Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-12-12T17:53:46Z No. of bitstreams: 1 MariaJoseSantosLima_TESE.pdf: 8256758 bytes, checksum: 2af332071bb76b3070e1cdcc7d8adcb2 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-12-13T17:58:53Z (GMT) No. of bitstreams: 1 MariaJoseSantosLima_TESE.pdf: 8256758 bytes, checksum: 2af332071bb76b3070e1cdcc7d8adcb2 (MD5) / Made available in DSpace on 2017-12-13T17:58:53Z (GMT). No. of bitstreams: 1 MariaJoseSantosLima_TESE.pdf: 8256758 bytes, checksum: 2af332071bb76b3070e1cdcc7d8adcb2 (MD5) Previous issue date: 2017-07-18 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Neste trabalho foram sintetizados p?s-comp?sitos WC-Ni atrav?s de Carborredu??o da mistura de paratungstato de am?nio hidratado (APT) com o nitrato de n?quel nas propor??es (5% p.Ni, 10% p.Ni e 15% p.Ni) a baixa temperatura (800?C a 950?C) e em curto tempo de rea??o (90 min a 150 min) em um ?nico processo de s?ntese. Os p?s foram caracterizados por difra??o de raios X, microscopia eletr?nica de varredura, espectroscopia de energia dispersiva (EDS), e fluoresc?ncia de raios X (FRX), an?lise de tamanho de part?culas e adsor??o de nitrog?nio pela t?cnica do BET, al?m de medidas de magnetiza??o, coercividade e reman?ncia. O estudo do tamanho de cristalito foi obtido a partir dos dados dos difratogramas de raios X dos p?s-comp?sitos, atrav?s da equa??o de Scherrer. Foi realizado um planejamento experimental fatorial 23 com tr?s pontos centrais com a finalidade avaliar a influ?ncia das condi??es de s?ntese nas vari?veis-resposta. Os par?metros de s?ntese avaliados neste trabalho foram: tempo de rea??o (90min, 120min e 150min), temperatura de s?ntese (800?C, 850?C e 900?C) e concentra??o de n?quel em peso (5%p.Ni, 10%p.Ni e 15%p.Ni). Foi poss?vel produzir p?s-comp?sitos de WC-Ni nonom?tricos nas propor??es desejadas com a pureza desejada, com tamanho m?dio de cristalito variando de 24,2 nm at? 38 nm, com ?rea superficial variando de 24,6 m?/g at? 46,7 m?/g. Os p?s apresentaram morfologia com part?culas de tamanhos e formas variadas, bastante aglomeradas, bem como uma boa dispers?o e homogeneiza??o das fases. As caracter?sticas espec?ficas desses materiais nanom?tricos proporcionam a sua utiliza??o tanto para a produ??o de metal duro como em rea??es catal?ticas. Os p?s-comp?sitos obtidos neste trabalho foram aplicados na produ??o de metal duro-WC-Ni atrav?s de sinteriza??o em fase s?lida e l?quida, utilizando as t?cnicas de sinteriza??o convencional e sinteriza??o por ?spark plasma sintering? para fins de compara??o. Nas amostras sinterizadas, foram realizadas medidas de dureza Vickers e densidade por picnometria. Tamb?m foram realizadas an?lises de DRX, MEV e EDS com mapeamento. Os melhores resultados para as os sinterizados de WC-Ni, foram obtidos para as amostras sinterizadas via SPS a 1350?C, apresentando dureza Vickers (2322 HV) e densidade (97,67 %) superiores as das amostras sinterizadas por sinteriza??o convencional a maiores temperaturas. / In this work WC-Ni composite powders were synthesized by carborreduction of the hydrated ammonium paratungstate (APT) mixture with the nickel nitrate in proportions (5% p.Ni, 10% p.Ni and 15% p.Ni) a low temperature (800 ? C to 950 ? C) and small reaction time (90min to 150min) in a single synthesis process. The powders were characterized mainly by X-ray diffraction, scanning electron microscopy (SEM), dispersive energy spectroscopy (EDS), X-ray fluorescence (FRX), particle size analysis and (BET) and measures of magnetization, coercivity and remanence. The study of crystallite size was obtained from the X-ray diffractograms of post-composites, using the Scherrer equation. A factorial experimental design 23 with three central points was carried out to evaluate the influence of the synthesis conditions on the response variables (crystallite size). The synthesis parameters evaluated in this work were: reaction time (90min, 120min and 150min), synthesis temperature (800 ? C, 850 ? C and 900 ? C) and concentration of nickel by weight (5% p.Ni, 10 % P.Ni and 15% p.Ni). It was possible to produce nanometric WC-Ni composite powders in the desired proportions with the desired purity, with a mean crystallite size varying from 24.2 nm to 38 nm, with a surface area ranging from 24.6m?/g to 46.7 m?/g. The powders presented morphology with particles of varied sizes and shapes, quite agglomerated and also presented a good dispersion and homogenization of the phases. The specific characteristics of these nanometric materials provide their use for both the hard metal in catalytic reactions.Therefore, the composite powders obtained in this work were applied in the production of WC-Ni hard metal by solid and liquid phase sintering using conventional sintering and Spark Plasma Sintering techniques for comparison purposes. In the sintered samples the measurements of Vickers hardness and density by pycnometry were performed. We also performed XRD, SEM and EDS analyzes with mapping. The best results for the sintered WC-Ni were obtained for the sintered samples via SPS at 1350?C, showing Vickers hardness (2322 HV) and density (97.67%) higher than the samples sintered by conventional sintering at higher temperatures. / 2018-08-23