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Master's Dissertation
DOI
https://doi.org/10.11606/D.46.2022.tde-01112023-181851
Document
Author
Full name
Elena Iraê Almeida Hummel Pimenta Santos
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2022
Supervisor
Committee
Vichi, Flavio Maron (President)
Polo, André Sarto
Gonçalves, Rogéria Rocha
Title in Portuguese
Síntese e caracterização de silicato de cádmio dopado com íons de metais de transição e ou Terras Raras para obtenção de materiais com luminescência persistente
Keywords in Portuguese
Luminescência persistente
Metassilicato de cádmio
Rotas sintéticas
Terras raras
Abstract in Portuguese
Materiais com luminescência persistente são materiais que emitem luz por longos períodos de tempo após cessada a excitação. Conhecer fatores que influenciam a luminescência, tanto na cor quanto no tempo de duração, são de extrema importância para ajustar esta propriedade conforme a aplicação. Assim, propôs-se a síntese de metassilicato de cádmio(CdSiO3) variando o método de síntese para estudo dos efeitos na luminescência. Os métodos foram precursor fundido, hidrotermal e sol-gel. Alterações nas condições de síntese foram conduzidas no pH e na temperatura de calcinação. Também foram conduzidas dopagens com manganês, praseodímio e térbio. Os materiais obtidos foram analisados por difratometria de raio X (DRX), adsorção de nitrogênio (BET). Espectros de emissão e excitação foram obtidos, assim como medidas de tempo de vida. Os materiais sintetizados no meio ácido foram obtidos e confirmados pela difratometria, enquanto no meio básico só foi possível a obtenção com boa pureza pelo método sol-gel a 800ºC. As amostras possuem uma variação de tamanho de cristalito entre 20-31 nm, com as amostras puras variando de 27-31 nm. As isotermas de adsorção de nitrogênio revelam uma maior área superficial para as amostras obtidas pelo método sol-gel, enquanto no método hidrotermal aparenta existir uma relação com a temperatura, possivelmente a formação de partículas maiores. Os espectros de emissão mostram cenários distintos para as amostras puras obtidas. A dopagem com manganês apresentou alterações no comprimento de onda da emissão, enquanto amostras com praseodímio apresentaram alterações na intensidade relativa de picos de transição, o que pode estar associado com alterações na rede cristalina devido às rotas sintéticas. As amostras com maior tempo de vida foram obtidas pelo método hidrotermal, seguido pelo sol-gel e por último precursor fundido. As de maior intensidade foram obtidas pelo método hidrotermal, a 800ºC.
Title in English
Synthesis and characterization of cadmium silicate doped with transition metal and/or Rare Earth ions to obtain materials with persistent luminescence
Keywords in English
Cadmium metasilicate
Persistent luminescence
Rare earth
Synthetic routes
Abstract in English
Materials with persistent luminescence are materials that emit light for long periods of time after the excitation is ceased. Knowing factors that influence luminescence, both in color and duration, are extremely important to adjust this property according to the application. Thus, to study the effects on luminescence the synthesis of cadmium metasilicate (CdSiO3) with different synthetic methods was proposed. The methods were molten precursor, hydrothermal and sol-gel. Changes in the synthesis conditions were carried out in the pH and calcination temperature. Dopings with manganese, praseodymium and terbium were also carried out. The resulting materials obtained were analyzed by X-ray diffraction (XRD), nitrogen adsorption (BET). Emission and excitation spectra were obtained, as well as lifetime measurements. Doped and undoped materials were obtained in acidic medium and confirmed by diffractometry, whereas in the basic medium it was only possible to obtain them with good purity by the sol-gel method at 800ºC. The samples have crystallite sizes varying between 20 and 31 nm, with non-doped samples ranging from 27-31 nm. Nitrogen adsorption shows samples with large surface area for those obtained by the sol-gel method, while in the hydrothermal method there appears to be a relationship with temperature, possibly due to precursor particle size. The emission spectra show different scenarios for undoped samples obtained, possibly due to the types of defects formed. Manganese doping leads to a shift in the emission wavelength, while samples with praseodymium showed changes in the relative intensity of transition peaks, which may be associated with changes in the crystal lattice due to synthetic pathways. The samples with the longest lifetime were obtained with the hydrothermal method, followed by sol-gel and finally the molten precursor method. The highest intensity was obtained by the hydrothermal method followed by calcination; at 800ºC.
 
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Publishing Date
2023-12-19
 
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