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Article

Strain and Grain Size Determination of CeO2 and TiO2 Nanoparticles: Comparing Integral Breadth Methods versus Rietveld, μ-Raman, and TEM

by
Yamerson Canchanya-Huaman
1,
Angie F. Mayta-Armas
1,
Jemina Pomalaya-Velasco
1,
Yéssica Bendezú-Roca
1,
Jorge Andres Guerra
2 and
Juan A. Ramos-Guivar
3,*
1
Laboratorio de No Metálicos, Facultad de Ingeniería Química, Universidad Nacional del Centro del Perú (UNCP), Av. Mariscal Ramón Castilla No. 3909, El Tambo, Huancayo 12000, Peru
2
Departamento de Ciencias, Sección Física, Pontificia Universidad Católica del Perú, Av. Universitaria 1801, Lima 15088, Peru
3
Grupo de Investigación de Nanotecnología Aplicada para Biorremediación Ambiental, Energía, Biomedicina y Agricultura (NANOTECH), Facultad de Ciencias Físicas, Universidad Nacional Mayor de San Marcos, Av. Venezuela Cdra 34 S/N, Ciudad Universitaria, Lima 15081, Peru
*
Author to whom correspondence should be addressed.
Nanomaterials 2021, 11(9), 2311; https://doi.org/10.3390/nano11092311
Submission received: 5 August 2021 / Revised: 1 September 2021 / Accepted: 1 September 2021 / Published: 6 September 2021
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Abstract

Various crystallite size estimation methods were used to analyze X-ray diffractograms of spherical cerium dioxide and titanium dioxide anatase nanoparticles aiming to evaluate their reliability and limitations. The microstructural parameters were estimated from several integral breadth methods such as Scherrer, Monshi, Williamson–Hall, and their variants: (i) uniform deformation model, (ii) uniform strain deformation model, and (iii) uniform deformation energy density model. We also employed the size–strain plot and Halder–Wagner method. For this purpose, an instrumental resolution function of an Al2O3 standard was used to subtract the instrumental broadening to estimate the crystallite sizes and strain, and the linear regression analysis was used to compare all the models based on the coefficient of determination. The Rietveld whole powder pattern decomposition method was introduced for comparison purposes, being the best candidate to fit the X-ray diffraction data of metal-oxide nanoparticles. Refined microstructural parameters were obtained using the anisotropic spherical harmonic size approach and correlated with the above estimation methods and transmission electron microscopy images. In addition, μ-Raman spectra were recorded for each material, estimating the mean crystallite size for comparison by means of a phonon confinement model.
Keywords: X-ray diffraction; CeO2; TiO2; crystallite size; strain; TEM; μ-Raman X-ray diffraction; CeO2; TiO2; crystallite size; strain; TEM; μ-Raman

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MDPI and ACS Style

Canchanya-Huaman, Y.; Mayta-Armas, A.F.; Pomalaya-Velasco, J.; Bendezú-Roca, Y.; Guerra, J.A.; Ramos-Guivar, J.A. Strain and Grain Size Determination of CeO2 and TiO2 Nanoparticles: Comparing Integral Breadth Methods versus Rietveld, μ-Raman, and TEM. Nanomaterials 2021, 11, 2311. https://doi.org/10.3390/nano11092311

AMA Style

Canchanya-Huaman Y, Mayta-Armas AF, Pomalaya-Velasco J, Bendezú-Roca Y, Guerra JA, Ramos-Guivar JA. Strain and Grain Size Determination of CeO2 and TiO2 Nanoparticles: Comparing Integral Breadth Methods versus Rietveld, μ-Raman, and TEM. Nanomaterials. 2021; 11(9):2311. https://doi.org/10.3390/nano11092311

Chicago/Turabian Style

Canchanya-Huaman, Yamerson, Angie F. Mayta-Armas, Jemina Pomalaya-Velasco, Yéssica Bendezú-Roca, Jorge Andres Guerra, and Juan A. Ramos-Guivar. 2021. "Strain and Grain Size Determination of CeO2 and TiO2 Nanoparticles: Comparing Integral Breadth Methods versus Rietveld, μ-Raman, and TEM" Nanomaterials 11, no. 9: 2311. https://doi.org/10.3390/nano11092311

APA Style

Canchanya-Huaman, Y., Mayta-Armas, A. F., Pomalaya-Velasco, J., Bendezú-Roca, Y., Guerra, J. A., & Ramos-Guivar, J. A. (2021). Strain and Grain Size Determination of CeO2 and TiO2 Nanoparticles: Comparing Integral Breadth Methods versus Rietveld, μ-Raman, and TEM. Nanomaterials, 11(9), 2311. https://doi.org/10.3390/nano11092311

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