Título: | SOFT CHEMISTRY APPROACHES FOR SYNTHESIS OF LESS AGGLOMERATED A2M3O12 AND STRUCTURALLY RELATED CERAMIC PHASES | ||||||||||||
Autor: |
MAYARA GUILHERME MARZANO |
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Colaborador(es): |
BOJAN MARINKOVIC - Orientador PATRICIA ISABEL PONTON BRAVO - Coorientador |
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Catalogação: | 27/FEV/2023 | Língua(s): | ENGLISH - UNITED STATES |
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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. |
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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 |
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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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