Made available in DSpace on 2014-10-09T12:37:19Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:09:05Z (GMT). No. of bitstreams: 1 02047.pdf: 7030823 bytes, checksum: edacc738c25ca0eb1c8ed2c023d5f1d6 (MD5) / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Made available in DSpace on 2014-10-09T12:29:56Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:09:55Z (GMT). No. of bitstreams: 1 00357.pdf: 772989 bytes, checksum: ccc94f3c8138d33bfe2494d41721d680 (MD5) / Dissertacao (Mestrado) / IEA/D / Instituto de Quimica, Universidade de Sao Paulo - IQ/USP

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Methods of temperature measurement by mass spectrometry have been critically reviewed. It was concluded that the most appropriate method depended critically on the availability of fundamental data, hence a database of fundamental spectroscopic constants, for diatomic ions which cause interferences in ICP-MS, was compiled. The equilibration temperature, calculated using the different methods and using various diatomic ions as the thermometric probes, was between c.a. 400 - 10,000 K in the central channel, and between c.a. 600 - 16,000 K when the plasma was moved 1.8 mm off-centre. The wide range in temperature reflected the range of temperature measurement methods and uncertainty in the fundamental data. Optical studies using a fibre optic connected to a monochromator were performed in order to investigate the presence of interferences both in the plasma and the interface region of the ICP-MS, and the influence of a shielded torch on these interferences. It was possible to determine the presence of some species in the plasma, such as the strongly bound metal oxides, however, no species other than OH were detected in the interface region of the ICP-MS. The OH rotational temperature within the interface region of the ICP-MS was calculated to be between 2,000 - 4,000 K. The effect of sampling depth, operating power, radial position and solvent loading, with and without the shielded torch, on the dissociation temperature of a variety of polyatomic interferences was investigated. These calculated temperatures were then used to elucidate the site of formation for different polyatomic interferences. Results confirmed that strongly bound ions such as MO+ were formed in the plasma, whereas weakly bound ions such as ArO+ were formed in the interface region due to gross deviation of the calculated temperatures from those expected for a system in thermal equilibrium.

Made available in DSpace on 2014-10-09T12:49:49Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:02:19Z (GMT). No. of bitstreams: 1 09819.pdf: 15341022 bytes, checksum: 089b1783177dd73c7433320bd2e0de7c (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP / FAPESP:98/05906-6

Made available in DSpace on 2014-10-09T12:34:52Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:08:21Z (GMT). No. of bitstreams: 0 / O carbeto de boro é um material sintético com ligações químicas essencialmente covalentes, tem um alto ponto de fusão só é sinterizável em elevada temperatura. Possui excepcional dureza, baixa densidade, resistência a abrasão, elevada velocidade sônica e boas propriedades mecânicas, características ideais para as aplicações balísticas. Tem como principal característica a alta seção de choque para nêutrons térmicos para aplicações nucleares. O presente trabalho teve por objetivo avaliar as propriedades mecânicas do carbeto de boro, pela introdução de diferentes teores de diboreto de titânio, pela reação in situ com pós de carbeto de titânio, e adição do carbono durante a sinterização, em forno resistivo sem pressão e prensagem isostática a quente dos componentes cerâmicos. Em menores temperaturas valores obtidos da densidade teórica para o carbeto de boro puro, foram alcançados com o emprego do aditivo. Os resultados obtidos na sinterização mostram a eficiência da introdução do carbeto de titânio para o aumento da densificação do material. Com percentuais de 20% de carbeto de titânio, obteve-se os máximos valores para microdureza (HV) de 35 GPa e tenacidade a fratura (KlC) de 3,16 MPa.m1/2. Comprovadamente a dificuldade de sinterização em elevadas temperaturas, para maior densificação, de componentes cerâmicos de carbeto de boro pode ser minimizada com a introdução de percentuais de carbeto de titânio. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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