Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review

This review reports the structural characterization of titanium dioxide nanomaterials and their composites, which are widely applied in catalysis, coatings, and thermal systems. A consistent dimensional hierarchy has been reported across studies: crystallite size (X-ray diffraction) < grain size...

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Main Authors: Sukarman, Budi Kristiawan, Eko Prasetya Budiana, Khoirudin, Amri Abdulah
Format: Article
Language:English
Published: Elsevier 2025-12-01
Series:Hybrid Advances
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Online Access:http://www.sciencedirect.com/science/article/pii/S2773207X25001472
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author Sukarman
Budi Kristiawan
Eko Prasetya Budiana
Khoirudin
Amri Abdulah
author_facet Sukarman
Budi Kristiawan
Eko Prasetya Budiana
Khoirudin
Amri Abdulah
author_sort Sukarman
collection DOAJ
description This review reports the structural characterization of titanium dioxide nanomaterials and their composites, which are widely applied in catalysis, coatings, and thermal systems. A consistent dimensional hierarchy has been reported across studies: crystallite size (X-ray diffraction) < grain size (transmission electron microscopy) < particle size (scanning electron microscopy or dynamic light scattering). The deviations between these dimensions ranged from ∼3 % to >130 % depending on the synthesis temperature, agglomeration, and instrumental resolution. Crystallite sizes as low as 2.12 nm have been reported, whereas the corresponding grain sizes typically exceed 20 nm. The microstrain values derived from the Williamson–Hall, uniform deformation, and Warren–Averbach models ranged from 0.06 % to 1.14 %, indicating variable lattice distortion. The dislocation density values ranged from 0.0389 to 0.224 × 1016 m−2, often correlating inversely with the crystallite size. The phase compositions confirmed by Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy included anatase, rutile, and iron oxide phases. ζ-potential and dynamic light scattering analyses consistently revealed colloidal stability and aggregation. These findings highlight the limitations of single-technique characterizations and support integrated multi-method approaches alongside artificial intelligence-based calibration for reliable structure–property optimization in titanium dioxide nanomaterials.
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spelling doaj-art-7ffe0eeadc7e4cb1aa6411cf715d10f32025-07-17T04:45:14ZengElsevierHybrid Advances2773-207X2025-12-0111100523Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review Sukarman0Budi Kristiawan1Eko Prasetya Budiana2 Khoirudin3Amri Abdulah4Department of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Department of Mechanical Engineering, Faculty of Engineering, Universitas Buana Perjuangan Karawang, Jl. HS. Ronggo Waluyo, Karawang, 41361, IndonesiaDepartment of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Studies Group of Sustainable Thermofluids, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Corresponding author. Department of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia.Department of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Studies Group of Sustainable Thermofluids, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Corresponding author. Department of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia.Department of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Department of Mechanical Engineering, Faculty of Engineering, Universitas Buana Perjuangan Karawang, Jl. HS. Ronggo Waluyo, Karawang, 41361, IndonesiaDepartment of Mechanical Engineering, Faculty of Engineering, Universitas Sebelas Maret, Jl. Ir. Sutami 36A Kentingan, Surakarta, 57126, Indonesia; Department of Mechanical Engineering, Sekolah Tinggi Teknologi Wastukancana, Jl. Cikopak No.53, Purwakarta, 41117, IndonesiaThis review reports the structural characterization of titanium dioxide nanomaterials and their composites, which are widely applied in catalysis, coatings, and thermal systems. A consistent dimensional hierarchy has been reported across studies: crystallite size (X-ray diffraction) < grain size (transmission electron microscopy) < particle size (scanning electron microscopy or dynamic light scattering). The deviations between these dimensions ranged from ∼3 % to >130 % depending on the synthesis temperature, agglomeration, and instrumental resolution. Crystallite sizes as low as 2.12 nm have been reported, whereas the corresponding grain sizes typically exceed 20 nm. The microstrain values derived from the Williamson–Hall, uniform deformation, and Warren–Averbach models ranged from 0.06 % to 1.14 %, indicating variable lattice distortion. The dislocation density values ranged from 0.0389 to 0.224 × 1016 m−2, often correlating inversely with the crystallite size. The phase compositions confirmed by Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy included anatase, rutile, and iron oxide phases. ζ-potential and dynamic light scattering analyses consistently revealed colloidal stability and aggregation. These findings highlight the limitations of single-technique characterizations and support integrated multi-method approaches alongside artificial intelligence-based calibration for reliable structure–property optimization in titanium dioxide nanomaterials.http://www.sciencedirect.com/science/article/pii/S2773207X25001472Titanium dioxideCrystallite sizeMicrostrainPhase identificationX-ray diffractionRaman spectroscopy
spellingShingle Sukarman
Budi Kristiawan
Eko Prasetya Budiana
Khoirudin
Amri Abdulah
Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
Hybrid Advances
Titanium dioxide
Crystallite size
Microstrain
Phase identification
X-ray diffraction
Raman spectroscopy
title Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
title_full Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
title_fullStr Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
title_full_unstemmed Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
title_short Multi-technique characterization of TiO2 nanoparticles: Crystallite size, microstrain, and phase analysis for nanomaterial applications – a review
title_sort multi technique characterization of tio2 nanoparticles crystallite size microstrain and phase analysis for nanomaterial applications a review
topic Titanium dioxide
Crystallite size
Microstrain
Phase identification
X-ray diffraction
Raman spectroscopy
url http://www.sciencedirect.com/science/article/pii/S2773207X25001472
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