Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis
Novel crystallographic investigation of sol-gel-derived anatase TiO2 nanocrystals synthesized using tetra isopropyl orthotitanate (TIOT) as a precursor at pH 9.0 for hydrolysis promoter. Unlike conventional methods integrated whole powder pattern fitting (WPPF) based Rietveld refinement to quantitat...
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| Format: | Article |
| Language: | English |
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Elsevier
2025-08-01
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| Series: | Chemistry of Inorganic Materials |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2949746925000229 |
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| author | Md. Tarikul Islam Sahil Aman Taiful Bayzid Md. Ashikur Rahaman Upoma Podder Gazi. Md. Arifuzzaman Khan Md. Ashraful Alam |
| author_facet | Md. Tarikul Islam Sahil Aman Taiful Bayzid Md. Ashikur Rahaman Upoma Podder Gazi. Md. Arifuzzaman Khan Md. Ashraful Alam |
| author_sort | Md. Tarikul Islam |
| collection | DOAJ |
| description | Novel crystallographic investigation of sol-gel-derived anatase TiO2 nanocrystals synthesized using tetra isopropyl orthotitanate (TIOT) as a precursor at pH 9.0 for hydrolysis promoter. Unlike conventional methods integrated whole powder pattern fitting (WPPF) based Rietveld refinement to quantitatively analyze the crystal structure, phase purity and microstructural features of the synthesized nanoparticles (NPs). The refinement confirmed the formation of 100 % pure anatase phase with a tetragonal structural shape [a=b= 3.7893 Å, c= 9.492 Å]. Notably, the study employed seven different crystallite size determination identical models where Scherrer method estimating an average size of 8.87 nm. The calculated unit cell volume (136.287 Å3), lattice strain (0.76 %), microstrain (0.00312), crystallinity (61.399 %), crystallinity index (1.44) and dislocation density (0.0127 nm−2) indicated lattice expansion and high defect tolerance critical features for catalytic and electronic applications. Peak profiling showed highest preferred orientation along the (101) plane at 2θ= 25.289°, with a d-spacing of 0.35190 nm and an intensity of 6542 cps. SEM confirmed uniformly dispersed, non-agglomerated NPs, while EDS analysis validated elemental purity with 60 % Ti and 40 % O. This comprehensive structural and surface morphological analysis, combining simple synthesis with advanced refinement, provides a reliable framework for optimizing TiO2 nanocrystals in functional applications. |
| format | Article |
| id | doaj-art-e0cda1a1f5e24e68b5b7d4d31d887072 |
| institution | Kabale University |
| issn | 2949-7469 |
| language | English |
| publishDate | 2025-08-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Chemistry of Inorganic Materials |
| spelling | doaj-art-e0cda1a1f5e24e68b5b7d4d31d8870722025-08-20T03:30:45ZengElsevierChemistry of Inorganic Materials2949-74692025-08-01610010810.1016/j.cinorg.2025.100108Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysisMd. Tarikul Islam0Sahil Aman1Taiful Bayzid2Md. Ashikur Rahaman3Upoma Podder4Gazi. Md. Arifuzzaman Khan5Md. Ashraful Alam6Department of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, Bangladesh; Corresponding author.Department of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, BangladeshDepartment of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, BangladeshDepartment of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, BangladeshDepartment of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, BangladeshDepartment of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, Bangladesh; Corresponding author.Institute of Glass and Ceramic Research and Testing (IGCRT), Bangladesh Council of Scientific and Industrial Research (BCSIR), Dhaka, 1205, Bangladesh; Corresponding author. Department of Applied Chemistry and Chemical Engineering, Islamic University, Kushtia, 7003, Bangladesh.Novel crystallographic investigation of sol-gel-derived anatase TiO2 nanocrystals synthesized using tetra isopropyl orthotitanate (TIOT) as a precursor at pH 9.0 for hydrolysis promoter. Unlike conventional methods integrated whole powder pattern fitting (WPPF) based Rietveld refinement to quantitatively analyze the crystal structure, phase purity and microstructural features of the synthesized nanoparticles (NPs). The refinement confirmed the formation of 100 % pure anatase phase with a tetragonal structural shape [a=b= 3.7893 Å, c= 9.492 Å]. Notably, the study employed seven different crystallite size determination identical models where Scherrer method estimating an average size of 8.87 nm. The calculated unit cell volume (136.287 Å3), lattice strain (0.76 %), microstrain (0.00312), crystallinity (61.399 %), crystallinity index (1.44) and dislocation density (0.0127 nm−2) indicated lattice expansion and high defect tolerance critical features for catalytic and electronic applications. Peak profiling showed highest preferred orientation along the (101) plane at 2θ= 25.289°, with a d-spacing of 0.35190 nm and an intensity of 6542 cps. SEM confirmed uniformly dispersed, non-agglomerated NPs, while EDS analysis validated elemental purity with 60 % Ti and 40 % O. This comprehensive structural and surface morphological analysis, combining simple synthesis with advanced refinement, provides a reliable framework for optimizing TiO2 nanocrystals in functional applications.http://www.sciencedirect.com/science/article/pii/S2949746925000229AnataseNanocrystalRietveld refinementTetra isopropyl orthotitanate (TIOT)WPPF |
| spellingShingle | Md. Tarikul Islam Sahil Aman Taiful Bayzid Md. Ashikur Rahaman Upoma Podder Gazi. Md. Arifuzzaman Khan Md. Ashraful Alam Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis Chemistry of Inorganic Materials Anatase Nanocrystal Rietveld refinement Tetra isopropyl orthotitanate (TIOT) WPPF |
| title | Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis |
| title_full | Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis |
| title_fullStr | Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis |
| title_full_unstemmed | Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis |
| title_short | Crystal growth behavior of nanocrystal anatase TiO2: A Rietveld refinement in WPPF analysis |
| title_sort | crystal growth behavior of nanocrystal anatase tio2 a rietveld refinement in wppf analysis |
| topic | Anatase Nanocrystal Rietveld refinement Tetra isopropyl orthotitanate (TIOT) WPPF |
| url | http://www.sciencedirect.com/science/article/pii/S2949746925000229 |
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