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Strategies for in situ laser heating in the diamond anvil cell at an X-ray diffraction beamline

Journal of Synchrotron Radiation (2014) 21(1) 89-96
DOI: 10.1107/S1600577513027434
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Abstract

An overview of several innovations regarding in situ laser-heating techniques in the diamond anvil cell at the high-pressure beamline ID27 of the European Synchrotron Radiation Facility is presented. Pyrometry measurements have been adapted to allow simultaneous double-sided temperature measurements with the installation of two additional online laser systems: a CO2 and a pulsed Nd:YAG laser system. This reiteration of laser-heating advancements at ID27 is designed to pave the way for a new generation of state-of-the-art experiments that demand the need for synchrotron diffraction techniques. Experimental examples are provided for each major development. The capabilities of the double pyrometer have been tested with the Nd:YAG continuous-wave lasers but also in a time-resolved configuration using the nanosecond-pulsed Nd:YAG laser on a Fe sample up to 180 GPa and 2900 K. The combination of timeresolved X-ray diffraction with in situ CO2 laser heating is shown with the crystallization of a high-pressure phase of the naturally found pyrite mineral MnS2 (11 GPa, 1100-1650 K).© 2014 International Union of Crystallography.

Figures

  • Figure 1 Schematic layout of the different laser-heating systems available at ID27. Red, blue and dashed blue lines indicate the incident CO2 and its HeNe alignment laser, Nd:YAG solid-state laser and pulsed Nd:YAG laser, respectively. In green are the incident X-ray beam and the X-ray cone of diffraction to the MAR CCD camera. In orange is the path for double-sided temperature measurement. Double-arrow signs refer to optics mounted on pneumatic stages.
  • Figure 2 Typical temperature measurements on a Fe foil at 180 GPa. The Fe sample is laser heated from side 1 with a CW Nd:YAG laser, and the temperature is recorded on both sides simultaneously through the double pinhole entrance of the spectrometer. (a) Two-dimensional image of the CCD strip, and (b) picture of the Fe sample embedded in KBr at 180 GPa. (c), (d) Data integrated, calibrated and fitted with Wien’s law from 600 to 900 nm to retrieve the temperature from both sides (only the portion from 600 to 800 nm is shown here).
  • Figure 3 Simultaneous temperature measurements from both sides of the sample during laser heating on side 1 with laser 1 (a) and on side 2 with laser 2 (b) from 63 to 180 GPa. Temperatures measured from side 2 (i.e. upstream of the X-rays, see Fig. 1) are reported on the vertical axis, and temperatures measured from side 1 are reported on the horizontal axis. Circles indicate temperature measurements obtained during laser heating from side 1 only (a) and diamonds represent the temperature measured on both sides of the samples while laser heating from side 2 only (b). The dark thick line is representative of an absence of gradient in the sample, i.e. equal temperature from both sides of the sample. The dashed line refers to isotherms, shifted from the thick line.
  • Figure 4 Pulse laser-heating results showing the time delay of the collected light from 180 to 100 GPa. The pulse laser is focused on the sample from side 1 (see Fig. 1). (a), (b), (c) Plots of near-IR intensity collected from the sample versus time (in ns) at 180 GPa, 140 GPa and 100 GPa, respectively. Red points are collected from side 1 (laser-heating side) and green points from side 2. The black curves are the pseudo-Voigt fits for the curve obtain from side 1, with black dashed curves for side 2. The time delay is calculated using the position of the two FWHMs for each side as illustrated in (a). (d) Plots of the inverse delay (in ns 1) (left scale) at the three investigated pressures (red circles); also reported are the results for thermal conductivity of molten iron (right-hand scale) as a function of pressure (blue squares) (Pozzo et al., 2012).
  • Figure 5 An in situ X-ray diffraction stack plot of the mineral MnS2 during CO2 laser heating. Temperature measurements were taken every 30 s and the full time lapse of this plot is 5 min.

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Petitgirard, S., Salamat, A., Beck, P., Weck, G., & Bouvier, P. (2014). Strategies for in situ laser heating in the diamond anvil cell at an X-ray diffraction beamline. Journal of Synchrotron Radiation, 21(1), 89–96. https://doi.org/10.1107/S1600577513027434

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