Fine Characterization of Co/Fe-Based Materials: Insights into the Influence of Cation Ratios Between 2/2 and 10/2 on Obtaining Layered Double Hydroxides.
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| Title: | Fine Characterization of Co/Fe-Based Materials: Insights into the Influence of Cation Ratios Between 2/2 and 10/2 on Obtaining Layered Double Hydroxides. |
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| Authors: | Abi Khalil, Almaza1,2 (AUTHOR), Betelu, Stéphanie1,2 (AUTHOR) n.maubec@brgm.fr, Delpeux, Sandrine2,3 (AUTHOR), Bouillet, Corinne3 (AUTHOR), Maubec, Nicolas1 (AUTHOR), Muller, Fabrice2 (AUTHOR), Seron, Alain1 (AUTHOR) a.seron@brgm.fr |
| Source: | Materials (1996-1944). Mar2026, Vol. 19 Issue 5, p838. 28p. |
| Subjects: | Layered double hydroxides, Rietveld refinement, Metal ions, Stoichiometry, Crystallinity, Materials analysis, Scientific method, Chemical synthesis |
| Abstract: | Co/Fe layered double hydroxides (LDHs) are among the most promising materials for advanced industrial and energy applications. Controlling the synthesis conditions of LDH materials is thus crucial to precisely tailoring cation composition and distribution, thereby regulating surface charge, ion sorption, and electron transfer required for optimal chemical and electrochemical performance. Therefore, characterizing Co/Fe precipitates (chemical composition, purity, morphology, and crystallinity) is also required to further exploit their controlled properties. Thus, solids with Co/Fe cation ratios between 2/2 and 10/2 were synthesized under an air atmosphere, at pH 8 or 11.5. For the first time, multiscale physicochemical techniques (FTIR, TEM-EELS, SEM, AAS, TGA, CHN elemental analysis, and XRD complemented by Rietveld refinement) were used to provide a fully documented characterization of the structure, texture, purity, chemical composition, and thermal properties of Co/Fe LDH-based materials. The combined interpretation of data from these complementary techniques enabled the precise identification and chemical characterization of the mineralogical phases formed. Both acid–base and redox reactions govern the overall CoII/FeIII LDH formation process. Well-crystallized LDHs were synthesized, except for the 2/2 ratio at pH 11.5, which led to the formation of α-Co(OH)2, γ-Fe2O3, and Co3O4 byproducts. A pH value of 8.0 provides valuable LDH materials made of quasi-hexagonal particles with diagonal lengths between 200 and 500 nm. Rietveld refining showed the presence of LDH phases in the range of 95–98%. Multiple local chemical analyses using EDX on chosen particles demonstrated pure 4/2 and 6/2 LDHs. For the 2/2 ratio, the cumulative mass fraction of two LDH-type products consistently reached 97%, distributed between Co/Fe 1.5/2 (71%) and Co/Fe 4/2 (29%). For the 10/2 ratio, only partial Co precipitation was observed, forming 95% Co/Fe LDH phases distributed between Co/Fe 10/2 (72%) and 7/2 (28%). [ABSTRACT FROM AUTHOR] |
| Copyright of Materials (1996-1944) is the property of MDPI 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.) | |
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| Header | DbId: egs DbLabel: Engineering Source An: 192640110 AccessLevel: 6 PubType: Academic Journal PubTypeId: academicJournal PreciseRelevancyScore: 0 |
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| Items | – Name: Title Label: Title Group: Ti Data: Fine Characterization of Co/Fe-Based Materials: Insights into the Influence of Cation Ratios Between 2/2 and 10/2 on Obtaining Layered Double Hydroxides. – Name: Author Label: Authors Group: Au Data: <searchLink fieldCode="AR" term="%22Abi+Khalil%2C+Almaza%22">Abi Khalil, Almaza</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Betelu%2C+Stéphanie%22">Betelu, Stéphanie</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<i> n.maubec@brgm.fr</i><br /><searchLink fieldCode="AR" term="%22Delpeux%2C+Sandrine%22">Delpeux, Sandrine</searchLink><relatesTo>2,3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Bouillet%2C+Corinne%22">Bouillet, Corinne</searchLink><relatesTo>3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Maubec%2C+Nicolas%22">Maubec, Nicolas</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Muller%2C+Fabrice%22">Muller, Fabrice</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Seron%2C+Alain%22">Seron, Alain</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> a.seron@brgm.fr</i> – Name: TitleSource Label: Source Group: Src Data: <searchLink fieldCode="JN" term="%22Materials+%281996-1944%29%22">Materials (1996-1944)</searchLink>. Mar2026, Vol. 19 Issue 5, p838. 28p. – Name: Subject Label: Subjects Group: Su Data: <searchLink fieldCode="DE" term="%22Layered+double+hydroxides%22">Layered double hydroxides</searchLink><br /><searchLink fieldCode="DE" term="%22Rietveld+refinement%22">Rietveld refinement</searchLink><br /><searchLink fieldCode="DE" term="%22Metal+ions%22">Metal ions</searchLink><br /><searchLink fieldCode="DE" term="%22Stoichiometry%22">Stoichiometry</searchLink><br /><searchLink fieldCode="DE" term="%22Crystallinity%22">Crystallinity</searchLink><br /><searchLink fieldCode="DE" term="%22Materials+analysis%22">Materials analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Scientific+method%22">Scientific method</searchLink><br /><searchLink fieldCode="DE" term="%22Chemical+synthesis%22">Chemical synthesis</searchLink> – Name: Abstract Label: Abstract Group: Ab Data: Co/Fe layered double hydroxides (LDHs) are among the most promising materials for advanced industrial and energy applications. Controlling the synthesis conditions of LDH materials is thus crucial to precisely tailoring cation composition and distribution, thereby regulating surface charge, ion sorption, and electron transfer required for optimal chemical and electrochemical performance. Therefore, characterizing Co/Fe precipitates (chemical composition, purity, morphology, and crystallinity) is also required to further exploit their controlled properties. Thus, solids with Co/Fe cation ratios between 2/2 and 10/2 were synthesized under an air atmosphere, at pH 8 or 11.5. For the first time, multiscale physicochemical techniques (FTIR, TEM-EELS, SEM, AAS, TGA, CHN elemental analysis, and XRD complemented by Rietveld refinement) were used to provide a fully documented characterization of the structure, texture, purity, chemical composition, and thermal properties of Co/Fe LDH-based materials. The combined interpretation of data from these complementary techniques enabled the precise identification and chemical characterization of the mineralogical phases formed. Both acid–base and redox reactions govern the overall CoII/FeIII LDH formation process. Well-crystallized LDHs were synthesized, except for the 2/2 ratio at pH 11.5, which led to the formation of α-Co(OH)2, γ-Fe2O3, and Co3O4 byproducts. A pH value of 8.0 provides valuable LDH materials made of quasi-hexagonal particles with diagonal lengths between 200 and 500 nm. Rietveld refining showed the presence of LDH phases in the range of 95–98%. Multiple local chemical analyses using EDX on chosen particles demonstrated pure 4/2 and 6/2 LDHs. For the 2/2 ratio, the cumulative mass fraction of two LDH-type products consistently reached 97%, distributed between Co/Fe 1.5/2 (71%) and Co/Fe 4/2 (29%). For the 10/2 ratio, only partial Co precipitation was observed, forming 95% Co/Fe LDH phases distributed between Co/Fe 10/2 (72%) and 7/2 (28%). [ABSTRACT FROM AUTHOR] – Name: AbstractSuppliedCopyright Label: Group: Ab Data: <i>Copyright of Materials (1996-1944) is the property of MDPI 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: 10.3390/ma19050838 Languages: – Code: eng Text: English PhysicalDescription: Pagination: PageCount: 28 StartPage: 838 Subjects: – SubjectFull: Layered double hydroxides Type: general – SubjectFull: Rietveld refinement Type: general – SubjectFull: Metal ions Type: general – SubjectFull: Stoichiometry Type: general – SubjectFull: Crystallinity Type: general – SubjectFull: Materials analysis Type: general – SubjectFull: Scientific method Type: general – SubjectFull: Chemical synthesis Type: general Titles: – TitleFull: Fine Characterization of Co/Fe-Based Materials: Insights into the Influence of Cation Ratios Between 2/2 and 10/2 on Obtaining Layered Double Hydroxides. Type: main BibRelationships: HasContributorRelationships: – PersonEntity: Name: NameFull: Abi Khalil, Almaza – PersonEntity: Name: NameFull: Betelu, Stéphanie – PersonEntity: Name: NameFull: Delpeux, Sandrine – PersonEntity: Name: NameFull: Bouillet, Corinne – PersonEntity: Name: NameFull: Maubec, Nicolas – PersonEntity: Name: NameFull: Muller, Fabrice – PersonEntity: Name: NameFull: Seron, Alain IsPartOfRelationships: – BibEntity: Dates: – D: 01 M: 03 Text: Mar2026 Type: published Y: 2026 Identifiers: – Type: issn-print Value: 19961944 Numbering: – Type: volume Value: 19 – Type: issue Value: 5 Titles: – TitleFull: Materials (1996-1944) Type: main |
| ResultId | 1 |
