Propriedades estruturais e controle da estequiometria de filmes finos de BiFeO3
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Data
2019-08-09
Autores
Sena, Wellington Adriano Fernandes
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Universidade Estadual Paulista (Unesp)
Resumo
O objetivo do trabalho foi estudar as propriedades estruturais dos filmes finos de ferrita de bismuto (BFO) ao se adicionar excesso de nitrato de ferro ao invés de nitrato de bismuto conforme muitas referências na literatura vêm praticando com a intenção de obter um BFO puro. Filmes finos de BFO foram preparados sobre substratos Pt/TiO2/SiO2/Si(100) usando o método de Pechini pertencente a rota química sol-gel polimérica. Foram produzidos filmes de estequiometria nominal e de variação de 2, 4, 6, 8, 10 e 12 mol% de excesso de nitrato de Ferro. O processo de síntese dos filmes passou por quatro deposições, quatro pirólises a 300 ºC por 20 minutos e cristalização a 600 ºC por 40 minutos. As propriedades físicas dos filmes foram investigadas usando técnicas de MEV, DRX, Raman e EDS. Rietveld foi usado para calcular os parâmetros de rede e o modelo de Williamson-Hall foi usado para calcular o tamanho do cristalito e o microstrain. Resultados do DRX revelaram o aparecimento da fase secundária Bi2O3, ela aparece quando há o excesso de bismuto. Resultados do EDS confirmam o excesso de Bi. A técnica de EDS apontou uma maior At% do bismuto em relação ao ferro em todas as amostras, sendo que, a de 12 mol% foi a que apresentou características mais próxima de uma estequiometria desejável para a produção de um BFO puro.
The objective of this work was to study the structural properties of bismuth ferrite (BFO) thin films by adding excess iron nitrate instead of bismuth nitrate as many references in the literature have been practicing with the intention of obtaining a pure BFO. BFO thin films were prepared on Pt / TiO2 / SiO2 / Si (100) substrates using the Pechini method belonging to the polymeric sol-gel chemical route. Films of nominal stoichiometry and variation of 2, 4, 6, 8, 10 and 12 mol% of iron nitrate excess were produced. The synthesis process of the films went through four depositions, four pyrolysis at 300 ºC for 20 minutes and crystallization at 600 ºC for 40 minutes. The physical properties of the films were investigated using SEM, XRD, Raman and EDS techniques. Rietveld was used to calculate lattice parameters and the Williamson-Hall model was used to calculate crystallite size and microstrain. XRD results revealed the appearance of the secondary phase Bi2O3, it appears when there is excess bismuth. EDS results confirm excess Bi. The EDS technique showed a higher At% of bismuth in relation to iron in all samples, and the 12 mol% was the one that presented characteristics closer to a desirable stoichiometry for the production of a pure BFO.
The objective of this work was to study the structural properties of bismuth ferrite (BFO) thin films by adding excess iron nitrate instead of bismuth nitrate as many references in the literature have been practicing with the intention of obtaining a pure BFO. BFO thin films were prepared on Pt / TiO2 / SiO2 / Si (100) substrates using the Pechini method belonging to the polymeric sol-gel chemical route. Films of nominal stoichiometry and variation of 2, 4, 6, 8, 10 and 12 mol% of iron nitrate excess were produced. The synthesis process of the films went through four depositions, four pyrolysis at 300 ºC for 20 minutes and crystallization at 600 ºC for 40 minutes. The physical properties of the films were investigated using SEM, XRD, Raman and EDS techniques. Rietveld was used to calculate lattice parameters and the Williamson-Hall model was used to calculate crystallite size and microstrain. XRD results revealed the appearance of the secondary phase Bi2O3, it appears when there is excess bismuth. EDS results confirm excess Bi. The EDS technique showed a higher At% of bismuth in relation to iron in all samples, and the 12 mol% was the one that presented characteristics closer to a desirable stoichiometry for the production of a pure BFO.
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Palavras-chave
Filmes finos, Ferrita de bismuto, Fases secundárias, Thin films, Bismuth ferrite, Secondary phases