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PP3000T User manual - Quorum Technologies

1. Desk Lamp e 6 04E 01 mbar Gas Flow ea 2011 06 08 02 14 50 USB 4751 board connected ok Auto ut 2011 06 08 02 14 52 SEM Camera fault 2011 0608 02 14 52 Prep Camera fault 2011 0608 02 15 22 Startup sequence begun Sublime finished 2011 06 08 02 15 22 Roughing out system 2011 06 08 02 15 28 Pumping to high vacuum 2011 06 08 02 17 30 System ready Sublime 2011 06 08 18 08 32 Failed to reach vacuum 2011 0606 18 09 57 Failed to reach vacuum 2011 06 08 18 45 27 Shutting down 2011 06 08 18 45 32 Shutdown Complete 2011 06 08 18 46 06 Startup sequence begun 2011 0608 18 46 06 Roughing out system Y E ee oe Camera O N2 Pressure System OK O H p 89 90 6 41 v 6 36 19 50 Figure 42 Message history 3 10 Shutting down the software and access to reserved functions Touching the logo in the bottom left hand corner opens a window where the software can be shut down and also gives access to the password protected area for diagnostics and service Issue 1 3 November 2011 42 Issue 1 3 November 2011 PP3000T User Manual V1 3 PP3000T User Manual V1 3 43 4 Running the system 4 1 Initial preparation Before using the system it is advisable to pump out the vacuum isolated transfer line especially after any long period without use This is best done overnight before the planned cryo session but can be done during start up if necessary See section 6 2 for details on how to pump out the line
2. Issue 1 3 November 2011 78 PP3000T User Manual V1 3 Time allowed for the user to stop pressing the Vent Airlock button If the user keeps pressing the button the venting will be cancelled automatically value in seconds lt SlushDelaySeconds gt 3600 lt SlushDelaySeconds gt Time allowed for the user to press the Vent button once the Slush is active If the user does not press the button in time the pumping will be cancelled automatically value in seconds lt TemperatureRampPerMinute gt 100 lt TemperatureRampPerMinute gt Requested heating rate for stages value in degrees per minutes lt TemperatureCoolPerMinute gt 50 lt TemperatureCoolPerMinute gt Requested cooling rate for stages value in degrees per minutes lt BleedVacuumValue gt 0 05 lt BleedVacuumValue gt Default setting for the sputter bleed valve vacuum level value in millibars lt BleedVacuumDelaySeconds gt 30 lt BleedVacuumDelaySeconds gt Time to wait before sputter bleed vacuum setting is checked value in seconds lt BleedVacuumTimeoutSeconds gt 60 lt BleedVacuumTimeoutSeconds gt Timeout if sputter bleed vacuum setting is not reached value in seconds lt CoatingVoltage gt 600 lt CoatingVoltage gt Default voltage for sputter coating value in volts lt CoatingVoltageCheckSeconds gt 5 lt CoatingVoltageCheckSeconds gt Time to wait for sputter voltage to rise to set value value in seconds lt CoatingCurrentCheckLevel gt 0 5 lt CoatingCurrentCheckLevel
3. November 2011 PP3000T User Manual V1 3 59 6 3 Lubricating the vacuum transfer device rod The stroke of the transfer device rod is quite long and it requires periodic lubrication This should be done at the beginning of each cryo session and as necessary during a long session if the rod does not slide easily and freely A small container of high vacuum compatible lubricant is supplied with the installation kit see Figure 65 Figure 65 Lubricant for transfer rod Pull the insertion rod fully out and using a soft lint free tissue carefully wipe the rod to remove any old lubricant and dirt which may have accumulated Retaining cover Figure 66 Rear of transfer device Unscrew the retaining cover see Figure 66 from the back of the rod ball joint Pull the rod sharply outwards to reveal the O rings Figure 67 Lubricating transfer rod Place a drop of lubricant on the rod near the ball joint at the back of the transfer device see Figure 67 Replace the retaining cover Slide the rod backwards and forwards a few times to distribute the lubricant along the rod Issue 1 3 November 2011 60 Issue 1 3 November 2011 PP3000T User Manual V1 3 PP3000T User Manual V1 3 61 7 Troubleshooting The system is designed to be mostly self diagnosing should there be a problem Any malfunction of a main system component such as temperature control unit power supply etc will be displayed in the message window at
4. During this time the vacuum isolated line continues to be pumped When purging is complete the user is prompted to close the pump out valve and remove it Startup Flease close the pumpout valve Figure 46 Close pump out valve prompt Startup Please remove the pumpout valve fram the CHESDOOD Cancel Figure 47 Remove pump out valve prompt Once this is confirmed the next prompt asks the user to insert the CHE3000 into the 12L dewar and increase the gas flow to 5L min to rapidly cool the SEM cold stage and anti contaminator Once at the Set temperatures the gas flow can be reduced and if required AUTO pressed to start a PID control loop to maintain the set temperature Often it is better to use manual control with a set flow to minimise gas usage The system will prompt the user that it is ready If non default temperatures are required they can now be set 4 4 Preparing a standard specimen Issue 1 3 November 2011 46 PP3000T User Manual V1 3 Make sure tools specimen mounting shuttles stubs hair dryer etc are available as needed 4 4 1 Making nitrogen slush e Decide which slusher to use Normally for direct freezing of fresh material the smaller one e Fill the polystyrene beaker with liquid nitrogen taking care not to overfill e Place the lid on the slusher pot and press the corresponding SLUSH button Pressing the SLUSH button again will stop the pump e Wait for nitrogen slu
5. Four focussed high intensity white LEDs illuminate the specimen These are adjustable and easily removed for cleaning Shadowing of the specimen by fracturing tools is minimised 2 3 4 CCD camera see Figure 4 A small CCD camera looks through one of the side windows and is focussed on the specimen shuttle and bayonet fitting area The image from this camera is displayed on the touch screen and can be enlarged to fill the screen making viewing of fracturing and bayonet engagement very easy The window is protected from sputtered material by a solenoid operated shutter Issue 1 3 November 2011 PP3000T User Manual V1 3 17 Figure 4 CCD camera on preparation chamber 2 3 5 Sputtering and carbon coating heads The standard coating option supplied is metal sputtering A carbon head is available as an option for those wishing to do EDS analysis The whole sputtering process is automated from argon gas introduction to striking of the plasma and current control Many different metal targets are available for the sputter head Platinum is supplied as standard Iridium is the recommended option for the finest grain size 2 3 6 Film thickness monitor An optional film thickness monitor mounted behind the cold block enables actual coating thickness to be measured if required 2 3 7 Liquid nitrogen dewar The large integral liquid nitrogen dewar with high thermal efficiency and low boil off cools the cold block and stage The inner sur
6. switches between full screen view and small window view PF30007 Control Version 0 7 1 7 Elida oe logies Camera Q M2 Pressure System LIF 18 48 Figure 40 Full screen video window 3 9 Messaging areas There are several areas of the screen used to display messages to the user Issue 1 3 November 2011 PP3000T User Manual V1 3 41 Process message history Scroll buttons General process messages Warning 3 d N2 Pressure System OK O P ii Prep 19 47 for message history Nitrogen pressure status Figure 41 Messaging areas of the screen System status General process messages are displayed above the process buttons Warning and error messages are displayed in the area below the buttons A history of all the messages displayed since system start up is shown at the bottom of the screen Touching the Prev and Next buttons allows the user to scroll through these messages By touching the message itself the frame is expanded to show a scrollable window of all the messages PP3000T Control Version 0 7 1 7 Anticontaminator SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T Startup Pump Prep Vent Prep Shion R Storage Storage Open circuit Open circuit 121 Set T Set T Over View View Log Vacuum Turbo Speed Functions ANN 175 Prep Chamber Vacuum Buffer Tank Vacuum 1E 4 E1 Gas Flow Heater Heat Level ato
7. A s Pumping line Knurled knob Dewar fitting Figure 64 Pumping the vacuum isolated line A flexible pumping line with a fitting which slides onto the pump out port of the vacuum isolated line is supplied The fitting has a threaded shaft which engages in a piston sealed plug in the port Slide the fitting over the pump out port and screw the shaft into the plug for about five turns As the vacuum isolated line will only be pumped out occasionally the control buttons to pump it are found under the Vacuum functions button Touching this button opens a window with the controls Firstly check there are no leaks in the line or connection by touching the Pump vacuum isolated line button The right hand vacuum gauge will then indicate the pressure in the line Make sure this comes below 1e mbar If this is the case then gently pull the threaded shaft out of the pump out valve until it comes to a stop The line should then be left to pump for several hours or overnight A vacuum of 5e mbar should be reached Once the line has been pumped press the threaded rod back into the pump out tool and unscrew it until it disengages from the piston sealed plug The pumping line may now be vented and removed from the pump out fitting by touching the Vent vacuum isolated line button When not pumping the vacuum isolated line the line should be removed from the CHE3000 to avoid any vibration being transmitted to the microscope Issue 1 3
8. Prep NEUE Service Menu i Storage Storage Open circuit 165 Turbo Speed Diagnostics Ho PPS3000T Buffer Tank Vacuum Quorum Technologies Version D 7 1 7 Check Config Copyright uerum Technologies 2011 uorum Technologies Sputter Unit Software Version 262 6 18E 01 mbar Sputter Unit Hardware Version 17 Chamber Unit 1 Software Version 8192 Chamber Unit 1 Hardware Wersian 32 Chamber Unit 2 Software Version 15 Chamber Unit 2 Hardware Version 15 Evaporation Unit Software Version 0 Evaporation Unit Hardware Version 0 Save Contig Prev system ready Next Prep Large hnologies Camera Pressure Heu H p 134 98 i 4 26 y 4 39 23 03 Save Config writes any new parameters which have been set in the configuration to the XML file To access the first 2 menu items the user must supply an access code Issue 1 3 November 2011 PP3000T User Manual V1 3 85 PP3DODT Control Version 0 7 1 7 Anticontaminatoar SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T Sann Pump Prep ps cA ce E Storage Service Men Siria Open circuit 147 Turbo Speed Diagnostics Buffer Tank Vacuum E1 Check Contig A 75E 01 mbar Gas Flow Auto iiid un Camera e M2 Pressure System LIF 29 41 Save Contig Typing in the correct code will open either of the 2 windows These 2 modes are not intended for normal usage as it is possible to cause damage to the system by
9. PrepDek specimen preparation desk The workstation trademarked PrepDek houses the dual slusher pots for specimen preparation and manipulation the control electronics and the panel PC Each of the slusher pots may be evacuated and vented independently The larger of the two pots is fitted with a manipulator for loading pre frozen specimens from high pressure freezers plunge freezers cryo microtomes or those prepared off site A bright flexible LED lamp provides illumination of the pots Each pot can have a dark coloured disk fitted in the bottom to give high contrast when loading under liquid nitrogen Issue 1 3 November 2011 20 PP3000T User Manual V1 3 A storage tube is provided for the transfer device which enables it to be stored under vacuum keeping it clean and moisture free Desk lamp Large slusher pot Small slusher pot Figure 8 PrepDek slusher pots Figure 9 Transfer device in storage tube 2 4 1 Control electronics All the control electronics are mounted in a sealed case fitted below the PrepDek Connections are made from below to prevent any ingress of water or liquid nitrogen The power supplies and valving are all controlled from a touch screen computer mounted on an adjustable arm on top of the workstation Control of stage and anti contaminator temperatures and cooling gas flow is via a dedicated multi channel temperature control system Valving and sensing is controlled by another d
10. Vent Prep Storage The transfer device is normally kept under vacuum in the storage tube To vent this tube and remove the transfer device simply touch this button 3 4 2 2 Vacuum Functions 3 4 2 2 1 Pump Vacuum Isolated Line This button starts the pump out of the CHE3000 vacuum isolated line NB The quick release valve should be fitted to the top of the CHE3000 before touching this button 3 4 2 2 2 Vent Vacuum Isolated Line Where the CHE3000 vacuum isolated lines have been pumped and the sorb pump regenerated pressing this button will vent the pumping line and it may then be disconnected from the vacuum isolated line NB The quick release valve on the top of the CHE3000 must be closed first 3 4 2 2 3 System vent This button will vent the entire system provided it is not cold LY 2 el ee ey eee Y SCUL n EL n cons Pump Vacuum Cancel Isolated Line Operation Vent Vacuum Isolated Line System Vent Clase Figure 19 Vacuum functions window 3 4 2 3 Overview This button calls up a graphical representation of the system showing the status of all valves switches etc It is read only 3 4 2 4 View Log This button will call up the graphs of pump down and cool down Issue 1 3 November 2011 30 PP3000T User Manual V1 3 3 4 3 Logging the system parameters If the Log vacuum and temperature values tick box is selected on Startup the system will store data for
11. and dry the end of the insertion rod 4 5 Advanced specimen handling pot For clarity the images below are shown without the main cover and with no liquid nitrogen Top loading shuttle 10246 Rotating shuttle holder Figure 58 Loading position Firstly load a top loading shuttle into the rotating shuttle holder and turn it so that it is horizontal Figure 58 Fill the polystyrene cup with liquid nitrogen taking care not to overfill Place the Perspex cover onto the pot and press Slush Once nitrogen slush forms the pot may be vented and the cover removed Top loading shuttle 10246 is supplied with the system Other types can be purchased Figure 59 Pick up position Issue 1 3 November 2011 PP3000T User Manual V1 3 53 Transfer the pre prepared specimen into the pot and load it into the shuttle Rotate the shuttle holder so that it is vertical Figure 59 Pre cool the tip of the transfer rod in the liquid nitrogen and locate the bayonet fitting into the shuttle Figure 61 Rotate 90 degrees to lock onto the shuttle Slide the transfer device down the insertion rod and locate it on top of the pot cover Figure 60 Press Slush Just before slush re forms slide the insertion rod back into the transfer device and close the small swing valve Continue the transfer as normal Figure 61 Picking up shuttle Issue 1 3 November 2011 54 PP3000T User Manual V1 3 Issue 1 3 Novem
12. button Touching OK will transfer the new value to the set temperature window Touching the Cancel button will exit with no change being made to the set temperature 3 3 Gas flow monitoring and control Two independent gas flow circuits control the flow of cold nitrogen gas through the heat exchangers of the SEM anti contaminator and SEM cold stage The flow of gas is regulated by a proportional valve and the flow measured by a mass flow meter The flows are displayed below their respective temperature displays Figure 14 Issue 1 3 November 2011 26 PP3000T User Manual V1 3 Gas Flow Current gas flow Touch here to open calculator window for large changes Increment or decrement gas flow in manual mode az Toggle gas flow lowy between auto and Manual manual control Figure 14 Gas flow control The temperatures may be controlled by gas flow alone or by a combination of gas flow and heating depending on the mode selected To minimise the gas consumption it is usual to control with gas flow only when not subliming The system defaults to manual gas control 3 4 Vacuum monitoring and control The top right hand area of the touch screen displays the vacuum monitoring and control functions Vacuum System Startup Pump Prep vent Prep EM MS storage Storage Ciyer view View Log Vacuum Turbo Speed Functions i Frep Chamber Vacuum Buffer Tank Vacuum 1E 4 Units label 3 89E 06
13. desk e Turbo pumping stack CHE3000 cold gas cooling system SEM cold stage and anti contaminator 2 2 1 SEM cold stage Figure 1 The SEM cold stage has two cartridge heaters and a Pt100 temperature sensor fitted It sits on high efficiency thermal mounts and is cooled by cold nitrogen gas supplied by the off column cooling system The temperature is controlled by a combination of gas flow and heating between about 193 C and 50 C If required the specimen may be sublimated in the microscope whilst simultaneously imaging to establish optimal thermal and temporal conditions which can then be used in the preparation chamber The cold stage does not normally limit the tilt or translation of the microscope stage An optional rotate stage allows full 360 rotation of the specimen A STEM version of the cold stage is also available Issue 1 3 November 2011 14 PP3000T User Manual V1 3 When not in use and where space in the SEM chamber allows the cold stage may be parked in the supplied retainer inside the microscope chamber and does not need to be removed for normal microscope operation The anti contaminator may be left in place and used in addition to the standard microscope cold trap or swung to one side The cold stage is mounted on the standard SEM stage using an adapter plate In most installations it will be necessary to remove the normal SEM specimen holding device in order to fit the cryo stage Figure 1 Example S
14. files lt SavedCoatingRecipes gt lt SavedSublimeRecipes gt lt string gt lt string gt lt string gt lt string gt lt string gt Names of the saved sublimation recipe files lt SavedSublimeRecipes gt lt SavedEvaporationRecipes gt lt string xsi nil true gt lt string xsi nil true gt lt string xsi nil true gt Names of the saved evaporation recipe files lt SavedEvaporationRecipes gt lt PP3000TConfig gt Issue 1 3 November 2011 PP3000T User Manual V1 3 83 11 Appendix Il Service and diagnostics mode 11 1 Accessing the configuration and diagnostic modes Touching the logo at the lower left of the screen opens a fly out menu PPSO00T Control Version 0 7 1 7 Anticontaminatar SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T startup Service Menu Open circuit 137 Set T Set T Overview Diagnostics 134 Prep Chamber vacuum 1E 4 Check Contig Save Contig iiti Camera d M2 Pressure System LIF 22 40 Figure 87 Fly out menu The Exit App About and Save Config buttons are not password protected Exit App closes down the software About brings up a small window with details of the system Issue 1 3 November 2011 84 PP3000T User Manual V1 3 PP3DODT Control Version 0 7 1 7 Anticontaminator SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T ua d ua ua ciem Pump Prep Vent
15. gt Minimum current value to be read from sputter supply to know plasma achieved value in milliamps lt CoatingVacuumMinimum gt 0 01 lt CoatingVacuumMinimum gt Minimum vacuum level for coating to proceed value in millibars lt CoatingShortCircuitVoltage gt 80 lt CoatingShortCircuitVoltage gt Default minimum HT voltage to decide if there is a short circuit on the sputter head value in volts lt EvaporationVoltage gt 10 lt EvaporationVoltage gt Default evaporation voltage in volts lt EvaporationBurnOutSeconds gt 15 lt EvaporationBurnOutSeconds gt Time allowed to burn out carbon string in seconds lt DegasCurrent gt 7 lt DegasCurrent gt Default carbon string degas current in amps lt DegasSeconds gt 20 lt DegasSeconds gt Default degas time in seconds Issue 1 3 November 2011 PP3000T User Manual V1 3 79 lt LeakDetectionTimeoutSeconds gt 30 lt LeakDetectionTimeoutSeconds gt Time allowed during start up for rotary pump to reach required airlock buffer tank or isolated line vacuum level before deciding there may be a leak value in seconds lt BackingVacuumAutoOn gt 1 lt BackingVacuumAutoOn gt Default buffer tank vacuum level read on buffer tank Pirani gauge where the buffer tank pump request will be generated value in millibars lt BackingVacuumAutoOff gt 0 07 lt BackingVacuumAutoOff gt Default buffer tank vacuum level read on buffer tank Pirani gauge where the buffer tank pumping will stop
16. mbar n 9E O1 mbar Figure 15 Vacuum monitoring and control area 3 4 1 Vacuum monitoring Vacuum levels in different parts of the system are displayed within the Vacuum System frame The left hand meter Figure 15 is for the Prep Chamber Vacuum and is read from a wide range gauge mounted directly on the preparation chamber This gauge can read from atmospheric pressure down to about 1e mbar The units may be displayed in either Pascal or millibars The units are changed by touching the units label Issue 1 3 November 2011 PP3000T User Manual V1 3 27 The right hand gauge displays one of the two Pirani gauges fitted to the system depending on the function which is running at the time The caption above the gauge changes to show which part of the vacuum system is being displayed Normally this is the turbo buffer tank vacuum When the airlock is being pumped out the Airlock Vacuum gauge is displayed When the vacuum isolated line is being pumped Isolated vacuum line is displayed The buffer tank vacuum is monitored above the gauge display Both analogue and digital displays are shown The analogue display makes checking vacuum levels easy from a distance as the needle only needs to be in the green band Version 0 7 2 0 EU Shutdown Storage BTank 1 85E 01 acum Functions Turbo Speed a Isolated Line Vacuum Buffer tank vacuum 3 92E 02 mbar Figure 16 Pumping the vacuum isolated line 3 4 2 Vacuum con
17. microscopy TEM grids Carbon fibre Carbon fibre normally in the form of a woven cord can be used to thermally evaporate thin layers of carbon onto a substrate The main application in electron microscopy EM is the production of thin electrically conducting coatings on scanning electron microscopy SEM specimens Carbon fibre can be used for transmission electron microscopy TEM applications but carbon rod is normally preferred due to superior control of the evaporation process Film thickness monitor Shuttle Stub A film thickness monitor can be used to monitor and control the thickness of sputtered and evaporated metal films A gold coated quartz crystal is mounted in the vacuum chamber of the coating system ideally close to the specimen or substrate The quartz crystal is made to oscillate at a defined frequency using an externally mounted oscillator As metal is deposited on the quartz crystal the frequency of oscillation alters and the change is converted to a digital eg LED display on the monitoring unit In this context a shuttle is the dovetail shaped gold plated copper block which is used to transfer specimens or specimen stubs between different parts of the system It fits onto the end of the insertion rod via a bayonet fitting A stub is a cylindrical metal disc usually 10mm diameter and between 5mm and 10mm thick It may be made of copper or aluminium for good thermal conductivity Specimens are mounted onto th
18. shield from the cold stage taking care no to damage the LED chamber light assemblies Issue 1 3 November 2011 76 PP3000T User Manual V1 3 These LED assemblies are fitted with a glass cover slip that should be cleaned as before with cotton buds and alcohol Thoroughly clean the cold stage taking care not the strain the flexible braids connecting the cold stage to the dewar or the electrical wires to the heater and thermometer Re assembly of the chamber is the reversal of dismantling Begin by re fitting the top cold shield to the cold stage leading the light wire to the left side of the cold stage so that it will connect to the feedthrough wire set without straining Lower the cold stage dewar assembly into the preparation chamber connecting the red yellow and black pink wires Lower the assembly completely into position engaging the bottom of the dewar into its three locating pegs and the cold stage onto its four supporting isolation pillars Check that the wires are not trapped and moreover that they are not in hard contact with the dewar cold stage or chamber wall Hard contact of the wires between cold and warm surfaces will leak heat into the cold assembly This must be avoided Replace the four countersunk screws into the support pillars through the front window using tweezers and the two into the SEM side support bracket using the screw retaining tool Tighten these six screws sufficiently using the correct size Alle
19. temperatures and vacuum in a log file Startup Menu Log vacuum and Auto Made Manual Made temperature values Logging enable tick box Figure 20 Activating the data logger The data can be displayed graphically by touching the View Log button This is a toggle button so the display may be masked by touching again Version Vacuum System Enabling the TE Pump Prep vent Prep log display F Storage Storage sl Functions Prep Chamber Vacuum Ill Butter Tar Figure 21 Enabling the log display Individual parameters are displayed by selecting the appropriate button below the graph The data is not live but can be refreshed by touching the Update button hd ded ee Selected param eter ee EE EE ROGA 4 z highlighted Yacuum Minutes Refresh data by touching Prep Bulfer button Figure 22 Logging window Issue 1 3 November 2011 PP3000T User Manual V1 3 31 3 5 Process control Once a specimen has been transferred to the preparation chamber it may be sublimed coated and then transferred into the SEM chamber These processes are activated by the process control buttons Figure 23 The buttons are laid out in the order they will most probably be used across the screen The Evaporation button only appears if the optional carbon evaporation board is fitted Cancel Figure 23 Process control buttons no evaporation board fitted 3 6 Sublimation Touchin
20. the bottom centre of the screen Any loss of communications will also be displayed here The system also logs data to three files in the Quorumtech folder in Program Files These can be useful for diagnostic when contacting the Quorum Service department Issue 1 3 November 2011 62 Issue 1 3 November 2011 PP3000T User Manual V1 3 PP3000T User Manual V1 3 63 8 PP3000T shuttles and stubs There are many styles of shuttles and stubs available for the PP3000T Some of the most common are shown below AL200077B E7449 Specimen shuttle with E7449 universal Universal cryo stubs multi stub stub Blank specimen stub bmm high E7402 aluminium E7403 copper E7449 5 universal cryo stub packet of five E7407 E7406 Copper stub with 1mm slot Copper stub with 3mm slot Issue 1 3 November 2011 64 E7404 Clamping stub 10247 Rivet shuttle bayonet fitting 10245 Shuttle for freeze fracture planchettes Issue 1 3 November 2011 PP3000T User Manual V1 3 328116510 Freezing rivets 10246 Shuttle for 10mm stub shown with E7433 rivet stub PP3000T User Manual V1 3 65 9 Maintenance With the exception of the regular maintenance tasks the service and repair of the PP3000 should be carried out by qualified service engineers Warning lethal voltages are present in this instrument disconnect power to the instrument when carrying out service tasks as indicated in the relevant section of thi
21. the dewar spout and knife shaft to make sure that you are not putting strain on any of the internal components It is likely that the knife shaft will lift out of the prep chamber cold stage but this is normal Just do not strain anything The argon feed capillary tube may be inclined to catch at the back of the chamber so take great care with this Place the top plate so that it will not be damaged You may decide that it is better off upside down You will now have access to the internal parts of the chamber Using a long M3 Allen key and screw holding tool remove the two screws that retain the SEM side support bracket Using a long M2 Allen key remove the four countersunk screws that hold the cold stage in place on its isolating pillars You will now be able to lift out the entire cold stage and dewar assembly but it will still be connected but the electrical leads Support the stage and dewar assembly while you locate the electrical wire connections in the red yellow and black pink and with care disconnect each of the three connections They pull apart It should not be necessary to disconnect the white wires as these are for the sputtering shutter solenoid which will remain in the preparation chamber Place the assembly on the clean work place that you prepared earlier You will now be able to thoroughly clean the inside of the preparation chamber but take care of the wires from the electrical feedthrough Remove the top cold
22. with these lights as it is possible to dislodge the cover glasses Inspect the inside of the chamber to be sure that there are no damaged cooling braids or wires Check the operation of the chamber lights and knife mechanism At this stage you should re fit the sputtering head if it has been removed Inspect the o ring and place the sputter head through the top plate place the dewar top cover in place taking care to position the sputter power lead clear of the other parts under the cover Connect the argon feed tube Fit the four screws that retain the dewar top cover Now press down on the sputter head with your finger and view the sputter head from below with a dental mirror to ensure that there is clearance between the sputter head and the top cryo shield Any contact will cause a cooling breech and must be rectified Figure 81 Checking the sputter head clearance The front window may now be re fitted but it is likely to need cleaning first Sputtered material will have coated the inside of the window which will greatly reduce visibility Take great care in handling the window as its edges will be very easily chipped It should once again be noted that the knife manipulator fitted to the front window has a scalpel blade as its cutting edge There is a high risk of personal injury Issue 1 3 November 2011 PP3000T User Manual V1 3 73 Figure 82 Cleaning the knife Make sure that the window seal O ring is clean and c
23. 011 80 PP3000T User Manual V1 3 lt PrepVacuum gt lt AirlockVacuum gt lt MinVacuum gt 0 001 lt MinVacuum gt Lowest value displayed on the airlock vacuum analogue scale value in millibars lt MaxVacuum gt 1000 lt MaxVacuum gt Highest value displayed on the airlock vacuum analogue scale value in millibars lt AirlockVacuum gt lt Anticontaminator gt lt Temperature gt lt MinTemperature gt 196 lt MinTemperature gt Lowest temperature which can be entered by the anti contaminator controls value in degrees Centigrade lt MaxTemperature gt 30 lt MaxTemperature gt Highest temperature which can be entered by the anti contaminator controls value in degrees Centigrade lt InitialTemperature gt 175 lt InitialTemperature gt Default temperature setting for the anti contaminator value in degrees Centigrade lt HeaterGain gt 0 5 lt HeaterGain gt Default heater gain for anti con arbitrary units lt HeaterDerivative gt 0 5 lt HeaterDerivative gt Default heater derivative for anti con arbitrary units lt Heaterlntegral gt 0 lt Heaterlntegral gt Default heater integral for anti con arbitrary units lt Temperature gt lt GasFlow gt lt MinGasFlow gt 0 lt MinGasFlow gt Lowest gas flow which can be entered for the anti contaminator value in litres minute lt MaxGasFlow gt 5 lt MaxGasFlow gt Highest gas flow which can be entered for the anti contaminator value in litres minute lt InitialGasFlow gt 0
24. EM cold stage 2 2 2 SEM anti contaminator Figure 2 The SEM anti contaminator is mounted on a ball jointed support and can be swung out of the way when not in use The anti contaminator is fitted with a Pt100 temperature sensor The temperature may be varied between 193 C and ambient and allows rapid warm up of the system The shape of the anti contaminator is tailored to suit the SEM to which it is fitted Figure 2 Example SEM anti contaminator 2 2 3 SEM chamber illumination To ensure good visibility when inserting a specimen the SEM chamber is fitted with high intensity LED illumination The LEDs are located close to the transfer rod axis and give excellent visibility when loading the specimen shuttle Issue 1 3 November 2011 PP3000T User Manual V1 3 15 2 2 4 SEM chamber CCD camera Where no chamberscope is available and space allows a CCD camera may also be fitted to the SEM chamber The image is displayed on the touch screen and can be enlarged to fill the screen when transferring 2 3 Column mounted preparation chamber Figure 3 The preparation chamber has been designed to maximise visibility of the specimen during specimen preparation and transfer Large cold surfaces provide excellent trapping of sublimed water vapour as well as cryo pumping the chamber The integral non boiling dewar cools the cold stage cold shields and specimen manipulators Vibration from boiling liquid nitrogen which could be trans
25. Make sure that a microscope is under vacuum and fully operational Set a low operating voltage beam current and magnification Move the SEM stage to the stored cryo load position b nitrogen vent gas is turned on c liquid nitrogen dewar for the CHE3000 is filled but the heat exchanger not inserted d liquid nitrogen for slushing is available e nitrogen gas for cooling circuits is turned on f argon supply is turned on g specimen preparation tools etc are to hand h PP3000T preparation chamber is isolated from the microscope with both gate valves closed and locked 4 2 Start up Switch on the PrepDek using the on off switch mounted under the rear left hand corner followed by the panel PC using the switch in the centre of its bottom cover Start the software by double tapping on the PP3000T shortcut on the desktop On power up and before the program starts the LEDs should all briefly light up orange and the LED lamps come on as the self test runs Wait for the main control screen to be displayed If all the processors and services are running the system status will show green Press the START UP button and select the Auto Mode or Manual mode option Figure 17 A window will pop up reminding the user to set the microscope to cryo operation Issue 1 3 November 2011 44 PP3000T User Manual V1 3 Startup Please configure the microscope for cryo operation Figure 43 Microscope configuration reminde
26. P3000T shuttles and stubs Users can also modify blank stubs E7402 supplied with the system with slots or holes 4 4 3 Freezing Once the specimen is mounted press and hold the VENT button to admit dry nitrogen gas to the nitrogen slushing pot Remove the lid and plunge the specimen shuttle under the nitrogen surface Wait for the nitrogen to stop boiling Slide the transfer device down the insertion rod keeping the specimen shuttle below the surface of the liquid nitrogen until the transfer device engages with the top of the slusher and the airlock pin enters the hole in the slusher lid Press the SLUSH button again Just before the nitrogen turns to slush again withdraw the insertion rod into the transfer device and close the small swivel valve by turning the black knob on the back of the transfer device a few turns Once the valve is closed press and hold VENT until the transfer chamber can be removed Replace the Perspex cover on the slushing pot 4 4 4 Transferring to the preparation chamber Mount the transfer device on the preparation chamber airlock making sure the pin locates in the guide and the device is square to the flange To evacuate the airlock e Press the airlock PUMP button e The PUMP LED turns red the airlock valve opens and the rotary pump starts pumping down the airlock e Open the small swivel valve by unscrewing the black knob about 3 turns e Wait for green LEDs on PUMP and
27. V1 3 51 4 4 6 Sublimation Once a fresh surface has been exposed it is usually necessary to sublime the surface The sublime button is touched and brings up the sublimation screen Once the desired profile has been selected either from one of the stored recipes or a new recipe defined the user needs only to press Start for the process to run automatically see the software section 3 6 4 4 7 Coating Following sublimation the specimen will usually need to be coated with a thin conductive film of metal This is done via the Coating button Pressing this button calls up the coating screen and again once the required current and time have been selected pressing Start runs the process automatically see the software section 3 7 4 4 8 Transferring the specimen into microscope Following coating the specimen is transferred into the SEM chamber and is mounted on the SEM cold stage To initiate a transfer the Transfer button is touched If the preparation chamber pressure is low enough the SEM gate valve solenoid will be released and the gate valve LED will turn green The gate valve may now be opened by rotating the black knob clockwise and pulling down to the end stop As the SEM gate valve opens the SEM chamber lamp will automatically be turned on The specimen is now withdrawn from the preparation chamber cold stage by gently pulling back on the transfer rod and then advanced through the preparation chamber and SEM gate valve Lo
28. WebCamRegistryString gt Registry address of SEM web cam lt PrepWebCamRegistryString gt lt PrepWebCamRegistryString gt Registry address of Prep web cam lt VacuumUnits gt MBAR lt VacuumUnits gt Units used to display vacuum readings lt General gt lt StartLeakDetectVacuum gt 4 lt StartLeakDetectVacuum gt Vacuum level required to be reached on rotary pump start up read on airlock Pirani gauge with no valves open value in millibars lt StartHighVacuumTimeoutSeconds gt 10000 lt StartHighVacuumTimeoutSeconds gt Time allowed for turbo pump to reach required vacuum level before deciding there may be a leak value in seconds lt StartHighOkVacuum gt 0 0005 lt StartHighOkVacuum gt Required turbo vacuum level read from multi range gauge on prep chamber needed to decide system is OK value in millibars lt AirlockVacuumLevel gt 0 1 lt AirlockVacuumLevel gt Vacuum level required to be reached on rotary pump when pumping the airlock read on airlock Pirani gauge value in millibars lt PumpVacuumTimeoutSeconds gt 30 lt PumpVacuumTimeoutSeconds gt Time allowed for the vacuum to reach the AirlockVacuumLevel when pumping the airlock value in seconds lt PumpValveOpenTimeoutSeconds gt 30 lt PumpValveOpenTimeoutSeconds gt Time allowed for the user to open the Airlock Valve If the user is too slow the pumping of the airlock is cancelled value in seconds lt VentAirlockDelaySeconds gt 30 lt VentAirlockDelaySeconds gt
29. YUOrUM iecnno OQIE i 2 PP3000T User Manual V1 3 Issue 1 3 November 2011 PP3000T User Manual V1 3 3 Contents te Heatran a UN aos 7 1 1 Control of substances hazardous to health COSHH eene 7 IP MEME i is DONO PNE 7 13 COMON Y ES ES UAM et ade 8 I EE uel t 8 141 JDISclaltijeluse aure ceiatitenn Dui o e Se DS de 8 L42 Operators and service CNEIN COIS asia 8 t5 Hazard siena ls ANG PASA e dan de vae eun 8 151 Hazard SIENI WON OS eds deed asa 8 1 5 2 Hazard labels used on equipment 8 Eos RISK ANAVSIS ii sta 9 Lol Personalloperational FISKS suo aes utu Aa 9 1052 Hazardous Mate na sd 9 Efi GOOG working practices aii das 10 1 8 Quorum PP3000T specific safety hazards eese 10 Lu Ca 0 Tc 10 A SCODO A ios dnt atis RS A imn dvo mah tee e nd 11 LIO Return OT BOSS 2e s ut dE NE EIS Qe Ep a Vater Vb b en aer eru SENE Ie Ea ec 11 IJ Returns DO COC UNG ES Rd me tt P PUE PE 11 1 11 1 Warranty ca IM 11 1 11 2 Chareeable repasa 11 1 11 3 Packaging and cara 12 Ames a OU 0 ERE Re ee ane ne E es ed 13 2 1 Basicoverview OF SYSTEMS teo is 13 2 11 Stage bias VOltaBB ice aia 13 2 2 SEM cold stage and anti contaminator ccccoocccconcnnnonaconnnnacononnnonnonarononanronnnanos 13 2 2 1 SEM cold Stage FIBUEG Llar 13 222 SEN anti contaminator FIBUEe 2 diia 14 2 2 3 SEM champberilluminatio Mardi 14 2 2 4 SEN Chamber CCD Camer niaii de tte tee 15 2 3 Column mounted preparation ch
30. airlock valve This means that the airlock vacuum has reached the set point and the interlock solenoid has been released Issue 1 3 November 2011 50 PP3000T User Manual V1 3 e Rotate the airlock valve control knob anticlockwise 90 and pull it downwards to open the valve e Ifthe valve is not opened within 30 seconds the solenoid re locks and the pump down sequence must be re started e After the valve has been opened the solenoid re locks after 5 seconds e Slide the insertion rod into the preparation chamber and slide the specimen onto cold stage 4 4 5 Fracturing Two means of producing a fracture are provided a front mounted scalpel bladed probe and a top mounted micrometer advanced knife Both are actively cooled by copper braids connected to the cold block in the preparation chamber The scalpel blades can be exchanged and any size 5 blade may be used depending on the application or user preference This blade can be used to fracture thinner specimens to flick pieces of specimen away to open complementary fracture holders and to knock off rivets Figure 56 Front mounted probe The micrometer advanced knife is used for thicker specimens and the height of the blade is adjusted by turning the knurled knob below the actuating lever The knife should be raised before swinging back otherwise it may smear the top of the specimen Figure 57 Micrometer advanced knife Issue 1 3 November 2011 PP3000T User Manual
31. amber Figure 3 15 29435 GOld Stage SE ueni te beds ta OR en DEL Duc Lo Dora etus 15 Lada COMA A o ca o dd 16 A A ON en a D don du 16 234 CCD Camera See Figure dardos Nequi eps Sema un 16 2 3 5 Sputtering and carbon coating heads c irri brc Pos eam aad 17 2 3 0 Filrathickness MONITOR io EC tL P d a 17 2 29 2 Haud nitrogen de Wasi iaa 17 2 310 E o o niet d 18 2 3 9 CRYO transfer device see Figure 6 a 18 2 4 PrepDek specimen preparation desk 19 241 Control electrOBI S uon om a 20 29 TUDO DUMPING SICA AAA 21 2 6 CHE3000 cold gas oolIDB SYSTEM e pdt eer e bed A te ee 21 WM METTI 23 sE o e MD Ede dM sono nena 24 Issue 1 3 November 2011 4 PP3000T User Manual V1 3 3 2 Temperature monitoring and control 24 3 3 Gas flow monitoring and control ss 25 344 Vacuum monitoring and CONtrO lat 26 Sl Vacu m mODItOKIFiB qii e Aa 26 942 VaACUUNIN CobltrOolsssaestedimestolmitottum mds ntvimsedudivnde prd sedes bons esi 27 Sy adc m UT mmm 28 A Eur de dd td repu ipto Dd 28 AZ Pu lp PrepStOLdBB ioca 28 3402 Vent Prep Storage ui 29 34 22 Vacuum FUNCTIONS ii 29 34 22 Pump Vacuum Isolated Line 29 2342 2 2 MentVacuum Isolated line 29 342 2 3 COVEN Vell eee de utendo pme uS c pe UP cn S die 29 BAD OVER 29 Sup ISW LOB nr dd dates ste iiie dau Lal it to ane 29 3 4 3 Logging the system parameters ss 30 Dede PROCESS CONTO nescia bara dnas cess cens een nat Rte Ode en Cn d
32. an operator or in a service capacity Quorum Technologies is committed to providing a safe working environment for its employees and those that use its equipment and conducts its business responsibly and in a manner designed to protect the health and safety of its customers employees and the public at large It also seeks to minimise any adverse effects that its activities may have on the environment Quorum Technologies regularly reviews its operations to make environmental health and safety improvements in line with UK and European Community legislation Quorum Technologies cannot be held responsible for any damage injury or consequential loss arising from the use of its equipment for any other purposes or any unauthorised modifications made to the equipment All service work carried out on the equipment should only be undertaken by suitably qualified personnel Quorum Technologies is not liable for any damage injury or consequential loss resulting from servicing by unqualified personnel Quorum Technologies will also not be liable for damage injury or consequential loss resulting from incorrect operation of the instrument or modification of the instrument Issue 1 3 November 2011 8 PP3000T User Manual V1 3 1 3 Conformity This instrument is supplied in a form that complies with the protection requirements of the EC Electromagnetic Compatibility Directive 2004 108 EC and the essential health and safety requirements of the low vo
33. and wrap the string around it making sure it is under the spring loaded end Gently ease the string back so it is not taut as this may lead to premature failure Cut off any the excess length of string Electrodes Main head bodv Retaining screw Collimator Shield Electrode shield Figure 37 Carbon head components The carbon head will need periodic cleaning To do this vent the prep chamber and remove the head The collimator shield may then be pulled off to give access to the electrodes and electrode shield Remove any remaining carbon string Using a suitable Allen driver unscrew the electrode shield retaining screw Carefully clean all components with a lint free cloth and iso propyl alcohol Re assemble making sure the electrode shield is centred on both electrodes Issue 1 3 November 2011 PP3000T User Manual V1 3 39 Figure 38 Assembling the carbon head 3 8 Imaging control Where space allows the system may be fitted with two webcams One camera looks at the specimen whilst it is in the preparation chamber and the second is fitted inside the SEM chamber to provide a view of the specimen as it is loaded onto the SEM cold stage Issue 1 3 November 2011 40 PP3000T User Manual V1 3 Toggle Prep SEM cameras Full screen video nera ak Mesi Prep Camera Penge System OF 5 Figure 39 Camera window 13 47 A toggle button switches between the two cameras and the Large Small button
34. available materials If the Crystal usage shows Fail either the cable is unplugged or the crystal has been used to exhaustion and will need to be replaced Touching the edit button will allow the desired thickness to be entered To start the coating touch START The measured thickness will be zeroed and the sputter coating will run automatically and stop once the set thickness is reached 3 7 2 Replacing the FTM crystal The FTM is accessed through the front window e Ventthe system e Unscrew the 6 countersunk cap screws which hold the front bezel and glass in place e Loosen the cap screw which holds the front knife braid in place and remove the window e Wearing a pair of gloves lift the FTM body from the spring clip e Unplug the miniature BNC connector e Unscrew the top retaining ring on the FTM body e Remove the crystal e Insert the new crystal e Clean any sputtered material from the retaining ring and replace e Reconnect the miniature BNC connector e Replace the FTM body in the spring clip e Check the FTM control page to check the crystal usage is now zeroed e Replace the front window knife braid and front bezel e Re pump the system Retaining ring Crystal Spring clip Miniature BNC Mounting bracket A Ld 4 a y Figure 33 FTM head components Issue 1 3 November 2011 PP3000T User Manual V1 3 37 3 7 3 Using the optional carbon evaporator If the system detects the optional carbon
35. ber 2011 Figure 62 View of pick up PP3000T User Manual V1 3 55 5 Shutting the system down Drive the SEM stage to the cryo load position Remove the specimen from the microscope Remove CHE3000 from the 12L dewar Touch Shutdown on main screen Wait for Shutdown complete message Turn off PC and PrepDek Turn off the argon and nitrogen gas supplies Issue 1 3 November 2011 56 Issue 1 3 November 2011 PP3000T User Manual V1 3 PP3000T User Manual V1 3 57 6 General Maintenance 6 1 Pumping the transfer device storage tube A position is provided in the PrepDek where the transfer device can be stored under vacuum to keep it clean and free from moisture Figure 63 Transfer device fitted on storage tube Place the transfer device in the storage tube and slide the rod down to the stop Touch the Pump Storage Tube button on the screen in the Vacuum area The storage tube will be pumped down to a set vacuum and then the valve closed to leave it under vacuum To vent the device just touch the Vent Storage Tube button 6 2 Pumping the vacuum isolated pumping line In order to maintain a good vacuum in the vacuum isolated cold gas delivery line it needs to be evacuated periodically Pumping also regenerates the sorb material in the body of the line Issue 1 3 November 2011 58 PP3000T User Manual V1 3 Gas outlet Pump out valve tubes Gas inlet tubes Ao EA yg k J
36. ber body This will be referred to as the Thorough method and may only need to be carried out annually depending on instrument usage Figure 70 Cold stage and dewar Depending on the installation this should be possible without removing the chamber from the microscope but will involve removal of either the top or bottom plate of the chamber again depending on the installation configuration See details in the relevant section 9 3 Chamber cleaning short method This is a regular maintenance task that should be performed by the instrument user 9 3 1 Venting the preparation chamber During the chamber venting you should monitor the microscope vacuum level If the microscope pressure is increasing this will indicate a leak across the SEM gate valve which will need to be resolved In the case of a pressure increase it is recommended that controlled venting of the microscope chamber should be performed Issue 1 3 November 2011 68 PP3000T User Manual V1 3 The nitrogen gas supply must be connected and set to deliver the pressure required to enable the N2 pressure indicator of the PP3000 main operating page Refer to the instrument operation instructions to vent the system and select the VENT SYSTEM option The turbo pump will be switched off and after a short time the vent valve will open to vent the chamber The indication that the chamber has vented is that the sputter head will now be free Cancel th
37. chnologies should be contacted for advice Quorum Technologies will not be responsible for damage resulting from inadequate returns packaging or contamination of delicate structures by stray particles under any circumstances All non warranty goods returned to the factory must be sent carriage pre paid Free Domicile They will be returned carriage forward Ex Works Issue 1 3 November 2011 PP3000 2 Int T User Manual V1 3 13 roduction The PP3000T Cryotransfer system allows users to prepare load process and transfer cryo specimens into an SEM The specimen may then be imaged at cryogenic temper 2 1 atures in the SEM chamber Basic overview of system 2 1 1 Stage bias voltage Please note that the standard cryo SEM sample stage supplied with the Quorum Technologies Ltd cryo SEM system is not suitable for use with stage bias We have become aware of instances where the Quorum Technologies Ltd cryo SEM instrument has been used in conjunction with sample stage high voltage bias resulting in considerable damage to the control electronics of the cryo instrument Use of sample stage bias with the cryo SEM system will void all warranty Damage resulting from use of stage bias with the cryo SEM and standard stage will be extensive and costly to repair The system can be broken down into five main units 2 2 e SEM cold stage and anti contaminator e Column mounted preparation chamber PrepDek specimen preparation
38. components are sold with a return to factory warranty unless otherwise stated which covers failure during the first 12 months after delivery This is extended by a further 2 years if the warranty form is returned to Quorum Technologies Returns must be sent carriage paid Quorum Technologies will cover the return carriage costs This covers defects which arise as a result of a failure in design or manufacturing It is a condition of warranty that equipment must be used in accordance with the manufacturers instructions and not have been subjected to misuse This warranty does not cover consumable items such as sputter coating targets and carbon evaporation material To make a claim under the terms of this warranty provision contact the Customer Service Department of your local Quorum Technologies representative in the first instance 1 11 2 Chargeable repairs Always contact your local Quorum Technologies representative in the first instance They will be pleased to assist you and will be able to provide an estimate of repair costs many offer local repair facilities For routine repairs where down time is not critical the target standard return time at Quorum Technologies is 20 working days Issue 1 3 November 2011 12 PP3000T User Manual V1 3 1 11 3 Packaging and carriage All goods shipped to the factory must be sealed inside a clean plastic bag and packed in a suitable carton If the original packaging is not available Quorum Te
39. d area e Mop up any spillages immediately e When handling or decanting mineral oils wear protective clothing e Aerosols of mineral oils such as that produced by gas ballasting can prove to be hazardous and an exhaust is recommended e Before attempting to service electrical apparatus isolate from the mains e Treat all unknown substances as hazardous e Dispose of substances in an appropriate manner e Use the correct tool for the job e Keep a straight back and bend from the knees when lifting heavy objects e Wear protective clothing when using liquid nitrogen e Affix pressurised gas cylinders firmly to walls or racks Use the correct regulating valves on gas cylinders and always transport cylinders using the appropriate specialist trolley e Obey safety regulations regarding lifts hoists and machine tools e Always make sure you understand a procedure well before attempting it for the first time 1 8 Quorum PP3000T specific safety hazards The following Safety Hazards are specific to the Quorum PP3000T Cryo Transfer System 1 8 1 Gases Nitrogen and argon gas supplies This instrument uses nitrogen and argon gas supplies for operation the customer is responsible for maintaining the supply to the instrument This supply should be regulated and kept to the lowest pressure and flow rate as is practical to minimise the effects of any leaks Extreme care to be used when filling the slusher assembly with liquid nitrogen foll
40. date If this is a change to an existing recipe touching the Save button will store the recipe under the same file name and overwrite the current values Touching the Save as button will open another window where the recipe may be saved under a new file name using the touch screen keyboard Enter String File name for sublime recipe MEN Fem EN Pe ee Pe ibt EN EN EN ee EN EN ed Figure 27 Saving a new recipe Issue 1 3 November 2011 34 PP3000T User Manual V1 3 Once the required recipe has been loaded the user just has to press Start for the sublimation to proceed automatically A red snail trail line shows the actual sublimation profile as compared to the set profile Sublimation can be aborted at any time by touching the Abort button Once sublimation is completed the window can be closed using the Close button PP3000T Control Version 0 7 1 7 Anticontaminator SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T Startup Pump Prep Vent Prep CH g E Storage Storage Open circuit Open circuit Set T Oe View Log Vacuum Turbo Speed A EL Prep Chamber Vacuum Buffer Tank Vacuum 1E 4 1E0 1E 1 en E1 ES E 3 AT a 2 1E2 ic 1E 2 reall 1E3 3 99E 06 mbar 5 97E 0 mbar Sublime Recipe minus90for5mins In Prep In SEM Subliming 5 mins Cancel 3 Minutes Recipes 1 minusS forbmins Figure 28 Sublimation started 3 7 Coating the specimen Once the spec
41. e specimen and anti contaminator for optimal cryo trapping The twin heat exchanger has integrated drying stacks to remove any water in the supplied nitrogen gas The transfer tubes are vacuum isolated and a sorb pump maintains this vacuum so the vacuum isolation only needs occasional pumping The CHE3000 is fitted as standard to PP3000T and has a number of significant advantages e Although column mounted dewars fitted to many previous Quorum cryo systems are very efficient because the volume of the dewar is actively pumped by the SEM pumping system their capacity is relatively small and therefore they only offer a limited hold time between refills e This limited hold time can be problematic for some users and limiting for some cryo applications e g unattended operation It also adds weight and surface area which can transfer vibration to the microscope column e On some heavily loaded SEMs there is often a lack of clearance to other accessories to enable the fitting of an on column dewar there may be a free SEM port but no space above for the dewar e The CHE3000 has a 12 litre liquid nitrogen capacity allowing run times between refills of over 16 hours Issue 1 3 November 2011 22 PP3000T User Manual V1 3 Typically the CHE3000 needs to be located behind the SEM and is connected to the SEM through tubes Access is needed to the dewar for filling The system has been designed with ease of use in mind The entire system i
42. e thicker emulsions Figure 51 Hole mount preparation 4 4 2 5 Film emulsion mounting This is useful when the specimen is small and would be obscured by Tissue Tek or when specimens need to be recovered Specimens need to be damp to use this method i e Nematodes Mount exposed unused film with the emulsion side up to the stub with mounting media Lay the damp specimen on the surface The specimen dampness slightly dissolves the film emulsion allowing the specimen to adhere to the film surface Issue 1 3 November 2011 48 PP3000T User Manual V1 3 Figure 52 Film mount preparation 4 4 2 6 Liquid film mounting Liquid specimens can be thinly spread on a plain stub which has been roughened with fine abrasive paper Figure 53 Liquid preparation 4 4 2 7 Rivet mounting Use rivets for liquids and when specimens need to be frozen off the stub to achieve fast freezing rates The rivet is placed in a hole and filled with liquid prior to freezing or if the specimen needs to be frozen rapidly off the stub 2 rivets are held together filled with liquid and plunge frozen prior to mounting in the rivet holder Rivets part 39996300 will push fit into the two holes of the E7449 multi stub supplied with the system Figure 54 E7449 stub Issue 1 3 November 2011 PP3000T User Manual V1 3 49 O O O O Figure 55 Rivet mounting preparation Other specimen stubs and shuttles are available see section 8 P
43. e venting operation if it has not cancelled automatically Remove the front window retaining bezel This is held by six M3 countersunk screws Hold the glass and bezel as you remove the last screw and do not let the bezel fall against the probe feed through Figure 71 Removing the front bezel Holding the glass window in place put the bezel to one side Now draw the window out squarely The window is quite thick and if it turns at an angle as it comes out it may jam and this will cause the glass to flake and chip If this occurs a replacement window will be required Figure 72 Front window removed Issue 1 3 November 2011 PP3000T User Manual V1 3 69 You will need to have the 2 5mm hexagon wrench ready as the window is withdrawn so that you can detach the cooling braid for the front window knife mum M s N Figure 73 Knife braid screw Place the window plate with its knife manipulator on a soft surface It should be noted that the knife manipulator fitted to the front window has a scalpel blade as its cutting edge There is a high risk of personal injury You now have access to the chamber though the front opening You may decide to remove the sputter head at this stage although it is not entirely necessary To do this you will need to release the argon gas feed capillary This will require the 5 16 spanner Issue 1 3 November 2011 70 PP3000T User Manual V1 3 Figure 75 A
44. en dU 31 3 01 SUDIIMATIONE a a NONIS UU dE 31 3 6 1 1 Defining a new sublimation recipe ss 31 3 6 1 2 Editing an existing sublimation recipe cccooccnccncnnncnocnononacononacononanonnnnos 32 3 6 1 3 Assigning a recipe to a quick access button 32 3 5 14 sSavimnpgadermneg rec Dei tete ne Let sde te 33 37 Coating the SPECIMEN iia ras 34 3 7 1 Using the optional film thickness monitor 35 3 5 2 Replacing tbe FIM CNS an ud uta rit A bes osi uses peu ide 36 3 7 3 Using the optional carbon evaporator E ENEA 37 3 5 44 Loading the carbon string sas re nee ta eps etu E teo Maiden 38 3 90 Magma CONTOUR iu deni E eoe eee 39 3 9 Messie me d 6d5 cose n vied cedi aede Dee redde BY eun s ide hn eee e 40 3 10 Shutting down the software and access to reserved functions 41 4 RBRunninethesyStelm uus radice Ai 43 Ad Milt lal preparacion atate tae RE Rb dag 43 EE quot 43 273 KOON QOWDsu RSR ac A Dei di 45 A Preparing a standard specimens 45 441 Making nitrogen luslhi a eas ro GA 46 AAD Mounting methods Nr a 46 442 1 Sirrace Mounn ASE ASS ES 46 BAD EdSe MOUNN aa 46 AA FIterMOUNUNBS ES 2 annee dois te ls seems vessie ns 47 WAZA HONE TMOUNUING an 47 AAD Film emulsib mounte seii o utet npud Pa ds dd io Nes 47 24 235 Loti TINO UNTING tati rats 48 4357 dANVetmolntllBssseustasie au n EAE aV a a nang RAS eee te 48 AAS i um pnr 49 4 4 4 Transferring to the preparatio
45. entering incorrect values Issue 1 3 November 2011 86 PP3000T User Manual V1 3 11 2 Configuration mode 4015 O 4017 O 4024 Command Send 1 T Set Address Gas Flow Control Values Head Interlock 7 e Anticontaminator Q SEMCryoStage on On Y ni en SEM Heater Prep Heater Heater Control Values Vacuum Units a nticontaminator O SEMCryoStage Q Prep Chamber m mbar 0 400 Gain 0 000 Derivative 500 Integral O Fascal Configuration StartLeakDetectVacuum v BB PSU Comms a Sputter O Chamber 1 Q Chamber 2 Q Evaporator Figure 88 Configuration page Issue 1 3 November 2011 PP3000T User Manual V1 3 87 9 4015 O 4017 O 4024 1 A command a Set Address Gas Flow Control Values Head Interlock 7 a Antilontaminator Q SEMCryostage on on 0 015 0 050 SEM Heater Prep Heater i d 4 Control Control StartLeakDetectVacuum StartLowVacuumTimeoutSeconds Vacuum Units StartHighVacuumTimeoutSeconds E mbar StartHighOkVacuum AirlockVacuumLevel 0 500 ew PumpVacuumTimeoutSeconds Pascal PumpValveOpenTimeoutSeconds VentAirlockDelaySeconds StartLeakDetectVacuum PSU Comms e Sputter O Chamber 1 Chamber 2 O Evaporator 24 a Figure 89 Configuration drop down menu Issue 1 3 November 2011 88 PP3000T User Manual V1 3 11 3 Diagnostics mode Vacuum System Prep Chamber Workstation Rotary Pump Turbo Purp Buffe
46. ese stubs which can have multiple holes and slots machined in them Preparation chamber The preparation chamber is a vacuum chamber mounted on the side of the SEM It has an integral cold stage and anti contaminator as well as coating and fracturing facilities This is where all cryo specimens will be processed before transfer into the SEM Issue 1 3 November 2011 PP3000T User Manual V1 3 91 Penning gauge Penning gauges are ionization gauges which operate with a cold discharge cold cathode The discharge which takes place in a measuring tube is very similar to that of a sputter ion pump The gauge has two electrodes cathode and anode between which a discharge is struck and maintained by a high DC voltage approx 2 kV A magnetic field is applied to make the paths along which electrons sufficiently long that their collision rate with gas molecules is large creating a large number of ions required to maintain the discharge The magnetic field lines confine the electrons to a spiral path The ions produced by these collisions move to the electrodes and form a pressure dependent discharge current The value current is dependent on the type of gas molecules present in the vacuum Pirani gauge Pirani gauges are gauges for measuring vacuum that use a heated sensor wire Pressure is determined by measuring the current needed to keep the wire at a constant temperature A Pirani gauge will only measure vacuum levels in the lower range dow
47. evaporation unit is fitted an extra button appears on the main screen in the process area PP3000T Control version 0 7 3 0 Anticontaminator SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T Startup 2466 05 mbar 4 06E 01 Cancel Operation Evaporate button Prep Save Camera Image System OF Figure 34 Main screen with carbon option fitted Touching the Evaporate button opens the evaporate sub menu Evaporation Edit Edit Figure 35 Evaporate sub menu The evaporation is fully automatic Firstly the carbon string is outgassed during which time the specimen should be shielded using the micrometer knife A message on the screen reminds the user to do this Once outgassed the user us prompted to retract the micrometer knife Once this is confirmed the string will be rapidly heated until it fuses Issue 1 3 November 2011 38 PP3000T User Manual V1 3 Should the user wish to alter the default parameters the SETUP button should be touched This will activate the settings and they may be changed using the EDIT buttons Current Current A Time Time 10 15 Figure 36 Editing the evaporate parameters 3 7 4 Loading the carbon string The carbon string is held in place by two spring loaded electrodes Wrap the string around one of the electrodes under the spring loaded part Make sure no frayed ends are sticking out Gently pull the string across to the other electrode
48. face of the dewar is coated to prevent boiling and is made of aluminium to reduce weight The dewar is mounted from the top lid and is located by plastic isolators to prevent vibration Issue 1 3 November 2011 18 PP3000T User Manual V1 3 2 3 8 Gate valves Two gate valves isolate the prep chamber from the SEM and transfer airlock These valves are solenoid interlocked to prevent opening when the vacuum levels are incorrect A bi colour LED shows the valve status The SEM valve provides interlocking signals to the SEM and where the necessary signals are made available by the SEM manufacturer can be disabled by the microscope 2 3 9 Cryo transfer device see Figure 6 The specimen is transferred cold and under vacuum from the PrepDek slusher to the airlock using a dedicated transfer device This device has a sealed chamber which is pumped out on the slusher and then closed The specimen shuttle Figure 5 latches onto the thermally isolated transfer rod via a bayonet fitting which engages and disengages by rotating through 90 A pointer on the outer end of the transfer rod indicates the orientation of the bayonet A window in the back of this device allows observation of the specimen as it is transferred into the preparation chamber or onto the SEM cold stage Figure 5 Specimen dovetail and bayonet fitting Issue 1 3 November 2011 PP3000T User Manual V1 3 19 2 4 Figure 7 Cryo transfer device rear view
49. ferred to the SEM are eliminated A multi range vacuum gauge is mounted directly on the chamber giving an accurate reading of the vacuum level close to the specimen Main pumping line ul OO o Multi range gauge aa Nitrogen dewar De Cooled adjustable knife L TM i Airlock control switches and LEDs Transfer pot SEM gate valve Cooled knife Prep gate valve Figure 3 Preparation chamber Within the preparation chamber are 2 3 1 Cold stage The cold stage fitted to the preparation chamber has twin cartridge heaters and a Pt100 temperature sensor It sits on a cold block and is separated from this Issue 1 3 November 2011 16 PP3000T User Manual V1 3 block by a thermal break This allows the cold stage temperature to be varied without boiling off a considerable amount of liquid nitrogen The cold stage temperature can be varied between about 185 C and 50 C with a stability of 1 C and is controlled by one channel of the three channel dedicated temperature control system The low thermal mass of the cold stage allows rapid temperature stabilisation The main cold block is connected to the liquid nitrogen dewar via copper braids which allow for any movement due to thermal contraction 2 3 2 Cold trap The cold trap is mounted directly onto the cold block and sits close to liquid nitrogen temperature It is made of gold plated copper for optimal thermal performance 2 3 3 Illumination
50. g the Sublime button calls up the sublimation control screen Sublimation is done via recipes which the user can define and save for future use Up to three commonly used recipes can be assigned to quick access buttons for instant recall The profile of the defined sublimation curve is shown graphically in the centre of the frame with an approximation of the warming and cooling ramps The profile can be edited or a new one defined using the New or Edit buttons Sublimation can be carried out in the preparation chamber or in the SEM chamber The stage SEM or Prep which is to be used for sublimation is selected by a radio button Sublime Recipe minus90for5mins x ETUR am Q In SEM Minutes 1 minusS farSmins 2 3 Figure 24 Main sublimation screen Recipes 3 6 1 1 Defining a new sublimation recipe When the New button is touched a pop up window appears which is very similar to the Edit screen but there will be no temperatures or times defined The window is described below in 3 6 1 2 Issue 1 3 November 2011 32 PP3000T User Manual V1 3 3 6 1 2 Editing an existing sublimation recipe Touching the Edit button opens a pop up window Figure 25 which displays the shape of the current defined sublimation curve and buttons which allow the values to be edited new steps to be added at any point in the overall curve or to delete certain points Touching the up and down arrow buttons scrolls throu
51. gh the defined steps Edit Sublime Recipe Temperature Minutes 5 Minutes Figure 25 Editing the sublime recipe The Edit button allows the user to change the temperature or time of the currently selected point The Add button will add another temperature and hold time to the end of the list The Insert button will add another temperature and hold time above the currently selected point The Remove button will delete the currently selected temperature and hold time As the curve is edited the graphic will change to reflect the edits Touching the Close button will transfer the updated curve to the sublime window and close the editing window 3 6 1 3 Assigning a recipe to a quick access button In the Recipe frame are three quick access buttons labelled 1 2 and 3 and a Setup button When Setup is touched another pop up window appears with the available recipes displayed The user touches the file name of the required recipe and touches the OK button The selected recipe will be assigned to the quick access button Touching Cancel will close the window with no changes Issue 1 3 November 2011 PP3000T User Manual V1 3 33 Load Recipe select Recipe File Name 10010710 pst 0dedg2rnins psb two psb Figure 26 Loading a stored recipe 3 6 1 4 Saving a defined recipe If a recipe has been defined which will be used again it can be saved to disk Figure 27 for recalling at a later
52. igital I O card and all gauge readings are made via the vacuum control board The system is designed to be modular and simple to diagnose should any fault occur The main power unit supplies the sputter high voltage the evaporation low voltage high current and the system 24V Each unit is stand alone and communicates via RS485 protocol with the main control PC Issue 1 3 November 2011 PP3000T User Manual V1 3 21 2 5 Turbo pumping stack The system is evacuated by a turbo pumping stack This stack has an integral buffer tank which means the backing pump only runs a few minutes in each hour A Pirani gauge monitors the buffer tank pressure and triggers the control PC when the tank needs to be pumped Another Pirani gauge monitors the backing pressure and is also used for system and airlock pump monitoring The pump stack has a heavy anti vibration base block to prevent transfer of vibration to the SEM chamber Connection from the turbo to the preparation chamber is by a stainless steel vacuum bellows All valving is integrated into the pump stack and is controlled via the PC Caution The pump stack is heavy Use the supplied strap if it needs to be moved This requires two people 2 6 CHE3000 cold gas cooling system An off column dual circuit gas cooling system CHE3000 provides the cooling for the SEM cold stage and anti contaminator Each circuit is controlled independently allowing a large temperature differential to be set between th
53. imen has been sufficiently sublimated it can then be coated with a fine layer of metal to render it conductive Once again coating is done using recipes in much the same way as for sublimation Touching the Sputter button opens the sputter coating window Figure 29 Recipes 1 1 maforB secs 2 3 Coating Recipe Cancel Figure 29 Coating recipe screen Editing saving and defining recipes in this window function in the same way as for the sublimation menu Only one set of time and current may be defined Issue 1 3 November 2011 PP3000T User Manual V1 3 35 Once a recipe is defined the user just has to touch the Start button for the sputter coating to run under fully automated control Figure 30 Sputter plasma under automatic control 3 7 1 Using the optional film thickness monitor If the optional film thickness monitor is fitted the sputtering may be controlled by the monitor The FTM button should be touched to access the FTM control panel Sputter Recipe Tw button Use FTM Cancel Recipes Figure 31 FTM button The FTM menu will then appear Measured thickness 0 000 Material Platinum Cancel Crystal usage Fail Figure 32 FTM menu FTM settings The default target material will be displayed as well as the measured thickness To change the target material touch either the NEXT or PREV buttons to cycle Issue 1 3 November 2011 36 PP3000T User Manual V1 3 through
54. lt InitialGasFlow gt Default gas flow for the anti contaminator value in litres minute lt GasFlowGain gt 0 02 lt GasFlowGain gt Default gas flow gain arbitrary units lt GasFlowDerivative gt 0 3 lt GasFlowDerivative gt Default gas flow derivative arbitrary units Issue 1 3 November 2011 PP3000T User Manual V1 3 81 lt GasFlowIntegral gt 0 05 lt GasFlowIntegral gt Default gas flow integral arbitrary units lt GasFlow gt lt Anticontaminator gt lt SEMCryoStage gt lt Temperature gt lt MinTemperature gt 196 lt MinTemperature gt Lowest temperature which can be entered by the SEM stage controls value in degrees Centigrade lt MaxTemperature gt 50 lt MaxTemperature gt Highest temperature which can be entered by the SEM stage controls value in degrees Centigrade lt InitialTemperature gt 140 lt InitialTemperature gt Default temperature for the SEM stage value in degrees Centigrade lt HeaterGain gt 0 1 lt HeaterGain gt Default heater gain for SEM stage arbitrary units lt HeaterDerivative gt 0 1 lt HeaterDerivative gt Default heater derivative for SEM stage arbitrary units lt Heaterintegral gt 0 1 lt Heaterintegral gt Default heater integral for SEM stage arbitrary units lt Temperature gt lt GasFlow gt lt MinGasFlow gt 0 lt MinGasFlow gt Lowest gas flow which can be entered for the SEM stage value in litres minute lt MaxGasFlow gt 5 lt MaxGasFlow gt Highest gas fl
55. ltage directive EN61326 1 2006 EN61000 4 2 EN61000 4 3 EN61000 4 4 EN61000 4 6 EN61000 4 8 EN61000 4 11 as well as EN61010 Safety requirements for Electrical Equipment for measurement control and laboratory use Part 1 General requirements Any modifications to the equipment including electronics or cable layout may affect the compliance with these directives 1 4 Servicing 1 4 1 Disclaimer All service work on the equipment should be carried out by qualified personnel Quorum Technologies cannot be liable for damage injury or consequential loss resulting from servicing from unqualified personnel Quorum Technologies will also not be liable for damage injury or consequential loss resulting from incorrect operation of the instrument or modification of the instrument 1 4 2 Operators and service engineers A normal operator of the equipment will not be trained in or qualified for service work on the equipment and may cause a hazard to themselves or others if such work is attempted Operators should therefore restrict themselves to the normal operation of the equipment and not by removing covers from the electronic equipment or dismantling of the instruments Service Engineers who are suitably trained to assess and isolate electrical mechanical and vacuum hazards should be the only personnel who access the equipment 1 5 Hazard signals and signs 1 5 1 Hazard signal words The standard three hazard signal words are defined a
56. n chamber 49 AA e CNO n su uoce NES oi aps taal beam danes Eu rua na NO Ran EUN ME DE 50 Issue 1 3 November 2011 PP3000T User Manual V1 3 5 465 _ SUDIIMATIOMS RUE naive free detu atium busdam tocando E 51 v COINS rM 51 4 4 8 Transferring the specimen into microscope LL 51 4449 Removing the Specimens reed uere ug Neteco eara a eee rires Face etu as con 51 4 5 Advanced specimen handling pot ss 52 5 Shuttihethe systemidoWL e endtaniet estis dte D acte ae ne 55 6 General Maintenant x ita Care dnt 57 6 1 Pumping the transfer device storage tube 57 6 2 Pumping the vacuum isolated pumping line oocccooccccccnonnnonacononanononnnonnos 57 6 3 Lubricating the vacuum transfer device rod 59 Te ShpoubleshoOLlf dg O e o os 61 o PR SOOO MT SMUETICS ANS EDS E Dean ent ue 63 9 Mantena NCO android 65 gie Preparation chamb aia 65 9 2 Cleaning the preparation chamber n i a 66 AE MEOE COM mmm 66 9 2 2 REASONS Tor Cleans die urmasa E 66 Ss Chambercleaningssnortmethiod aas ee eo IE VERE ei sad eee ant Eben sd 67 9 3 1 Venting the preparation chamber ss 67 9 4 Chamber cleaning thorough method top access 73 9 4 1 Remove the top plate ars 74 10 Appendix The XML control parameters file 77 11 Appendix ll Service and diagnostics mode c oocccccncccnonoconcnnaronccnnnnnonacononaronnnnanononos 83 11 1 Accessing the configuration and diagnostic modes oocccconccnccnonnn
57. n key in the way described in the introduction Do not over tighten any screws Carefully inspect the O ring in the top edge of the preparation chamber If necessary the O ring may be removed for cleaning Removal will not require any tools as it is a loose fit in the O ring groove Clean the O ring using lint free tissue and clean alcohol If the O ring is damaged it must be replaced Inspect the seal face of the chamber top plate and clean the seal surface with alcohol Place to chamber top plate over the dewar top and lower it down to meet the O ring surface Push the lid forwards so it is aligned with the chamber body and place screws in the two front corner holes and one in the back centre hole leaving the screws loose Place the remaining screws into their holes and progressively tighten them all in rotation sequence until they are all sufficiently tight Replace the dewar Issue 1 3 November 2011 PP3000T User Manual V1 3 77 10 Appendix The XML control parameters file All parameters for the control system are saved in an XML file There are very few hard coded values in the software Each parameter has limit values to prevent erroneous values being entered The contents of the XML file are described below xml version 1 0 encoding utf 8 gt PP3000TConfig xmins xsi http www w3 org 2001 XMLSchema instance xmins xsd http www w3 org 2001 XMLSchema gt lt SEMWebCamRegistryString gt lt SEM
58. n to 10 mbar and is typically used in low vacuum systems such as rotary pumped sputter coaters A Pirani gauge is sometimes used in conjunction with a high vacuum gauge such as Penning to measure vacuum in the low pressure range Most of our high vacuum products now use full range gauges a single gauge which measures vacuum from atmosphere to high vacuum Rotary pump A rotary pump is a type of vacuum pump where pumping is produced by moving air from one side of a rotating cylinder to another by means of an eccentric drum Rotary pumps are used with all of our coaters either to evacuate instruments directly or to rough pump and back high vacuum sputter coaters and vacuum evaporators Turbo pump A turbo molecular turbo pump is a type of vacuum pump used to obtain and maintain high vacuum The principle of operation is that gas molecules within a vacuum chamber can be given momentum in a desired direction by repeated collisions with a rapidly spinning turbine rotor The rotor hits gas molecules from the inlet of the pump towards the exhaust in order to create or maintain a vacuum A turbo pump normally works in tandem with a low vacuum pump such as a rotary vacuum pump which is used to rough pump the vacuum system e g sputter coater or vacuum evaporator during initial pump down period and to back the turbo pump i e remove gases from the back of the pump during high vacuum operation Liquid nitrogen f
59. nsure adequate ventilation Lifting of Heavy Items Service engineer Protective footwear Use Dropping on foot Back strain lifting equipment 1 6 2 Hazardous materials Isopropanol IPA For certain service tasks isopropanol is suggested for cleaning components before use in the vacuum system It should be noted that isopropanol is a flammable liquid and as such should not be used on hot surfaces In addition it is recommended that protective gloves are worn when using isopropanol Liquid nitrogen Only operators with experience in the safe handling of liquid nitrogen should use the equipment under these conditions Thermally insulated gloves and goggles should be worn at all times when handling and using liquid nitrogen The instrument uses nitrogen and argon gas supplies for its operation the customer is responsible for maintaining the supply to the instrument This supply should be Issue 1 3 November 2011 10 PP3000T User Manual V1 3 regulated and kept to the lowest pressure and flow rate as is practical to minimise the effects of any leaks 1 7 Good working practices It is essential that good hygienic working practices are adopted at all times especially in an ultra high vacuum or cleanroom environment and are generally of the common sense type Some simple good practice rules are e If in doubt don t e If in doubt ask e When handling solvents wear face mask gloves apron and work only in a well ventilate
60. oking through the transfer device window or at the CCD image slide the specimen dovetail onto the SEM cold stage Rotating the insertion rod 90 degrees will release the bayonet and the insertion rod may be retracted into the transfer device The SEM gate valve should now be closed and the solenoid will lock and the SEM lamp will extinguish Close the transfer gate valve The specimen should be imaged and if the preparation is successful the transfer device should be removed from the preparation chamber to reduce any induced vibration This is done by pressing and holding the Vent button on top of the airlock and once vented lift the transfer device off the airlock and place in the storage tube 4 4 9 Removing the specimen Drive the SEM stage to the cryo load position If the transfer rod has been removed from the preparation chamber it must be re fitted and evacuated as per inserting a specimen Open the gate valve and check the prep chamber pressure recovers Press Transfer to release the SEM column valve and open the valve Slide the insertion rod fully into the Issue 1 3 November 2011 52 PP3000T User Manual V1 3 SEM and engage the bayonet into the specimen shuttle Slide the rod fully back into the transfer device close the SEM valve followed by the prep valve Partially close the small transfer device cover to make sure it clears the prep valve body Vent the airlock and remove the transfer device Remove the specimen shuttle warm
61. onannnnonarononanos 83 11 2 Conte ura tion OGG quist cene etri tec ac ue Civ cite m enone ane ee 86 11 35 Did notes Mode a NECI meee 88 12 Glossary OF TENSA Ad 89 15 SWC CE DAS aMSN nice neo 93 Issue 1 3 November 2011 6 PP3000T User Manual V1 3 For technical and applications advice plus our on line shop for spares and consumable parts visit www quorumtech com Quorum Technologies Ltd is the manufacturer of a range of EM preparation equipment 2 Acorn House The Broyle Ringmer East Sussex BN8 5NN Tel 44 0 1273 815340 UK Fax 44 0 1273 813439 Email sales Q quorumtech com Web http www quorumtech com For further information regarding any of the other products designed and manufactured by Quorum Technologies contact your local representative or directly to Quorum Technologies at the address above o Carbon and sputter coaters o Plasma reactor for ashing and etching o High vacuum bench top evaporators o Cryo transfer systems e Critical point dryers o Service and spares For technical and applications advice plus our on line shop UK only for spares and consumable parts visit www quorumtech com Disclaimer The components and packages described in this document are mutually compatible and guaranteed to meet or exceed the published performance specifications No performance guarantees however can be given in circumstances where these component packages are used in conjunction with equipment s
62. orrectly located in its groove Holding the window adjacent to the window opening extend the knife manipulator into the chamber and re connect the knife cooling braid Slide the window into place and hold in position Place the window bezel in place and fit a screw top and bottom so that the window is held in place Re fit the remaining screws and gently tighten them in turn until they are all secure Please note that that this does not mean too tight Once the chamber is sealed check That the prep chamber lights are working Check that there is a sensible temperature reading for the prep chamber stage software test function required Check that the side window sputtering shutter works Check that the stage heater is working To do this set a temperature for the stage that is above the read temperature and set the heater operation to AUTO You will see the heat power reading bar show an indication of applied power and the temperature of the stage should rise If all of these functions are working satisfactorily the chamber may be evacuated by selecting the START option and choosing CRYO or A LOCK mode Observe the vacuum recovery and turbo speed The turbo should reach 100 and a pressure of XXx10 X within XX minutes Failure to reach this vacuum level or failure of the turbo pump to reach full speed will indicate a vacuum leak 9 4 Chamber cleaning thorough method top access This is a regular maintenance task tha
63. ow your company s standard Health and Safety instruction when using this liquid gas Issue 1 3 November 2011 PP3000T User Manual V1 3 11 1 9 Scope This manual is intended for all users of the PP3000T Cryo System manufactured by Quorum Technologies and provides information on the operation and maintenance of the instrument Please note that the servicing and maintenance procedures should only be carried out by qualified service personnel and it is essential that all users should read the Health and Safety section of this manual 1 10 Return of goods If goods are to be returned to Quorum Technologies for repair or servicing the customer should contact their local distributor or the factory direct before shipment A Returns Authorisation Number should be obtained in advance of any shipment This number is to be clearly marked on the outside of the shipment All returned goods are to be accompanied by a completed Returned Goods Health and Safety Clearance form HSC 100 attached to the outside of the package to be accessible without opening the package and a copy of the forms should be faxed in advance to the factory A copy of this form can be found at the end of the manual or requested directly from Quorum Technologies the details can be found on page two of this document 1 11 Returns procedure 1 11 1 Warranty claim Electronic and basic servicing capabilities exist at most in country appointed agents however all
64. ow which can be entered for the SEM stage value in litres minute lt InitialGasFlow gt 0 lt InitialGasFlow gt Default gas flow for the SEM stage value in litres minute lt GasFlowGain gt 0 02 lt GasFlowGain gt Default gas flow gain arbitrary units lt GasFlowDerivative gt 0 15 lt GasFlowDerivative gt Default gas flow derivative arbitrary units lt GasFlowIntegral gt 0 05 lt GasFlowIntegral gt Default gas flow integral arbitrary units Issue 1 3 November 2011 82 PP3000T User Manual V1 3 lt GasFlow gt SEMCryoStage lt PrepChamber gt lt MinTemperature gt 196 lt MinTemperature gt Lowest temperature which can be entered by the Prep stage controls value in degrees Centigrade lt MaxTemperature gt 50 lt MaxTemperature gt Highest temperature which can be entered by the Prep stage controls value in degrees Centigrade lt InitialTemperature gt 140 lt InitialTemperature gt Default temperature for the prep stage value in degrees Centigrade lt HeaterGain gt 0 5 lt HeaterGain gt Default heater gain for prep stage arbitrary units lt HeaterDerivative gt 0 3 lt HeaterDerivative gt Default heater derivative for prep stage arbitrary units lt Heaterintegral gt 0 1 lt Heaterintegral gt Default heater integral for prep stage arbitrary units lt PrepChamber gt lt SavedCoatingRecipes gt lt string gt lt string gt lt string gt lt string gt Names of the saved sputter coating recipe
65. r Once the user confirms by pressing OK another window pops up reminding the user to fit the pump out valve to the CHE3000 Startup Please fit the pumpout valve to the CHESOUU Figure 44 CHE insertion reminder On seeing OK the system will pump down the valve pumping line and check for leaks If this test is passed another window will pop up requesting the user to open the pump out valve Startup Flease open the pump out valve Figure 45 Open valve reminder The automatic pump down sequence will start The rotary pump is switched on first and the vacuum in the lines checked for leaks If this test is passed the buffer tank valve will open and the system will be roughed out Again if no leaks are suspected and the vacuum comes down to the set trip point the turbo pump is started and the system pumped to high vacuum This may take some time if the system has been at atmospheric pressure for any length of time Issue 1 3 November 2011 PP3000T User Manual V1 3 45 4 3 Cool down If the system has been started in Auto mode a message to cool down the preparation chamber will appear once the system has reached high vacuum When the system sees the temperature of the prep chamber dropping it will start a low 1L min gas flow through the CHE3000 to purge the lines This is to make sure the lines are clean and free from any moisture which could cause a blockage in the gas lines The purging lasts for 20 minutes
66. r Tank Valve System ent Valve Prep fac 4 00E 05 Airlock vac 1 00E 01 But Tank sac 1 66E00 Turbo Speed 100 Sputter Unit Enable 0 0 Current 0 0 0 Voltage Airlock Pump LED Airlock vent LED Airlock ent Valve Airlock Pump Valve Accessory Vent Valve e Buffer Contral Evaporation Unit Enable 0 0 0 0 0 0 0 0 Pump Airlock Pra Airlock Valve Status Slushing Pump Vent Airlock Pra Valve 1 Airlock Valve Cle Column false Slushing Vent Valve 1 Status Airlock Fitted Sputter Shield Solenoid Airlock Yale Solenoid Slushing Pump Valve 2 Trolley Chamber valve Prep Lamp Solenoid ushi Pre e verti prs e uzr D vert 2prs Slushing ent Valve 2 O Desk lamp d Storage Valve Gas Flows Temperatures A ConF 0 74 c 1 0 Set Flow Heaters SEMF 0 10 i limin SEM A ConT 25 58 0 set Current Prep SEMT 25 82 PrepT 175 38 System Chamber Vacuum Isolated Auto e Chamber Valve Cle D Line valve 0 050 Bleed State Current z vacuum SEM lamp E Nitrogen Pressure 1 00 open otage Unit 4 Bt On Ott v Close Issue 1 3 November 2011 Figure 90 Diagnostics page Switch PP3000T User Manual V1 3 89 12 Glossary of terms Buffer tank In a standard vacuum pump configuration a rotary pump is used to provide a backing vacuum to a turbo molecular pump The rotary pump
67. r electron microscopy EM specimen coating the magnetron sputtering head design ensures that minimal heat energy electrons reach the specimen surface This is important as it reduces heat damage to specimen and is a significant factor in ensuring the grain size within the sputtered film is optimally small essential for high resolution field emission scanning electron microscopy FE SEM Sputter coating with metals such as platinum gold palladium or chromium is widely used for depositing fine grain high resolution films onto field emission scanning electron microscopy FE SEM specimens Chromium oxidises on contact with air which can present specimen storage problems For this reason iridium Ir sputter coating is increasingly preferred by many workers Fracturing Issue 1 3 November 2011 90 PP3000T User Manual V1 3 Carbon coating The thermal evaporation of carbon C is widely used for preparing specimens for electron microscopy EM A carbon source either in the form of woven fibre or graphite rod is mounted in a vacuum system between two high current electrical terminals When the carbon source is heated to its evaporation temperature a fine stream of carbon is deposited onto specimens The main applications of carbon coating in EM are making scanning electron microscopy SEM specimens conductive for subsequent examination by X ray microanalysis and being used as specimen support films on transmission electron
68. reezing Using liquid nitrogen is the cheapest and easiest way to prepare cryo SEM specimens Normally the specimen is plunged rapidly under slushed nitrogen see Liquid nitrogen slush Although the freezing is not that rapid it is usually enough for cryo SEM Issue 1 3 November 2011 92 PP3000T User Manual V1 3 Liquid nitrogen slush When pumped by a rotary vacuum pump liquid nitrogen can be solidified Liquid nitrogen freezes at 63 K 210 C The freezing efficiency of liquid nitrogen is severely limited by the fact that it boils immediately on contact with a warm object This creates an insulating nitrogen gas layer around the object This effect is known as the Leidenfrost effect By plunging an object into slushed nitrogen more rapid cooling may be obtained than plunging into liquid nitrogen at its boiling point 77K 196 C Rivets Rivets are used for liquid specimens and rapid freezing Two rivets are sandwiched together and plunged into nitrogen slush Their thin wall section and small volume give good freezing rates The rivets are then mounted in a stub and transferred to the preparation chamber where the upper rivet if knocked off to reveal the fractured surface Anti contaminator SEM cold stage Flushing Heat exchanger Argon gas Argon Ar is widely used as the process gas during sputter coating The use of argon is essential for clean contamination free coating of scanning electron microscopy SEM specimens Mo
69. rgon union There is a cover over the top of the LN2 dewar through which the sputter head cable passes The cover is retained by four M3 countersunk screws You will need a 2 5mm hexagon wrench for this Figure 76 Top plate cover removal Lift the dewar top cover and sputter head away from the top of the preparation chamber and place on a soft surface to avoid damage Take care to retrieve the seal ring from the dewar neck above the cover plate Please note the sputter head is of the Magnetron type and as so has a powerful magnet behind the target foil Take care to keep magnetic particles away from this Use tweezers to remove dropped samples and discarded rivets from any accessible surfaces If possible use a small vacuum cleaner pipe to remove debris from the cold shield top surface and from the lower front of the chamber Issue 1 3 November 2011 PP3000T User Manual V1 3 71 Figure 77 Chamber cleaning with vacuum adapter Using cotton buds remove the worst of the stray sputter coating from the cold shield taking care not to leave any debris from the cleaning materials Figure 79 Cleaning chamber with tissue Clean the cold stage and cryo shields with lint free tissues and cotton buds Use clean alcohol Issue 1 3 November 2011 72 PP3000T User Manual V1 3 Figure 80 Cleaning the LED cover glasses Clean the cover glasses of the LED chamber lights with cotton buds and alcohol Be very gentle
70. runs continuously In electron microscopy applications the vibrations from the rotary pump could be transmitted to the microscope To avoid this a vacuum reservoir is used between the rotary pump and the turbo pump This reservoir is called a buffer tank and is pumped to a low vacuum by the rotary pump and then a valve between the rotary pump and buffer tank is closed and the rotary pump turned off A Pirani gauge is then used to monitor the vacuum level in the buffer tank and when this rises to a pre set value the rotary pump is started again and the valve opened to re evacuate the buffer tank The rotary pump then only runs for a few minutes each hour Sublimation Cryo electron microscopy Cryo SEM Cryo SEM is a method for preparing liquid semi liquid or beam sensitive specimens for examination in a scanning electron microscope SEM The technique has huge benefits compared to alternative methods such as critical point drying and freeze drying because all of the specimen s water is retained Cryo transfer Cryo transfer device Slusher Pot Sputter coating Magnetron sputtering using a crossed field electromagnetic configuration keeps the ejected secondary electrons near the cathode target surface and in a closed path on the surface This allows a dense plasma to be established near the sputter target surface The ions that are accelerated from the plasma do not sustain energy loss by collision before they bombard the sputter target Fo
71. s manual Recommended tools Set of metric Allen keys 1 5 to 8mm Long reach magic ring M3 Allen key Dewar top nut spanner 5 16 1 4 spanner 395020220 Mini vacuum cleaner LED hand light 21mm open ended spanner 22mm open ended spanner 2 paint brush Peg spanner or circlip pliers transfer device Dental mirror Screw retaining tool Small size nozzle to suite vacuum cleaner Vacuum cleaner not supplied 9 1 Preparation chamber Please note the preparation chamber and many of the parts of the cryo system are manufactured from light aluminium alloy This material is highly suitable for this application and with care the instrument will last many years It is however easily damaged if mistreated Great care must be taken of seal faces and in the tightening of Screws Figure 68 Using an Allen key Issue 1 3 November 2011 66 PP3000T User Manual V1 3 Without exception screw threads into aluminium must not be over tightened and it is acceptable to use only the short arm of a standard Allen key for tightening Mistreatment of the chamber components will void warranty cover 9 2 Cleaning the preparation chamber This is a regular maintenance task 9 2 1 Introduction Cleaning of the preparation chamber is required in order to keep the instrument operational The frequency of this cleaning will be determined by the amount of use and sample type 9 2 2 Reasons for cleaning are To remove debris from sample frac
72. s control e Imaging control e Messaging areas Parameters on the screen which can be changed by the user are surrounded by a dark outline parameters which are read only are surrounded by a grey frame PP3OUD UT Control version D 7 1 7 Anticontarminator SEM Cryo Stage Prep Chamber Vacuum System Actual T Actual T Actual T Ex d za Startup peu Shutdown Open circuit Open circuit 166 Set T Set T Set T servie vacuum Turbo Speed nos JA Prep Chamber vacuum 1E 4 na 3 89E 06 mbar n 9E 01 mbar m e E E T SEM Camera ak Met Frep LENTE i Quorum Techno ogies Camera O N2 Pressure System OF OO 13 47 Figure 10 Main start up screen Issue 1 3 November 2011 24 PP3000T User Manual V1 3 3 1 Top data bar Software version number Version 0 7 1 YELLEN Shutdown Storage Figure 11 Blanking button and software version number Screen blank control The screen may be blanked at any time by touching the down arrow icon in the top right hand corner of the screen Touching anywhere on the blanked screen will restore the control interface The software version number is displayed next to the blanking icon 3 2 Temperature monitoring and control The temperature of the SEM anti contaminator SEM cold stage and preparation chamber cold stage are continuously monitored and displayed Prep Chamber Current read temperature Actual T 166 Current set temperature SetT Touch inside this box
73. s controlled by a touch screen PC This is mounted on a monitor arm attached to the PrepDek allowing it to be positioned to suit the user Most functions have been automated and the user can save personal settings for specimen coating and sublimation as recipes for future use The PrepDek workstation allows the user to work with pre frozen specimens as well as to freeze their own PrepDek designed as an expandable system where additional features will be added in the future Holders are available for virtually any type of specimen from liquids to rocks Special holders can also be developed to suit the users specimens if required Once the system has been cooled down and reached base temperature it will run all day without the need to refill the CHE3000 dewar The preparation chamber dewar hold time will depend on the number and temperature of sublimation cycles Continuing the ease of use philosophy disassembly and cleaning of the chamber is simple with a minimum of tools or dismantling required Windows are piston sealed and can be pulled out for cleaning The top and base are easily removable Issue 1 3 November 2011 PP3000T User Manual V1 3 23 3 Software On start up the system loads the control software and displays the main control window This window is split into logical functional areas e Top data bar e Temperature monitoring and control e Gas flow monitoring and control e Vacuum monitoring and control e Proces
74. s follows DANGER imminently hazardous situation or unsafe practice that if not avoided will result in death or severe injury WARNING potentially hazardous situation or unsafe practice that if not avoided could result in death or severe injury CAUTION potentially hazardous situation or unsafe practice that if not avoided may result in minor or moderate injury or damage to equipment 1 5 2 Hazard labels used on equipment Several hazard symbols may be found on the equipment they are shown in Table 1 below with their meaning Issue 1 3 November 2011 PP3000T User Manual V1 3 9 Table 1 Hazard warning symbols HIGH VOLTAGE Caution Equipment is heavy Caution refer to accompanying o Risk of injury Caution risk of electric shock documents 1 6 Risk analysis 1 6 1 Personal operational risks The following is a list of tasks carried out by both the operator and service engineer where recognised risks have been observed Listed is the personnel protection equipment PPE which is suggested for use for various tasks on any system Table 2 Personal operational risks Nature of hazard Cleaning of parts samples Operator service engineer Protective goggles protective with isopropanol IPA Splash hazard to eyes drying gloves of skin Use of liquid nitrogen in Operator service engineer Thermally protective gloves sample cooling etc Burn risk Asphyxiation risk and goggles should be worn E
75. sh to form Nitrogen ice pops up Prepare the specimen and mount it on the specimen shuttle using whichever mounting technique is suitable Fit the shuttle to the transfer rod bayonet 4 4 2 Mounting methods There are many ways to mount a specimen depending on the geometry and consistency Below are a few examples 4 4 2 1 Surface mounting For leaf samples etc Roughen the stub surface with fine abrasive paper place a small amount of mounting media mixture of 50 Tissue Tek 50 colloidal graphite onto the stub and lay the specimen on top of the mounting media Figure 48 Leaf sample preparation 4 4 2 2 Edge mounting For edge observations and fracture Roughen the surfaces of a stub with fine abrasive paper Mount the specimen on edge secured with mounting media or mount the specimen standing on edge in a machined slot secured with mounting media This is important if the specimen is to be fractured Issue 1 3 November 2011 PP3000T User Manual V1 3 47 Figure 49 Edge mount preparation 4 4 2 3 Filter mounting For liquid suspensions Secure the filter paper to the stub with four droplets of mounting media Secure the membrane filter to filter paper base using mounting media Pipette liquid suspension onto membrane filter Figure 50 Filter mounting preparation 4 4 2 4 Hole mounting For thicker emulsions and liquids i e oil toothpaste Use a hole or holes drilled in stub to locat
76. t should be performer by the instrument user This procedure will allow full access to the internal parts of the preparation chamber but should only be required if the chamber has become excessively soiled or in order to rectify faults that may have occurred Issue 1 3 November 2011 74 PP3000T User Manual V1 3 9 4 1 Remove the top plate Isolate the supply of argon gas to the PP3000 Loosen the argon supply union at the back of the chamber below the main pumping pipe connection with the 5 16 spanner and disconnect the capillary tube Figure 83 Argon union loosening Begin by performing the short method cleaning procedure to the point where the sputter head has been removed but do not carry out any cleaning at this stage cleaning will be done once the chamber has been further dismantled Loosen the dewar to nut with the special spanner supplied with the instrument tool kit You may need to remove the bracket that holds the pipes and electrical plug in order to gain access to the dewar nut Remove the nut and the plastic washer that will be found under it Issue 1 3 November 2011 PP3000T User Manual V1 3 75 Figure 86 Knife knob screw Loosen the grub screw in the knife control knob and lift the knob clear of the knife shaft Loosen all of the M4 screws that hold the top plate to the top of the preparation chamber Carefully lift the top plate away from the chamber applying gentle downward force to
77. to open the calculator window Increase decrease temperature by 1 C Toggle heater between off and Heater power level automatic control bargraph Figure 12 Temperature control area The temperature controls work in the same way for each of the three areas SEM cold stage SEM anti contaminator preparation chamber cold stage The current temperature is displayed at the top of the box This is read only If a sensor is not connected or a wire broken the current temperature will read Open circuit Below this the current set temperature is displayed This can be changed by using either the up down arrow buttons to make small increments or decrements or if a larger change is required by touching the set temperature display area This will call up a calculator window Figure 13 where the desired temperature may be entered Issue 1 3 November 2011 PP3000T User Manual V1 3 25 PP3O00T Control Version 0 7 1 7 Anticontaminator SEM Cryo Stage Prep Chamber Vacuum System i Storage Storage Open circuit Open circuit 30 set T Vacuum Turbo Speed Enter New Value IE LAE E1 T Clear rd y 3 N i 1E3 DES PN Failed to reach vacuum Prep Large Quorum Technologies Camera C3 M2 Pressure System OF O 19 43 Figure 13 Changing the set temperature The minus sign may be pressed at any time when entering the new set temperature If a data entry error is made it can be corrected by touching the Clear
78. trol Within the Vacuum System frame are several control buttons Startup Shutdown Pump Prep Storage Vent Prep Storage Vacuum Functions Overview View Log as well as the turbo speed indicator The speed indicator bar will change colour from red 8096 through orange lt 90 to green gt 90 depending on the turbo speed Issue 1 3 November 2011 28 PP3000T User Manual V1 3 3 4 2 1 Startup The vacuum system is automated and will begin its start up procedure when this button is touched On touching the Startup button a small options window opens Here the user can decide if they want to run a fully automated cryo session which guides the user though the full start up and loading procedure or to use the PP3000T in manual mode Should the user want to log the pump down and cool down the tick box labelled Log vacuum and temperature values should be touched Log vacuum and Auto Mode Id anual Made temperature values Figure 17 Start up pop up 3 4 2 2 Shutdown Pressing this button starts the automated shut down procedure PP3000T Confirm shutdown Figure 18 Shutdown initial screen Figure 18 shows the shutdown confirmation screen 3 4 2 3 Pump Prep Storage This button starts the pump out of the transfer device storage tube NB The transfer device should be in the tube before starting to pump Issue 1 3 November 2011 PP3000T User Manual V1 3 29 3 4 2 1
79. ture To retrieve sample mounting rivets if used To remove build up of sputtered material on internal chamber surfaces viewing windows and chamber lights Cleaning of the preparation chamber will normally be done at the end of a cryo work run in readiness for the next cryo work run and having allowed the instrument to come up to ambient temperature It will be assumed that the instrument is being pumped and is in good working order Clean gloves must be worn throughout the maintenance routine to avoid contamination of vacuum surfaces The cleaning process is simple and should not give any problems if conducted in a methodical manner Prepare by placing a soft mat on the microscope work top below the preparation chamber and have space enough to lay out the parts It is a good idea to have small dishes to keep screws safe Some of the work may need to be done away from the cryo chamber and microscope so prepare workspace in advance Two levels of chamber cleaning are possible Cleaning through the front window port will allow cleaning of accessible surfaces removal of debris used rivets and dropped samples This will be referred to as the Short method and may be required on a weekly basis depending on instrument usage Issue 1 3 November 2011 PP3000T User Manual V1 3 67 Figure 69 Working though the front window A more thorough cleaning will be possible if the cold stage and liquid nitrogen dewar is removed from the cham
80. unting media In order to attach a specimen to a shuttle or stub some sort of glue is needed The glue should not shrink when frozen nor bubble nor crack The usual media used for cryo SEM is a 1 1 mixture of Tissue Tek and colloidal graphite Issue 1 3 November 2011 PP3000T User Manual V1 3 93 13 Circuit Diagrams Issue 1 3 November 2011
81. upplied by companies other than Quorum Technologies Issue 1 3 November 2011 PP3000T User Manual V1 3 7 1 Health and safety Safety is very important when using any instrumentation and this chapter should be read by all users of our equipment This section of the manual applies to all equipment supplied by Quorum Technologies range of products not just the particular instrument to which the manual refers Included in this chapter are details on warning notations good working practices and information on European Community EC legislation regarding Control of Substances Hazardous to Health COSHH and risk analysis 1 1 Control of substances hazardous to health COSHH The EC legislation regarding the Control of Substances Hazardous to Health requires Quorum Technologies to monitor and assess every substance entering or leaving their premises Consequently any returned goods of whatever nature must be accompanied by a declaration form available from Quorum Technologies reference number HSC100 Without this declaration Quorum Technologies reserves the right not to handle the substance item Also in accordance with EC regulations we will supply on request hazard data sheets for substances used in our instruments 1 2 Safety policy This section contains important information relating to all health and safety aspects of the equipment As such it should be read and understood by all personnel using the instrument whether as
82. value in millibars lt TransferVacuumLevel gt 0 0001 lt TransferVacuumLevel gt Default vacuum level where column gate valve can be opened and a specimen transferred measured on prep chamber multi range gauge value in millibars lt PumpLineVaccumLevel gt 0 02 lt PumpLineVaccumLevel gt Vacuum level required to be reached when pumping the prep storage read on airlock Pirani gauge value in millibars lt AntiConFlowZeroOffset gt 320 lt AntiConFlowZeroOffset gt Default offset for anti con flow gauge calibration arbitrary units lt AntiConFlowLitreFactor gt 0 035 lt AntiConFlowLitreFactor gt Default gain factor for anti con flow gauge calibration arbitrary units lt SEMFlowZeroOffset gt 325 lt SEMFlowZeroOffset gt Default offset for SEM stage flow gauge calibration arbitrary units lt SEMFlowLitreFactor gt 0 038 lt SEMFlowLitreFactor gt Default gain factor for SEM stage flow gauge calibration arbitrary units lt General gt lt ComPorts gt lt PSUPort gt COM3 lt PSUPort gt COM port used on PC to address the power supply lt AdamPort gt COM1 lt AdamPort gt COM port used on the PC to address the ADAM modules lt ComPorts gt lt PrepVacuum gt lt MinVacuum gt 1E 06 lt MinVacuum gt Lowest value displayed on the prep vacuum analogue scale value in millibars lt MaxVacuum gt 0 01 lt MaxVacuum gt Highest value displayed on the prep vacuum analogue scale value in millibars Issue 1 3 November 2

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