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Comparative Study of Crystallite Size and Microstrain of Synthesized Analcime Using X-Ray Diffraction Profile Analysis

DOI: 10.4236/ampc.2026.169019, PP. 333-353

Keywords: Analcime, X-Ray Diffraction, Crystallite Size, Microstrain, Microstructure

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Abstract:

The present study consisted of a comparative investigation of crystallite size and microstrain through the analysis of X-ray diffraction peak broadening of analcime synthesized by the hydrothermal method. Several characterization techniques, including X-ray diffraction (XRD), scanning electron microscopy coupled with energy-dispersive spectroscopy (SEM/EDS), Fourier transform infrared spectroscopy (FTIR), and X-ray fluorescence (XRF), were employed to characterize the synthesized material. XRD analysis revealed the presence of a single phase corresponding to analcime. SEM analysis revealed a trapezohedral or deltoidal icositetrahedral morphology, while EDS confirmed the presence of the expected elements accross the analyzed regions, with some local variations in their relative abundances. XRF analysis demonstrated the aluminosilicate nature of the material with a Si/Al ratio of 2.8, while FTIR spectroscopy revealed absorption bands in the range 500 - 1000 cm1, characteristic of zeolitic materials. Several XRD peak broadening analysis methods were applied, including the Scherrer, Monshi-Scherrer, Williamson-Hall, size-strain plot, Halder-Wagner, and modified Warren-Averbach methods. The results highlight significant differences in crystallite size and microstrain values, arising from the assumptions specific to each model. The Scherrer and Monshi-Scherrer methods provided crystallite size estimates ranging from 75.47 nm to 98.71 nm. The UDM, USDM, and UDEDM approaches of the Williamson-Hall method revealed crystallite sizes of 158.54 nm, 149.46 nm, and 155.21 nm, respectively, with corresponding microstrain values of 0.931 × 10?3, 0.902 × 10?3, and 0.924 × 10?3. The Halder-Wagner, size-strain plot, and modified Warren-Averbach methods yielded crystallite sizes of 115.54 nm, 115.54 nm, and 128.38 nm, respectively, and microstrain values of 1.02 × 10?3, 6.26 × 10?3, and 8.13 × 10?4.

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