Electron Probe Microanalysis of Transition Metals using L lines: The Effect of Self-absorption

Electron microprobe-based quantitative compositional measurement of first-row transition metals using their L $\alpha$ X-ray lines is hampered by, among other effects, self-absorption. This effect, which occurs when a broad X-ray line is located close to a broad absorption edge, is not accounted for by matrix corrections. To assess the error due to neglecting self-absorption, we calculate the L $\alpha$ X-ray intensity emitted from metallic Fe, Ni, Cu, and Zn targets, assuming a Lorentzian profile for the X-ray line and taking into account the energy dependence of the mass absorption coefficient near the absorption edge. We find that calculated X-ray intensities depart increasingly, for increasing electron beam energy, from those obtained assuming a narrow X-ray line and a single fixed absorption coefficient (conventional approach), with a maximum deviation of $\sim$ 15% for Ni and of $\sim$ 10% for Fe. In contrast, X-ray intensities calculated for metallic Zn and Cu do not differ significantly from those obtained using the conventional approach. The implications of these results for the analysis of transition-metal compounds by electron probe microanalysis as well as strategies to account for self-absorption effects are discussed.

Development and synthesis of orthophosphate single crystals of YPO4 and LuP4 activated with Er3+

Crystals of xenotime-structured phosphates doped with erbium had been grown from molybdate flux at a temperature 1220 ° C followed by slow cooling. The crystals synthesized had been studied using X-ray diffraction and electron probe microanalysis in combination with optical microscopy and luminescence studies.

A Novel Reconstruction Method to Increase Spatial Resolution in Electron Probe Microanalysis

The spatial resolution of electron probe microanalysis (EPMA), a non-destructive method to determine the chemical composition of materials, is currently restricted to a pixel size larger than the volume of interaction between beam electrons and the material, as a result of limitations on the underlying k-ratio model. Using more sophisticated models to predict k-ratios while solving the inverse problem of reconstruction offers a possibility to increase the spatial resolution. Here, a k-ratio model based on the deterministic M1-model in Boltzmann Continuous Slowing-Down approximation (BCSD) will be utilized to present a reconstruction method for EPMA which is implemented as a PDE-constrained optimization problem. Iterative gradient-based optimization techniques are used in combination with the adjoint state method to calculate the gradient in order to solve the optimization problem efficiently. The accuracy of the spatial resolution still depends on the number and quality of the measured data, but in contrast to conventional reconstruction methods, an overlapping of the interaction volumes of different measurements is permissible without ambiguous solutions. The combination of k-ratios measured with various electron beam configurations is necessary for a high resolution. Attempts to reconstruct materials with synthetic data show challenges that occur with small reconstruction pixels, but also indicate the potential to improve the spatial resolution in EPMA using the presented method.