Quantitative analysis of anatase-rutile mixtures of TiO2 employing X-ray diffractometry and visible-Raman spectroscopy at normal heating and superheating conditions- Implications and limitations of the Spurr-Mayers equation.
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| Title: | Quantitative analysis of anatase-rutile mixtures of TiO2 employing X-ray diffractometry and visible-Raman spectroscopy at normal heating and superheating conditions- Implications and limitations of the Spurr-Mayers equation. |
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| Authors: | Aswathappa, Sivakumar1 (AUTHOR), Dai, Lidong1 (AUTHOR) dailidong@vip.gyig.ac.cn, Sathiyadhas, Sahaya Jude Dhas2 (AUTHOR), Kumar, Raju Suresh3 (AUTHOR), Almansour, Abdulrahman I.3 (AUTHOR), Freire, P.T.C.4 (AUTHOR), Athiruban, Sakthisabarimoorthi5 (AUTHOR), Kang, Gyeongwon5 (AUTHOR) |
| Source: | Ceramics International. Dec2025:Part B, Vol. 51 Issue 29, p61025-61034. 10p. |
| Subjects: | Titanium dioxide, X-ray diffractometers, Photocatalysts, Raman spectroscopy, High temperatures, Equations |
| Abstract: | Titanium dioxide (TiO 2) is a multifunctional material that has been extensively studied, mainly because of its superior optical, electronic, and photocatalytic properties. Since the invention of the Spurr and Mayers equation (Spurr et al., Anal. Chem. 1957 , 29, 760–762), the proposed mathematical formulation based on the X-ray diffraction intensity ratio of anatase [ Int (101) A ] and rutile [ Int (110) R ] phases has been widely used to estimate the relative amounts of anatase (A) and rutile (R) in TiO 2 mixtures. However, our findings reveal that this formula is valid only under conventional (steady-state) heating conditions-assisted synthesis of AR-TiO 2 nanoparticles (NPs). It becomes unreliable when applied to AR-TiO 2 NPs synthesized under superheating conditions (e.g., unsteady-state involving acoustic shock waves). To support this claim, we present comparative XRD and Raman spectral results for AR-TiO 2 NPs synthesized under both normal heating and superheating conditions. The X-ray intensity ratio of (101) A /(110) R remains constant in the superheating samples; however, the Raman spectral results demonstrate significant changes occurring in the intensity ratio of the anatase (B 1g -399 cm−1) and rutile (A g -447 cm−1) TiO 2 NPs, which substantiates the changes occurring in the proportion of the anatase and rutile phases of AR-TiO 2. Based on these findings, it is authenticated that the Spurr-Mayers equation has significant limits in its ability to provide the precise ratio of the anatase and rutile proportion in superheating-based synthesis of AR-TiO 2 NPs. Its inaccuracy is attributed to the dominance of dynamic microstructure recrystallization processes and surface crystallographic changes, which were not accounted for in the original formulation. [ABSTRACT FROM AUTHOR] |
| Copyright of Ceramics International is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) | |
| Database: | Engineering Source |
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| Header | DbId: egs DbLabel: Engineering Source An: 189412854 AccessLevel: 6 PubType: Academic Journal PubTypeId: academicJournal PreciseRelevancyScore: 0 |
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| Items | – Name: Title Label: Title Group: Ti Data: Quantitative analysis of anatase-rutile mixtures of TiO2 employing X-ray diffractometry and visible-Raman spectroscopy at normal heating and superheating conditions- Implications and limitations of the Spurr-Mayers equation. – Name: Author Label: Authors Group: Au Data: <searchLink fieldCode="AR" term="%22Aswathappa%2C+Sivakumar%22">Aswathappa, Sivakumar</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Dai%2C+Lidong%22">Dai, Lidong</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> dailidong@vip.gyig.ac.cn</i><br /><searchLink fieldCode="AR" term="%22Sathiyadhas%2C+Sahaya+Jude+Dhas%22">Sathiyadhas, Sahaya Jude Dhas</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kumar%2C+Raju+Suresh%22">Kumar, Raju Suresh</searchLink><relatesTo>3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Almansour%2C+Abdulrahman+I%2E%22">Almansour, Abdulrahman I.</searchLink><relatesTo>3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Freire%2C+P%2ET%2EC%2E%22">Freire, P.T.C.</searchLink><relatesTo>4</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Athiruban%2C+Sakthisabarimoorthi%22">Athiruban, Sakthisabarimoorthi</searchLink><relatesTo>5</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kang%2C+Gyeongwon%22">Kang, Gyeongwon</searchLink><relatesTo>5</relatesTo> (AUTHOR) – Name: TitleSource Label: Source Group: Src Data: <searchLink fieldCode="JN" term="%22Ceramics+International%22">Ceramics International</searchLink>. Dec2025:Part B, Vol. 51 Issue 29, p61025-61034. 10p. – Name: Subject Label: Subjects Group: Su Data: <searchLink fieldCode="DE" term="%22Titanium+dioxide%22">Titanium dioxide</searchLink><br /><searchLink fieldCode="DE" term="%22X-ray+diffractometers%22">X-ray diffractometers</searchLink><br /><searchLink fieldCode="DE" term="%22Photocatalysts%22">Photocatalysts</searchLink><br /><searchLink fieldCode="DE" term="%22Raman+spectroscopy%22">Raman spectroscopy</searchLink><br /><searchLink fieldCode="DE" term="%22High+temperatures%22">High temperatures</searchLink><br /><searchLink fieldCode="DE" term="%22Equations%22">Equations</searchLink> – Name: Abstract Label: Abstract Group: Ab Data: Titanium dioxide (TiO 2) is a multifunctional material that has been extensively studied, mainly because of its superior optical, electronic, and photocatalytic properties. Since the invention of the Spurr and Mayers equation (Spurr et al., Anal. Chem. 1957 , 29, 760–762), the proposed mathematical formulation based on the X-ray diffraction intensity ratio of anatase [ Int (101) A ] and rutile [ Int (110) R ] phases has been widely used to estimate the relative amounts of anatase (A) and rutile (R) in TiO 2 mixtures. However, our findings reveal that this formula is valid only under conventional (steady-state) heating conditions-assisted synthesis of AR-TiO 2 nanoparticles (NPs). It becomes unreliable when applied to AR-TiO 2 NPs synthesized under superheating conditions (e.g., unsteady-state involving acoustic shock waves). To support this claim, we present comparative XRD and Raman spectral results for AR-TiO 2 NPs synthesized under both normal heating and superheating conditions. The X-ray intensity ratio of (101) A /(110) R remains constant in the superheating samples; however, the Raman spectral results demonstrate significant changes occurring in the intensity ratio of the anatase (B 1g -399 cm−1) and rutile (A g -447 cm−1) TiO 2 NPs, which substantiates the changes occurring in the proportion of the anatase and rutile phases of AR-TiO 2. Based on these findings, it is authenticated that the Spurr-Mayers equation has significant limits in its ability to provide the precise ratio of the anatase and rutile proportion in superheating-based synthesis of AR-TiO 2 NPs. Its inaccuracy is attributed to the dominance of dynamic microstructure recrystallization processes and surface crystallographic changes, which were not accounted for in the original formulation. [ABSTRACT FROM AUTHOR] – Name: AbstractSuppliedCopyright Label: Group: Ab Data: <i>Copyright of Ceramics International is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.) |
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| RecordInfo | BibRecord: BibEntity: Identifiers: – Type: doi Value: 10.1016/j.ceramint.2025.10.297 Languages: – Code: eng Text: English PhysicalDescription: Pagination: PageCount: 10 StartPage: 61025 Subjects: – SubjectFull: Titanium dioxide Type: general – SubjectFull: X-ray diffractometers Type: general – SubjectFull: Photocatalysts Type: general – SubjectFull: Raman spectroscopy Type: general – SubjectFull: High temperatures Type: general – SubjectFull: Equations Type: general Titles: – TitleFull: Quantitative analysis of anatase-rutile mixtures of TiO2 employing X-ray diffractometry and visible-Raman spectroscopy at normal heating and superheating conditions- Implications and limitations of the Spurr-Mayers equation. Type: main BibRelationships: HasContributorRelationships: – PersonEntity: Name: NameFull: Aswathappa, Sivakumar – PersonEntity: Name: NameFull: Dai, Lidong – PersonEntity: Name: NameFull: Sathiyadhas, Sahaya Jude Dhas – PersonEntity: Name: NameFull: Kumar, Raju Suresh – PersonEntity: Name: NameFull: Almansour, Abdulrahman I. – PersonEntity: Name: NameFull: Freire, P.T.C. – PersonEntity: Name: NameFull: Athiruban, Sakthisabarimoorthi – PersonEntity: Name: NameFull: Kang, Gyeongwon IsPartOfRelationships: – BibEntity: Dates: – D: 05 M: 12 Text: Dec2025:Part B Type: published Y: 2025 Identifiers: – Type: issn-print Value: 02728842 Numbering: – Type: volume Value: 51 – Type: issue Value: 29 Titles: – TitleFull: Ceramics International Type: main |
| ResultId | 1 |
