Orientador: Celio Pasquini / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-08T16:03:21Z (GMT). No. of bitstreams: 1 Cortez_Juliana_M.pdf: 4343113 bytes, checksum: d1746c525a8d51ede4e8432a525eecf2 (MD5) Previous issue date: 2007 / Resumo: Neste trabalho um instrumento LIBS com resolução temporal (TRELIBS) foi construído e seu desempenho foi avaliado para análise qualitativa e quantitativa. Além disso, este trabalho apresenta estudos exploratórios acerca da influência de parâmetros que afetam as análises em LIBS. O instrumento foi montado empregando-se óptica e sistema de detecção de última geração: um detector ICCD, um policromador echelle e um laser Q-switched de Nd:YAG. Três configurações do sistema LIBS foram avaliadas. No último arranjo do sistema, o pulso de laser era refletido por um espelho dicróico à 45º para uma lente de distância focal de 25 cm que focava o pulso de laser na superfície da amostra. A radiação foi coletada por uma lente de curta distância focal e depois enviada para o echelle, por uma fibra óptica, e posteriormente para o ICCD. Na análise qualitativa foram avaliados os espectros de uma placa de cobre e zinco, obtendo-se espectros condizentes com a literatura, de acordo com a resolução do echelle. Na avaliação quantitativa, determinou-se manganês em aços acalmados. O sistema apresentou resposta às diferentes concentrações de manganês em 293,30 nm e curvas analíticas foram obtidas. A energia do pulso de laser mostrou ser um fator determinante no desempenho da análise quantitativa. Outros parâmetros como tempo de integração do sinal, tempo de atraso, ganho do MCP, co-adição de pulsos e distância foco-amostra também mostraram ter influência na análise quantitativa. Imagens de MEV e mapeamentos de EDS das crateras formadas pelo laser foram ferramentas importantes para o entendimento do processo de interação laser-amostra-atmosfera / Abstract: In this work a time resolved LIBS instrument (TRELIBS) was built and its performance evaluated in qualitative and quantitative analysis. Additionally, exploratory studies are presented on the influence of parameters that affect the LIBS analysis. The instrument was built employing optical systems and devices of modern technology: an ICCD device, an echelle polychromator and an Q-switched Nd:YAG laser. Three configurations of LIBS system were evaluated. In the last configuration, the laser pulse was reflected by a dicroic mirror at 45º to a lens of 25 cm focal distance that focused the laser pulse on the sample surface. The plasma emission was collected by a lens of short focal distance and sent to the echelle, through of an optical fiber, and later to the ICCD. In qualitative analysis, spectra of copper and zinc foils were evaluated and the spectral lines were found in agreement with literature, considering the echelle resolution. In quantitative analysis, manganese was determined in killed steel. The system presented signals at 293,30 nm whose intensities changes in function of manganese concentration and analytical curves were obtained. The laser pulse energy showed to be an important factor for the success of quantitative analysis. Others parameters such as width, delay time, MCP gain, accumulated laser pulses and distance sample-focusing lens also showed have influence in quantitative analysis. MEV images and surface scanner by EDS of the craters formed by laser were important tools to understanding laser-sample-atmosphere interaction processes / Mestrado / Quimica Analitica / Mestre em Química

The present thesis focuses on the interaction between refractory and liquid steel. The aim of this work is to understand the interaction behavior between refractory and liquid steel regarding steel cleanliness. The effect of different refractories on different inclusions in Al-killed steel was studied in a furnace. The sintering mechanism of filler sand were also investigated in laboratory. In the industrial trials, the attachments of different oxides on the walls of submerged entry nozzle (SEN) were discussed in the cases of high strength low alloy steel (HSLA) and ultra-low carbon steel (ULC). It is found that the effect of alumina and spinel refractory on all the three types of inclusions is very little, while MgO refractory influences the inclusions depending on the activity of dissolved oxygen in liquid steel. At low oxygen level, alumina inclusions could transform into spinel inclusions with the help of MgO refractory, while the effect on spinel and calcium aluminate inclusions is not evident. On the other hand, when the activity of dissolved oxygen is high enough, the evolution of spinel inclusions from alumina inclusions could not be seen. The reaction between chromite and silica grains leading to liquid formation is the main mechanism for the sintering of filler sand. The factors viz. steel composition, silica size and content, operation temperature and process holding time have a strong influence on the sintering of the filler sand. Smaller size and higher content of silica in sand, steel grades containing higher Mn and Al contents, higher temperature and longer holding time would result in serious sintering. The choice of the sand needs to take those factors into account. The results show that solid alumina particles are always agglomerated on the inner wall of SEN in the case of ULC steel. The top slag with high FeO and MnO contents is considered as the main reason of this kind of attachments. The removal of slag might be a good method to avoid the attachments. In the case of HSLA steel, liquid calcium aluminate inclusions could attach on the inner wall of SEN as well. The smoothness of the inner wall of the SEN holds the key of liquid attachments. In addition, the attachment situation on the outer wall of SEN depends on the operations. The oxygen entrainment through the mold powder would result in the formation of plate-like alumina attachments. The control of reoxidation due to oxygen entrainment would help to avoid this situation. / <p>QC 20160816</p>

QC 20101203

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