Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions

In this project, a method was developed to synthesize ammoniacal niobium oxalate (NH4)(NbO(C2O4)(H2O)ᵧ)·XH2O, aimed at its application in the preparation of niobium-incorporated materials. This transition metal exhibits excellent properties and is widely available in Brazil. Its versatility makes it...

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Main Authors: Vitor Manoel Silva Fernandes de Souza, Vinícius Gomes de Sousa Duarte, Kivia Fabiana Galvão Araújo, Maria José dos Santos Lima, Gerlânea Silva Oliveira, Sibele Berenice Castella Pergher, Uilame Umbelino Gomes
Format: Article
Language:English
Published: Associação Brasileira de Metalurgia e Materiais (ABM); Associação Brasileira de Cerâmica (ABC); Associação Brasileira de Polímeros (ABPol) 2025-08-01
Series:Materials Research
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Online Access:http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392025000200294&tlng=en
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author Vitor Manoel Silva Fernandes de Souza
Vinícius Gomes de Sousa Duarte
Kivia Fabiana Galvão Araújo
Maria José dos Santos Lima
Gerlânea Silva Oliveira
Sibele Berenice Castella Pergher
Uilame Umbelino Gomes
author_facet Vitor Manoel Silva Fernandes de Souza
Vinícius Gomes de Sousa Duarte
Kivia Fabiana Galvão Araújo
Maria José dos Santos Lima
Gerlânea Silva Oliveira
Sibele Berenice Castella Pergher
Uilame Umbelino Gomes
author_sort Vitor Manoel Silva Fernandes de Souza
collection DOAJ
description In this project, a method was developed to synthesize ammoniacal niobium oxalate (NH4)(NbO(C2O4)(H2O)ᵧ)·XH2O, aimed at its application in the preparation of niobium-incorporated materials. This transition metal exhibits excellent properties and is widely available in Brazil. Its versatility makes it essential for metal alloys and electronic components. The synthesis was based on physical and chemical processes, including fusion, decantation, filtration, and complexation, using niobium pentoxide and potassium bisulfate. Rigorous procedures were implemented to ensure precursor quality. Material characterization was performed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and thermogravimetric analysis (TGA), which collectively confirmed the material's morphology, structure, and thermal stability. The results confirmed the efficient synthesis of high-purity niobium oxalate, with the developed method demonstrating technical feasibility by preserving the material's essential physicochemical properties, as verified by the characterization techniques. Key innovations included replacing acid leaching with a more efficient method, implementing neutral-pH decantation instead of traditional acidic processes, and the strategic use of an aqueous acetic acid solution in the washing step. This combination of advancements enabled a 75% reduction in water consumption during the washing stage, thus establishing a significantly more sustainable synthesis protocol for producing this precursor without compromising final product quality.
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institution Kabale University
issn 1516-1439
language English
publishDate 2025-08-01
publisher Associação Brasileira de Metalurgia e Materiais (ABM); Associação Brasileira de Cerâmica (ABC); Associação Brasileira de Polímeros (ABPol)
record_format Article
series Materials Research
spelling doaj-art-d58ad2ea31e14f96bc96acbb25bfd90e2025-08-26T07:45:26ZengAssociação Brasileira de Metalurgia e Materiais (ABM); Associação Brasileira de Cerâmica (ABC); Associação Brasileira de Polímeros (ABPol)Materials Research1516-14392025-08-0128suppl 110.1590/1980-5373-mr-2025-0210Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical ReactionsVitor Manoel Silva Fernandes de Souzahttps://orcid.org/0009-0000-1496-4853Vinícius Gomes de Sousa DuarteKivia Fabiana Galvão Araújohttps://orcid.org/0000-0002-7197-2582Maria José dos Santos Limahttps://orcid.org/0000-0001-8957-9204Gerlânea Silva OliveiraSibele Berenice Castella PergherUilame Umbelino GomesIn this project, a method was developed to synthesize ammoniacal niobium oxalate (NH4)(NbO(C2O4)(H2O)ᵧ)·XH2O, aimed at its application in the preparation of niobium-incorporated materials. This transition metal exhibits excellent properties and is widely available in Brazil. Its versatility makes it essential for metal alloys and electronic components. The synthesis was based on physical and chemical processes, including fusion, decantation, filtration, and complexation, using niobium pentoxide and potassium bisulfate. Rigorous procedures were implemented to ensure precursor quality. Material characterization was performed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and thermogravimetric analysis (TGA), which collectively confirmed the material's morphology, structure, and thermal stability. The results confirmed the efficient synthesis of high-purity niobium oxalate, with the developed method demonstrating technical feasibility by preserving the material's essential physicochemical properties, as verified by the characterization techniques. Key innovations included replacing acid leaching with a more efficient method, implementing neutral-pH decantation instead of traditional acidic processes, and the strategic use of an aqueous acetic acid solution in the washing step. This combination of advancements enabled a 75% reduction in water consumption during the washing stage, thus establishing a significantly more sustainable synthesis protocol for producing this precursor without compromising final product quality.http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392025000200294&tlng=enSynthesisAmmonium Niobium Oxalate TrihydrateNiobiumPrecursor
spellingShingle Vitor Manoel Silva Fernandes de Souza
Vinícius Gomes de Sousa Duarte
Kivia Fabiana Galvão Araújo
Maria José dos Santos Lima
Gerlânea Silva Oliveira
Sibele Berenice Castella Pergher
Uilame Umbelino Gomes
Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
Materials Research
Synthesis
Ammonium Niobium Oxalate Trihydrate
Niobium
Precursor
title Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
title_full Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
title_fullStr Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
title_full_unstemmed Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
title_short Development of a Method for the Synthesis of Ammoniacal Niobium Oxalate Trihydrate for Use as a Precursor in Chemical Reactions
title_sort development of a method for the synthesis of ammoniacal niobium oxalate trihydrate for use as a precursor in chemical reactions
topic Synthesis
Ammonium Niobium Oxalate Trihydrate
Niobium
Precursor
url http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14392025000200294&tlng=en
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