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Heating experiments at high pressure are extremely
valuable in understanding fundamental physical and chemical behavior
of materials as well as in examining phase stability and phase diagrams.
Diamond-anvil cell (DAC) experiments usually have been very productive
at room temperature. In order to perform experiments at high temperature
using a DAC, one has to develop a heating technique either using
ohmic heating or optical lasers. Ohmic heating is relatively simple
and the workable temperature can reach to 1000 K. We have tested
various wire heating configurations coupled with DAC experiments.
Initially we used a band heater to heat samples inside DAC’s
to ~750 K. To aid thermal coupling between the heater and the cell
body, we used aluminum filler. As the temperature goes up, the pressure
starts decreasing largely due to the thermal expansion of the cell
body. However, it stays stable once P and T are adjusted to the
conditions of a measurement. We used a similar heating method to
measure x-ray powder diffraction and Raman spectra. To reach higher
temperatures, a simple wire heating method has been adapted. A Ni-Cr
wire wound into a 4-5 mm diameter loop is placed around sample area
covering the gasket and two diamond anvils. A small ceramic ring
is cut and used to hold the heater wire in place. To prevent oxidation
of the heating wire, the DAC with an external heater is placed in a
vacuum jacket.
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Externally heated cell under Ar/H2 condition (left)
and in vacuum jacket (right), respectively for angle-resolved x-ray
diffraction at the SSRL and energy-dispersive x-ray diffraction at
the NSLS.
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Various cw- and pulsed-lasers (YAG,
YLF, CO2, and pulsed-YAG lasers) are used to heat the samples to
a few thousand degrees at Mbar pressures in diamond-anvil cells.
This technique is capable of generating the pressure-temperature
conditions of the interiors of the Earth and Jovian planets, thermal
and nuclear explosions, and metallic-hydrogen. These laser heating
techniques are often coupled with synchrotron x-ray diffraction
and laser spectroscopy to discover and characterize new
materials and novel phases with advanced materials properties and
determine high pressure materials properties in-situ at high pressures
and temperatures.
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Operating high-pressure diamond anvil cells at cryogenic
conditions permits us to load molecular fluids and perform studies
including low temperature phases and phase transitions. The High
Pressure Physics Group has several cryostats suited to low temperature
work.
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The simplest of these systems is a sealed vessel
that can be cooled to an appropriate temperature for condensing
and capturing molecular fluids such as nitrogen or methane. This
permits us to load these fluids at extremely high purity in a sealed
environment. This technique is limited to the temperature of liquid
nitrogen, 77 Kelvin.
For temperature below 77 K and low temperature optical studies,
the High Pressure Physics Group has two continuous flow cryostats
that can achieve temperatures of ~1.5 Kelvin, and several closed
cycle refrigerators that can achieve temperatures of ~ 10 Kelvin.
These cryostats have optical windows that permit the diamond anvil
cell sample to be imaged and studied spectroscopically at low temperatures.
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