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OXFORD CRYOSYSTEMS PheniX Operation & Instruction Manual

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OXFORD CRYOSYSTEMS
PheniX
Operation &
Instruction Guide

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  • Page 1 OXFORD CRYOSYSTEMS PheniX Operation & Instruction Guide...
  • Page 2 Operation & Instruction Guide v2.6 Oxford Cryosystems Ltd 3 Blenheim Office Park Lower Road Long Hanborough Oxford OX29 8LN United Kingdom Phone +44 1993 883488 • Fax +44 1993 883988 Email Support@oxcryo.com © 2012 Oxford Cryosystems Ltd. All Rights Reserved.

  • Page 3: Table Of Contents

    How the PheniX works ..............................4 1.2. Items required for assembling your PheniX ......................... 5 Setting Up ........................6 2.1. Matching the PheniX Coldhead and 730 Series Controller ..................6 2.2. Operating voltage ................................6 2.3. Electrical supply connection for Cryodrive ........................6 2.4.
  • Page 4 8.1. Returns procedure ................................42 Oxford Cryosystems - Warranty Certificate ..............43 Registration ..................................... 43 Copyright 2012 Oxford Cryosystems Ltd...
  • Page 5 Figure 11 – Ballast valve in the closed position........................16 Figure 12 – Turbo station display unit ..........................17 Figure 13 – Venting the vacuum from the PheniX ......................19 Figure 14 – Front of a Controller ............................21 Figure 15 – Cryopad Settings page and Search dialog .....................32 Figure 16 –...

  • Page 6: Introduction

    The PheniX cryostat is designed for the cooling of flat plate powder samples down to temperatures of around 12 K. The PheniX is designed to fit to vertical powder diffractometers and be used in both the theta - theta and theta - 2 theta modes. This is made possible by a uniquely designed rotating seal between the integrated Gifford-McMahon Cryocooler and the sample stage.

  • Page 7: Items Required For Assembling Your Phenix

    Coldhead otherwise achieving extremely low temperatures at the sample becomes impossible. The PheniX can cool the sample stage to temperatures as low as 12 K and as high as 310 K with a stability of better than 0.1 K.

  • Page 8: Setting Up

    This pump unit will automatically run on the correct voltage. Oxford Cryosystems ships all Cryodrives set to 240 V and 50 Hz as this is how they are commissioned in the UK. It will be necessary to refer to Section 2.3 to set the Primary Tap Connections for the local voltage and frequency.

  • Page 9: Figure 2 - Transformer Showing Different Electrical Supply Connections

    • Use a small screwdriver to adjust the current-limit potentiometer to the recommended value. • Replace the lid of CryoController and the Cryodrive. • Make sure that the Cryodrive ON/OFF switch is in the OFF position and connect the Cryodrive to your electrical supply. Copyright 2012 Oxford Cryosystems Ltd...

  • Page 10: Figure 3 - Overload Relay Showing Stop And Reset Buttons

    16 A 16 A 16 A Cryodrive 3.0, 60 Hz supply 18 A 17 A 16 A Table 2 – Recommended protection switch current limit setting Figure 3 – Overload relay showing stop and reset buttons Copyright 2012 Oxford Cryosystems Ltd...

  • Page 11: Layout Of Cryodrive

    2.5. Helium gas hose connection WARNING If you are unsure on how to connect the helium gas hoses, please contact Oxford Cryosystems. Failure to connect the hoses properly might result in complete loss of helium pressure within the Cryodrive. The main layout is illustrated schematically on the diagram in Figure 1 and connections are generally labelled equivalently at each end.

  • Page 12: Figure 5 - Helium Gas Hoses

    (red arrow) to fully tighten the coupling. 10. When tightening the hoses both at the Cryodrive and the PheniX coldhead, ensure the fittings are tightened until a good resistance is felt. In the case of the Cryodrive fittings, the helium connections should be tightened so that the two faces of the male and female fittings meet.

  • Page 13: Figure 6 - Connection Of A Helium Hose To The Cryodrive Using Two Spanners

    16.5 bar (240 psi). If this pressure reads less than 15.5 bar (220 psi), contact Oxford Cryosystems. This check should be repeated, if possible, each time the unit is to be turned on. Under normal operating conditions it should be about 22 bar and will noticeably oscillate by around 0.5 bar.

  • Page 14: Figure 7 - Front Of Cryodrive Showing The Pressure Gauge

    Connect the PheniX Coldhead cable connector from the Cryodrive to the bayonet fitting on the Cryocooler Coldhead of the PheniX. Connect the serial cable from the Cryodrive to the ‘Cryodrive’ socket on the back of the PheniX Controller. Connect the PheniX Coldhead Cable from the ‘Coldhead’ socket on the back of the Controller to the multi-pin bayonet socket on the side of the PheniX cryostat body located next to the relief valve.

  • Page 15: Figure 8 - Cooling Water Requirements

    Figure 8 – Cooling water requirements Cooling water flow rate vs pressure drop (with outlet flow to open drain) Water flow rate (Litre per minute) Figure 9 – Cooling water flow rate vs pressure drop Copyright 2012 Oxford Cryosystems Ltd...

  • Page 16: Vacuum System

    NOTE A variety of manuals are supplied with the Pfeiffer Vacuum System for all its components. The information below outlines the simple steps needed to use this system with the PheniX. Further information is available in the manuals, if necessary.
  • Page 17 Cryo Vac Turbo Station and integrated Diaphragm Pump - this turbo system pumps the main body of the PheniX. Seal Vac Diaphragm Pump - this pump evacuates the rotating seal of the PheniX to ensure that when the seal moves, the main body vacuum is then unaffected.

  • Page 18: Figure 11 - Ballast Valve In The Closed Position

    To ensure a good vacuum, open both Gas Ballast Valves for an hour during initial pumping to ensure any residual water vapour and air in the lines and PheniX are removed. Figure 11 below illustrates how sleeve ‘43’ should be moved to position ‘Y’ to open the gas ballast valve. Be sure not to leave the valve open permanently.

  • Page 19: Figure 12 - Turbo Station Display Unit

    Turbo Station, see Figure 11. This will remove any residual water vapour and air in the vacuum lines and body of the PheniX. This is necessary if the vacuum reading begins to rise (or does not drop) during the early stages of pumping down. Open the Ballast Valve for an hour.

  • Page 20: Table 3 - Options On The Turbomolecular Pumping Station

    Table 3 Symbol Arrow Explanation No arrow Not accelerating Pump acceleration Accelerating (flashing) Heating Not in use for PheniX No arrow Not in standby mode Standby In standby mode Under remote control Not in use for PheniX Switch-point not No arrow...

  • Page 21: Releasing Vacuum Into The Phenix

    Turbo pump on the Cryo Vac Turbo Station. Once the PheniX Cooler has warmed up and been shut down it can simply be reprogrammed to start the system up again. IT IS NOT NECESSARY TO SWITCH THE SYSTEM OFF. Simply press START to re-initialise.

  • Page 22: Checklist To Start The Phenix Running

    The height of the sample stage can be adjusted by turning the red dial on the bottom of the dovetail of the PheniX. There is also a dial on the side to allow the PheniX to be moved horizontally, if necessary.

  • Page 23: Phenix 730 Series Controller

    ON indicates the higher speed. In addition, during a COOL phase the SPEED lamp will flash. This indicates a mode in which the PheniX Cooler fixes the Cryodrive speed at the higher value in order to minimise the cooling time.

  • Page 24: Display Modes

    START. NOTE It is not safe to release the PheniX Cooler’s vacuum or open the cryostat until the system has been warmed up. This can be achieved via a WARM phase, which is the approved method of shutting the system down.
  • Page 25 The system has been shut down due to a programmed END WARM The system has been shut down due to a programmed WARM (see Further Programming on the PheniX Controller, Section 4.2) POWER The power has been switched off at the mains...
  • Page 26 Description: Phase Table Mode The PheniX lists the phases in the current program, with the current phase at the top of the list. The current phase is indicated with a ‘>’. Use the IntelliKnob to scroll through the list. Press DISPLAY or PROGRAM to enter the Display Modes 5 & 6.
  • Page 27 Program Mode This mode allows the user to program the PheniX as described in Programming the PheniX, Section 4. New phases are added at the end of the list of phases. If the system is in a HOLD, press HOLD to begin the next phase.

  • Page 28: Programming The Phenix

    Using the quick start facility and the COOL function To cool as quickly as possible simply rotate the IntelliKnob to the appropriate temperature and press START. The PheniX will remember the last value requested here and store it for the next time the Quick Start facility is used.
  • Page 29 Change temperature at a controlled rate. When ramping down Add Phase: Ramp in temperature, if the selected rate is too fast for the PheniX to follow, the Controller will automatically enter the RAMP/WAIT mode (this will be indicated on the screen). The effect of this is...
  • Page 30 Controller will automatically enter a HOLD phase at the end of the program if one has not already been programmed. If the system is running and already in a HOLD phase, pressing the HOLD button will make the program continue to the next instruction in the Phase Table. Copyright 2012 Oxford Cryosystems Ltd...

  • Page 31: Phase Table

    The Cryodrive includes a variable-speed compressor. The speed at which the compressor is running is indicated by the speed meter on the Front Panel. In order to minimise wear, PheniX will automatically reduce the compressor speed to the minimum compatible with maintaining the current set temperature.

  • Page 32: Alarm Conditions

    4.7. Safety features during power failures The PheniX Controller is designed to protect itself and the sample during power interruptions. It is possible for the Controller to maintain cooling and not reset the Controller during electrical interruption indicated by the term ‘Brown-Out’ of between 0-2 seconds. If a ‘Brown-Out’ is detected, this is indicated on the screen.

  • Page 33: Phenix Shut Downs

    4.8. PheniX shut downs The 730 Series PheniX Controller has been designed to fully protect the PheniX Cooler under its normal mode of operation as outlined in this manual. The Controller will shut down the PheniX Cooler if: 1. The Sample Temp registers an error greater than ±25 K.

  • Page 34: Running The Phenix With Cryopad

    5 Running the PheniX with Cryopad Cryopad is a PC program which allows remote monitoring and control of any 700 series Oxford Cryosystems device. This includes the 700 series Cryostream / Plus, Cobra / Plus, PheniX and N- HeliX systems.

  • Page 35: Figure 16 - Cryopad Display Page

    Cryo Speed 5.2.3. The Command page The Command page allows commands to be sent to your PheniX exactly as if they were entered using the controller. Commands sent in this way will immediately overwrite the contents of the controller’s Phase table. Refer to section 4 above for details of the commands.

  • Page 36: Figure 17 - Cryopad Command Page

    For monitoring purposes a 60 s interval is suitable whereas for diagnosing problems an interval of 1 s provides the most information but will produce a larger log file. Check the Logging Active box to commence logging. Figure 18 – Cryopad Data Logging page Copyright 2012 Oxford Cryosystems Ltd...

  • Page 37: Phenix User Maintenance

    6 PheniX User Maintenance The PheniX has been designed to be as easy to use as possible and should run without the need for constant attention, once the user is accustomed to the system. However, some parts of the system will eventually require maintenance, with the following maximum service intervals:...

  • Page 38: Replacing The Cryodrive Adsorber

    Replacing the Cryodrive Adsorber When the Cryodrive has been operating for approximately 16000 hours, you must replace the Adsorber with a new one to avoid permanent damage to the PheniX Coldhead. Please contact Oxford Cryosystems for more information. The new Adsorber is supplied pressurised with helium, so you should not have to re-charge the Cryodrive with helium after you fit the new Adsorber.

  • Page 39: Topping Up The Cryodrive With Helium

    Topping up the Cryodrive with helium The PheniX system involves a closed helium gas circuit. The helium in this circuit will eventually leak out over time and will require topping up from a high pressure helium gas cylinder (99.9995%). Note: that this should only be performed when the system is off.

  • Page 40: Liquid And Gaseous Nitrogen Safety Sheet

    All users are requested to read this safety sheet before handling the PheniX. Oxford Cryosystems accept no responsibility for injury or damage caused by the mishandling of liquid or gaseous nitrogen.

  • Page 41: Precautions

    Where large spills of liquid nitrogen occur a fog forms in the vicinity of the spill caused by the condensation of water vapour in the surrounding air. The fog, in addition to severely reducing visibility, may contain oxygen concentrations appreciably lower than that of the air presenting a local asphyxiation hazard. Copyright 2012 Oxford Cryosystems Ltd...

  • Page 42: First Aid

    Thawing may take from 15-60 minutes and should be continued until the blue, pale colour of the skin turns to pink or red. Morphine, or some potent analgesic, is required to control the pain during thawing and should be administered under professional medical supervision. Copyright 2012 Oxford Cryosystems Ltd...
  • Page 43 Slow restoration of temperature is necessary and forms of locally applied heat should not be used. Summon medical attention. 7.5.3. Liquid nitrogen spillage If large spills of liquid nitrogen occur, large quantities of water should be used to increase the rate of liquid vaporisation. Copyright 2012 Oxford Cryosystems Ltd...

  • Page 44: Technical Support

    8 Technical Support To allow Oxford Cryosystems to offer fast and accurate technical support, please quote your PheniX Serial Number with all technical issues. It is worth keeping a record of this number in a convenient place: PheniX SERIAL NUMBER This PheniX serial number is _______ Before you return your equipment you must warn Oxford Cryosystems by contacting us.
  • Page 45 Oxford Cryosystems - Warranty Certificate This warranty is subject to the Oxford Cryosystems Ltd (OCL) Terms and Conditions of Sale. OCL warrants to the Buyer that the goods sold for use hereunder will be free from defects in material and workmanship under normal use and operation for 12 months from the date of shipment from OCL’s premises.

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