Microfabrication of controlled-geometry samples for the laser-heated diamond-anvil cell using focused ion beam technology

The pioneering of x-ray diffraction with in situ laser heating in the diamond-anvil cell has revolutionized the field of high-pressure mineral physics, expanding the ability to determine high-pressure, high-temperature phase boundaries and equations of state. Accurate determination of high-pressure, high-temperature phases and densities in the diamond-anvil cell rely upon collinearity of the x-ray beam with the center of the laser-heated spot. We present the development of microfabricated samples that, by nature of their design, will have the sample of interest in the hottest portion of the sample. We report initial successes with a simplified design using a Pt sample with dimensions smaller than the synchrotron-based x-ray spot such that it is the only part of the sample that absorbs the heating laser ensuring that the x-rayed volume is at the peak hotspot temperature. Microfabricated samples, synthesized using methods developed at The Ohio State University's Mineral Physics Laboratory and Campus Electron Optics Facility, were tested at high P-T conditions in the laser-heated diamond-anvil cell at beamline 16 ID-B of the Advanced Photon Source. Pt layer thicknesses of ≤0.8 μm absorb the laser and produce accurate measurements on the relative equations of state of Pt and PtC. These methods combined with high-purity nanofabrication techniques will allow for extension by the diamond-anvil cell community to multiple materials for high-precision high-pressure, high-temperature phase relations, equations of state, melting curves, and transport properties.