Abstract

A scanning angle diffraction technique with an energy-dispersive solid-state detector (SSD) and white synchrotron radiation has been developed for high-pressure structure studies in diamond anvil cells (DACs). This technique is similar to the CAESAR technique [Y. Wang, T. Uchida, R. Von Dreele, M.L. Rivers, N. Nishiyama, K. Funakoshi, A. Nozawa, and H. Kaneko, A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation, J. Appl. Cryst. 37 (2004), p. 947] developed for large-volume presses, but extended to DAC applications with high spatial resolution. The main feature of the technique is the well-defined collimation in the beam path to the detector, which improves the signal-to-noise ratio significantly, compared to routine monochromatic angle-dispersive powder diffraction with area detectors. This is particularly useful and essential for low-scattering materials and for amorphous and liquid diffraction/scattering studies using DACs. Data collected from crystalline and amorphous samples in DACs show that a coarse 2θ scan (0.1–0.2° for crystals and 0.5° for amorphous structure) is sufficient to obtain reasonable diffraction resolution. The scanning angle energy-dispersive X-ray diffraction technique provides angle-dispersive X-ray diffraction (ADXD) data in multiple energies. Such multi-energy ADXD data carry much more information than regular single-energy ADXD, which could provide site-specific atomic structure information for full structure refinement.

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