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The work in this thesis relates to the preparation and structural and electrical characterisation of calcium and strontium hydrides, imides and nitride hydrides. Conventional solid state methods in controlled atmospheres were used to synthesise these materials. High temperature neutron diffraction, thermal analysis and conductivity studies performed on calcium and strontium hydride suggest an order – disorder transition in these materials at 350 – 450°C. Disordering is believed to involve rapid exchange of hydride ions across two crystallographic sites. This manifests itself in a lowering of the activation energy for bulk hydride ion conduction. The hydride ion conduction is good in these undoped materials: σ[total]subscript = 0.01 S/cm for CaH₂ at 1000K; for SrH₂, σ[total]subscript = 0.01 S/cm at 830K. Doping of SrH₂ with NaH causes a significant increase in the low temperature conductivity, due to presence of extrinsic defects. The high temperature conductivity is negatively affected by NaH doping. Calcium nitride hydride (Ca₂NH) was obtained as a single phase material by reacting either calcium metal or calcium hydride (CaH₂) in an argon atmosphere containing 5 – 7% H₂ and 1 – 7% N₂. Imide ions substituting for hydride and nitride ions constitute a major chemical defect in this material. Long range ordering of the nitride and hydride ions occurs, giving rise to a double cubic crystal symmetry. This order breaks down at 600 – 650°C. Applying the same reaction conditions to strontium metal results in a mixed phase of strontium nitride hydride and imide. No long range order in the nitride hydride phase could be observed. Doping Ca₂NH with lithium hydride (LiH) causes the appearance of a second calcium imide phase, whereas doping with sodium hydride (NaH) increases the amount of imide ions as a defect in the nitride hydride structure, thereby decreasing the long range ordering of nitride and hydride ions.

Made available in DSpace on 2014-10-09T12:34:02Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:59:37Z (GMT). No. of bitstreams: 0 / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-10-09T12:34:02Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:59:37Z (GMT). No. of bitstreams: 0 / Composições cerâmicas de CaxSr1-xTi1-yFeyO3-&delta;, x = 0, 0,5 e 1,0, y = 0 e 0,35, foram preparadas por meio de síntese reativa de CaCO3, SrCO3, TiO2 e Fe2O3 e pela técnica dos precursores poliméricos. Os pós-cerâmicos foram avaliados por meio de análise térmica (termogravimétrica e térmica diferencial), difração de raios X e microscopia eletrônica de varredura. Compactos cerâmicos sinterizados foram analisados por difração de raios X, microscopia eletrônica de varredura, microscopia de varredura por sonda e espectroscopia de impedância. A força eletromotriz gerada entre duas faces paralelas de amostras cilíndricas foi monitorada na faixa de temperatura 600 - 1100 oC para pressão parcial de oxigênio de ~50 ppm, utilizando-se uma bomba eletroquímica de oxigênio com transdutores de zircônia estabilizada com ítria. Foram refinadas, por meio de análise de Rietveld as estruturas cristalinas determinadas na análise por difração de raios X: perovskita cúbica (x = 0) e perovskita ortorrômbica (x 0). A condutividade elétrica foi analisada por medidas de espectroscopia de impedância na faixa de freqüências 5 Hz-13 MHz da temperatura ambiente até ~200 C. A deconvolução dos diagramas de impedância [-Z\"() x Z\'()] na faixa de temperaturas 300 < T(K) < 500 mostra dois semicírculos atribuídos às contribuições intragranular (grãos) e intergranular (contornos de grão) à resistividade elétrica. Os compactos sinterizado utilizando pós preparados pela síntese de estado sólido apresentam valores de resistividade intergranular e intragranular maiores que os compactos preparados com pós obtidos pela síntese química. O sinal elétrico (força eletromotriz) gerado sob exposição a oxigênio mostra que esses compostos podem ser utilizados em dispositivos sensores de oxigênio entre 600 e 1100C. Análises topográficas em microscópio de varredura por sonda em superfícies polidas e atacadas termicamente mostram detalhes morfológicos dos grãos, permitindo concluir que compactos sinterizados preparados com pós obtidos pela rota química são menos porosos que os preparados com pós obtidos pela rota convencional de síntese de estado sólido. Estes resultados estão de acordo com os resultados de medidas de espectroscopia de impedância. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

No / Recent casework in Belgium involving the search for human remains buried with lime, demonstrated the need for more detailed understanding of the effect of different types of lime on cadaver decomposition and its micro-environment. Six pigs (Sus scrofa) were used as body analogues in field experiments. They were buried without lime, with hydrated lime (Ca(OH)(2)) and with quicklime (CaO) in shallow graves in sandy loam soil in Belgium and recovered after 6 months of burial. Observations from these field recoveries informed additional laboratory experiments that were undertaken at the University of Bradford, UK. The combined results of these studies demonstrate that despite conflicting evidence in the literature, hydrated lime and quicklime both delay the decay of the carcass during the first 6 months. This study has implications for the investigation of clandestine burials and for a better understanding of archaeological plaster burials. Knowledge of the effects of lime on decomposition processes also has bearing on practices involving burial of animal carcasses and potentially the management of mass graves and mass disasters by humanitarian organisations and DVI teams. / No

No / Contradictions and misconceptions regarding the effect of lime on the decay of human remains have demonstrated the need for more research into the effect of different types of lime on cadaver decomposition. This study follows previous research by the authors who have investigated the effect of lime on the decomposition of human remains in burial environments. A further three pig carcasses (Sus scrofa), used as human body analogues, were observed and monitored for 78 days without lime, with hydrated lime (Ca(OH)2) and with quicklime (CaO) in the taphonomy laboratory at the University of Bradford. The results showed that in the early stages of decay, the unlimed and hydrated lime cadavers follow a similar pattern of changes. In contrast, the application of quicklime instigated an initial acceleration of decay. Microbial investigation demonstrated that the presence of lime does not eliminate all aerobic bacteria. The experiment also suggested that lime functions as a sink, buffering the carbon dioxide evolution. This study complements the field observations. It has implications for the investigation of time since death of limed remains. Knowledge of the effects of lime on decomposition processes is of interest to forensic pathologists, archaeologists, humanitarian organisations and those concerned with disposal of animal carcasses or human remains in mass disasters.

Indiana University-Purdue University Indianapolis (IUPUI) / Brasseler USA (Savannah, GA) developed and introduced a bioceramic putty called EndoSequence Root Repair Material (ERRM) that can be used as a retrofilling material for surgical endodontics. The material is said to have many of the same chemical, physical, and biological properties as mineral trioxide aggregate (MTA), but with superior handling characteristics. The material is composed of calcium silicates, monobasic calcium phosphate, zirconium oxide, tantalum oxide, proprietary fillers, and thickening agents. ERRM is said by the manufacturer to bond to adjacent dentin, have no shrinkage, be highly biocompatible, hydrophilic, radiopaque, and antibacterial due to a high pH during setting. Investigations on the sealing properties of this material have not yet been conducted. The purpose of this study was to compare the microbial leakage of Enterococcus faecalis in teeth with root-end fillings using ProRoot MTA and Brasseler’s ERRM in a dual-chamber bacterial leakage model as described by Torabinejad and colleagues. The aim of this investigation was to compare the bacterial microleakage of these two root-end filling materials exists. Sixty-two human, single-rooted, mandibular premolars in which extraction was indicated were accessed and instrumented in an orthograde fashion with hand and rotary files. Root resection of the apical 3 mm was then completed and root-end retropreparations were created for placement of root-end filling material. Twenty-seven of these premolars had root-end fillings using ProRoot MTA and 27 had root-end fillings using ERRM. Two teeth were used as a positive control group with no root-end filling, and two other teeth were used as a negative control group and were sealed and coated with dentin bonding agent. The teeth were then evaluated for microleakage using a dual-chamber bacterial microleakage model for 40 days as described by Torabinejad and colleagues. Microleakage was determined by the presence of turbidity in the lower chamber of the apparatus and was assessed each day. Fresh samples of E. faecalis were used every three days to inoculate the apparatus and serve as a bacterial challenge for the materials. Results were recorded every day for 30 days. The outcome of interest (bacterial turbidity) and time-to-leakage (in days) were determined for each of the samples. Survival analysis was used to compare the two groups with a Kaplan-Meier plot to visualize the results and a nonparametric log-rank test for the group comparison. The microleakage of ERRM was not statistically different (p > 0.05) than leakage of ProRoot MTA when subjected to E. faecalis over the 40 day observation period. Both groups had a small number of early failures (within 4 days) and no leakage was observed for the remaining 40 days of the study. Therefore, the null hypothesis was rejected. The results of this research support the use of either of these two materials when compared with the controls. The microleakage of Brasseler’s EndoSequence Root Repair Material was at least as good as ProRoot Mineral Trioxide Aggregate when tested with E. faecalis.