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Oxford Instruments OptistatDry BLV User Manual - Original Instructions

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User Manual - Original Instructions
OptistatDryBLV

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Summary of Contents for Oxford Instruments OptistatDry BLV

  • Page 1 User Manual - Original Instructions OptistatDryBLV...
  • Page 2 OptistatDry BLV Manual Oxford Instruments Nanoscience Sep 2017...

  • Page 3: Table Of Contents

    5.8 Setting up the compressor ..........© 2017 Oxford Instruments Nanoscience...
  • Page 4 7.5 Troubleshooting ........... . . 8 OptistatDry BLV Specifications 8.1 Performance .

  • Page 5: Optistatdryblv - Principles Of Operation

    All such warranties are hereby excluded to the fullest extent permitted by law. Oxford Instruments will not be responsible for the accuracy of the information contained in this document, which is used at your own risk and should not be relied upon. The information could include technical inaccuracies or typographical errors. Changes are periodically made to the information contained herein;...

  • Page 6: Introduction

    If you sell or give away the product to someone else, please give them the manuals too. If you have bought a complete system from Oxford Instruments, separate manuals will have been supplied describing the other components. Please ensure you have reviewed the information supplied in all of the manuals before you attempt to operate your system.

  • Page 7: Restrictions On Use

    Any resultant non-compliance damage, or personal injury would be the fault of the owner or user. Use of the equipment for purposes other than those intended and expressly stated by Oxford Instruments, as well as incorrect use or operation of the equipment, may relieve Oxford Instruments or its agent of the responsibility for any resultant non-compliance damage or injury.

  • Page 8: Acronyms

    OptistatDry BLV Manual 2.7 Acronyms A number of acronyms may be used throughout this document. Please refer to the document Practical Cryogenics for a glossary of terms. • Next - Safety Information © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 9: Safety Information

    3.1 Disclaimer Oxford Instruments assumes no liability for use of any document supplied with the system if any unauthorised changes to the content or format have been made.

  • Page 10: Specific Hazards

    The electrical supply to the system must include an isolation box to ensure that mains electrical power to the system can be isolated. The isolation box must allow the supply to be locked OFF, but must NOT allow the supply to be locked ON. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 11: Protective Earth

    The correct operation of these relief valves is critical to the safety of the system. 3.9 Weight and lifting Incorrectly lifting heavy objects can cause severe injury. Use the appropriate lifting equipment, operated by fully © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 12: Magnetic Fields

    Areas where these chemicals are stored or used must be well ventilated to avoid the danger of suffocation. Oxygen level detection equipment should be installed in suitable locations to warn personnel if the oxygen concentration falls below a threshold value. Take precautions to prevent spillage of liquid cryogens. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 13: Fire

    • Hazard warning signs, barriers or controlled entry systems to ensure that personnel approaching the system are aware of the potential hazards. This precaution is especially important if you system includes a superconducting magnet. 3.14 Maintenance Observe the necessary maintenance schedule for the system. Consult Oxford Instruments if you are unsure about the required procedures. 3.15 Pressure relief valves There is an over-pressure relief plate on the front of the cryostat, shown below.

  • Page 14: Compressor And Cold Head

    OptistatDry systems will normally be supplied with a MercuryiTC. Safety features for this temperature controller are described in the corresponding manual, as supplied with the system. You should ensure that you understand and comply with all safety warnings and cautions. • Next - System Description © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 15: System Description

    The OptistatDry range is designed to be versatile, upgradeable, simple to use, and to provide optical excellence. 4.1 The cryostat The OptistatDry BLV (Bottom Loading in Vacuum) system provides a temperature controlled sample-in-vacuum measurement environment within a cryofree cryostat. The system enables optical and electrical measurements to be carried out on the user’s sample.
  • Page 16 OptistatDry BLV Manual Figure 4.1: Cryostat front view © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 17 OptistatDry BLV Manual Figure 4.2: Cryostat rear view © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 18 • Controls and monitors the heating and thermometry for the VTI heat exchanger. • Controls and monitors the heating and thermometry for the sample probe. • Monitors the thermometry for the 1 and 2 stages of the GM cooler. • Next - Installation © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 19: Installation

    An optional spares kit containing the tools required for assembly is available. 5.1 Site preparation Figure 5.1: System configuration (photograph) © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 20: Toolkit Lists

    The total weight of the cryostat and the vertical support stand is approximately 23kg. This is too heavy for one person to manage safely. All processes that require lifting or moving the partly or fully assembled system require two people. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 21 The system is shipped with the blanking windows fitted (black, opaque). It is a good idea to keep these in position whilst the system is installed. These can be removed and swapped for the system windows after the system has been cooled for the first time to check its performance. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 22: Mounting The Cryostat

    OptistatDry BLV Manual The OptistatDry BLV system is fitted with transit fixtures that must not be removed until the cryostat is as close as practical to its final operating position. The cryostat and frame should be placed upright on a firm flat surface. Note that the weight of the cryostat and frame assembly is 23kg, therefore two people are required to lift and move the assembly safely.
  • Page 23 Required A / mm Use side panel holes Note 280 - 310 1 and 2 255 - 280 2 and 3 230 - 255 3 and 4 205 - 230 4 and 5 © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 24 Replace the four M6 washers and nuts on the cradle. Turn the nuts until they just make contact with the L brackets; there is no need to fully tighten them at this stage. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 25 OptistatDry BLV Manual Figure 5.5: Defining the window height, A © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 26 OptistatDry BLV Manual Figure 5.6: Side panel hole numbering © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 27 OptistatDry BLV Manual Figure 5.7: Cradle height adjustment © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 28 OptistatDry BLV Manual Figure 5.8: Removing the upper nuts from the anti-vibration (AV) mounts © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 29 OptistatDry BLV Manual Figure 5.9: Removing the OptistatDry from its packaging © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 30 OptistatDry BLV Manual Figure 5.10: Do not lift by the cover © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 31 OptistatDry BLV Manual Figure 5.11: Inserting the cryostat © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 32 OptistatDry BLV Manual Figure 5.12: Mounting the cryostat Figure 5.13: The AV mounts and L-brackets © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 33: Cryostat Height Adjustments

    Note that the stand must be securely bolted to the optical table before attempting this procedure. • If the cryostat is to be raised, remove the four lower bolts holding the cradle to the side panels. Loosen, but do not remove, the four upper bolts. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 34 OptistatDry BLV Manual Figure 5.15: Support the cryostat weight with a lab jack © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 35: Fitting The Radial Restraints

    Pins at the ends of each restraint match recesses in a locator block on each side panel leg and a similar recess on the corners of the cryostat. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 36: Setting Up The Compressor

    10mm open-ended spanner, to fix the overall length. 5.8 Setting up the compressor You must read and follow the following procedures described in the SHI compressor technical manual installation section: © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 37 OptistatDry BLV Manual Figure 5.18: Mount the locator blocks Figure 5.19: Adjust the positon of the blocks © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 38 OptistatDry BLV Manual Figure 5.20: Diagram of a radial restraint Figure 5.21: Adjusting the restraints © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 39 OptistatDry BLV Manual Figure 5.22: Fixing the restraint length © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 40: Setting Up The Compressor Lines

    With all the helium gas line connections made, check that the static pressure indicated on the gauge of the compressor is within the range specified for your combination of cold head, gas line length and compressor. The nominal charge is 16.6bar / 240psi © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 41 OptistatDry BLV Manual Figure 5.23: Support the lines horizontally Figure 5.24: Restrain the supply line without damaging it © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 42 OptistatDry BLV Manual Figure 5.25: Support, but do not restrain, the return line Figure 5.26: Connections to the compressor © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 43: Electrical Connections To The Temperature Controller

    5.10 Electrical connections to the temperature controller The Mercury iTC has been configured by Oxford Instruments to suit the system ordered. When you first switch on the Mercury iTC you will see the instrument home screen, similar to that shown below: The Mercury iTC temperature controller should be connected to the cryostat as follows: •...
  • Page 44 OptistatDry BLV Manual Figure 5.28: Mercury home screen Figure 5.29: Electrical connections to the Mercury iTC © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 45 OptistatDry BLV Manual • Next - System Operation © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 46: System Operation

    System Operation This section describes how to cool the OptistatDry BLV to base temperature for the first time with blanking pieces fitted to the radiation shield openings and the OVC window mounts. The test sequence includes running the system to base temperature, controlling the sample position at 300K and then warming the entire system to room temperature.

  • Page 47: Conditioning The Sorption Pump

    Hence, just before cooling the system the sorption pump must be conditioned by heating and pumping the removable radiation shield plate. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 48 Figure 6.3: Replacing the sample access plate Always try to minimize the time the OVC and sorption pump are left exposed to atmosphere. It is advisable to refit the radiation plate (with © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 49: Evacuate The Cryostat

    6.3 Evacuate the cryostat Refer to the manual supplied with the pump for details of how to operate your pump. Optional turbo pumps supplied by Oxford Instruments (H4-600 or H4-601) have their own manuals. If using another pump, the pump should be oil-free and capable of achieving a base pressure of <1x10...

  • Page 50: Running The System To Base Temperature

    Select the Sensor that you want to use for control (either VTI or Probe), set the desired control temperature in the Set Point box and then switch the heater control from Manual to Auto. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 51: Control The Sample Region At 300K

    • Next, remove the window or blank. A vacuum tool (such as the Oxford Instruments DRYLOAD) or plastic tweezers can be helpful. • Remove the radiation shield window/blank by removing the spring clip. Fit the new window as required, or leave the mounting point on the radiation shield open.

  • Page 52: Sample Holders

    When the radiation shield plate is refitted the bolts should be tightened to a torque ~1.0Nm. Lift up the plate and remove it, storing carefully. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 53 Remove the six T20 Torx bolts holding the window block to the main OVC body. Hold the block in position as the last bolt is removed. When the window block is refitted the bolts should be tightened to a torque ~1.8Nm. Lower the optical window block, remove it and store in a clean, dry, sealed bag. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 54 OptistatDry BLV Manual Figure 6.7: Removing the standard sample holder © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 55 OptistatDry BLV Manual Figure 6.8: DRYLX20 connector near the sample positon Figure 6.9: Remove the bolts in the OVC © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 56: Puck Sample Holder - Fitting And Removing

    Prepare your sample and thermally attach it to the puck. Make electrical connections, if applicable. The surface of the puck has an “ENIG” surface finish. ENIG is an electroless nickel layer capped with a thin layer of immersion gold. It is a multifunctional surface finish, © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 57 OptistatDry BLV Manual Figure 6.11: Remove the bolts in the radiation shield Figure 6.12: Remove the radiation shield tail © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 58: Conditioning The Sorption Pump

    Do not set a control temperature in excess of 300K. When the set temperature is reached, the system will control at the set temperature until the control temperature is changed. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 59 OptistatDry BLV Manual • Next - Service and Maintenance © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 60: Service And Maintenance

    Adsorber replacement must occur every 30,000 hours, as it is critical in ensuring the helium gas circuit remains contaminant free. The adsorber replacement and helium gas charging procedures are described in the SHI Helium compressor technical manual. © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 61: Troubleshooting

    HC4E2) Cryocooler operation manual. Diagnosis of MercuryiTC temperature controller faults should be made using the MercuryiTC manual Troubleshooting chapter. Refer to the following table for problems arising from the OptistatDry BLV cryostat or a combination of the above. Problem Possible cause...
  • Page 62 OptistatDry BLV Manual If you are unable to resolve the problem, please direct allqueries through your nearest support facility. • Next - Appendices © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 63: Optistatdry Blv Specifications

    The refrigerator is a Sumitomo SHI 101D cold head with Standard A SHI HC4A2 air-cooled or Option W SHI HC4E2 water-cooled compressor. • Service intervals – Displacer replacement: 10,000 hrs – Compressor absorber: 30,000 hrs © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 64: Electrical Power

    • Base temperature may be reduced by fitting blanks to each of the windows. Radial window blanks are supplied as spares with the system. • The maximum operating temperature will be set accordingly in the Mercury iTC supplied with the system. 8.9 Further Information • Test Specifications • OptistatDry Index © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 65: Appendices

    Copper 36SWG Firerod heater (I+) 40 Ω other not used 9.2.2 21-way micro D connector to DRYLX20 Hermetic micro-D connector pin Wire type Solder pin number Constantan 42SWG Constantan 42SWG Constantan 42SWG © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

  • Page 66: Appendix C - Sample Puck Options

    Wire type Track number DRYPUCK12R / 12T Constantan 42SWG Constantan 42SWG Constantan 42SWG Constantan 42SWG Constantan 42SWG Copper 36SWG 6, 7, 8, 9 not used 17, 18, 19, 20 not used © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 67 OptistatDry BLV Manual Figure 9.1: 15-way pin numbering © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 68 OptistatDry BLV Manual Figure 9.2: 21-way pin numbering © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 69 OptistatDry BLV Manual Figure 9.3: DRYPUCK12R and 12T puck schematics © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 70 OptistatDry BLV Manual Figure 9.4: Puck track numbers and sample position © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...
  • Page 71 The internal wiring between these terminations consist of five twisted pairs of constantan 42 SWG wires and one twisted pair of copper 36 SWG wires. • Back to - OptistatDry BLV front page © 2017 Oxford Instruments Nanoscience MAN-OPTDRY-BLV-2.1.0 (28ff3d8) Sep 2017...

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