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A method for the refinement of atomic and experimental parameters applicable to several spectroscopic techniques is presented. This kind of procedure, previously used in x‐ray diffraction, is shown to be a powerful tool in electron probe microanalysis (EPMA). This method consists of minimizing the differences between an experimental x‐ray spectrum and a function proposed to account for the bremsstrahlung and characteristic peaks from the corresponding sample, and also for detection artifacts. This complicated function involves several parameters related to different sources (x‐ray production, x‐ray attenuation, sample composition, x‐ray detection, etc.). Initial values must be supplied for them, and after a numerical iterative procedure is performed, improved values are achieved. Depending on the particular situation, certain parameters may be known a priori, so that they can be fixed, allowing the others to vary. In this way, the method can be used for different purposes: determination of atomic parameters such as fluorescence yields, transition rates or photoelectric cross‐sections, quantitative standardless analysis, determination of detector characteristics, etc. This work is intended to present the general aspects of the method for refining EPMA parameters, and to give some examples of its application to the aforementioned issues. Even when only EPMA spectra are included in this work, the method can be applied to different spectroscopic techniques, such as x‐ray fluorescence, particle‐induced x‐ray emission, etc. Copyright © 2001 John Wiley & Sons, Ltd.

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The emission of x rays in the Kβ region of Mg, Al, Si, Sc, Ti, Cr, Fe, Ni, and Zn induced by electron bombardment was studied by means of wavelength dispersive spectroscopy. The lines studied were: the Kβ III and Kβ IV spectator hole transitions, the 1s → 3s quadrupole decay, the Kβ 2 and Kβ 5 diagram transitions, the structures related to radiative Auger processes, and the Kβ and Kβ lines. Relative energies and probabilities were determined through a careful spectral processing based on a parameter refinement method. The results obtained were compared with other experimental and theoretical determinations when available.

Scanning electron microscopy (SEM) is widely used in the science of materials and different parameters were developed to characterize the surface roughness. In a previous work, we studied the surface topography with fractal dimension at low scale and two parameters at high scale by using the variogram, that is, variance vs. step log-log graph, of a SEM image. Those studies were carried out with the FERImage program, previously developed by us. To verify the previously accepted hypothesis by working with only an image, it is indispensable to have reliable three-dimensional (3D) surface data. In this work, a new program (EZEImage) to characterize 3D surface topography in SEM has been developed. It uses fast cross correlation and dynamic programming to obtain reliable dense height maps in a few seconds which can be displayed as an image where each gray level represents a height value. This image can be used for the FERImage program or any other software to obtain surface topography characteristics. EZEImage also generates anaglyph images as well as characterizes 3D surface topography by means of a parameter set to describe amplitude properties and three functional indices for characterizing bearing and fluid properties.

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