Derivation of d-Values from Digitized X-ray and Synchrotron Diffraction Data

Abstract

AbstractA precise and practical method for the determination of d-values and lattice parameters from digital diffraction data is described. Systematic errors are corrected mathematically during a d-spacing / lattice-parameter least-Squares refincment process making it unnecessary to use internal standards. X-ray and synchrotron diffraction data of an ICDD alumina plate obtained with a wide variety of experimental conditions and analysis parameters were used to study the precision in the derivation of d-values and the accuracy in the determination of lattice parameters. Results showed that the precision in determining d-values was high with |Δd/d|avg ranging from 2x105 to 4x10-5. Using the results obtained from the high precision XRD analysis as a reference standard, the accuracy in the lattice parameter determinations from the synchrotron diffraction data reached the l-2x10-6] range. Lattice parameters, with an accuracy in the high 10-5 range, were also obtained using parameters commonly used in a routine XRD analysis such as a wide RS (0.11°) for high intensity, peaks only in the front reflection region, no Kα2 stripping, and a Single 2θo parameter for systematic error corrections.