6 Operation
28
C58IB004EN-D
6.5 Performing a Measurement
After having mounted and aligned the sample you
are now ready to start with your measurements (for
sample mounting and alignment refer to
).
If the sample stage temperature does not exceed
200 °C during the entire measurement, the mea-
surement can be carried out without dome and cool-
ing air. Above 200 °C, dome and cooling air are
necessary. Use the configuration cOFF on the
CCU 100.
Use cOn on the CCU 100, if it is required to start
cooling the sample stage at a starting temperature
of dSP + 1 °C or to cool down to dSP + 1 °C contin-
uously.
6.5.1 Before Starting
Before you start the measurement:
• Check the dome. In case of any defect do
not
use it.
• Make sure that the dome is mounted correctly
and the three fixing screws provide tight connec-
tion between dome and the DHS 1100 housing.
• Make sure that the pressure relief valve is not
blocked or closed with a blind plug.
• Make sure that the temperature of your experi-
ment is below the melting point of the sample
and that no sample components react with the
sample stage.
• Make sure that the goniometer is operated in a
way so that it
always
moves back to its starting
position. This is important to avoid that the
hoses wind up.
If changes in the diffractometer software are
necessary, contact the diffractometer manufac-
turer.
• Make sure that cooling air is supplied to the
CCU 100 temperature controller and that the
cooling air is connected to the DHS 1100 (refer
to
chapter 3.4 Installing the Compressed Air
).
• If the PEEK dome is required, make sure that
the dome cooling nozzle is installed (see
ter 3.8: Installing the Cooling Nozzle
6.5.2 Creating a Sample Environment
With DHS 1100 samples can be investigated in vac-
uum or different gas atmospheres.
6.5.2.1 Operation with Air
No special measures must be taken if the sample is
measured in air. The sample stage can be heated
up to the maximum temperature of 1100 °C, de-
pending on the used dome.
6.5.2.2 Operation with Non-Reactive Gases
In order to prevent oxidation of samples, the
DHS 1100 can be filled with non-reactive gases like
helium or nitrogen. We recommend not to use argon
because of its high X-ray absorption.
The
pressure relief valve
in the DHS 1100 housing
is set to 0.35 ± 0.05 bar. This is the maximum pres-
sure which can be achieved inside the dome.
NOTICE
We recommend to move the goniometer with the
DHS 1100 on it over the complete range of
angles intended for the measurement to ensure
that the hoses are not caught by any parts of the
diffractometer.
CAUTION
• The temperature control of the DHS 1100 is
optimized for
stationary atmospheres
around the sample. Do not measure with a
gas flow onto the sample or through the
dome.
• The atmosphere inside the dome has an
influence on the maximum achievable sam-
ple heating/cooling rates and on the tempera-
ture offset between sample stage and probed
sample surface.
• When the DHS 1100 is filled with
helium
, the
maximum operating temperature
is
limited
(see technical specifications appendix A) due
to the large heat transfer from the heating
plate to the dome.
CAUTION
All pressure values in this section are relative to
atmospheric pressure!
Содержание DHS 1100
Страница 2: ......
Страница 38: ...Appendix B Declaration of Conformity 38 C58IB004EN D Appendix B Declaration of Conformity ...
