8 Performing a Measurement
58
D52IB001EN-G
beam during the height scan, before a small peak in
intensity appears representing the gap between the
top part of the sample holder and the Kapton foil.
The sample holder height should be aligned to the
position of the reflection battery sample holder lid.
So that the sample is correctly aligned in the X-ray
beam and peak shifts due to height errors are avoid-
ed, the height should be increased by the following
amounts depending on the foils being used:
• only Kapton foil: +2.28 mm
• Kapton and graphite foils: +2.32 mm
Battery Sample Holder (Transmission):
Fig. 60: Transmission sample holder
To mount the battery sample holder (transmission),
proceed exactly as described for the battery sample
holder (reflection).
To align the sample in the beam, a height scan
should be performed with ? = 0° and 2? = 0°. This
will show intensity where the window opens on the
back side of the sample holder. The sample height
should be aligned to be in the middle of this intensity
peak.
8.5 Creating a Gas/Vacuum Environ-
ment
An overview of the possible in-situ XRD experi-
ments that are possible with the TTK 600 Low-Tem-
perature Chamber is given in chapter 2.2.
8.5.1 Operation with Air
There are no special requirements for the operation
with air inside the chamber.
Leave the vacuum flange open to allow release of
gas during heating in order to avoid overpressure in-
side the chamber.
8.5.2 Operation under Vacuum
TTK 600 can be evacuated to approx.1x10
-2
mbar
with a rotary pump (4.2 m
3
/h).
In case that high vacuum is needed, TTK 600 can
also be evacuated to approx. 1x10
-4
mbar using a
turbomolecular pump.
Experiments in vacuum can be performed in the full
temperature range of the TTK 600 Low-Tempera-
ture Chamber from -190 °C to 600 °C.
TIP:
The thermal conductivity of powder material is
much lower than that of the corresponding bulk
material. As a consequence, significant tempera-
ture deviation between the sample holder and the
NOTICE
Risk of damage
Take care that no setpoint > 130 °C is applied to
the instrument as this can cause destruction of
the components of the battery sample holder.
1
3
4
5
2
CAUTION
Risk of injury.
The gas inside the chamber expands when
heated. Above 3 bar rel. the gas will be released
through the overpressure relieve valve on the lid
of the instrument.
This overpressure relieve valve MUST NOT be
used for the control of the pressure inside the
instrument. Instead a separate adjustable over-
pressure relieve valve has to be installed in the
gas line.
CAUTION
Risk of injury.
Be aware that experiments in air can be per-
formed at temperatures between room tempera-
ture and 450 °C for the standard sample holder.
Summary of Contents for TTK 600
Page 2: ......
Page 74: ...Appendix B Sample Chamber Dimensions 74 D52IB001EN G Appendix B Sample Chamber Dimensions ...
Page 75: ...Appendix C Declaration of Conformity D52IB001EN G 75 Appendix C Declaration of Conformity ...
Page 77: ...Appendix D Spare Parts and Accessories D52IB001EN G 77 176383 COOLING MODE SWITCHING VALVE ...
