Crystallinity integration of anatase (TiO2) nanocrystal by whole powder pattern fitting (WPPF) method: A Rietveld refinement study

Shanawaz Ahmed , Md. Khalid Hossain Shishir , Md. Tarikul Islam , Md. Ashikur Rahaman , Sahil Aman , Allah Rakha Aidid , Sumaiya Islam Sadia , Md. Masud Rana , Md. Ashraful Alam
{"title":"Crystallinity integration of anatase (TiO2) nanocrystal by whole powder pattern fitting (WPPF) method: A Rietveld refinement study","authors":"Shanawaz Ahmed ,&nbsp;Md. Khalid Hossain Shishir ,&nbsp;Md. Tarikul Islam ,&nbsp;Md. Ashikur Rahaman ,&nbsp;Sahil Aman ,&nbsp;Allah Rakha Aidid ,&nbsp;Sumaiya Islam Sadia ,&nbsp;Md. Masud Rana ,&nbsp;Md. Ashraful Alam","doi":"10.1016/j.rinma.2025.100673","DOIUrl":null,"url":null,"abstract":"<div><div>High crystalline anatase synthesized by a unique simple route using titanium isopropoxide (TTIP) as precursor and isopropyl alcohol (IP) as peptizing agent. The Rietveld refinement analysis showed that the synthesized material is composed of 99.0 % anatase and 1.0 % brookite phases of titanium dioxide (TiO<sub>2</sub>). XRD characterized the prominent crystalline phase, providing insights into lattice parameters where a=b= 3.79068 Å, c= 9.50400 Å; α=β=γ= 90.0°; lattice strain 0.718, lattice volume 136.565 Å<sup>3</sup>, specific surface area 429.26 m<sup>2</sup>/g, dislocation density 0.0755 nm<sup>− 2</sup>, preference growth 0.119 and packing efficiency 70.09 %. The most intense diffraction was attributed to the (101) plane at 2θ = 25.39°. The average crystallite size through six identical models those were 3.64 nm (Scherrer equation), 6.47 nm (Williamson-Hall plot) confirming the formation of nano-crystalline anatase. Furthermore, the synthesized anatase exhibited a higher degree of crystallinity at 67.21 % compared to the ICDD standard of 65.06 %. This enhanced crystallinity and other crystallographic data, confirm the successful synthesis of the highly crystalline anatase with improved properties compared to the standard material. The Z-average size of 342.05 nm indicates the hydrodynamic diameter and 63.05 mV zeta potential depicted excellent stability of synthesized anatase in colloidal. The TEM images revealed the uniform crystal growth and average crystallite size ranges in size 8.712 nm. The SAED pattern computed the high crystalline anatase diffracted in individual crystal planes as well as HR-TEM revealed d-spacing 0.3501 nm corresponding to the (101) planes and TEM couple EDS confirmed 100.0 % unified anatase crystal. This research advances the understanding of the controlled synthesis of anatase nanoparticles and demonstrates the effectiveness of characterizing their crystalline structure.</div></div>","PeriodicalId":101087,"journal":{"name":"Results in Materials","volume":"26 ","pages":"Article 100673"},"PeriodicalIF":0.0000,"publicationDate":"2025-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Results in Materials","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S2590048X25000184","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0

Abstract

High crystalline anatase synthesized by a unique simple route using titanium isopropoxide (TTIP) as precursor and isopropyl alcohol (IP) as peptizing agent. The Rietveld refinement analysis showed that the synthesized material is composed of 99.0 % anatase and 1.0 % brookite phases of titanium dioxide (TiO2). XRD characterized the prominent crystalline phase, providing insights into lattice parameters where a=b= 3.79068 Å, c= 9.50400 Å; α=β=γ= 90.0°; lattice strain 0.718, lattice volume 136.565 Å3, specific surface area 429.26 m2/g, dislocation density 0.0755 nm− 2, preference growth 0.119 and packing efficiency 70.09 %. The most intense diffraction was attributed to the (101) plane at 2θ = 25.39°. The average crystallite size through six identical models those were 3.64 nm (Scherrer equation), 6.47 nm (Williamson-Hall plot) confirming the formation of nano-crystalline anatase. Furthermore, the synthesized anatase exhibited a higher degree of crystallinity at 67.21 % compared to the ICDD standard of 65.06 %. This enhanced crystallinity and other crystallographic data, confirm the successful synthesis of the highly crystalline anatase with improved properties compared to the standard material. The Z-average size of 342.05 nm indicates the hydrodynamic diameter and 63.05 mV zeta potential depicted excellent stability of synthesized anatase in colloidal. The TEM images revealed the uniform crystal growth and average crystallite size ranges in size 8.712 nm. The SAED pattern computed the high crystalline anatase diffracted in individual crystal planes as well as HR-TEM revealed d-spacing 0.3501 nm corresponding to the (101) planes and TEM couple EDS confirmed 100.0 % unified anatase crystal. This research advances the understanding of the controlled synthesis of anatase nanoparticles and demonstrates the effectiveness of characterizing their crystalline structure.
用全粉末模式拟合(WPPF)方法整合锐钛矿(TiO2)纳米晶的结晶度:Rietveld细化研究
以异丙醇(IP)为助剂,异丙醇(TTIP)为前驱体,采用独特的简单工艺合成了高结晶锐钛矿。Rietveld细化分析表明,合成的材料由99.0%的锐钛矿相和1.0%的钛矿相组成。XRD表征了突出的晶相,提供了对晶格参数的深入了解,其中a=b= 3.79068 Å, c= 9.50400 Å;α=β=γ= 90.0°;晶格应变0.718,晶格体积136.565 Å3,比表面积429.26 m2/g,位错密度0.0755 nm - 2,偏好生长0.119,封装效率70.09%。衍射强度最大的是(101)平面在2θ = 25.39°。通过六个相同的模型,平均晶粒尺寸分别为3.64 nm (Scherrer方程)和6.47 nm (Williamson-Hall图),证实了纳米锐钛矿的形成。此外,合成的锐钛矿结晶度为67.21%,高于ICDD标准的65.06%。这种增强的结晶度和其他晶体学数据,证实了高结晶锐钛矿的成功合成,与标准材料相比,其性能得到了改善。z -平均尺寸为342.05 nm,表明该锐钛矿的水动力直径为342.05 nm, zeta电位为63.05 mV,表明该锐钛矿具有良好的胶体稳定性。TEM图像显示晶体生长均匀,平均晶粒尺寸为8.712 nm。SAED图计算出了在单个晶体平面上衍射的高结晶锐钛矿,HR-TEM显示出(101)平面对应的d间距为0.3501 nm, TEM对EDS证实了100.0%的统一锐钛矿晶体。本研究促进了对锐钛矿纳米颗粒控制合成的理解,并证明了表征其晶体结构的有效性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
求助全文
约1分钟内获得全文 求助全文
来源期刊
CiteScore
5.30
自引率
0.00%
发文量
0
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:604180095
Book学术官方微信