Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)

Detalhes bibliográficos
Autor(a) principal: Carvalho, Emanoel Silva
Data de Publicação: 2021
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Repositório Institucional da UFS
Texto Completo: http://ri.ufs.br/jspui/handle/riufs/17260
Resumo: In this work, the structural properties of crystalline nanoparticles of pure and doped zinc oxide with different nominal concentrations of cerium, [Zn1-xCexO1-δ (x = 0,00, 0,03, 0,06, 0,10 and 0,15)], obtained through the microwave assisted hydrothermal synthesis route, are studied. Xray diffraction measurements, refinement by the Rietveld method and Raman spectroscopy were performed. The XRD analyzes indicate that the samples have good crystallinity, with all peaks allowed for the hexagonal wurtzite type structure of the space group P63mc and point group C4 6v. It was observed non-linear displacement of the diffraction peak (100) to lower angles caused by the increase of dopant in the ZnO matrix. Increase in the relative intensity of the peak (002) due to the increase in the size of the crystallite in the direction [001] and increase in the intensity of the peak (110) associated with the conditions of production of the samples. Increasing of the full width at half maximum of the peaks due to the increase amount of defects in the material. A secondary phase was found, at first, not identified in position 2θ≈34º. The profiles observed and calculated with the Rietveld refinement are in good fit and indicate that the material has a hexagonal wurtzite structure, confirming the results of the XRD. The density of the material increases from 5,7 g/cm3 to 6,1 g/cm3, the volume of the unit cell from 47,2 Å3 to 47,8 Å3, the parameters “a” from 3,24 Å to 3,25 Å and “c” from 5,19 Å to 5,21 Å and the normalized relative height of oxygen from 0,38 to 0,40 with the increase of cerium. The c/a factor remains 1.60 for all samples. The size of the crystallite increases from 30 nm to 31 nm for the sample with 3% cerium and decreases for the other samples staying close to 25 nm. The stress decreases for samples with 3% and 6% of cerium and increases for other samples. The secondary phase could not be identified with the Rietveld refinement. Raman spectrograms have vibration modes A1(TO), E1(TO), E2(H), A1(LO) and E1(LO) characteristic of the hexagonal structure of the wurtzite type. Present E2(H)-E2(L) and A1(LO)-E2(H) modes assigned to second-order Raman processes and a mode of approximately 205 cm-1 assigned to oxygen vacancies. Another vibrational mode was identified at 452 cm-1, 465,6 cm-1 and 453,5 cm-1 for samples with cerium doping with 6%, 10% and 15% respectively, attributed to the symmetric vibration of oxygen in around the cerium atoms identified as F2g mode characteristic of the cubic structure of the fluorite type belonging to cerium oxide crystals. The existence of this mode in these samples indicates that the ZnO matrix has a solubility limit due to the non-compatibility between the cerium and zinc atoms.
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spelling Carvalho, Emanoel SilvaFerreira, Nilson dos Santos2023-03-21T19:57:21Z2023-03-21T19:57:21Z2021-01-25CARVALHO, Emanoel Silva. Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15). 2021. 66 f. Dissertação (Mestrado em Física) – Universidade Federal de Sergipe, São Cristóvão, 2021.http://ri.ufs.br/jspui/handle/riufs/17260In this work, the structural properties of crystalline nanoparticles of pure and doped zinc oxide with different nominal concentrations of cerium, [Zn1-xCexO1-δ (x = 0,00, 0,03, 0,06, 0,10 and 0,15)], obtained through the microwave assisted hydrothermal synthesis route, are studied. Xray diffraction measurements, refinement by the Rietveld method and Raman spectroscopy were performed. The XRD analyzes indicate that the samples have good crystallinity, with all peaks allowed for the hexagonal wurtzite type structure of the space group P63mc and point group C4 6v. It was observed non-linear displacement of the diffraction peak (100) to lower angles caused by the increase of dopant in the ZnO matrix. Increase in the relative intensity of the peak (002) due to the increase in the size of the crystallite in the direction [001] and increase in the intensity of the peak (110) associated with the conditions of production of the samples. Increasing of the full width at half maximum of the peaks due to the increase amount of defects in the material. A secondary phase was found, at first, not identified in position 2θ≈34º. The profiles observed and calculated with the Rietveld refinement are in good fit and indicate that the material has a hexagonal wurtzite structure, confirming the results of the XRD. The density of the material increases from 5,7 g/cm3 to 6,1 g/cm3, the volume of the unit cell from 47,2 Å3 to 47,8 Å3, the parameters “a” from 3,24 Å to 3,25 Å and “c” from 5,19 Å to 5,21 Å and the normalized relative height of oxygen from 0,38 to 0,40 with the increase of cerium. The c/a factor remains 1.60 for all samples. The size of the crystallite increases from 30 nm to 31 nm for the sample with 3% cerium and decreases for the other samples staying close to 25 nm. The stress decreases for samples with 3% and 6% of cerium and increases for other samples. The secondary phase could not be identified with the Rietveld refinement. Raman spectrograms have vibration modes A1(TO), E1(TO), E2(H), A1(LO) and E1(LO) characteristic of the hexagonal structure of the wurtzite type. Present E2(H)-E2(L) and A1(LO)-E2(H) modes assigned to second-order Raman processes and a mode of approximately 205 cm-1 assigned to oxygen vacancies. Another vibrational mode was identified at 452 cm-1, 465,6 cm-1 and 453,5 cm-1 for samples with cerium doping with 6%, 10% and 15% respectively, attributed to the symmetric vibration of oxygen in around the cerium atoms identified as F2g mode characteristic of the cubic structure of the fluorite type belonging to cerium oxide crystals. The existence of this mode in these samples indicates that the ZnO matrix has a solubility limit due to the non-compatibility between the cerium and zinc atoms.Neste trabalho são estudadas as propriedades estruturais de nanopartículas cristalinas de óxido de zinco puro e dopado com diferentes concentrações nominais de cério, [Zn1-xCexO1-δ (x= 0,00, 0,03, 0,06, 0,10 e 0,15)], obtidas através da rota de síntese hidrotermal assistida por micro-ondas. Foram realizadas medidas de difratômetria de raios-X, refinamento pelo método de Rietveld e espectroscopia Raman. As análises de DRX indicam que as amostras possuem boa cristalinidade, com todos os picos permitidos para a estrutura hexagonal do tipo wurtzita do grupo espacial P63mc e grupo pontual C4 6v. Foi observado deslocamento não linear do pico de difração (100) para ângulos mais baixos, provocado pelo incremento de dopante na matriz de ZnO. Aumento da intensidade relativa do pico (002) devido ao aumento do tamanho do cristalito na direção [001] e aumento da intensidade do pico (110) associado às condições de produção das amostras. Aumento da largura à meia altura máxima dos picos devido ao aumento da quantidade de defeitos no material. Foi encontrada ainda uma fase secundária inicialmente não identificada, na posição 2θ≈34º. Os perfis observados e calculados com o refinamento Rietveld estão em bom ajuste e indicam que o material possui estrutura hexagonal tipo wurtzita confirmando os resultados do DRX. A densidade do material aumenta de 5,7 g/cm3 para 6,1 g/cm3, o volume da célula unitária de 47,2 Å3 para 47,8 Å3, os parâmetros de rede “a” de 3,24 Å para 3,25 Å e “c” de 5,19 Å para 5,21 Å e a altura relativa normalizada do oxigênio de 0,38 para 0,40 com o incremento de cério. O fator c/a permanece 1,60 para todas as amostras. O tamanho do cristalito aumenta de 30 nm para 31 nm para a amostra com 3% de cério e diminui para as outras amostras ficando próximo de 25 nm. O estresse de rede diminui para as amostras com 3% e 6% de cério e aumenta para as outras amostras. A fase secundária não pôde ser identificada com o refinamento Rietveld. Os espectrogramas Raman apresentam modos os de vibração A1(TO), E1(TO), E2(H), A1(LO) e E1(LO) característicos da estrutura hexagonal do tipo wurtzita. Apresenta os modos E2(H)- E2(L) e A1(LO)-E2(H) atribuídos a processos Raman de segunda ordem e um modo em aproximadamente 205 cm-1 atribuído a vacâncias de oxigênio. Foi identificado ainda outro modo vibracional em 452 cm-1, 465,6 cm-1 e 453,5 cm-1 para as amostras com dopagem de cério com 6%, 10% e 15% respectivamente, atribuído à vibração simétrica do oxigênio em torno dos átomos de cério, identificado como modo F2g característico da estrutura cúbica do tipo fluorita pertencente a cristais de óxido de cério. A existência desse modo nessas amostras indica que a matriz de ZnO possui um limite de solubilidade devido à não compatibilidade entre os átomos de cério e zinco.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão CristóvãoporPropriedades estruturaisNanopartículasÓxido de zincoDopagemCérioStructural propertiesNanoparticlesZinc oxideDopingCeriumCIENCIAS EXATAS E DA TERRA::FISICAEstudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPós-Graduação em FísicaUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/17260/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALEMANOEL_SILVA_CARVALHO.pdfEMANOEL_SILVA_CARVALHO.pdfapplication/pdf2929353https://ri.ufs.br/jspui/bitstream/riufs/17260/2/EMANOEL_SILVA_CARVALHO.pdf4950763af8bea7df7b60eb548cd3b1bdMD52TEXTEMANOEL_SILVA_CARVALHO.pdf.txtEMANOEL_SILVA_CARVALHO.pdf.txtExtracted texttext/plain108912https://ri.ufs.br/jspui/bitstream/riufs/17260/3/EMANOEL_SILVA_CARVALHO.pdf.txtbe502fb3e94aa25df8f1b692617534cbMD53THUMBNAILEMANOEL_SILVA_CARVALHO.pdf.jpgEMANOEL_SILVA_CARVALHO.pdf.jpgGenerated Thumbnailimage/jpeg1227https://ri.ufs.br/jspui/bitstream/riufs/17260/4/EMANOEL_SILVA_CARVALHO.pdf.jpgfaea00c38f610060b109747b90fedbfaMD54riufs/172602023-03-21 16:57:21.84oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2023-03-21T19:57:21Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false
dc.title.pt_BR.fl_str_mv Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
title Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
spellingShingle Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
Carvalho, Emanoel Silva
Propriedades estruturais
Nanopartículas
Óxido de zinco
Dopagem
Cério
Structural properties
Nanoparticles
Zinc oxide
Doping
Cerium
CIENCIAS EXATAS E DA TERRA::FISICA
title_short Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
title_full Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
title_fullStr Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
title_full_unstemmed Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
title_sort Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15)
author Carvalho, Emanoel Silva
author_facet Carvalho, Emanoel Silva
author_role author
dc.contributor.author.fl_str_mv Carvalho, Emanoel Silva
dc.contributor.advisor1.fl_str_mv Ferreira, Nilson dos Santos
contributor_str_mv Ferreira, Nilson dos Santos
dc.subject.por.fl_str_mv Propriedades estruturais
Nanopartículas
Óxido de zinco
Dopagem
Cério
topic Propriedades estruturais
Nanopartículas
Óxido de zinco
Dopagem
Cério
Structural properties
Nanoparticles
Zinc oxide
Doping
Cerium
CIENCIAS EXATAS E DA TERRA::FISICA
dc.subject.eng.fl_str_mv Structural properties
Nanoparticles
Zinc oxide
Doping
Cerium
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::FISICA
description In this work, the structural properties of crystalline nanoparticles of pure and doped zinc oxide with different nominal concentrations of cerium, [Zn1-xCexO1-δ (x = 0,00, 0,03, 0,06, 0,10 and 0,15)], obtained through the microwave assisted hydrothermal synthesis route, are studied. Xray diffraction measurements, refinement by the Rietveld method and Raman spectroscopy were performed. The XRD analyzes indicate that the samples have good crystallinity, with all peaks allowed for the hexagonal wurtzite type structure of the space group P63mc and point group C4 6v. It was observed non-linear displacement of the diffraction peak (100) to lower angles caused by the increase of dopant in the ZnO matrix. Increase in the relative intensity of the peak (002) due to the increase in the size of the crystallite in the direction [001] and increase in the intensity of the peak (110) associated with the conditions of production of the samples. Increasing of the full width at half maximum of the peaks due to the increase amount of defects in the material. A secondary phase was found, at first, not identified in position 2θ≈34º. The profiles observed and calculated with the Rietveld refinement are in good fit and indicate that the material has a hexagonal wurtzite structure, confirming the results of the XRD. The density of the material increases from 5,7 g/cm3 to 6,1 g/cm3, the volume of the unit cell from 47,2 Å3 to 47,8 Å3, the parameters “a” from 3,24 Å to 3,25 Å and “c” from 5,19 Å to 5,21 Å and the normalized relative height of oxygen from 0,38 to 0,40 with the increase of cerium. The c/a factor remains 1.60 for all samples. The size of the crystallite increases from 30 nm to 31 nm for the sample with 3% cerium and decreases for the other samples staying close to 25 nm. The stress decreases for samples with 3% and 6% of cerium and increases for other samples. The secondary phase could not be identified with the Rietveld refinement. Raman spectrograms have vibration modes A1(TO), E1(TO), E2(H), A1(LO) and E1(LO) characteristic of the hexagonal structure of the wurtzite type. Present E2(H)-E2(L) and A1(LO)-E2(H) modes assigned to second-order Raman processes and a mode of approximately 205 cm-1 assigned to oxygen vacancies. Another vibrational mode was identified at 452 cm-1, 465,6 cm-1 and 453,5 cm-1 for samples with cerium doping with 6%, 10% and 15% respectively, attributed to the symmetric vibration of oxygen in around the cerium atoms identified as F2g mode characteristic of the cubic structure of the fluorite type belonging to cerium oxide crystals. The existence of this mode in these samples indicates that the ZnO matrix has a solubility limit due to the non-compatibility between the cerium and zinc atoms.
publishDate 2021
dc.date.issued.fl_str_mv 2021-01-25
dc.date.accessioned.fl_str_mv 2023-03-21T19:57:21Z
dc.date.available.fl_str_mv 2023-03-21T19:57:21Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
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dc.identifier.citation.fl_str_mv CARVALHO, Emanoel Silva. Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15). 2021. 66 f. Dissertação (Mestrado em Física) – Universidade Federal de Sergipe, São Cristóvão, 2021.
dc.identifier.uri.fl_str_mv http://ri.ufs.br/jspui/handle/riufs/17260
identifier_str_mv CARVALHO, Emanoel Silva. Estudo das propriedades estruturais de nanopartículas de Zn1-xCexO1-δ (0≤x≤0,15). 2021. 66 f. Dissertação (Mestrado em Física) – Universidade Federal de Sergipe, São Cristóvão, 2021.
url http://ri.ufs.br/jspui/handle/riufs/17260
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