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Título: SOFT CHEMISTRY APPROACHES FOR SYNTHESIS OF LESS AGGLOMERATED A2M3O12 AND STRUCTURALLY RELATED CERAMIC PHASES
Autor: MAYARA GUILHERME MARZANO
Colaborador(es): BOJAN MARINKOVIC - Orientador
PATRICIA ISABEL PONTON BRAVO - Coorientador
Catalogação: 27/FEV/2023 Língua(s): ENGLISH - UNITED STATES
Tipo: TEXT Subtipo: THESIS
Notas: [pt] Todos os dados constantes dos documentos são de inteira responsabilidade de seus autores. Os dados utilizados nas descrições dos documentos estão em conformidade com os sistemas da administração da PUC-Rio.
[en] All data contained in the documents are the sole responsibility of the authors. The data used in the descriptions of the documents are in conformity with the systems of the administration of PUC-Rio.
Referência(s): [pt] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=61910&idi=1
[en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=61910&idi=2
DOI: https://doi.org/10.17771/PUCRio.acad.61910
Resumo:
The aim of this work was to synthesize Al2W3O12 and ZrMgMo3O12 submicronic powders using different soft-chemical routes, such as: co-precipitation and non-hydrolytic sol-gel (NHSG) to evaluate the effect of the methods on agglomeration degree of the as-prepared powders. Al2W3O12 was synthesized via co-precipitation, which includes i) simultaneously mixing reactants at room temperature, ii) simultaneously mixing reactants at 3.5 degrees C, iii) simultaneously mixing reactants with CTAB surfactant addition, and by non-hydrolytic sol-gel (NHSG). The purpose of each method was to study the effect of the synthesis parameters, such as, molarity (0.1 M and 0.005 M), calcination temperature on the morphology, size, and agglomeration of the powders, evaluated through specific surface areas. The best combination of synthesis parameters in both methods, coprecipitation, and NHSG, resulted in Al2W3O12 nanometric powders, with average primary particle sizes of 40 nm, and 45 nm, respectively. Al2W3O12 nanopowder, with high surface area (26 m2g-1), was prepared by the NHSG through a less laborious way than commonly reported in the literature for this type of ceramics. In addition, attempts to synthesize crystalline Al2W3O12 in one step by hydrothermal treatment at 180 degrees C have been performed, however, the desired phase did not crystallize. ZrMgMo3O12 was synthesized via co-precipitation by total evaporation route. The influence of the calcination parameters such as temperature and time of the synthesized powders were assessed. Even though different calcination temperatures were tested a completely monophasic powder was not fully attained by total evaporation route, presenting at least, 27 percent of secondary phases. Two additional different co-precipitation routes have been applied which include i) coprecipitation by simultaneously mixing reactants, ii) co-precipitation by dropwise addition of reactants and controlled pH at 9, however, both methods were unsuccessful since the desired phase was not crystallized.
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