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X-Ray Dynamical Diffraction in Powder Samples with Time-Dependent Particle Size Distributions

Published online by Cambridge University Press:  02 December 2019

Adriana Valério ,
Sérgio L. Morelhão ,
Alex J. Freitas Cabral ,
Márcio M. Soares  and
Cláudio M. R. Remédios
Adriana Valério*
Affiliation:
Institute of Physics, University of São Paulo, São Paulo 05508-090, Brazil
Sérgio L. Morelhão
Affiliation:
Institute of Physics, University of São Paulo, São Paulo 05508-090, Brazil
Alex J. Freitas Cabral
Affiliation:
Instituto de Ciências Exatas e Naturais, Universidade Federal do Pará, Belém, PA, Brazil Universidade Federal do Oeste do Pará, Santarém, PA, Brazil
Márcio M. Soares
Affiliation:
Laboratório Nacional de Luz Síncrotron - LNLS/CNPEM, Campinas, SP, Brazil
Cláudio M. R. Remédios
Affiliation:
Instituto de Ciências Exatas e Naturais, Universidade Federal do Pará, Belém, PA, Brazil
*
*(Email: avalerio@if.usp.br)
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Abstract

In situ X-ray diffraction is one of the most useful tools for studying a variety of processes, among which crystallization of nanoparticles where phase purity and size control are desired. Growth kinetics of a single phase can be completely resolved by proper analysis of the diffraction peaks as a function of time. The peak width provides a parameter for monitoring the time evolution of the particle size distribution (PSD), while the peak area (integrated intensity) is directly related to the whole diffracting volume of crystallized material in the sample. However, to precisely describe the growth kinetics in terms of nucleation and coarsening, the correlation between PSD parameters and diffraction peak widths has to be established in each particular study. Corrections in integrated intensity values for physical phenomena such as variation in atomic thermal vibrations and dynamical diffraction effects have also to be considered in certain cases. In this work, a general correlation between PSD median value and diffraction peak width is deduced, and a systematic procedure to resolve time-dependent lognormal PSDs from in situ XRD experiments is described in details. A procedure to correct the integrated intensities for dynamical diffraction effects is proposed. As a practical demonstration, this analytical procedure has been applied to the single-phase crystallization process of bismuth ferrite nanoparticles.

Keywords

in situnucleation & growthx-ray diffraction (XRD)crystallization
Type
Articles
Information
MRS Advances , Volume 5 , Issue 29-30: Materials Theory, Computation and Characterization , 2020 , pp. 1585 - 1591
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Copyright
Copyright © Materials Research Society 2019

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References

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