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Previous issue date: 2013-07-23 / Compounds of CoFe(2-x)YxO4, with 0 x 0.05, were synthesized by
combustion reaction. On the synthesis we used as oxidizing reagents, iron
nitrate Fe(NO3)3.9H2O, cobalt nitrate Co(NO3)2.6H2O, yttrium nitrate
Y(NO3)3.6H2O and as a fuel reducer, was used urea CO(NH2)2 with 300% in
excess. Post nanometric of cobalt ferrite in the spinel structure was obtained,
wich formed crystalline aggregates, with crystallite average size of 20 ± 3 nm.
The results of X-ray diffraction showed well defined diffraction peaks
characteristic of the pure phase CoFe2O4, not showing secondary phase for
all the compounds stoichiometries. The infrared spectra showed bands
characteristic of the metal and the oxygen bonds in the octahedral and
tetrahedral sites around 590-600 cm-1 and 400 cm-1 respectively, as well as,
shifting of the same to higher frequencies, also showed bands relating to
residual compounds bonds of the synthesis stage, that was eliminated during
the heating to obtain the thermograms. The thermograms showed the
material chemical stability and the residual compounds elimination and the
crystallization of the same starting at 400°C. The micrographs achieved
through transmission electron microscopy showed crystalline agglomerates
and using the program Image J. was possible to make 301 counts of the
particles diameters and to obtain a mean value for the sample x = ~ 1.5% of
18.58 nm, close to that obtained by the Scherrer equation, which for this
sample was ~19 nm. The scanning electron microscopy via Energy
Dispersive Spectrometer (EDS) was used to determine the chemical
composition of the experimental material, and along with the stoichiometric
calculate the values were tabulated. The data exposed in the table showed
an agreement with the calculated values whit the obtained. The magnetic
analysis revealed that the samples show the typical ferrimagnetism of the compound nature dependent of the Y3+ concentration. / Compostos de CoFe(2-x)YxO4, com 0 x 0,05, foram sintetizados por
reação de combustão. Na síntese foram empregados como reagentes
oxidantes; nitrato de ferro, Fe(NO3)3.9H2O, nitrato de cobalto
Co(NO3)2.6H2O, nitrato de ítrio Y(NO3)3.6H2O e como redutor, combustível,
foi usado uréia CO(NH2)2 com 300% em excesso. Pós nanométricos de
ferritas de cobalto na estrutura de espinélio foram obtidos, formaram
agregados cristalinos, com tamanho médio dos cristalitos de 20 ± 3 nm. Os
resultados de Difração de raios X mostraram os picos de difração bem
definidos característicos da fase de CoFe2O4 pura, não apresentando fase
secundária para todas as estequiometrias do composto. Os espectros de
infravermelho mostraram as bandas característica das ligações metal e
oxigênio nos sítios tetraédricos e octaédricos em torno 590-600 cm-1 e 400
cm-1 respectivamente, bem como deslocamento das mesmas para
freqüências maiores, apresentaram também bandas referente a ligações de
compostos residuais da etapa de síntese eliminados durante o aquecimento
para obtenção dos termogramas. Os termogramas mostraram a estabilidade
química do material, a eliminação de compostos residuais e a cristalização
do mesmo a partir de 400°C. As micrografias obtidas através da
microscopia eletrônica de transmissão mostraram aglomerados cristalinos e
através do programa Image J. foi obtido o valor médio dos diâmetros das
partículas para a amostra x=1,5% de ~19±6 nm, próximo ao obtido pela
equação de Scherrer, que para a referida amostra foi de ~19±3 nm. A
microscopia eletrônica de varredura através do Espectrômetro de Energia
Dispersiva (EDS) foi usado para determinar a composição química
experimental do material e juntamente com o calculado
estequiometricamente os valores foram tabelados. Os dados exposto na tabela mostraram uma concordância dos valores calculados com os obtidos.
As análises magnéticas revelaram que as amostras apresentam
ferrimagnetismo característico da natureza do composto dependente da
concentração de Y3+.
| Identifer | oai:union.ndltd.org:IBICT/oai:repositorio.bc.ufg.br:tede/3192 |
| Date | 23 July 2013 |
| Creators | Nascimento, Thaísa Cardoso |
| Contributors | Franco Júnior, Adolfo, Ruggiero, Marçal Antonio, Gomes, Danielle Cangussu de Castro |
| Publisher | Universidade Federal de Goiás, Programa de Pós-graduação em Química (IQ), UFG, Brasil, Instituto de Química - IQ (RG) |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | Portuguese |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/masterThesis |
| Format | application/pdf |
| Source | reponame:Biblioteca Digital de Teses e Dissertações da UFG, instname:Universidade Federal de Goiás, instacron:UFG |
| Rights | http://creativecommons.org/licenses/by-nc-nd/4.0/, info:eu-repo/semantics/openAccess |
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