Anton Paar TTK 600 User manual

Measure
what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)
Reference Guide
TTK 600
Low Temperature Chamber with
CCU 100 Control Unit

Reference Guide
TTK 600
Low Temperature Chamber with
CCU 100 Control Unit
Disclaimer
This document may contain errors and omissions. If you discover any such errors or if you would like to see
more information in this document, please contact us at our address below. Anton Paar assumes no liability
for any errors or omissions in this document.
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Further information
Published and printed by Anton Paar GmbH, Austria
Copyright © 2018 Anton Paar GmbH, Graz, Austria
Address of the instrument producer: Anton Paar GmbH
Anton-Paar-Str. 20
A-8054 Graz / Austria – Europe
Tel: [phone]
Fax: [phone]
E-Mail: [email protected]
Web: www.anton-paar.com
Date: October 2018
Document number: D52IB001EN-G

Contents
4D52IB001EN-G
Contents
1 Safety Instructions.................................................................................................................................. 7
1.1 General Safety Instructions............................................................................................................... 7
1.2 Conventions for safety messages..................................................................................................... 8
1.3 Safety Signs on the Instrument......................................................................................................... 9
2 TTK 600 - An Overview......................................................................................................................... 10
2.1 Intended Use of the Instrument...................................................................................................... 10
2.2 Operating Principle ......................................................................................................................... 11
2.3 TTK 600 Sample Chamber ............................................................................................................. 12
2.3.1 Chamber Main Parts............................................................................................................... 12
2.3.2 Chamber Housing with Connectors ........................................................................................ 12
2.3.3 Chamber Lid ........................................................................................................................... 13
2.3.4 Internal Parts .......................................................................................................................... 13
2.3.5 Sample Holders ...................................................................................................................... 14
2.3.5.1 Standard Sample Holder ................................................................................................ 14
2.3.5.2 Standard Sample Holder Heating Environment.............................................................. 14
2.3.5.3 Capillary Sample Holder ................................................................................................. 14
2.3.5.4 Transmission Sample Holder.......................................................................................... 15
2.3.5.5 Antechamber for TTK 600 .............................................................................................. 15
2.3.5.6 Battery Sample Holder....................................................................................................15
2.4 Sample Cooling............................................................................................................................... 16
2.4.1 Liquid Nitrogen Cooling Equipment ........................................................................................ 16
2.4.2 Compressed-Air Cooling Equipment ...................................................................................... 17
2.5 CCU 100 Combined Control Unit.................................................................................................... 18
2.5.1 CCU 100 Front Panel ............................................................................................................. 18
2.5.2 CCU 100 Rear Panel .............................................................................................................. 18
2.5.3 Control of the Sample Cooling................................................................................................ 19
2.5.4 Overheat Protection................................................................................................................ 19
2.6 Water Flow Controller ..................................................................................................................... 19
3 Checking the Supplied Parts ............................................................................................................... 20
4 Installation............................................................................................................................................. 21
4.1 Installation Overview....................................................................................................................... 21
4.2 Installation Requirements ............................................................................................................... 22
4.2.1 X-Ray Diffractometer Requirements....................................................................................... 22
4.2.2 Electrical Requirements.......................................................................................................... 23
4.2.3 Cooling Water Requirements.................................................................................................. 23
4.2.4 Requirements for Liquid Nitrogen Cooling.............................................................................. 23
4.2.5 Requirements for Compressed-air Cooling ............................................................................ 23
4.2.6 Vacuum Equipment Requirements (optional) ......................................................................... 23
4.3 Mounting the Adapter on the Sample Chamber.............................................................................. 24
4.4 Mounting the Chamber on the Goniometer..................................................................................... 25
4.5 Installing CCU 100 .......................................................................................................................... 25
4.6 Connecting CCU 100 with a Computer........................................................................................... 25
4.7 Installing the Cooling Water Circuit................................................................................................. 26
4.8 Installing the Liquid Nitrogen Equipment ........................................................................................ 26
4.9 Installing the Air-Cooling Equipment............................................................................................... 27
4.10 Cooling Mode Switching Valve (optional) .....................................................................................29
4.11 Mounting the Gas/Vacuum Connector.......................................................................................... 29
4.11.1 Installing the Gas Supply (optional) ......................................................................................29
4.11.2 Installing the Vacuum Equipment (optional) ......................................................................... 30
4.11.3 Installing the Gas/Vacuum system for using the Antechamber ............................................ 31
4.12 Convection Heater ........................................................................................................................ 31
4.13 Mounting the Electrode Connector and the Connector Box.......................................................... 32
5 Putting TTK 600 into Operation........................................................................................................... 34

Contents
D52IB001EN-G 5
5.1 Alignment of the Standard Sample Holder......................................................................................34
5.1.1 Height Alignment with Rigid Adapter ...................................................................................... 34
5.1.2 Height Alignment with Motorized Alignment Stage................................................................. 35
5.1.3 Alignment of the Chamber Rotation........................................................................................ 35
5.2 Alignment of the Standard Sample Holder......................................................................................35
5.3 Preparing the Cooling Equipment ................................................................................................... 36
5.3.1 Preparing the Liquid-Nitrogen Cooling.................................................................................... 36
5.3.2 Preparing the Compressed-Air Cooling .................................................................................. 36
5.4 Checking the Instrument Condition................................................................................................. 36
5.5 Turning on the Instrument............................................................................................................... 37
6 Operating CCU 100 ............................................................................................................................... 38
6.1 Front Panel of the Instrument ......................................................................................................... 38
6.2 Keypad............................................................................................................................................ 38
6.2.1 Status LEDs............................................................................................................................ 39
6.3 Display ............................................................................................................................................ 39
6.3.1 Navigation Diagram of CCU 100 ............................................................................................ 40
6.4 Turning the Heater On and Off ....................................................................................................... 41
6.5 Controlling the Cooling Device........................................................................................................ 41
6.5.1 Controlling the Liquid Nitrogen Cooling .................................................................................. 41
6.5.2 Controlling the Compressed-Air Cooling ................................................................................ 42
6.6 Manual Control of CCU 100............................................................................................................ 42
6.7 Remote Control of CCU 100 ........................................................................................................... 42
7 Operating the LN2 Cooling Equipment............................................................................................... 43
7.1 LN2 Consumption and Operating Time .......................................................................................... 43
7.2 Typical Cooling Curves ................................................................................................................... 43
8 Performing a Measurement.................................................................................................................. 44
8.1 Adjusting the Knife Edge................................................................................................................. 44
8.2 Preparing the Sample ..................................................................................................................... 44
8.2.1 Additional Information for the Standard Sample Holder ......................................................... 44
8.2.2 Additional Information for the Transmission Sample Holder................................................... 45
8.2.3 Samples for the Capillary Sample Holder............................................................................... 45
8.2.4 Taking out the Sample Holder ................................................................................................ 46
8.2.4.1 Standard Sample Holder ................................................................................................ 46
8.2.4.2 Transmission Sample Holder.......................................................................................... 46
8.2.4.3 Battery Sample Holder....................................................................................................47
8.2.5 Applying the Sample............................................................................................................... 48
8.2.5.1 Powder Samples for the Standard Sample Holder ......................................................... 48
8.2.5.2 Bulk Samples for the Standard Sample Holder .............................................................. 48
8.2.5.3 Powders and Pastes for the Transmission Sample Holder ............................................ 48
8.2.5.4 Foils for the Transmission Sample Holder...................................................................... 50
8.2.5.5 Coin Cells for the Battery Sample Holder ....................................................................... 50
8.3 Guideline for the correct choice of conditions and foil materials..................................................... 51
8.3.1 Temperature Range................................................................................................................ 51
8.3.2 Temperature accuracy and influence of convection heater .................................................... 51
8.3.3 Background of the foil materials ............................................................................................. 52
8.3.4 Foil Materials for the Battery Sample Holders ........................................................................ 52
8.4 Mounting the Sample Holder .......................................................................................................... 53
8.4.1 Mounting the Standard Sample Holder................................................................................... 53
8.4.2 Mounting the Standard Sample Holder Heating Environment ................................................ 53
8.4.3 Mounting the Capillary Sample Holder ................................................................................... 54
8.4.4 Mounting the Transmission Sample Holder............................................................................ 55
8.4.5 Mounting and use of the Antechamber for TTK 600............................................................... 56
8.4.6 Mounting and Use of the Battery Sample Holders.................................................................. 57
8.5 Creating a Gas/Vacuum Environment ............................................................................................58
8.5.1 Operation with Air ................................................................................................................... 58
8.5.2 Operation under Vacuum........................................................................................................ 58
8.5.3 Operation with Gases Other than Air...................................................................................... 59

Contents
6D52IB001EN-G
8.6 Heating and Cooling the Sample .................................................................................................... 60
8.7 Carrying out the Measurement ....................................................................................................... 60
8.8 Temperature Control Information.................................................................................................... 61
8.8.1 Sample Temperature Accuracy .............................................................................................. 61
8.8.2 Effective Heating and Cooling Rate........................................................................................ 61
8.8.2.1 Standard Sample Holder ................................................................................................ 61
9 Putting TTK 600 out of Operation........................................................................................................ 62
10 Troubleshooting.................................................................................................................................. 63
10.1 Error Messages............................................................................................................................. 63
10.2 General Messages on Display ...................................................................................................... 63
10.3 Error Analysis................................................................................................................................ 63
10.4 Technical Support ......................................................................................................................... 66
11 Maintenance........................................................................................................................................ 67
11.1 Routine Maintenance .................................................................................................................... 67
11.2 Check the Functioning of the Flow Controller ............................................................................... 67
11.3 Exchanging of Parts...................................................................................................................... 67
11.3.1 Switching off the Instrument ................................................................................................. 67
11.3.2 Exchanging the Graphite Foil ............................................................................................... 67
11.3.3 Replacing the Window Foil ................................................................................................... 69
11.3.4 Replacing the O-rings ........................................................................................................... 69
11.4 Checking and Replacing Mains Fuses..........................................................................................70
Appendix A: Technical Data ................................................................................................................... 71
Appendix B: Sample Chamber Dimensions.......................................................................................... 74
Appendix C: Declaration of Conformity................................................................................................. 75
Appendix D: Spare Parts and Accessories ...........................................................................................76
Appendix E: Safety Data Sheet for Liquid Nitrogen ............................................................................. 78
Appendix F: Warranty.............................................................................................................................. 85

1 Safety Instructions
D52IB001EN-G 7
1 Safety Instructions
• Read the documentation before using TTK 600.
• Follow all hints and instructions contained in the
documentation to ensure the correct use and
safe functioning of TTK 600.
• The documentation is a part of the product.
Keep this document for the complete working
life of the product and make sure it is easily
accessible to all people involved with the prod-
uct. If you receive any additions or revisions to
the documentation from Anton Paar GmbH,
these must be treated as part of the documenta-
tion.
1.1 General Safety Instructions
Liability
• This documentation does not claim to address
all safety issues associated with the use of the
instrument and samples. It is your responsibility
to establish health and safety practices and
determine the applicability of regulatory limita-
tions.
• Anton Paar GmbH only warrants the proper
functioning of TTK 600 if no adjustments have
been made to the mechanics, electronics, and
firmware.
• Only use TTK 600 for the purpose described in
the documentation. Anton Paar GmbH is not lia-
ble for damages caused by incorrect use of
TTK 600.
Installation and use
• TTK 600 is not an explosion-proof instrument
and therefore must not be operated in areas
with risk of explosion.
• The installation procedure should only be car-
ried out by authorized personnel who are famil-
iar with the installation instructions.
• Do not use any accessories or spare parts other
than those supplied or approved by Anton Paar
GmbH (see chapter 3).
• Make sure all operators are trained to use the
instrument safely and correctly before starting
any applicable operations.
• In case of damage or malfunction, do not con-
tinue operating TTK 600. Do not operate the
instrument under conditions which could result
in damage to goods and/or injuries and loss of
life.
• Check TTK 600 for chemical resistance to the
samples and cleaning agents.
Maintenance and service
• The results delivered by TTK 600 not only
depend on the correct functioning of the instru-
ment, but also on various other factors. We
therefore recommend you have the results
checked (e.g. plausibility tested) by skilled per-
sonnel before consequential actions are taken
based on the results.
• Service and repair procedures may only be car-
ried out by authorized personnel or by Anton
Paar GmbH.
Disposal
• Concerning the disposal of TTK 600, observe
the legal requirements in your country.
Returns
• For repairs send the cleaned TTK 600 to your
Anton Paar representative. Only return the
instrument together with the filled out RMA
(Return Material Authorization) and the form
"Safety Declaration for Instrument Repairs".
Please download the Safety Declaration form
from our website www.anton-paar.com.
• Do not return instruments which are contami-
nated by radioactive materials, infectious agents
or other harmful substances that cause health
hazards.
Precautions for highly inflammable samples
and cleaning agents
• Observe and adhere to your national safety reg-
ulations for handling the measured samples
(e.g. use of safety goggles, gloves, respiratory
protection etc.).
• Only store the minimum required amount of
sample, cleaning agents and other inflammable
materials near the TTK 600.
• Do not spill sample/cleaning agents or leave
their containers uncovered. Immediately remove
spilled sample/cleaning agents.
• Make sure that the setup location is sufficiently
ventilated. The environment of TTK 600 must be

1 Safety Instructions
8D52IB001EN-G
kept free of inflammable gases and vapors.
• Connect TTK 600 to the mains via a safety
switch located at a safe distance from the instru-
ment. In an emergency, turn off the power using
this switch instead of the power switch on
TTK 600.
• Supply a fire extinguisher.
• Ensure the sufficient supervision of TTK 600
during operation.
Work with liquid nitrogen
• For detailed safety information on working with
liquid nitrogen, please refer to appendix E.
1.2 Conventions for safety messages
The following conventions for safety messages are
used in this instruction manual:
TIP: Tip gives extra information about the situation
at hand.
DANGER
Description of risk.
Danger indicates a hazardous situation which, if
not avoided, will result in death or serious injury.
WARNING
Description of risk.
Warning indicates a hazardous situation which, if
not avoided, could result in death or serious
injury.
CAUTION
Description of risk.
Caution indicates a hazardous situation which, if
not avoided, could result in minor or moderate
injury.
NOTICE
Description of risk.
Notice indicates a situation which, if not avoided,
could result in damage to property.
CAUTION
Hot surface
This symbol calls attention to the fact that the
respective surface can get very hot. Do not
touch this surface without adequate protective
measures.
CAUTION
High voltage
This symbol calls attention to the risk of high
voltage. Do not proceed until the indicated con-
ditions for averting this threat are fully under-
stood and met.
CAUTION
Cold surface
This symbol calls attention to the fact that the
respective surface can get very cold. Do not
touch this surface without adequate protective
measures.
WARNING
Electrostatic sensitive device
Warning indicates a situation which, if not
avoided, could result in damage to property.
Wear protective gloves
Wear protective gloves when handling
the TTK 600.
Wear safety goggles
Wear safety goggles when handling
the TTK 600.

1 Safety Instructions
D52IB001EN-G 9
1.3 Safety Signs on the Instrument
1 CAUTION - Hot surface
Fig. 1: Position of warning signs on the instrument
1CAUTION
2 CAUTION - Cold surface
Fig. 2: Position of warning signs on the safety box
CAUTION
Hot surface
This symbol calls attention to the fact that the
respective surface can get very hot. Do not
touch this surface without adequate protective
measures.
1
1
1
CAUTION
Cold surface
This symbol calls attention to the fact that the
respective surface can get very cold. Do not
touch this surface without adequate protective
measures.
Wear protective gloves
Wear protective gloves when handling
the TTK 600.
Wear safety goggles
Wear safety goggles when handling
the TTK 600.
NOTICE
Take care that the warning symbols remain
clearly legible.
1
2

2 TTK 600 - An Overview
10 D52IB001EN-G
2 TTK 600 - An Overview
The TTK 600 Low-Temperature Chamber is an attachment for 2-circle X-ray diffractometers with vertical
goniometer to cool and heat samples for in-situ X-ray diffraction.
Fig. 3: Main Components of the instrument
1 Combined Control Unit CCU 100 to control the sam-
ple temperature
2 Sample chamber (mounted on the stage mount)
2.1 Intended Use of the Instrument
The TTK 600 Low-Temperature Chamber has been
designed for use on powder X-ray diffractometers
with a vertical goniometer. The sample chamber is
mounted on the goniometer instead of the standard
(ambient) sample holder in order to heat or cool the
sample to a defined temperature while scanning the
sample with X-rays.
Different types of sample holders are available that
allow to perform X-ray scans either in reflection ge-
ometry, transmission geometry using capillaries or
transmission geometry for foils, pastes and also
powders. Two cooling options are available for the
instrument. With the liquid nitrogen cooling equip-
ment, the temperature range is -190 °C to 600 °C.
With the compressed-air cooling equipment the
temperature range is -20 °C to 600 °C. The sample
can be cooled/heated in vacuum or various gas at-
mospheres.
The sample temperature is controlled by a control
unit (CCU 100). This control unit is installed in spe-
cial compartments in the diffractometer or in an ex-
ternal rack beside the diffractometer.
TTK 600 should be used for powder samples (all
three types of sample holders) or foils and pastes
(transmission sample holder). The following sample
materials must not be investigated with TTK 600:
• radioactive samples
• samples that are self-igniting in air or when
exposed to humid gas.
If TTK 600 is operated under dynamic gas condi-
tions, gas flows through the chamber and sample
material can be released to the environment. This
must be taken into account when measuring sam-
ples that present a health hazard.
1
2
CAUTION
Risk of injury
Observe that in case of an unlikely malfunction
the highest possible temperature in the instru-
ment can be up to 900 °C. Do not use samples
that are self-igniting or form poisonous gases at
that temperature.