Absolute x-ray energy calibration over a wide energy range using a diffraction-based iterative method

In this paper, we report a method of precise and fast absolute x-ray energy calibration over a wide energy range using an iterative x-ray diffraction based method. Although accurate x-ray energy calibration is indispensable for x-ray energy-sensitive scattering and diffraction experiments, there is still a lack of effective methods to precisely calibrate energy over a wide range, especially when normal transmission monitoring is not an option and complicated micro-focusing optics are fixed in place. It is found that by using an iterative algorithm the x-ray energy is only tied to the relative offset of sample-to-detector distance, which can be readily varied with high precision of the order of 10−5–10−6 spatial resolution using gauge blocks. Even starting with arbitrary initial values of 0.1 Å, 0.3 Å, and 0.4 Å, the iteration process converges to a value within 3.5 eV for 31.122 keV x-rays after three iterations. Different common diffraction standards CeO2, Au, and Si show an energy deviation of 14 eV. As an application, the proposed method has been applied to determine the energy-sensitive first sharp diffraction peak of network forming GeO2 glass at high pressure, exhibiting a distinct behavior in the pressure range of 2–4 GPa. Another application presented is pair distribution function measurement using calibrated high-energy x-rays at 82.273 keV. Unlike the traditional x-ray absorption-based calibration method, the proposed approach does not rely on any edges of specific elements, and is applicable to the hard x-ray region where no appropriate absorption edge is available.