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.
Changes, copyright, trademarks etc.
This document and its contents may be changed or amended by Anton Paar at any time without prior notice.
All rights reserved (including translation). This document, or any part of it, may not be reproduced, changed,
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process) without prior written permission by Anton Paar GmbH.
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as such. They are the property of their respective owner.
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.

2 TTK 600 - An Overview
D52IB001EN-G 11
TTK 600 can be operated under vacuum or stan-
dard gases like nitrogen or air. Certain other gases
can be used as well, but the following types of gases
are not permitted:
• poisonous gases
• explosive gases
• corrosive gases
• gases which can create explosive gas mixtures
with air.
TTK 600 must not be pressurized to more than 2 bar
rel. under all operating conditions.
2.2 Operating Principle
TTK 600 uses so called direct heating/cooling to
control the temperature of the samples. Heating is
done by a resistive heater underneath the sample
holder. Cooling is provided by either compressed air
or liquid nitrogen which cools down a cryostat which
is located directly under the heater of the instru-
ment. Measurement of the temperature is done by a
thermocouple inside the heater and depending on
the actual setup a second temperature is measured
with a Pt100 which is directly integrated in the sam-
ple holder to ensure accurate temperature mea-
surement.
The following table gives an overview of the acces-
sible temperature range in dependence of the used
atmosphere and the used type of sample holder. 1 This is a nominal limit. The true limit is the dew point
temperature of the (ambient) air.
2 Observe the pressure dew point requirements for the
compressed-air given in appendix A in order to avoid
icing of the cryostat.
3 Recommended heating rate/slope for the battery
sample holder transmission: < 20 °C for the tem-
perature range < CL (cooling limit; refer to chapter
6.3.1).
The standard sample holder of the instrument is
used in reflection geometry, whereas the transmis-
sion sample holder and the capillary sample holder
are made for transmission geometry.
Standard Sample Holder
Cooling
Equipment
Ambi-
ent Air
Dry Air/
N2/He
Vacuum
Liquid Nitro-
gen Cooling
+25 °C1
+450 °C
-150 °C
+450 °C
-190 °C
+600 °C
Compressed
Air Cooling
+25 °C1
+450 °C
-10 °C2
+450 °C
-20 °C2
+600 °C
Transmission Sample Holder
Cooling
Equipment
Ambi-
ent Air
N2 Vacuum
Liquid Nitro-
gen Cooling
+25 °C1
+450 °C
-175 °C
+600 °C
-190 °C
+600 °C
Compressed
Air Cooling
+25 °C1
+450 °C
-10 °C2
+600 °C
-20 °C2
+600 °C
Capillary Sample Holder
Cooling Equip-
ment
Ambient Air N2
Liquid Nitrogen
Cooling
+25 °C1
+450 °C
-175 °C
+600 °C
Compressed Air
Cooling
+25 °C1
+450 °C
-10 °C2
+600 °C
Battery Sample Holder
Cooling
Equipment
Ambi-
ent Air
N2 Vacuum
Liquid Nitro-
gen Cooling3
+25 °C1
+130 °C
-150 °C
+130 °C
-180 °C
+130 °C
Compressed
Air Cooling
+25 °C1
+130 °C
-10 °C2
+130 °C
-15 °C2
+130 °C

2 TTK 600 - An Overview
12 D52IB001EN-G
2.3 TTK 600 Sample Chamber
The following chapters describe the chamber and its
parts in detail.
2.3.1 Chamber Main Parts
Fig. 4: Main components of the sample chamber
1 Chamber housing
2 X-ray beam window
3Lid
4 Adapter for z-alignment stage (mechanical interface)
A suitable mechanical interface is necessary to
mount TTK 600 on the goniometer. Two types of in-
terfaces are available:
• Rigid adapters with a simple z-alignment device
which requires manual alignment of the sample
stage.
• Motorized z-alignment stages for PC-controlled
alignment of the sample stage.
If a motorized z-alignment stage is used, the align-
ment stage is mounted on the base-plate of
TTK 600 and the interface to the goniometer is
mounted on the z-alignment stage.
The sample position can change due to thermal
movement of the sample holder or sample shrink-
ing/expansion. If correction of the sample surface
displacement during a series of X-ray scans is re-
quired, we recommend to use a motorized z-align-
ment stage. For TTK 600 the sample holder
displacement during heating and cooling is
approx. ±0.1 mm.
2.3.2 Chamber Housing with Connectors
Fig. 5: Chamber housing with connectors
1 Blind plug (for optional additional connections)
2 Cooling water hose inlet
3 Cooling water hose outlet
4 Connection cable to CCU 100
5 Connector for sample cooling (liquid nitrogen or com-
pressed air)
6 Overpressure relieve valve (3 bar)
7 Gas connectors
The TTK 600 chamber housing is made of alumi-
num and is water-cooled. The housing is slotted
along the radiation path (entrance and exit of X-
rays). The X-ray window is covered with a Kapton
foil, which is pressed onto an O-ring by two clamp-
ing pieces.
There is one cable to connect TTK 600 to CCU 100.
This cable is responsible for providing the heating
current to the heater and for transferring the tem-
perature read-out and the signals from the sensors
within the instrument.
At the bottom of the housing is the connector for the
sample cooling device, either the liquid nitrogen
cooling equipment or the compressed-air cooling
unit.
1
2
3
4
1
2
3
4
56
7

2 TTK 600 - An Overview
D52IB001EN-G 13
2.3.3 Chamber Lid
T
Fig. 6: Chamber lid
1 Vacuum flange
2 Bayonet fitting
3 Fixing screws
4 Viewing window
The lid of the TTK 600 is fixed to the housing by two
bayonet fittings as well as two fixing screws and is
sealed with an O-ring.
TIP: There is a special lid for the use of the Capillary
Sample Holder. For further information refer to
chapter 2.3.5.3 and the Instruction manual for the
Capillary Sample Holder.
2.3.4 Internal Parts
Fig. 7: Main parts inside the sample chamber
1 O-ring seal
2 Knife edge
3 Guiding rods for beam stop
4 Beam Stop (only for transmission configuration)
5 Sample holder fixing ring
6 Graphite foil
7Cryostat
8 Pt100 plug connector
For detailed information on the materials used in the
TTK 600, please refer to appendix A.
The temperature of the sample holder is controlled
with a combination of resistance heater and cryo-
stat. The cryostat can either be cooled with liquid ni-
trogen or compressed air (refer to chapter 2.4).
Temperature measurement is performed with a
Pt100 temperature sensor which is embedded in the
sample holder. For sample exchange the sensor
can be disconnected with a plug.
1
2
3
42
3
1
2
3
4
5
6
8
7

2 TTK 600 - An Overview
14 D52IB001EN-G
2.3.5 Sample Holders
There are four sample holders for the TTK 600. De-
tailed information is contained in the chapters be-
low.
2.3.5.1 Standard Sample Holder
Fig. 8: Standard Sample Holder
1 Sample holder
2 Fixing screw for sample holder
3 Sheath resistance Pt100
4 Pt100 connector
The standard sample holder of TTK 600 is opti-
mized for measurements in reflection geometry.
The sample holder is made of nickel. To provide
good heat transfer from the heater to the sample
holder, a graphite foil is placed in between. The
sample holder is fixed onto the heating/cooling
block with a screw (see Fig. 8-2).
2.3.5.2 Standard Sample Holder Heating Environ-
ment
Optionally, to minimize the deviation between the
real sample surface temperature and the displayed
temperature a standard sample holder environment
can be used which inhibits the loss of heat to the
surrounding atmosphere inside the TTK 600. The
sample holder environment can be equipped with a
graphite, nickel or Kapton foil (others on request).
To mount the sample holder environment see chap-
ter 8.4.2 Mounting the Standard Sample Holder
Heating Environment.
Fig. 9: Standard sample holder heating environment
1 Standard sample holder heating environment
2 Sample holder
3 Heater insulation
2.3.5.3 Capillary Sample Holder
Fig. 10: Capillary Sample Holder
1 Window foil of the capillary sample holder
2 Fixing screw for sample holder
3 Sheath resistance Pt100
4 Pt100 connector
5 Hose for convection heating of the capillary
The Capillary Sample Holder is used for transparent
samples in transmission geometry. The tempera-
ture distribution around the capillary is improved by
the use of an additional convection heater. For fur-
ther information on the Capillary Sample Holder, re-
fer to the instruction manual
Capillary Sample Holder for TTK 600.
1
2
4
3
12
3
12
3
54

2 TTK 600 - An Overview
D52IB001EN-G 15
2.3.5.4 Transmission Sample Holder
Fig. 11: Transmission Sample Holder
1 Transmission sample holder heating environment
2 Fixing screw for sample holder
3 Sheath resistance Pt100
4 Pt100 connector
5 Hose for convection heating of the sample
The Transmission Sample Holder is used for pow-
ders, foils and pastes in transmission geometry. The
temperature distribution around the sample is im-
proved by the use of an additional convection heater
(necessary for Kapton foil only).
2.3.5.5 Antechamber for TTK 600
The Antechamber for TTK 600 is used for the trans-
fer of air-sensitive samples to TTK 600.
Fig. 12: Antechamber for TTK 600
1 Antechamber TTK 600
2 Mount of Antechamber
This can be done by loading the sample to the ante-
chamber within a glove box. Detailed information
about the necessary steps can be found in
chapter 8.4.5.
The sample holder for the antechamber is different
compared to the standard sample holder. The most
important difference is that this type of sample hold-
er has no integrated Pt100 temperature sensor. If
the antechamber for TTK 600 is used, the tempera-
ture of the thermocouple inside the heater is used to
measure the temperature.
For the recognition of this type of sample holder, the
Pt100 blind plug, which is delivered together with
the antechamber has to be connected to the Pt100
plug connector.
2.3.5.6 Battery Sample Holder
The battery sample holder is used to measure coin
cell battery samples in either reflection or transmis-
sion geometry. An anode and a cathode are located
on either side of the sample so that the behavior of
the coin cell can be monitored in-situ and in-operan-
do.
Reflection:
Fig. 13: Battery Sample Holder (Reflection)
1 Fixing screw for sample holder
2 Pt100 connector
3 Lid of battery sample holder
4 Sheath resistance Pt100
5 Electrode cable
1
2
3
4
5
1
2
3
4
5
2
1

2 TTK 600 - An Overview
16 D52IB001EN-G
Transmission:
Fig. 14: Battery Sample Holder (Transmission)
1 Fixing screw for sample holder
2 Pt100 connector
3 Lid of battery sample holder
4 Sheath resistance Pt100
5 Electrode cable
2.4 Sample Cooling
TTK 600 Low-Temperature Chamber can be oper-
ated with two types of sample cooling equipment,
depending on the desired temperature range:
• liquid nitrogen cooling
temperature range -190 °C to +600 °C
• compressed-air cooling
temperature range -20 °C to +600 °C
Both types of cooling equipment are connected to
TTK 600 via the connector for sample cooling (see
chapter 2.3.2) and controlled by CCU 100.
CCU 100 automatically turns off the cooling when it
is not needed to save liquid nitrogen/compressed-
air.
2.4.1 Liquid Nitrogen Cooling Equipment
The LN2 cooling equipment consists of the following
components:
• Low Temperature Equipment for Venturi Nozzle
(cat. no. 164578)
• Liquid Nitrogen Container, Dewar 60 L
(cat.no.166462)
or
• Liquid Nitrogen Container, Dewar 100 L
(cat.no.166463)
Other dewar vessels can be used, provided they
have the same specification and opening dimension
as the ones offered by Anton Paar GmbH (see
chapter 4.2.4 for further information).
Fig. 15: Low Temperature Equipment mounted on
TTK 600
1 LN2 connector
2 LN2 supply hose
3 Exhaust hose for evaporated nitrogen
Fig. 16: LN2 Dewar
1 LN2 Dewar vessel
2 LN2 inlet connection
3
4
1
5
2
1
23
2
1

2 TTK 600 - An Overview
D52IB001EN-G 17
Fig. 17: "Venturi-Nozzle - Safety Box"
1 "Venturi-Nozzle - Safety Box"
2 N2 inlet hose
3 N2/Air exhaust hose
4 Compressed-air connector
5 Overpressure-relieve valve
On top of the safety box is a Venturi nozzle which
creates a vacuum if the compressed air is switched
on. This vacuum ensures that liquid nitrogen is
sucked from the Dewar vessel through TTK 600 and
provides in this regard the cooling power that is
needed for low-temperature experiments. The
evaporated nitrogen is removed through the ex-
haust hose of the Low-Temperature Equipment and
directed into the Venturi-Nozzle - Safety Box. This
box is made as additional safety device for the cool-
ing system.
Liquid nitrogen that may escape from the gas ex-
haust hose of the Low-Temperature Equipment
would accumulate in the Venturi-Nozzle - Safety
Box until a certain filling level is reached and a float-
er inside the box closes the gas outlet of the box to
a minimum level. Due to that the flow through the
system is decreased which results in a warming of
the whole cooling system. For the error case that the
outlet hose of the box is blocked, an additional over-
pressure relief valve that opens at a pressure of
3 bar is integrated in the lid of the box. In this way a
safe use of liquid nitrogen is ensured that prevents
liquid nitrogen to escape from the system in case of
an error or mishandling.
The compressed air that is needed for the activation
of the Venturi nozzle is provided by CCU 100. Active
cooling is only needed to cool the sample holder to
temperatures around room temperature and be-
low.The so-called Cooling Limit (CL) defines the
threshold temperature for active cooling. The value
can be changed between 20 and 55 °C (see
chapter 6.3.1 for further information). If the tempera-
ture set point is <CL, CCU 100 opens the com-
pressed-air connection to the Venturi nozzle and
enables in this way the cooling of the system. If the
sample is heated above the threshold temperature,
CCU 100 closes the compressed-air connection
and thus stops the supply of LN2 to the cryostat of
TTK 600.
For further details see chapter 6.5.1 Controlling the
Liquid Nitrogen Cooling.
2.4.2 Compressed-Air Cooling Equipment
The compressed-air cooling equipment consists of
the following components:
• Air-Cooling Set TTK 600 (cat.no.165420)
In order to meet the requirements for the com-
pressed air regarding pressure and purity, Anton
Paar GmbH recommends to use the following pres-
sure regulator with filters:
• Air-Service Unit (cat.no. 6931)
For frequent or long-time cooling of the sample hold-
er to < 10 °C Anton Paar GmbH recommends to use
the following component in order to prevent prob-
lems with condensed water or ice inside the cooling
unit:
• Compressed-air Dryer (cat.no. 81393)
When compressed-air is supplied to the cooling unit,
it generates a flow of cold gas which is directed into
the cryostat inside the sample chamber and cools
the sample holder. The supply of compressed-air to
the cooling unit is controlled by CCU 100.
1
2
3
4
5
DANGER
Risk of injury.
Never open the lid of the Venturi-Nozzle - Safety
Box during operation.

2 TTK 600 - An Overview
18 D52IB001EN-G
Fig. 18: Compressed-air cooling
1 Air cooling unit
2 Compressed air connector
3 Air exhaust
4 Cooling nozzle
Fig. 19: Air service unit
1 Air pressure regulator
2 Air pressure gauge
3 Coarse filter cartridge
4 Fine filter cartridge
For further details see chapter 6.5.2 Controlling the
Compressed-Air Cooling.
2.5 CCU 100 Combined Control Unit
CCU 100 is designed to control the sample holder
temperature in TTK 600 and to guarantee safe op-
eration of the entire instrument. In order to reach
and maintain the desired sample holder tempera-
ture, CCU 100 controls the resistance heater inside
the sample chamber and the cooling devices (liquid
nitrogen cooling equipment or compressed-air cool-
ing unit.)
CCU 100 can be operated manually by means of
the push - buttons on the front panel, or it can be re-
mote-controlled via a serial RS 232 interface.
The main parts of CCU 100 are the main board, the
micro controller for the temperature control and the
power module. The micro controller controls the
sample holder temperature based on the measured
temperature and the user defined target values. The
power module provides variable electrical power for
the heater inside TTK 600, depending on the control
signal from the micro controller.
2.5.1 CCU 100 Front Panel
The front panel of CCU 100 contains all control but-
tons, status LEDs and the display.
Fig. 20: CCU 100 front panel with control elements
1 Mains switch
2 Display and keypad
All elements of the front panel are described in detail
in chapter 6.2.
2.5.2 CCU 100 Rear Panel
The rear panel of CCU 100 contains all the connec-
tors of the instrument.
Fig. 21: CCU 100 rear panel
1 Power connector
2 Connector air out
3 Connector air in
4 RS 232 connector
5 LAN connector (currently not used)
6 Low power module for TTK 600
7 Connector Flow Sensor
8 Connector OUT1/2 (optional connectors)
9 Connector Heater (not used for TTK 600)
10 Connector Sensors/Heater
1
2
3
4
1
2
34
12
123 4678910 5

2 TTK 600 - An Overview
D52IB001EN-G 19
2.5.3 Control of the Sample Cooling
Depending on the instrument configuration,
CCU 100 controls either the liquid nitrogen cooling
(LN2) or the compressed-air cooling equipment.
In order to be able to cool the sample, the com-
pressed-air source has to be connected to the con-
nector AIR IN on the rear panel of CCU 100. If the
controlling of the LN2 cooling equipment is active,
CCU 100 switches a valve inside which is connect-
ed to the AIR OUT connector. By switching this
valve the compressed air is directed to the Venturi
nozzle on the safety box or not. The Venturi nozzle
is creating a vacuum in the hose to the Dewar ves-
sel if the compressed air is on. Due to that liquid ni-
trogen is transported from the Dewar vessel to the
cryostat of TTK 600. If no cooling is required, the
compressed air is switched off.
Cooling automatically starts if the set point tempera-
ture is below the Cooling Limit (CL) of the instru-
ment. This value can be changed between 20 and
50 °C. For further details on how to change this pa-
rameter see chapter 6.3.1.
If the compressed air cooling equipment is used, the
compressed air supply is also connected to the AIR
IN connector on CCU 100. If cooling is required, a
valve inside CCU 100 connects the AIR IN to the
AIR OUT connector, which is connected to the air
cooling unit on the sample chamber.
In case that no cooling is required, the valve be-
tween AIR IN and AIR OUT closes.
2.5.4 Overheat Protection
TTK 600 has two devices to prevent overheating of
the instrument. The water flow controller (cat.no.
164877) monitors the flow of cooling water through
the housing of the sample chamber. It is a water flow
dependent switch, which is connected to CCU 100.
If there is not enough water flow, CCU 100 switches
to Standby (heater off) mode, the Error LED on the
front panel starts to flash and shows an alarm mes-
sage (E03).
In addition, a thermoswitch is mounted on the sam-
ple chamber to protect the device from being over-
heated in case of a malfunction. The thermoswitch
interrupts the heating power circuit if the tempera-
ture of the chamber housing exceeds 70 °C.
CCU 100 automatically switches to Standby mode
(heater off) and shows an alarm (E04).
TIP: A list of all error messages can be found in
chapter 10.1 Error Messages.
2.6 Water Flow Controller
The Water Flow Controller (cat.no. 164877) con-
sists of two components to control and monitor the
cooling water flow through the TTK 600 sample
chamber housing. The pressure regulator is used to
reduce the pressure from the cooling water supply
and set it to the required value of 2 bar. The water
flow monitor is a flow dependent switch which de-
tects if the water flow is below the required minimum
value. The flow monitor is connected to CCU 100
and switches off the heating power in case of insuf-
ficient water flow.
Fig. 22: Pressure regulator
Fig. 23: Water flow monitor
WARNING
Risk of injury.
When the cooling water supply to the chamber
fails, the housing can have a hot surface. In case
of an E03 error, turn off the heater by pressing
the HEATER button and do not touch TTK 600.
Carefully check the temperature of the TTK 600
housing and make sure the housing is at room
temperature before you touch it. Make sure that
you have found and removed the cause of the
error before you continue operation of TTK 600
and CCU 100.

3 Checking the Supplied Parts
20 D52IB001EN-G
3 Checking the Supplied Parts
TTK 600 was tested and packed carefully before
shipment. However, damage may occur during
transport.
1. Keep the packaging material (box, foam piece,
transport protection) for possible returns and
further questions from the transport and insur-
ance company.
2. Check the delivery for completion by comparing
the supplied parts to those noted in Table 3-1.
3. If a part is missing, contact your Anton Paar rep-
resentative.
4. If a part is damaged, contact the transport com-
pany and your Anton Paar representative.
Table 3-1: Supplied Parts
Pcs. Article Description Mat. No.
1
1
8m
1
1
1
TTK 600 Low Temperature Chamber
Adapter or z-alignment stage
Cooling water hoses with quick coupling connectors (already mounted)
Standard Sample Holder (depth 0.8mm)
Gas/vacuum connector
Accessory box (content specified on label)
159900
*
159930
1
1
1
2
1
and/or
1
CCU 100 Combined Control Unit**
Mains cables
Connection cable to TTK 600 sample chamber
Mains fuses
RS232 cable to control PC
Low-Power Module CCU
135000
176730
1
1
1
Flow Controller CCU
Pressure regulator
Water flow monitor
164877
1
1
1
with Liquid-Nitrogen Cooling Equipment
Low-temperature equipment for Venturi nozzle
Liquid nitrogen container, Dewar 60L (optional)
Liquid nitrogen container, Dewar 100L (optional)
164578
166462
166463
1
1
1
with Compressed-air Cooling Equipment
Air cooling set TTK 600
Air service unit (optional)
Compressed-air dryer (optional)
165420
6931
81393
1
1
1
Instruction manual English
Software manual Nambicon
USB flash drive with Nambicon
* The catalog number of the adapter/alignment stage depends on the type of diffractometer.
** The CCU 100 is able to control more than one chamber. In case of ordering the chamber and controller,
the CCU 100 together with the preinstalled Low-Power Module is included; in case of adding a second
chamber to an existing CCU 100, only the Low-Power Module is included.