surface of the cryostat is composed of a fiberglass housing The cryostat cover on top can be removed by simply lifting it vertically This exposes the electronics and integrated gas handling hardware This includes the chamber vacuum gauge Node 13 on the CAN bus and
94. ion 2 2 Chapter 2 System Hardware Components Hardware Most measurement options and inserts require a connection between this port and one or more modules located in the CAN module bay The module bay hosts ten CAN modules One module in the back most bay is dedicated to the core DynaCool system operations chamber temperature control while the remaining nine are for optional measurement and control modules 2 2 2 1 CAN POWER SUPPLY AND POWER DISTRIBUTION Because of the large number of empty slots in the module bay it is usually not necessary to remove and install modules unless a new module is being installed for the first time or a defective module is being removed However if it becomes necessary to install or remove a module it is critical that the power switch on the back of the module bay be turned off The module power switch is located with the main power inlet as show in Figure 2 4 below WARNING You must turn off the power to the module bay using the switch on the back of the bay whenever removing or installing CAN modules Hot plugging can destroy a module CAN network controller USB from computer reset CAN network out to cabinet to cryostat spare AC power out amp breaker regulated power yy fuses for CAN out power switch amp light for modules turn off when installing modules magnet signal AC main power inlet patch from cabinet to cryostat from magnet power
95. l in the sequence window and are changed from black text to gray text With this feature you may decide to execute or not execute some commands just prior to run time based on the immediate circumstances For example you may wish to disable a series of commands that fall outside the meaningful measurement range for certain samples All of the commands found in the Edit menu are duplicated in a pop up menu when you right click any sequence window PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 3 Software 3 4 2 3 4 3 Section 3 4 Sequences view Sample Edt 3 7 3 F Cut Ctrl Copy Ctrl C Faste Ctrl y MO Delete Del Enable os Figure 3 10 Disabling Sequence Commands Advanced Script Editing Before running sequences MultiVu automatically compiles sequence files into Visual Basic for Applications VBA scripts Users with programming experience may compile this script without running the sequence and may then edit the script directly and run the edited script macro VBA scripts give the user the ability to perform branching and more sophisticated loops than standard sequences Also communication with third party instruments via GPIB is possible in VBA scripts You must supply GPIB hardware However Quantum Design cannot certify the instrument behavior when it is automated with user designed scripts Many checks and safeguard
96. lding the top of the cryostat in the crate Raise the landing pads on the cryostat feet as high has they will go to allow clearance of the ramp while rolling out 7 Carefully roll the cryostat down the ramp At the top of the cryostat you can hold on to the heavy steal ring that encircles the cryostat top Do not grab the aluminum brackets that stick up since these are fragile and must remain aligned for a later assembly step 8 Remove the cryostat cover from the top of the crate and place in a safe location You will install it later A 3 2 Unpack the Cabinet Crate Remove the front and the top of the wider but slightly shorter crate containing the pump cabinet 2 Remove the cables and small accessories from the space above the cabinet and set aside Also remove the wood shelf that is on top of the pump cabinet 3 Locate the ramp from the front of the cryostat cabinet and attach it to the front of the cabinet crate so the cabinet can roll down it Complete the ramp with the short lower section of the ramp also from the cryostat cabinet Roll the cabinet out of the crate and down the ramp Remove the CAN Module Bay and remaining parts from the crate A 3 3 Unpack and Inspect Fittings 1 Remove plastic from the cryostat and cut the ties holding the bundled cables stored on top of the cryostat 2 Make sure none of the VCO type fittings around the cryostat top plate have come loose during shipping There are seven of these
97. le format but export a subset of the data Click Select Data to specify which data items to export o Available data items are listed on multiple tabs o Check the box next to data items to write them to the export file o Specify the order of the data columns in the export file by entering numbers in the Col Order boxes o To exclude data that falls outside a certain range check the Select Range box and specify the range of data to keep Click Export to write the selected data to the exported file You will see a confirmation dialog when the operation is complete 3 6 Temperature Magnet and Cryostat Services Dynacool Services Temperature Service Magnet Service Cryostat Service Running Running Running T CEA Figure 3 15 DynaCool Services Control Dialog The Temperature Magnet and Cryostat services run as Windows services in the background While they can be started and stopped manually normally they start automatically when the computer is started and remain running continuously in the background even 1f MultiVu is not running Any temperature field or cryostat operation requested by MultiVu is controlled by one of these services For example if you enter a new temperature set point into MultiVu the request is passed to the Temperature Service which configures and manages the appropriate hardware components While the services do not have a user interface their operation is indicated by
98. ll Plots to apply the appearance settings to all plots in the graph window Plot 1 Appearance Wt Horizontal Grid Lines W Vertical Grid Lines Apply Show Data Markers Cancel Show Lines gt Show Both Apply to All Plots Figure 3 13 Plot appearance dialog 3 5 3 Template and Graph Files Groups of graph view settings may be saved in template files tpl and applied to other data files so the graph view of each data file will look similar The settings saved in template files include all settings in the Data Selection and Plot Appearance dialogs This feature helps view many different data files in the same graphic format The settings are specific to files a given type so applying a template file from a Log Data file to a VSM Data File will yield unexpected results A graph file gph is a template file that MultiVu automatically applies to the data file dat with the Same name whenever the data file is opened in graph view You may save template files as graph files gph but it is not necessary to do so MultiVu automatically saves a graph file for each data file whenever all graph views are closed so that the graph view of the data file will look the same next time it is opened To save a template file format the graph view as desired then o Select File gt Save Template OR o Select Graph gt Save Template OR o Right click the graph view window and select Save Template
99. located in the side of the pump cabinet This breaker should be off when opening the side panel on the cabinet future expansion NS thermometer amp heater control to cryostat power light for cryostat controller regulated power breakers for CAN out CAN network in from module bay gt CAN network out with terminator reset button cryostat controller only E cryocooler control to compressor valve amp flow control to cryostat Figure 2 7 Connectors to the Cryostat Controller electronics on the back of the Pump Cabinet Figure 2 7 shows the vertical back panel of the Pump Cabinet with the connectors to the cryostat controller electronics The cryostat controller contains thermometer bridges heater drivers valve drivers and various other instrument electronics for communicating with the cryostat and the cryocooler compressor Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 2 9 November 2011 Section 2 2 Chapter 2 System Hardware Components Hardware 224 Cryocooler Compressor Assembly helium return low start button A T helium send high stop button meet g kaa e compressor control serial power switch cold head power main breaker S 2 Ne service valve amp port 3 phase cooling water power inlet OS out amp in Figure 2 8 Helium Compressor Figure 2 8 shows the cryocooler compressor This unit drives the high pressure
100. mGas Supply Cynder esis Maleate cadeatant inte eit ya taueda anes a Aeneas 5 1 33 Replacing the Scroll Pump tip Seals Varian SH110 Scroll Pump osssooononneneessesssssssssseeerrsssssssssssssse 5 3 54 JTnspeciina and Maintains O N Soari erar E E E EAA e O E a EEEE 5 5 5 5 Replacing Busessand Reset Break ers nenea a a yeaa sa gee siaeu teen tonne aterees 5 5 5 5 1 Pump Cabinet P wer Input Breakers actinia e E E eta hate tee i 5 5 392 Pump Capiiet Extemal24 V Break Seo n A E T EA OA 5 6 5 5 3 Cryostat Controller Board FUSE Sree e a A 5 6 5 5 4 Magnet Controller Fuses and Breakers nnenneessessssssseseeeerrressssssssssssssssesetreersssssssssssssseeereressssssss 5 7 5 5 5 CAN Module Bav FUSES reann AA 5 7 5 6 shuttins Down the DynaCool System gccsciaicsee cceaceniactien eden vecunssenek E a E NE TKE 5 7 5 7 Saarne up a Colds DynaGool Sy Steniesstessci tnt sacicstae i tout at ores tenet E dovdaviaieventaeds 5 8 5 8 Compressor Adsoroer Replacement eaaa a E A nanan alates E 5 8 S9 Regord Manem LOS corporea EE pee eeseoeuneiiakeanes 5 8 APPENDIX A SySteni SCP eai E E E A 1 Al OVON OW mienge E E E ETA E E A A 1 A2 Sle REQUIFCINCINS hss ad cas odees iecechasacsasceaecihaeiesurecuiscuGieiucimees E E A 1 wW Saa Oe a EN E N A 1 A 3 1 Unpack the Cry OSIAE E AC iar scene intusatutanuatediua subi attns E S A 2 ROD Mpa thet bnet Crate e a a a ders dica ea tammeutucds A 2 A 3 3 Wn pack and IMS Pe CU PiU s Sorring aa a a a N A 2 A 3 4 Co
101. mme ce NI aan EEC Omit OIC sf acsac ashi strat seta a ute aeamatisa ienoe dausaauby vaseiategmnaeaussardamaeeditanas A 3 A 3 5 Makat abime OnnG CUONS siesena enn EAE EAE deine wail AN A 3 ASO Mo ntand Connect Me CAN Module Bay vic wait A A aie avennsieuatess A 3 A 3 7 istal Helium Gas RE SUIALOL sa noveccnanastecvercacetceoterenevoureiec nates ENEE a E ITEE ENEA E E ENEE PESER A AKERE ESEE A 4 A 3 8 Make COomipressor CONNEC COONS wc xn ssssccnsctacconesspinacsletanareteaneesdbedsanutibs Saeidat ateudtonidtees E A 4 A 3 9 Power up eS yS EIE 5 cts advances tusateste E E A 4 AS AO Attach Deck and Cryostal COVER aiserosce enteren aae OE E A 4 APPENDIX B Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO V November 2011 Contents Table of Contents Dianos tic SOWAT Caaan a a ewe eat aa B 1 BA OC VAC W aeoea EE E EE EE B 1 Be TOG Data eena EE E E EE E EE E B 1 B 2 1 Sandar TEMS ea a a a Ve Ont samines nae Aus nda aaoonwes B 2 B 2 2 PATO SUC Mem erennere e e E A al as B 3 B 2 3 Aneen EE EN B 3 Bo Backeronnd EOS eere E e a E B 3 B4 Eyventand Emor Cos Cie srnnin E a B 4 B 4 1 Nuli VEV nE EOT a a a a a a rte B 4 B 4 2 Temperature Magnet and Cryostat Service Logs sseseoeeeeessssssssssssssettrerresrressssssssssseseeeeeersessssss B 4 B 4 3 ODOR LOS DINGS onnon E a a E Mosente ivesaoasts B 4 APPENDIX C Pin out and Interconnect DiagramS eseesosesessoseseososeseososeseososeseososeseososessososcssososessososessos
102. n The compressor is a fairly noisy piece of equipment compared to the rest of the instrument Therefore you may wish to locate the compressor in a space that is separate from the DynaCool cabinet and cryostat In this case provision must be made to run the high pressure helium lines between the compressor and the cryostat Initial Installation Quantum Design service personnel will typically perform system set up It is possible for you to set up the equipment yourself so instructions are included here Please read this section and contact Quantum Design service before attempting to set up the instrument Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO A 1 November 2011 Section A 3 Appendix A Initial Installation System Setup Please refer to the DynaCool Installation Video for detailed installation instructions A 3 1 Unpack the Cryostat Crate 1 Remove the fasteners holding on the front side of the tall crate containing the cryostat The front side of the crate forms the upper ramp section for rolling the cryostat out of the crate Remove the ramp and flip it around and place against the crate base to form the start of the ramp Locate the lower section of the ramp inside the crate it may be screwed down and need to be removed and complete the lower section of the ramp with this Inside the crate remove the foot braces that prevent the cryostat from rolling around in the crate Remove the upper braces ho
103. n 9 T DynaCool systems contains two 8 Amp 20 mm delay type fuses in its power entry module There is also a switch not a breaker on the power entry module Before servicing these fuses turn this switch to the off position and disconnect the power cord from the magnet controller The magnet controller on 14 T DynaCool systems has a 16 Amp breaker switch in its power entry module There are not fuses in the power entry module on 14 T systems Normally the switch on the magnet controller is left in the On position and the MAG PWR 10 A or MAG PWR 12 A pump cabinet power input breaker is used to turn the magnet controller on and off CAN Module Bay Fuses Before servicing any of these fuses turn the CAN module bay power off using the switch on the back panel and disconnect the power cord The power entry module on the rear panel of the CAN module bay contains two 6 3 Amp 20 mm delay type fuses There is also a switch not a breaker on the power entry module The rear panel of the CAN module bay houses four additional fuses F1 F2 F3 and F4 All four of these fuses are 5 Amp 3AG standard fuses Fuses F1 and F2 control 24 VDC power to JQR 1 JQR 2 on the rear panel of the module bay and JQR 9 on the front panel of the module bay Fuses F3 and F4 control 24 VDC power to JQR 3 and JQR 4 on the rear panel of the module bay The breaker labeled AC OUTPUT on the rear panel of the module bay is a 5 Amp breaker that switches 2
104. n the sequence as soon as the temperature is set not when the temperature set point is achieved To wait for a stable temperature before executing the next command use the Wait command PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Software 3 5 Quantum Design Section 3 5 Graphing Data Files Shutdown Places the instrument in shutdown mode to conserve resources The field is set to zero the magnet controller is turned off the chamber heaters are turned off and the chamber is sealed Wait Waits for specified conditions to be achieved then delays a specified amount of time before continuing with sequence execution Conditions that can be specified to wait for are temperature stability field stability and chamber state This command is usually used immediately after another command in order to make sure the desired outcome of the first command is achieved before proceeding For example Set Temperature 77K at 10 K min Fast Settle Wait For Temperature Delay 10 secs No Action Measure Moment vs Field This sequence will wait 10 seconds after the instrument has achieved temperature stability at 77 K before beginning a series of moment measurements at various magnetic fields Specify also what the instrument should do if an error occurs while waiting for the specified conditions no action abort sequence or shutdown instrument 3 4 5 2 MEASUREMENT COMMANDS Log Data
105. nants in the chamber The second stage of the cryopump pumps the helium gas that is left behind after purging High Vacuum Valve Controls connection between chamber and cryopump The state of this stepper motor controlled bellows valve is stored in memory in the Cryostat Controller When the Cryostat Controller boots up it closes this valve to put it in a known state Chamber Isolation Valve Controls connection between chamber and chamber case gas line It is a normally closed solenoid valve Helium Vent Valve Controls connection between chamber gas gas line and helium supply line It is anormally closed solenoid valve Flush Valve Controls the connection between chamber case pump and chamber case gas line It is anormally closed solenoid valve Chamber Vacuum Gauge Records the pressure in the sample chamber Cryopump Heaters Apply heat to cryopump in order to regenerate it With the exception of the Chamber Pressure Gauge all of these components are controlled by the Cryostat Control Electronics 4 5 1 Chamber Operations DynaCool supports several chamber operations described below It is important to note that any chamber operation involving pumping should be performed only when the sample chamber KF flange is sealed Otherwise the chamber will not be pumped down as desired during these operations Quantum Design Seal Sealing the chamber simply closes all valves leaving the chamber atmosphere unchanged Purge and Seal
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107. of the cryostat to open the sample chamber After closing the sample chamber you can click Purge Seal to vent and flush the chamber with helium gas from the bottle Note that you can also bring up these instrument control dialogs by clicking on the corresponding panel in the status bar at the bottom of the DynaCool MultiVu window Installing and Removing Samples The Puck Sample mounting varies widely depending on the type of measurement you perform You should consult the appropriate measurement option manual for information about sample mounting methods However for most measurement options the sample holder is some variation on the basic PPMS puck design Figure 1 3 Example of a puck When installed into the DynaCool sample chamber this puck provides the sample with both electrical and thermal contact to the chamber Installing a Sample Puck A puck that you are installing in the sample chamber may have your sample mounted on it or it may have measurement hardware on it e g VSM coil set Either way use the following procedure to install a puck For a puck with a sample on it you should use the measurement option sample installation wizard to walk you through this process because the wizard also guides you through other important tasks such as setting up a data file The measurement option will not give you detailed instructions on use of the puck insertion tool so be sure to read these instructions first Q
108. on Pump Cabinet Flush Valve gt lt Chamber Case whence e ent Pump Chamber SAUL Wen Regulator Valve Helium gt o Supply Air Vent Valve gt q Ambient Chamber Air Top flange Chamb r ___Chamber Case High Vacuum teoiation Line Valve Case Valve v gt i YAN l Sample Chamber Cryopump First Stage Cryopump Second Stage m mm ee ee e m e e e e e m Figure 4 2 The DynaCool Cryostat showing components of the Chamber Atmosphere Control System and Case Vacuum System All items not shown in the box labeled Pump Cabinet are located on or in the cryostat Refer to Figure 4 1 for details about cryostat components not labeled in this figure 4 14 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Theory of Operation Section 4 5 Chamber Atmosphere Control System The chamber atmosphere control system consists of the following components most of which are shown in Figure 4 2 Chamber Case Pump Evacuates the chamber to pressures as low as 1 Torr Helium Vent Gas Vents chamber up to about 1 atmosphere with helium gas The pressure of gas entering the chamber is controlled by the chamber regulator on the pump cabinet manifold This regulator is set at the factory Cryopump Evacuates chamber to high vacuum when High Vacuum Valve is open The first stage of the cryopump pumps condensable gasses such as air and water which are present only as contami
109. on first set up the option hardware as described in the option manual Then select the menu item Utilities gt Activate Option You will be presented with a dialog showing available measurement options Select the desired option and press the Activate gt gt button The option software will start within the MultiVu window and will initialize the option hardware The measurement option will display a control center from which you can Configure the option Insert and remove samples e Set up data files e Perform immediate mode not sequenced measurements To perform sequenced measurements you write and execute a sequence in MultiVu as described in Section 3 4 1 VSM Log 2 VSM Sequence Command fe tf _ oro A r seer t Soat Aira wey DEUOSS Lt mR amp gt inaj Sebcted Sequence Sequence Commande Sequences seq Syston Canmante Jaen a Sequence o Soio Seque ce Status hoentes Nane Sequence lde Joma Ste Fale Soun Tomporatuc Sean T Cie i Pa neken ee F ab roe shade we crate a Messuerent Conrands oc Data CAND E na Unale te bilake Huka uduk SeaeliN ede Signa o Daa Iretalaing VSN modde a VSH CAN ID E ro Unable to males USA modiis Gasch iodel Ady Maange Unace to rvtialre VEM modde Carter S angi Papalia Crerenerr VS Not Fuly Monert vs Feki Honert ve Teme Nowe Data te u gt VSN SIM No Datafile nda Data Fie Savpe Advanced Diegroehe Chante Status Cotiau Hesuing
110. on software In MultiVu select the menu item Utilities gt Activate Option You will be presented with a dialog showing available options Select the desired option and press the Activate gt gt button The option software will start within the MultiVu window and will initialize the option hardware 4 Install your sample Use the measurement option installation wizard because it guides you through all the necessary steps including setting up data files and entering sample properties 5 Perform an immediate mode measurement using the measurement option control panel in order to verify that everything is working correctly 6 Write a sequence to automate the measurement Execute the sequence and allow the instrument to acquire data See Section 3 4 for information about writing and executing sequences 7 You can graph your measurement data while it is being acquired To open the data file from an activated option please see Section 3 5 8 When the measurement sequence is complete remove your sample using the option s wizard Then either install a new sample to measure or go back to step 1 to use a different measurement option 1 10 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 C H A PTER 2 Hardware 2 1 Overview This chapter describes the DynaCool hardware and contains instructions for operating some hardware components Be sure to read Chapter 1 Getting Started before read
111. ons and to help maintain and troubleshoot the instrument including cooling the system down and logging diagnostic data See Appendix B for more information WINDOW Window menu helps arrange the open windows in MultiVu HELP Help menu contains version and serial number information about DynaCool and access to the user documentation PPMS DynaCool User s Manual 1307 110 Rev AO 3 3 November 2011 Section 3 2 Chapter 3 MultiVu Software 3 2 2 Tool Bar New Sequence Lock Sequence Open Sequence Abort Sequence Save Sequence Pause Sequence y Run Sequence Open Graph File j Print P P About Open Data File i Copy Cut Figure 3 4 Tool Bar The Tool Bar contains shortcuts for common menu items 3 2 3 Control Center The Control Center Figure 3 5 shows the currently selected sequence file name and sequence execution status In addition there are buttons to change the selected sequence and edit run pause abort or lock the selected sequence Selected Sequence Sequence eq E dit Change Sequence Status Sequence Idle i Rur Pause Abort Lock Figure 3 5 Sequence Control Center rE 3 2 4 Sequence Command Bar The Sequence Command Bar Figure 3 6 is shown when you edit sequences You can toggle its display by selecting the View gt Sequence Command Bar entry while editing a sequence It contains commands you may insert into the sequence Commands are organized in a tree struc
112. opump chamber consisting of cold metal surfaces at about 70 K and charcoal cooled to about 4 K by the cryocooler system in the cryostat The high vacuum valve isolates the sample chamber volume from the cryopump chamber when high vacuum is not required Long term operation of the cryopump requires that the contaminant gases and adsorbed helium be removed from the metal surfaces and charcoal This process is called regeneration and is performed during a standard cryostat startup operation when the cryostat is still warm The capacity of the DynaCool cryopump is such that it should not require regeneration more often than the cryostat itself requires regeneration Heaters on the cryopump make it possible to regenerate the cryopump while the cryostat is cold Contact Quantum Design Service if you need to perform this operation You can prevent the need to perform an unscheduled regeneration by keeping the sample chamber clean Avoid placing wet objects such as a cold baffle set that has condensed water on it in the sample chamber Be sure to purge and seal the sample chamber before attempting to set high vacuum 2 3 5 Puck Adjustment Tool The puck adjustment tool Figure 2 13 is used to adjust the position of the fingers of the puck so that the fingers maintain solid thermal contact with the thermal interface located at the bottom of the sample chamber This is especially important for measurement options such as Heat Capacity or VSM Oven where the pu
113. osessososessososesses C 1 Col SOVEN IOW onei ERE TOET ANTO TO AE Go ONT EE C 1 C2 Sample Puck Connections Gray Lemo and JOP S sisitscntate suet snensoeeseinshdovesaandaeeonveneebedateh rS C 1 Co Temperi ConmolJOP I ea T E E E C 2 C4 Cryostat Temperature Control JOP hersien a once C 4 APPENDIX D Usine Third party Instruments ciori iior an aT NN OEE AEN D 1 B3 OVV Wa a S a a a ted es gated atanetenegaeatet D 1 D 2 WinWrap Visual Basic Scripting in Multi Vu eeeeeeesssssssssssssseeeeresssssssssssssseeceeeeressssssssssseeeeseeeessssss D 1 DS Nationalin mument LabVIEW Oedse p EE E EEEa D 2 D 4 Object Linking and Embedding ActiveX ccccccccecececeeeeceeeeeaeeeseeseeeeeeeeeeeeeeeeeaaaseaasseseeeseseeeeeeeeeeqaaas D 2 vi PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Contents Figures Figure 1 1 Figure 1 2 Figure 1 3 Figure 1 4 Figure 1 5 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 2 15 Figure 2 16 Figure 3 1 Figure 3 2 Figure 3 3 Figure 3 4 Figure 3 5 Figure 3 6 Figure 3 7 Figure 3 8 Figure 3 9 Figure 3 10 Figure 3 11 Figure 3 12 Figure 3 13 Figure 3 14 Figure 3 15 Figure 4 1 Figure 4 2 Figure 5 1 Figure 5 2 Figure 5 3 Quantum Design Table of Figures Photo of the Computer
114. ower 3 5 2 Pump Cabinet External 24 V Breakers There are two breakers located on the back of the pump cabinet under the label EXTERNAL see Figure 2 7 These breakers switch 24 VDC power to the CAN OUT connector labeled JQQ 3 Normally there is only a CAN termination dongle connected to JQQ 3 When one of these breakers trips a white section appears Push on the lever near the white section to reset the breakers 5 5 3 Cryostat Controller Board Fuses The cryostat controller board utilizes four fuses To access these fuses first shut down the computer power down the entire system using the MAIN PWR breaker and then disconnect the system from the wall power outlet Then remove the right panel from the pump cabinet by removing the two screws near the back of the panel and then pulling on the panel to disconnect the ball studs that hold the panel onto the cabinet The fuses on the cryostat controller PC board are F1 and F2 5 Amp 20 mm delay type These fuses control 24 VDC power to the controller board F3 and F4 10 Amp 20 mm delay type F3 controls 240 VAC power to the circulation pump and F4 controls 240 VAC power to the chamber case pump 5 6 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Maintenance and Servicing 5 5 4 5 5 5 5 6 Quantum Design Section 5 6 Shutting Down the DynaCool System Magnet Controller Fuses and Breakers The magnet controller o
115. pressor see Figure 2 8 e To prevent electrical shock disconnect the system from power before you install it adjust it or service it e The instrument must be plugged into a 200 240 VAC 50 60HZ outlet fused to 30 A e For continued protection against fire hazard electric shock and irreversible system damage replace fuses only with same type and rating of fuses for selected line voltage Information about user accessible fuses and their replacement is summarized in Section 5 6 e Keep this system away from radiators and heat sources Provide adequate ventilation to allow for air cooling around the instrument and compressor e Do not obstruct the ventilation openings in the front and back of the pump cabinet The ventilation openings in the front of the cabinet face down and are located between the light gray and dark gray sections e Do not obstruct the ventilation openings on the left side of the CAN module bay e Take care not to damage the high pressure helium gas lines which contain helium at approximately 2 MPa 300 psi Do not bend the lines tighter than 30 cm 12 inches radius Do not damage the lines with sharp objects and do not place any objects on top of the lines Damage to these lines could cause sudden release of high pressure gas e If this system is used in a way not specified by Quantum Design then the protection provided by the equipment may be impaired Xil PPMS DynaCool User s Manual 1307 110 Rev AO Quan
116. pter 3 Software o Selecting Run Sequence gt OR o _ Selecting the menu command Sequence gt Run OR o _ Selecting the Run button on the control center The status bar and the control center both display the status of the sequence execution The sequence window also highlights the line currently being executed in green The toolbar Sequence menu and command center all provide the ability to pause uf and abort m sequence execution also When paused the sequence window highlights the active line of the sequence in yellow Locking Sequence Execution When the sequence execution is locked a sequence cannot be run paused or aborted without first unlocking sequence execution You cannot exit MultiVu when sequence execution is locked No key or password is required to lock or unlock sequence execution The feature is intended only to prevent careless and accidental interference with instrument operation It is not a security device and does not protect against malicious behavior The instrument does not need to be running a sequence to lock sequence execution Lock sequence execution by clicking Lock Sequence l selecting the menu item Sequence gt Lock or click the Lock button on the control center Type in your name and additional information so other users know why the sequence is locked then click the Lock button All run pause and abort controls in the graphical user inter
117. pty the helium supply bottle High Vacuum This operation uses the cryopump to pump a high vacuum typically lt 10 Torr in the sample chamber First the chamber case pump evacuates the sample chamber to lt 5 Torr Then the high vacuum valve is opened exposing the sample chamber to the cryopump The system declares high vacuum when the pressure gets below 5x10 Torr 4 6 Case Vacuum System The cryostat vacuum case must be maintained at high vacuum in order to thermally isolate components at different temperatures DynaCool maintains its vacuum case without the need for user intervention or any high vacuum pumps The case vacuum system consists of the following components most of which are shown in Figure 4 2 Chamber Case Pump Evacuates case to 2 Torr Flush Valve Controls the connection between chamber case pump and chamber case gas line It is a normally closed solenoid valve e Case Valve Controls connection between chamber case gas line and vacuum case It is a normally closed solenoid valve Air Vent Valve Allows air to be vented into the chamber gas gas line and from there to the vacuum case when the case valve is open It is a normally closed solenoid valve e Charcoal Sorbs Adsorb gasses in vacuum case that are not removed by chamber case pump In addition to these components the chamber vacuum gauge is used to monitor the cryostat vacuum case pressure during some operations The chamber isolation valv
118. r 5 Section 5 9 Maintenance and Servicing Required Maintenance Log Maintenance Log DATE E On WORK PERFORMED BY AFFILIATION WORK COMPLETED Replace compressor adsorber LI Replace scroll pump tip seals L Other explain COMMENTS Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 5 15 November 2011 A P P EN DI XK A System Setup A l A 2 A 3 Overview This appendix contains instructions to physically install and set up DynaCool Once you have completed the steps described in this appendix refer to Section 1 4 to start up also called cool down the system Site Requirements Before installing the DynaCool system you should determine where to place the equipment The pump cabinet and cryostat should be placed next to each other preferably with the cabinet to the left of the cryostat as shown in Figure 1 1 The floor space required for these two components is about 3 m wide by 2 m deep The cabinet requires a 30 amp 220 VAC 50 60 Hz power connection Casters are provided on both the cabinet and cryostat so moving the systems on a flat hard floor is relatively easy The compressor assembly must be located within about 30 m of the cryostat While the compressor itself requires only about a 1 m square floor space the stiff high pressure helium lines have a large bending radius and may require an additional meter to make a 90 degree turn The compressor requires cooling water and a 3 phase power connectio
119. r at 4 2 K This temperature maintains 1 atmosphere pressure above the liquid in the bucket in order to drive helium flow for sample chamber temperature control The bucket pressure is reported in MultiVu Log Data as Tank Pressure Torr During the Warm Up operation the first and second stage heaters are used to rapidly warm the first and second stage to 300 K PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Section 4 3 Theory of Operation Chamber Temperature Control System 4 2 4 4 3 4 3 1 These thermometers and heaters are all controlled and read out by the cryostat controller electronics located in the pump cabinet The Cryostat Service see chapter 3 orchestrates the control of the cryostat The Cryostat Service receives requests for cryostat modes such as Startup then sends commands to the Cryostat Control Electronics to achieve the desired results The Cryostat Service also monitors the system when it is cold in order to ensure proper operation Startup Operation The Cryostat Control System is completely automated by the DynaCool software Therefore starting up or cooling down the system from a room temperature state is accomplished simply by pressing the Startup button in the Cryostat Monitor The DynaCool software then performs the operations described below These operations involve systems described later in this chapter Purge cryostat vacuum cas
120. r to quickly cool the high neck to 220 K before the system enters low temperature mode 4 3 3 Temperature Control Electronics and Software Three electronic modules are involved in temperature control Temperature Control Module Located in CAN module bay The Temperature Control Module TCM reads out the block thermometer neck thermometer and high neck thermometer The TCM also provides heater current to the block heater neck heater and high neck heater based on feedback temperature control using thermometer readings e Cryostat Control Electronics Located in pump cabinet The cryostat controller electronics control the mass flow controller for main flow the impedance heater and the pot heater The Cryostat Control Electronics also turn on and off the circulation pump and control solenoid valves as needed Cryostat Utility Controller Located on cryostat top plate The cryostat utility controller reads out the liquid level sensor located in the bottom of the cooling annulus Temperature control is orchestrated by the Temperature Service The Temperature Service receives temperature set points and then sends commands to the temperature control electronics to achieve the desired result 4 3 4 Temperature Values and Configurations There are several temperature values involved in sample temperature control and sample temperature measurement that are reported in MultiVu Software Option Software and Data Files The meaning of t
121. re for you WARNING Do not open the sample chamber if it is below room temperature Doing so may condense water and air in the sample chamber Such contaminants may form a plug in the chamber resulting in a dangerous over pressure condition on warming 1 8 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 1 Section 1 6 Getting Started Configure Measurement Option and Perform Measurement 2 Verify that the magnetic field is less than 1 T 10 000 Oe If the magnetic field is greater than 1 T set zero field and wait for the field to stabilize before continuing WARNING If you place the sample insertion tool into the sample chamber when the magnet is at high field the insertion tool will be strongly pulled into the sample chamber The force may overwhelm you and cause damage to the instrument Vent the sample chamber with helium An installation wizard may do this for you Open the hinge clamp and remove the KF blank flange and attached baffle set if present from the sample chamber access port If the blank flange is difficult to move due to low pressure in the chamber 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 Disengage the sample insertion tool by flipping up the black switch located on top of the tool or by fully depressing the swit
122. round the regulator fittings could result in most of the gas being lost rather than used in the system 4 Before connecting the helium gas transfer hose to the new cylinder purge the air from the regulator by installing and using the check valve assembly that is supplied with the DynaCool system see Figure 5 2 Open the needle valve to allow gas to flush for several seconds If you can t locate this fitting then skip this step and then be sure to perform 3 or 4 chamber purge operations from MultiVu when you are finished with step 6 Figure 5 2 Check valve assembly for purging air from the regulator of the helium gas supply cylinder part number 4095 243 5 Verify that the regulated pressure is set to 15 2 psi before proceeding Make adjustments as needed and open and close the needle valve to make sure the reading is consistent when closed 6 Remove the check valve assembly and connect the helium supply hose at the double sealing connector and open the needle valve 5 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 5 Section 5 3 Maintenance and Servicing Replacing the Scroll Pump tip Seals Varian SH110 Scroll Pump 5 3 Replacing the Scroll Pump Tip Seals Varian SH110 Scroll Pump Approximately every 6 months it will be necessary to service the circulation pump by performing this tip seal replacement procedure This procedure can be performed on a maintenance schedule or when it is
123. rtup procedure the Cryostat Monitor status will read Cold Cryostat and the Cryostat Status panel will indicate Cold Tank 667 Torr Cold Magnet 4 59 K Figure 1 2 Cryostat monitor status panel showing Cold cryostat 1 4 6 Shutting Down the System and Other Tasks It may be necessary to shut the system down from time to time or perform system level control tasks Please refer to Chapter 3 Section 3 2 8 Cryostat Monitor Dialog for a description of the shutdown and other cryostat commands 1 4 7 Temperature Field and Chamber Commands With the system now ready to be used you can perform various control tasks immediately To set temperature select the Instrument gt Temperature menu item enter a Set Point of 300 K and a Rate of 20 K min and click Set to bring the sample chamber to room temperature e To set magnetic field select the Instrument gt Field menu item then enter a Set Point of 10000 Oe and a Rate of 200 Oe sec and click Set to bring magnetic field to 1 Tesla 1 4 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 1 Section 1 5 Getting Started Installing and Removing Samples 1 5 1 5 1 1 5 2 e Once the sample chamber is stable at room temperature select Instrument gt Chamber and click Vent and Seal to vent up the chamber with helium gas You can then remove the KF flange cover at the top
124. s pressure circulation file name status setpoint State loop pressure execution time setpoint set rate and Status set rate and mode magnet temp mode Figure 3 7 MultiVu DynaCool Status Bar amp Panels 3 2 6 Sequence Window The Sequence Window is used for editing sequences More than one sequence window may be open at a time The selected sequence is always the sequence in the last sequence window that was active clicked The control center reports the selected sequence file name The selected sequence is the sequence into which commands will be inserted when selected with the sequence command bar The Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 5 November 2011 Section 3 2 MultiVu 3 2 7 3 2 8 3 6 Chapter 3 Software selected sequence is also the sequence that executes when Run Sequence is selected when the control center Run button is selected or when the menu command Sequence gt Run is selected Data Windows Graph Record and Table Views Data file contents can be viewed and browsed from within MultiVu using the graph record and table data view windows The Graph View data window shows a data file in graph format Each point on the graph corresponds to a line in the data file and represents a single data record A data record consists of several data items collected simultaneously such as sample temperature magnetic field and magnetic moment You may view a
125. s can be bypassed when running a VBA script directly Novice users should not use this feature Advanced users with programming experience should use this feature with caution Compile and edit the sequence script using the menu commands Sequence gt Advanced gt Compile Macro and Sequence gt Advanced gt Edit Macro A WinWrap Basic editor window will appear Run the script with the menu command Sequence gt Advanced gt Run Macro You will be prompted to locate the script file to run Or you may run the script by clicking the Start Resume button in the WinWrap Basic editor window Find more information about the WinWrap BASIC editor and scripting language by right clicking in the WinWrap BASIC editor window and selecting Help gt Editor Help and Help gt Language Help Running Sequences If the sequence file you want to run is not open you need to open it Open an existing sequence file by clicking Open Sequence B or selecting the menu item File gt Open gt Sequence You will be prompted to locate the file you want to open To execute a sequence it must be the selected sequence If more than one sequence window is open make sure the selected sequence is the sequence you want to execute Execute the selected sequence by Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 11 November 2011 Section 3 4 Sequences 3 4 4 3 4 5 3 12 Cha
126. sample space to a vacuum of lt 10 Torr This makes the PPMS DynaCool compatible with all existing Quantum Design cryogenic hardware or any other user designed experiments For temperature control DynaCool uses a novel gas flow regulation system to improve both cooling power and temperature stability as compared to the already state of the art PPMS temperature control Along with sophisticated control software this system provides seamless transitions between high temperatures 400 K with minimal cooling power needs intermediate temperatures with rapid slewing and large cooling needs and stable operation near the base temperature lt 1 8 K with cooling provided by evaporating liquid helium With this new control system PPMS DynaCool is capable of cooling a standard PPMS sample puck from 300 K to 1 9 K stable in less than 40 minutes The sample chamber design has also been improved for better thermal uniformity at both low and high temperatures while maintaining the robust 12 pin sample puck interface from the original PPMS Multiple thermometers and heaters manage temperature gradients and ensure smooth temperature control throughout the accessible temperature range The PPMS DynaCool comes with a built in cryopump and vacuum gauge for controlling the sample environment The cryopump can pump out the sample chamber to less than 104 Torr in under 10 minutes This feature is fully integrated allowing you to change the chamber environment during
127. section before using the tool WARNING Read section 1 5 2 before attempting to insert a puck into the sample chamber Failure to follow the directions correctly could damage the system 2 3 3 Sample Chamber Access Port and Chamber Baffles The sample chamber is accessed through the KF 40 flange mounted to the cryostat top plate manifold In order to seal the flange and prevent thermal radiation from reaching your sample you use the baffle set which is attached to the KF blank flange as shown in Figure 2 12 In order to prevent leaks into the sample chamber be sure to keep the sealing surfaces of the KF flange and baffle set clean Also be sure not to damage the O ring used to seal this flange A threaded adapter is present on the end of the rod in order to allow the attachment of accessories such as the contact baffle used with the Heat Capacity and Thermal Transport Options Note that some DynaCool options seal the sample chamber differently and do not use the components shown in the figure _7 HINGE CLAMP KF BLANK FLANG CS YAWWY _ CENTERING RING WITH O RIN CHAMBER KF FLANGE _ BAFFLE ASSEMBLY Ty Figure 2 12 Cross section of Sample Chamber Access Port and Baffle Set Quantum Design PPMS DynaCool User s Manual 1307 110
128. service instructions Chamber Case Pump This is a low capacity scroll pump for evacuating the sample chamber during chamber pump and purge operations Itis also used during initial system startup to evacuate the vacuum case e Gas handling manifold The gas handling manifold contains solenoid valves pressure gauges pressure regulators and various gas interconnections to manage the flow of gas in both the chamber gas circuit and the circulation loop circuit There are several modes of operation this serves Refer to Chapter 4 for more information Cryostat Controller Electronics The cryostat controller electronics contains thermometer and heater circuits for managing the operation of the cryostat The cryostat controller also 2 6 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Section 2 2 Hardware System Hardware Components communicates with the cryocooler system compressor and controls all the gas handling valves and gauges on the gas handling manifold and at the cryostat top plate It operates as Node 5 on the CAN bus Magnet Controller This is the power supply for the superconducting magnet in the cryostat It sources the 55 amps required to drive the 9 Tesla magnet to full field It operates as Node 6 on the CAN bus Personal Computer PC running the Windows operating system and MultiVu measurement software Main 240 VAC power inlet and distribution for the system For
129. single data record in its own window by double clicking any record in the graph view The record view and graph view are linked so that the highlighted point on the graph view corresponds to the record shown in the record view The appearance of the graph view may be manipulated extensively and templates may be applied to the graph view so that you do not need to set each graph characteristic individually To learn more about manipulating the graph view see Section 3 6 In addition to the record and graph views you can also view the data in a table where each row in the table is a data record Right click in the graph view and select Table View to open the table view Cells and groups of cells in the table view can be selected copied and pasted into spreadsheets and other graphing programs for additional analysis using the standard Windows copy and paste features Cryostat Monitor Dialog Dynacool Cryostat monitor Cryostat Monitor Cold Cryostat Cryocooler Running Magnet 4 30 K Holding 4K Plate 418K 1W Shield 51 80 K Loop 643 56 Torr Circulating Liquid Full Case Purged Figure 3 8 Cryostat Monitor The DynaCool Cryostat Monitor is used to perform basic system operations like starting up and shutting down the system It also shows current status and sensor information from the cryostat Open the Cryostat Monitor from the MultiVu Instrument gt gt Cryostat menu item or by clicking on the Cryostat status panel
130. t options that provide a control thermometer near the sample and provide temperature control outside the standard 1 8 400 K range In this mode the Measurement Temperature and Sample Temperature both report the value of the extended range control thermometer The Control Temperature is either the Block Temperature or the value read by a measurement option thermometer Measurement configurations that use this mode include 4 10 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 4 Section 4 3 Theory of Operation Chamber Temperature Control System Measurement Control Sample Measurement Control Configuration Thermometer Thermometer Thermometer Vibrating Sample Magnetometer with Oven Coil Oven Stick Oven Stick Thermometer Thermocouple Thermocouple Block Electro Transport Thermometer or or Resistivity Helium 3 with Helium 3 Sample Thermometer Electro Transport Dilution Dilution or Resistivity Block Refrigerator Refrigerator with Dilution Thermometer Sample Sample Refrigerator Thermometer Thermometer Helium 3 Sample Helium 3 Sample Thermometer Thermometer On Oreo Extended Range Option Temperature Control with Additional Measurement Option Thermometer This configuration is used when the measurement option provides a thermometer close to the sample that is used to measure the sample temperature and an additional option is providing extended range temperature control In this mode the
131. t the 44 pin TCM cable from the cryostat to JG 1 at the temperature control module in the CAN Module Bay Figure 2 3 Connect power cable from outlet on cabinet Figure 2 6 to CAN rack Figure 2 4 PPMS DynaCool User s Manual 1307 110 Rev AO A 3 November 2011 Section A 3 Initial Installation A 3 7 A 3 8 A 3 9 A 3 10 A 4 Appendix A System Setup Install Helium Gas Regulator l Unpack and install the helium regulator onto the helium cylinder Use a wrench to tighten the connection Close the needle valve and open the bottle valve Use soapy water to leak check the fitting Connect the helium supply hose to the double sealing connector at the regulator using two wrenches Connect the other end of the helium supply hose to the VCO connection on the cabinet Figure 2 5 Tighten using wrench 1 8 turn past finger tight Adjust regulator to about 15 psi and open the needle valve Make Compressor Connections 1 Refer to Cryomech instructions for connecting power and cooling water to the compressor unit 2 Connect cold head power cable from the cryostat to the compressor Figure 2 8 Connect compressor control RS232 cable to the 9 pin D sub connector on the compressor Figure 2 8 and connect the other end to the cabinet Figure 2 7 4 Connect the large helium hose from the LOW port on the compressor to the larger of the two helium connections at the back of the cryostat Figure 2 2 Use the prov
132. te that Option Software has configured the system to use a different control thermometer Sample Temperature This value reports the temperature that is being controlled to achieve the desired sample temperature If no extended range temperature option is active this is the same as the Control Temperature If an extended range temperature option such as Dilution Refrigerator is active then this value is measured by an option provided sample thermometer that is being controlled using a feedback loop implemented in Option Software not base DynaCool temperature software This value is reported in the MultiVu status bar in Log Data as Temp K Also the Log Data item Sample Therm ID reports an identification number for the control thermometer A value of 643 indicates the block thermometer Other values indicate that Option Software has configured the system to use a different sample thermometer Measurement Temperature This value is the temperature of the sample recorded in option data files with sample measurement results In many cases this value is the same as the Sample Temperature and may be derived by averaging multiple readings of the Sample Temperature In other cases the Measurement Temperature is derived from option thermometer readings not displayed elsewhere An example is Heat Capacity where the Measurement Temperature is the average of the platform thermometer during the relaxation measurement 4 3 4 2 TEMPERATURE CONTR
133. that the high temperature superconductor and NbTi sections are superconducting and to minimize heat load to the next stage 4 4 2 Magnet Controller and Software The DynaCool magnet controller is located in the center rear portion of the pump cabinet Depending on magnet model a controller capable of sourcing either 60 or 120 A is provided Due to an inherently 4 quadrant design and analog current feedback the system is able to achieve linear field ramps with no discontinuity or kink at zero field and negligible overshoot when stabilizing Magnet control is orchestrated by the Magnet Service in DynaCool Besides sending field set points to the controller the Magnet Service monitors the magnet for quenches and over temperature conditions If such a condition occurs the Magnet Service will instruct the Magnet Controller to discharge the magnet and the Cryostat Service will attempt to cool the magnet as quickly as possible 4 12 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 4 Section 4 5 Theory of Operation Chamber Atmosphere Control System 4 4 3 Magnetic Shielding The DynaCool Cryostat resides inside an enclosure that also functions as a magnet shield The enclosure is constructed of steel in order to reduce the field experienced outside the enclosure The extent of shielding depends on magnet model so see your system specifications for information about stray fields outside the enclosure 4 4 4 Ma
134. the block temperature is slewing at maximum rate Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 5 November 2011 Section 4 3 Chapter 4 Chamber Temperature Control System Theory of Operation The block heater is located below the puck interface Using a tight feedback loop the block heater controls the temperature of the block thermometer at the user requested set point The heater power balances a bias of cooling provided by helium gas flow as described in section 4 3 2 The block heater is also used for controlled temperature ramps and rapid warming of the sample chamber In addition to the block thermometer and heater there are two other thermometer heater pairs on the sample chamber One pair is the neck thermometer and neck heater located just above the isothermal region The other pair is the high neck thermometer and high neck heater located approximately at the vertical center of the sample chamber Each of these pairs is used in a feedback configuration to reduce thermal gradients in the sample chamber After rapid warming of the block from low temperature to room temperature the lower and middle sections of the sample chamber would normally be cold for gt 1 hour The neck and high neck thermometer heater pairs are used to keep the lower and middle sections of the sample chamber close to the block temperature during warming The high neck thermometer is also used to determine when the upper part of the sample ch
135. the cryostat utility controller Node 14 on the CAN bus Both the cryostat cover and the fiberglass side panels are attached to a steel magnet shield The lower part of the shield is shown in the figure With 9 Tesla systems this shield maintains less than 5 gauss stray fields very near the exterior surface of the cryostat cabinet allowing it to be installed close to other sensitive instruments in a laboratory The current sample temperature and magnetic field are displayed on the two red LED displays on the front of the cryostat Note that the sample temperature may be different than the temperature of the sample chamber itself For example when operated with the Dilution Refrigerator the temperature displayed would be that of the sample platform on the refrigerator See section 4 3 4 for details The sample chamber access port is shown on the top of the cryostat This port is a standard KF 40 flange the same as the standard PPMS All samples and experiment probes are inserted here The front deck is meant to stand on when installing and removing samples and measurement hardware The deck is designed to be removed if needed to fit through small doorways PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Section 2 2 Hardware System Hardware Components A high pressure helium from compressor low pressure helium moisture wick to compressor Figure 2 2 Back base of cryostat
136. the icon se located in the Windows tool tray in the lower right of the screen Double click this icon to open a utility see Figure 3 15 to start and stop the Services Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 3 19 November 2011 C H APTER 4 Theory of Operation 4 1 Overview This chapter describes the functional subsystems of PPMS DynaCool The information in this chapter is not necessary for normal use of DynaCool but will help you understand the underlying principals of the system s operation The subsystems and their respective sections are Section 4 2 Cryostat Control System maintains cryostat components at appropriate temperatures for normal operation Section 4 3 Chamber Temperature Control System controls the temperature of the sample chamber and sample puck contained inside it Also provides cooling and heating for insert probes such as the Helium 3 Refrigerator and Dilution Refrigerator Section 4 4 Magnetic Field Control System controls the magnetic field at the sample location Section 4 5 Chamber Atmosphere Control System controls the atmosphere inside the sample chamber Typical states are vented 760 Torr of helium gas purged 1 Torr of helium gas and high vacuum Section 4 6 Case Vacuum System prepares and maintains proper cryostat vacuum to allow the cryostat to achieve low temperatures The subsystems interact in many ways and even share components None
137. theless it is helpful to break the system down into subsystems in order to understand their operation 4 2 Cryostat Control System The Cryostat Control System is responsible for keeping the cryostat components at the correct temperatures to allow normal operation of the rest of the subsystems Figure 4 1 shows a diagram of the components described in this and the next two sections Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 4 1 November 2011 Section 4 2 Chapter 4 Cryostat Control System Theory of Operation Pump Cabinet p Bypass Circulation Ha tas Valve Pump alve xhaust Annulus Pumping Helium Line Chamber NL Supply Top flange Fill Biei Return Valve Regulator Sample Gas Line Chamber i l Ow LP ais Cooling Cryostat Annulus Vacuum Case Main Cooler _ First Stage re i Cooler i Second Stage i i Bucket Annulus i AARG j Counter flow l Heat 4K Plate i Exchanger i Helium Gas Magnet l Helium Liquid i i Isothermal r Region I j Sample i Puck i Liquid i Level i Sensor Case Nacuum Po ll Figure 4 1 The DynaCool Cryostat showing the components of the Cryostat Control System Chamber Temperature Control System and Magnetic Field Control System All items not shown in the box labeled Pump Cabinet are located on or in the cryostat 4 2 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 201 1 Chapter 4 Section 4 2
138. til the commands within the loop are completed This is intended for use with highly temperature hysteretic samples Sweep Controller will drive directly from the initial temperature to the final temperature without stopping Each time a temperature increment defined by the command is reached the commands inside the scan temperature loop will be executed but the temperature will continue to change while they execute Scan Time Creates a program loop for executing repeated commands at user defined time increments or immediate repetitions with no time increment All commands between the Scan Time line in the sequence and the End Scan line in the sequence will be repeated at each time specified by the scan time command Set the total time in seconds and specify whether the spacing of events should be uniform in time or logarithmic in time And specify the number of steps This is the number of times the loop will be repeated For uniform spacing in time you may alternatively specify the time increment If the total time is set to zero seconds then the number of steps defines how many times the loop will be repeated in rapid succession Sequence Message Displays a message on the computer screen and pauses sequence execution until the message is acknowledged or until a timer expires If the computer is set up with network access and access to a mail server a message can also be emailed with attachments such as data files
139. tions like the VSM provide an integrated thermometer on the puck assembly close to where the sample is positioned See Sections 4 3 1 and 4 3 4 for details about thermometry The base of the basic puck contains 12 solder pads to allow connection of the sample or other measurement option hardware to the experimental sample wiring These solder pads are connected to a set of 12 sockets on the base of the puck which contact pins in the bottom of the sample chamber Most option specific pucks are pre wired for a specific type of measurement like for example the ETO option pucks that extend the electrical connection to a convenient mounting frame on the top side of the puck The puck is keyed to ensure that the electrical connectors properly align See Section 2 3 7 for details on experimental wiring See Appendix C for an experimental wiring pin out diagram 2 3 2 Puck Insertion Tool The puck insertion tool is a long rod used for installing pucks 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 1 4 When the lever is engaged the tool grips the puck by a groove in its outer rim Figure 2 11 Puck Insertion Tool with Level in Engaged Position 2 12 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 2 Section 2 3 Hardware Measurement System Hardware The puck insertion procedure is described in Section 1 5 2 Please read that
140. tum Design November 2011 C H A P T E R 1 Getting Started 1 1 Overview This chapter provides a brief introduction to DynaCool and describes how to perform some common tasks Be sure to read the rest of the manual to become familiar with the details of the system 1 2 Introduction to PPMS DynaCool Figure 1 1 Photo of the Computer Pump Cabinet and Cryostat The Quantum Design DynaCool is an instrument designed to measure a variety of a sample s physical properties while controlling the conditions experienced by the sample The Quantum Design DynaCool is a next generation Physical Property Measurement System PPMS The PPMS DynaCool is a completely redesigned instrument that provides all the capabilities of the Quantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 1 1 November 2011 Section 1 3 Chapter 1 How to use this Manual Getting Started PPMS without the need for any liquid cryogens The system uses a single two stage pulse tube cooler to cool both the superconducting magnet and the temperature control system providing a low vibration environment for sample measurements The PPMS DynaCool employs a minimum amount of condensed liquid Helium 4 for cooling both the sample chamber and superconducting magnet As a result the system requires only a small volume of bottled helium gas for its fully automated startup and operation The PPMS DynaCool also comes standard with an integrated cryopump used to pump out the
141. ture Click and to expand or collapse tree branches Double click commands to insert them into the sequence 3 4 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Section 3 2 Software MultiVu Measurement option sequence commands are present in the Measurement Commands branch when a measurement option is active More on sequences is found in Section 3 3 Sequence Commands E System Commands Beep Call Sequence or Script Chamber Operations Remark Scan Field Scan Temperature Scan Time Sequence Message Set Field Set Temperature Standby walt El Measurement Commands Log Data Sigma Log Data Figure 3 6 Sequence Command Bar 3 2 5 Status Bar The Status Bar contains information about the status of the instrument Click on the panels in the status bar to access dialogs for setting temperature magnetic field and chamber atmosphere actions Click on the Cryostat status panel on the right to open the Cryostat Monitor dialog see Section 3 3 8 for system startup shutdown and other maintenance operations Sequence Idle 246 47 K Stable 0 11 Oe Holding 0 00 mTorr Tank 643 Torr l Seq lt none gt Set 246 47 E Set 0 00 Oe Sealed Cold lt none gt 10 00 K min Fast Settle 100 00 Oesec Linear Magnet 4 30 K Cryostat and sequence Temperature Magnetic Field sample Chamber Cryocooler status sample temp and field and statu
142. uantum Design PPMS DynaCool User s Manual 1307 110 Rev AO 1 5 November 2011 Section 1 5 Chapter 1 Installing and Removing Samples Getting Started 1 Disengage the sample insertion tool by flipping up the black switch located on top of the tool or by fully depressing the switch WARNING The part of the puck insertion tool shown at the bottom of Figure 1 5 is very fragile Even a smallest dent in this rim will prevent it from properly engaging a puck i l x 4 y oe ie cf cial ts if z z F se Me ia iia n eth aa ee gat ga Sa l ja j pa z a a is n A E n Peai ate ea ae ee ERNI hre ea i a a cone I M a ai EI RERE H i Si S aa aeaaeae ii me aie oe r a z z Aaa R m ii aS i E E A a S S i h h ik i ii i e k e ik i R a i i oe i E g i i a e i a r3 bata bate hate ate fata ate ie r H ki Fa mh Fa E ti a ae aa a Ha sm ate E i ea n cath ue i S r Disengaged Disengaged Engaged Figure 1 4 Operation of puck insertion tool 2 Insert the puck with the sample facing upward inside the hollow cylinder that is at the bottom of the sample insertion tool The sample will be inside the cylinder and the connectors and solder pads will be outside the cylinder Figure 1 5 Puck insertion tool connecting to puck 1 6
143. uestions about system maintenance The DynaCool system is designed to operate with minimal maintenance for 20 000 hours about two years Quantum Design recommends that you have the DynaCool system serviced every two years Some services must be performed only by a qualified Quantum Design representative Contact your local Quantum Design representative to schedule the maintenance visit The following sections describe various maintenance procedures you might need to perform on your DynaCool system Changing the Helium Gas Supply Cylinder Periodically you will need to change the helium gas supply cylinder that is used to supply helium to DynaCool Itis recommended to monitor the gauge on the cylinder pressure regulator and to change the cylinder before it is completely depleted This is because an empty bottle will interrupt normal chamber gas handling operations and other automated procedures such as System Startup and possibly result in unpredictable behavior For a standard K size cylinder Quantum Design recommends changing the cylinder when the pressure falls below 300 psi It is not necessary to shut down or warm up the DynaCool system in order to change the Helium Cylinder The system requires standard laboratory grade helium gas 99 9 pure or better Higher purity is not necessary for proper circulation loop operation but it may be desirable if extremely clean vent and purge gas is needed for your particular experiments Follow the steps
144. ular intervals one cycle every to 2 hours to consume the minimum power necessary to prevent loss of helium from the circulation loop Full operation can be resumed from the standby state in less than 1 hour by clicking the Restart Cryostat button Restart Cryostat Depending on the current state this will cancel the current shutdown operation and return to normal operation or exit the current standby state and resume normal cryostat operation Warmup This will warm the cryostat to room temperature and shut the system down This includes turning off the cryocooler evacuating the helium from the circulation loop venting the cryostat case with air to speed warming and turning on stage heaters until all cryostat PPMS DynaCool User s Manual 1307 110 Rev AO 3 7 November 2011 Section 3 2 MultiVu 3 2 9 Chapter 3 Software components are at room temperature At room temperature the case will be pumped out to remove excess air followed by power down Use this command if you will be performing maintenance or will need to cool the system down again shortly after warming it up As an alternative see the Shutdown command Shutdown This operation will turn off the cryocooler evacuate the circulation loop and turn off the power to the system Use this command if you plan to shut the system down for more than a week and you don t care how long it takes to warm up As an alternative see the Rapid Shutdown command Rapi
145. ximum field are 55 A for a9 Tesla magnet and 120 A for a 14 Tesla magnet While most magnets are cooled by liquid or gaseous helium the DynaCool magnet is cooled by solid conduction The magnet is cooled by solid contact to the 4 K plate Figure 4 1 shows how the magnet is directly connected to the 4 K Plate The DynaCool magnet does not have a superconducting switch Rather the magnet controller is directly connected via magnet leads to the superconducting solenoid The magnet leads are designed to present a very small heat load to the 4 K Plate so heat loads from magnet currents do not affect temperature control operation The heat load to the Main Shield is more substantial but easily handled by the large cooling power at the cryocooler first stage The magnet leads inside the cryostat consist of three stages The section between room temperature and the Main Shield which is constructed of copper wire The design minimizes the total heat load on the cryocooler first stage considering solid conduction and joule heating at maximum current The section between the Main Shield and 4 K Plate which is constructed of high temperature superconductor eliminating joule heating The section between the 4 K Plate and the magnet which is constructed of NbTi alloy also eliminating joule heating Low thermal resistance but electrically isolating thermal anchors cool the magnet leads at the Main Shield and 4 K Plate in order to make sure
146. xport Data 1 1 3 Data File CAQ dSquidysm Data MyS ample dat Browse Export File c QdS quid sm Data MySample csy Destination File Format Headers C Tab Delimited Column Headers Comma Delimited C Full Headers C Space Delimited C No Headers Select Data Export Close Figure 3 14 Exporting Data Select a graph view of the data file you want to export Select the menu item File gt Export Make sure Data File specifies the file you want to export You can browse to a different data file if desired Designate the path and file name of the exported file to write under Export File 3 18 PPMS DynaCool User s Manual 1307 110 Rev AO Quantum Design November 2011 Chapter 3 Section 3 6 Software Temperature Magnet Cryostat Services Under Destination File Format choose which character will separate data items in the exported file tab comma or space Choose whether you want column headers column labels full headers or no headers With full headers the file format must be comma delimited All of the header information at the beginning of the data file will be written to the new file including sample properties software revision and other information used by MultiVu This header information will appear at the beginning of the exported data file and may not be easily imported by other programs This option is used to keep the existing MultiVu data fi

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