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XRD Pattern Fitting as a Tool to Control Plating Parameters in Zinc Nickel Electroplates

Published online by Cambridge University Press:  06 March 2019

Lloyd Hammond  and
Don Wright
Lloyd Hammond
Affiliation:
Materials Research Laboratory Defence Science and Technology Organisation Melbourne, Australia
Don Wright
Affiliation:
Materials Research Laboratory Defence Science and Technology Organisation Melbourne, Australia
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Abstract

Rietveld X-ray powder diffraction (XRD) and uniaxial stress measurement procedures are being evaluated as a means of correlating the crystalline structure properties of zinc-nickel electroplate with observed plating properties. The study is being performed on a suite of six samples of varying composition (6 to 20%Ni) electrodeposited on mild steel. Rietveld refinement of the XRD data (Rietveld, 1969) has been performed on a specially prepared ingot (9%Ni:91%Zn) to determine the structural parameters and relative abundances for the γ(Ni4Zn22), δ(Ni3Zn22) and η(Zn) phases which could possibly be present in the electroplate. Relative phase abundances were verified by Atomic Absorption Spectrometry (AAS) and electron probe microanalysis (EPMA) image mapping techniques.

The structural parameters for the ingot zinc-nickel phases were subsequently used as initial parameters in Rietveld calculations for the six electroplate samples. Structure refinement of the electroplate XRD data was hampered by extremely high preferred orientation and the corresponding lack of quality diffraction peaks. However, Rietveld refinements produced accurate cell dimensions (which correlate linearly with nickel composition), a means of quantifying the degree of preferred orientation, and crystalline phase verification. For residual stress determination, d-sin2ψ plots were produced for each electroplate sample. The plots were found to be linear for Ni < 12%, allowing calculation of residual stress, and distinctly curved for Ni > 12%.

Type
VI. Whole Pattern Fitting, Phase Analysis by Diffraction Methods
Information
Advances in X-Ray Analysis , Volume 36: Forty-First Annual Conference on Applications of X-ray Analysis, August 3-7, 1992 , 1992 , pp. 315 - 325
Copyright
Copyright © International Centre for Diffraction Data 1992

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