OXFORD CRYOSYSTEMS PheniX Guida per l'amministratore

OXFORD CRYOSYSTEMS

PheniX

Operation &

Instruction Guide

O X F O R D C R Y O S Y S T E M S P H E N I X

Operation & Instruction Guide v2.6

Oxford Cr os stems Ltd

3 Blenheim Office Park

Lower Road

Long Hanborough

Oxford OX29 8LN

United Kingdom

Phone +44 1993 883488 • Fax +44 1993 883988

Email Support@oxcr o.com

Table of Contents

1 Introduction ............................................................................................................... 4

1.1. How the PheniX works .................................................................................................................................................... 4

1.2. Items required for assembling our PheniX ................................................................................................................. 5

2 Setting Up .................................................................................................................. 6

2.1. Matching the PheniX Coldhead and 730 Series Controller ........................................................................................ 6

2.2. Operating voltage ............................................................................................................................................................... 6

2.3. Electrical suppl connection for Cr odrive ................................................................................................................... 6

2.4. La out of Cr odrive ........................................................................................................................................................... 9

2.5. Helium gas hose connection ............................................................................................................................................ 9

2.6. Vacuum S stem ................................................................................................................................................................ 14

2.7. Releasing vacuum into the PheniX ............................................................................................................................... 19

2.8. Checklist to start the PheniX running .......................................................................................................................... 20

2.9. Adjusting the height of the PheniX sample stage ...................................................................................................... 20

2.10. How to shut down the PheniX...................................................................................................................................... 20

PheniX 7 0 Series Controller .................................................................................. 21

3.1. PheniX controller front panel ........................................................................................................................................ 21

3.2. Displa modes .................................................................................................................................................................. 22

4 Programming the PheniX ........................................................................................ 26

4.1. Using the quick start facilit and the COOL function .............................................................................................. 26

4.2. Further programming of the PheniX Controller ........................................................................................................ 26

4.3. Phase table ......................................................................................................................................................................... 29

4.4. Cr odrive speed and the SPEED button .................................................................................................................... 29

4.5. HOLD and ‘Un-HOLD’ ................................................................................................................................................ 29

4.6. Alarm conditions .............................................................................................................................................................. 30

4.7. Safet features during power failures ............................................................................................................................ 30

4.8. PheniX shut downs .......................................................................................................................................................... 31

5 Running the PheniX with Cryopad .......................................................................... 2

5.1. Installing Cr opad ............................................................................................................................................................ 32

5.2. Using Cr opad to run the PheniX ................................................................................................................................ 32

6 PheniX User Maintenance ....................................................................................... 5

6.1. Coldhead swap-out .......................................................................................................................................................... 35

6.2. Servicing the Turbomolecular Vacuum Pumping Station ........................................................................................ 35

6.3. Replacing the Cr odrive Adsorber ................................................................................................................................ 36

6.4. Topping up the Cr odrive with helium ........................................................................................................................ 37

7 Liquid and gaseous nitrogen safety sheet .............................................................. 8

7.1. General ............................................................................................................................................................................... 38

7.2. Fire and explosion hazards ............................................................................................................................................. 38

7.3. Health hazards .................................................................................................................................................................. 38

7.4. Precautions ........................................................................................................................................................................ 39

7.5. First aid .............................................................................................................................................................................. 40

8 Technical Support ................................................................................................... 42

8.1. Returns procedure ............................................................................................................................................................ 42

Oxford Cryosystems - Warranty Certificate ................................................................. 4

Registration ..................................................................................................................................................................................... 43

FiguresFigure 1 – PheniX la out .................................................................................................................................. 4

Figure 2 – Transformer showing different electrical suppl connections ...................................................................... 7

Figure 3 – Overload rela showing stop and reset buttons .............................................................................................. 8

Figure 4 – Front and back of Cr odrive .............................................................................................................................. 9

Figure 5 – Helium gas hoses ................................................................................................................................................10

Figure 6 – Connection of a helium hose to the Cr odrive using two spanners ..........................................................11

Figure 7 – Front of Cr odrive showing the pressure gauge ...........................................................................................12

Figure 8 – Cooling water requirements ..............................................................................................................................13

Figure 9 – Cooling water flow rate vs pressure drop .......................................................................................................13

Figure 10 – PheniX Vacuum Pump Station ......................................................................................................................14

Figure 11 – Ballast valve in the closed position. ...............................................................................................................16

Figure 12 – Turbo station displa unit ...............................................................................................................................17

Figure 13 – Venting the vacuum from the PheniX ..........................................................................................................19

Figure 14 – Front of a Controller ........................................................................................................................................21

Figure 15 – Cr opad Settings page and Search dialog .....................................................................................................32

Figure 16 – Cr opad Displa page ......................................................................................................................................33

Figure 17 – Cr opad Command page .................................................................................................................................34

Figure 18 – Cr opad Data Logging page ...........................................................................................................................34

Tables

Table 1 – Wire connections to primar tap connections .................................................................................................. 8

Table 2 – Recommended protection switch current limit setting ................................................................................... 8

Table 3 – Options on the turbomolecular pumping station ...........................................................................................18

Table 4 - PheniX Service Intervals ......................................................................................................................................35

1Introduction

The PheniX cr ostat 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 b a uniquel designed rotating seal

between the integrated Gifford-McMahon Cr ocooler and the sample stage. This allows the sample

stage to move in the full 2-theta range of the detector without the high pressure hoses and cables

becoming tangled up or interfering with other services in the enclosure.

The compact design means the PheniX can be easil fitted to the goniometer from the front with a

specific adapter plate designed for each t pe of goniometer.

1.1. How the PheniX works

The gas flow circuit of the PheniX is shown in Figure 1 below.

Helium compressor

Turbomolecular

vacuum pump

Controller

Power

Cable

Coldhead cable

Power

Cooling water in

Cooling water out

PheniX

Coldhead

SEAL VAC

(NW10)

CRY VAC

(NW16)

High pressure

helium hose

Low pressure

helium hose

Vacuum hoses

Cable

Figure 1 – PheniX layout

The closed c cle cooler is mounted within the bod of the PheniX and operates using

compressed helium gas provided b the Cr odrive compressor, which is water-cooled. It is

important to note that there is no helium gas consumption in this s stem and the helium gas

circuit in the Cr odrive/Coldhead combination is sealed. The sample stage is cooled b the

conduction of heat between the sample stage and the cold stages of the Coldhead.

A Vacuum S stem is used to continuousl pump the vacuum space around the PheniX internals

and also the Rotating Seal to minimise unwanted heat leaks into the s stem. It is important that a

good vacuum (<10-4 mbar) is maintained with the Coldhead otherwise achieving extremel 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 stabilit of better than 0.1 K.

1.2. Items required for assembling your PheniX

The component parts of the s stem are:

The PheniX Coldhead

730 Series Controller

Gre Cr odrive cable

Black Coldhead cable

Cr odrive compressor

2x Stainless steel flexible transfer lines

Pfeiffer Turbomolecular Vacuum Pump

CD with Operating Manuals and Cr opad software

PheniX Mounting Plate for Goniometer

2Setting Up

2.1. Matching the PheniX Coldhead and 7 0 Series Controller

The PheniX Coldhead and 730 Series Controller are supplied as a matched pair. The individual

characteristics of the Coldhead sensors are programmed into the Controller. Please contact our

supplier if ou believe ou ma have unmatched units.

2.2. Operating voltage

It is essential that the PheniX is configured to operate on the local mains electrical suppl .

Item O erating voltage requirements

730 Series Controller The voltage selector switch on the rear panel must be set to the

correct position:

200-240 Volts AC, 50 Hz, 3 Amps

100-120 Volts AC, 50-60 Hz, 6 Amps.

Make sure an ‘Anti-Surge’ (T) t pe fuse of the correct rating is fitted.

Cr odrive User configurable Suppl voltage:

200, 220 or 240 V at 50 Hz or

200, 208 or 220 V at 60 Hz

Suppl voltage tolerance: +10 %

Maximum suppl fuse rating: 30 A

Recommended Cr oController fuse t pe: Slow blow

Maximum Cr oController fuse rating: 5 A

Over voltage categor (IEC664): 2

Pfeiffer Turbomolecular

Vacuum Pump 90-132 V 50/60 Hz and 185-265 V 50/60 Hz.

This pump unit will automaticall run on the correct voltage.

Oxford Cryosystems shi s 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 Ta

Connections for the local voltage and frequency.

2. . Electrical supply connection for Cryodrive

We recommend that ou use a suitabl fused isolator at our electrical suppl outlet. Locate the

isolator switch close to the electrical outlet. It is also recommended that back-up fuses are installed at

the electrical suppl outlet. You must configure the Cr odrive to suit our electrical suppl . The

Cr odrive is despatched configured for use with 240 V and 50 Hz electrical suppl .

Figure 2 – Transformer showing different electrical su ly connections

Use the procedure below to change this configuration.

•Look at Table 1: find our electrical suppl in the left-hand column, look along this row to

find the connections ou must make for the wire 30 (W30) and wire 31 (W31).

•Remove the lid of the Cr odrive and locate the transformer.

•With reference to Figure 2, change the position of wire 30 (W30) and wire 31 (W31) so that

the are in the correct position for our electrical suppl . Ensure the connections are full

tightened. Do not move the wires attached to the red 0 V and 230 V connectors, as

these rovide ower to the secondary ste er motor transformer and are not art of

the rocedure.

•Locate the protection switch on the current-limit potentiometer which is situated in the

Cr oController, refer to Figure 3. The switch can be accessed b removing the lid of the

Cr oController unit.

•Look at Table 2: find our Cr odrive t pe and electrical suppl frequenc in the left-hand

column, look along this row to find the recommended limit for the protection switch current.

•Use a small screwdriver to adjust the current-limit potentiometer to the recommended value.

•Replace the lid of Cr oController and the Cr odrive.

•Make sure that the Cr odrive ON/OFF switch is in the OFF position and connect the

Cr odrive to our electrical suppl .

Electrical Su ly

Primary Ta Connection

N 200 V 208 V 220 V 230 V 240 V

50 Hz, 200 V W32 W31 W30 - - -

50 Hz, 220 V W32 - W30 W31 - -

50 Hz, 240 V W32 - W30 - - W31

60 Hz, 200 V W32 W31 - - W30 -

60 Hz, 208 V W32 - W31 - W30 -

60 Hz, 220 V W32 - - W31 W30 -

60 Hz, 240 V W32 W30 W31

Table 1 – Wire connections to rimary ta connections

Cryodrive model Electrical su ly voltage

200 V 208 V 220 V 240 V

Cr odrive 1.5, 50 Hz suppl 11 A - 10 A 10 A

Cr odrive 1.5, 60 Hz suppl 11 A 11 A 11 A -

Cr odrive 3.0, 50 Hz suppl 16 A - 16 A 16 A

Cr odrive 3.0, 60 Hz suppl 18 A 17 A 16 A -

Table 2 – Recommended rotection switch current limit setting

Figure 3 – Overload relay showing sto and reset buttons

Indice

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