8 Performing a Measurement
48
D52IB001EN-G
8.2.5 Applying the Sample
In general the most suitable way of sample prepara-
tion strongly depends on the sample, temperature
range and goal of the experiment. Therefore, regard
the following instructions as suggestions only.
8.2.5.1 Powder Samples for the Standard Sample
Holder
Prepare the sample as follows:
Use a spatula to press the powder into the groove of
the sample holder and then smooth the powder's
surface with a glass platelet.
If required, mix the powder with a small quantity of
diluted Zapon lacquer solution.
1. Again, use the spatula to uniformly apply this
"slurry" into the groove of the sample holder.
2. Allow sufficient time for the sample to dry and
become an adhesive and solid substance.
8.2.5.2 Bulk Samples for the Standard Sample
Holder
Bulk samples are usually difficult to measure be-
cause of irreproducible deviations between the tem-
perature displayed on the CCU 100 and the
temperature of the sample surface scanned with the
X-ray beam.
Main properties which determine the temperature
gradient are:
• thermal conductivity and thickness of the sam-
ple
• flatness and smoothness of the sample surface.
Place solid samples into the groove of the sample
holder. The depth of the groove in the sample holder
is 0.8 mm (a sample holder with a depth of 0.2 mm
and a flat sample holder are also available). The
alignment stage allows you to compensate for the
difference in height between the sample holder and
sample holder groove.
8.2.5.3 Powders and Pastes for the Transmission
Sample Holder
The procedure for preparing powder and paste
samples for the transmission sample holder is de-
scribed below:
1. Place the delivered mounting tool on a flat sur-
face and place the transmission sample holder
NOTICE
Risk of damage.
Sample components might react with the sample
holder and destroy it.
- Check the chemical resistance of the
sample holder for the respective sample in
the applied atmosphere and at the desired
temperature BEFORE the experiment.
- Refer to appendix A for technical data of
the TTK 600 Low -Temperature Chamber.
NOTICE
Risk of damage.
Do not heat fast, because rapidly evaporating
liquid creates holes in the sample.
- Make sure that the sample completely
covers the sample holder. Holes in the
sample can cause large background sig-
nal from the sample holder.
- For organic samples with high X-ray trans-
mission, use the zero back- ground
holder.
NOTICE
Make sure that the sample is thermally con-
tacted to the sample holder to achieve a uniform
temperature distribution within the sample.
NOTICE
If possible, do not measure bulk samples in vac-
uum. Heat transfer in vacuum is usually very
bad. Use inert gas (He) instead of vacuum.
Bulk samples often bend upon heating, which
changes the thermal contact and the tempera-
ture gradients in an undefined way.
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 ...
