Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-09-19T20:22:47Z No. of bitstreams: 1 IgorOliveiraNascimento_TESE.pdf: 5575757 bytes, checksum: c19dabd04c4f5dd3dd95968e649af7af (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-09-20T21:21:32Z (GMT) No. of bitstreams: 1 IgorOliveiraNascimento_TESE.pdf: 5575757 bytes, checksum: c19dabd04c4f5dd3dd95968e649af7af (MD5) / Made available in DSpace on 2017-09-20T21:21:32Z (GMT). No. of bitstreams: 1 IgorOliveiraNascimento_TESE.pdf: 5575757 bytes, checksum: c19dabd04c4f5dd3dd95968e649af7af (MD5) Previous issue date: 2017-06-23 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Filmes finos de nitreto de tit?nio foram depositados em superf?cies de sil?cio e de vidro, utilizando as t?cnicas de deposi??o: descarga em Gaiola Cat?dica e Magnetron Sputtering, a fim de verificar a influ?ncia da corrente e da temperatura na taxa de deposi??o, na estequiometria dos filmes finos e nas propriedades estruturais dos filmes finos. As deposi??es por Gaiola Cat?dica foram realizadas nas configura??es gaiola alta, gaiola baixa e por uma inova??o da t?cnica utilizando a gaiola dupla, em atmosfera gasosa composta de 75% de hidrog?nio e 25% de nitrog?nio, sob temperaturas de 300?C e 350?C, e tempos de deposi??es de 2 e 4 horas. As deposi??es foram realizadas em Magnetron Sputtering em atmosfera gasosa composta de 75% de arg?nio e 25% de nitrog?nio, utilizando correntes de 0,40 A e 0,50 A, nos tempos de deposi??es de 2 e 4 horas. Para a caracteriza??o dos filmes finos de nitreto de tit?nio, utilizou-se a espectroscopia Rama (RAMAN) que forneceu a medida direta das energias dos nodos da primeira ordem dos ?tomos constituintes dos filmes finos. Os espectros mostraram interdifusividade at?mica que comprovaram a forma??o de nitreto de tit?nio o que permitiu o c?lculo da raz?o da concentra??o N/Ti, As an?lises de difra??o de raios-X (DRX) comprovaram que os filmes finos obtidos s?o compostos por TiN, apresentando varia??es nos planos cristalinos indicando a n?o exist?ncia de um plano preferencial para o crescimento dos filmes, A espectroscopia de energia de dispers?o (EDS) analisou quantitativamente a composi??o dos filmes finos de nitreto de tit?nio, A microscopia eletr?nica de varredura (MEV) evidenciou a estrutura dos filmes finos de nitreto de tit?nio e foi poss?vel calcular as espessuras dos mesmos, A microscopia de for?a at?mica (AFM) mostrou algumas caracter?sticas microestruturais como a diferen?a entre picos e vales da topografia dos filmes finos de nitreto de tit?nio. De maneira geral, os filmes finos de nitreto de tit?nio depositados por Gaiola Cat?dica apresentaram menor cristalinidade devido ? baixa quantidade de nitrog?nio na atmosfera e, evidenciaram que quanto mais elevada a temperatura, maior ser? a espessura do filme fino. Os filmes finos depositados por Magnetron Sputtering apresentaram crescimento na espessura com o aumento da corrente e s?o mais estequiom?tricos. / Thin films of titanium nitride deposited on silicon surfaces and glass deposition techniques using: Download cathodic cage and Magnetron Sputtering to verify the influence of flow and temperature in the deposition rate in stoichiometry of thin films and structural properties of thin films. Deposits of cathodic cage was carried out in high cage configurations and cage low an innovation of the technique using atmospheric gas double cage consisted of 75% hydrogen and 25% nitrogen to temperatures of 300 ? C and 350 ? C Y deposits both 2 and 4 hours. The deposits were made in an atmosphere of sputter gas Magnetrons consisting of 75% argon and 25% nitrogen using current 0.40 A and 0.50 A in the deposition time of 2 and 4 hours. Rama spectroscopy (Raman), which makes available for the characterization of thin layers of titanium nitride direct measurement of the energy of the node of the first order of the constituent atom of the thin films. The spectra showed interdifusivity atomic of the titan nitride formation that the calculation of the concentration ratio N / Ti, X-ray diffraction analysis (XRD) showed that the thin films obtained from TiN is composite with variations of the crystal planes indicating the non-existence of preference plan for The growth of films, microscopy of the energy dispersion spectroscopy (EDS) quantitatively analysed the composition of the thin films of titanium nitride, electron scanning (MEV) structure highlight thin films of titanium nitride was able to calculate the thickness thereof, the scanning force microscopy (AFM) showed microstructural properties, Which is the difference between the peaks and valleys of the topography of the thin films of titanium nitride. In general, thin films deposited by cathodic titanium nitride cage deposited a lower crystallinity due to the small amount of nitrogen in the atmosphere, and showed that the higher the temperature, the greater the thickness of the thin film. Thin films deposited by Magnetron Sputtering have increased thickness with increasing current and are stoichiometric.

Made available in DSpace on 2014-12-17T14:07:01Z (GMT). No. of bitstreams: 1 NataliaFD_DISSERT.pdf: 4136751 bytes, checksum: 47b384d6442f251d58542735c23ae300 (MD5) Previous issue date: 2012-02-27 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film / Filmes finos de nitreto de tit?nio foram crescidos sobre vidro utilizando a t?cnica de deposi??o por descarga em gaiola cat?dica a fim de averiguar a influ?ncia das vari?veis de processo nas propriedades ?pticas e estruturais do filme. Como atmosfera do plasma foi utilizada a mistura de gases Ar, N2 e H2, fixando o fluxo de Ar e N2 em 4 e 3 sccm, respectivamente, e usando fluxos de 0, 1 e 2 sccm de H2. O processo de deposi??o foi monitorado por Espectroscopia de Emiss?o ?ptica (OES) para investiga??o das esp?cies ativas no plasma. Observou-se que com o aumento fluxo de H2 as intensidades das esp?cies luminescentes no plasma sofrem altera??es e que a esp?cie N2 (391,4 nm) n?o teve um crescimento proporcional ao fluxo de H2. Outros par?metros investigados foram o di?metro e o n?mero de furos da gaiola. As an?lises de difra??o de raios X com ?ngulo de incid?ncia rasante (GIXRD) comprovaram que os filmes obtidos s?o compostos por TiN, podendo ter varia??es quanto a quantidade de nitrog?nio na rede e o tamanho de cristalito; a microscopia ?ptica forneceu dados sobre a homogeneidade, a partir da microscopia de for?a at?mica (AFM) observou-se algumas caracter?sticas microestruturais do filme e a rugosidade. A espessura foi quantificada atrav?s das an?lises de elipsometria. As propriedades ?pticas como reflet?ncia e transmit?ncia (medidas por espectrofotometria) s?o bastante sens?veis a altera??es na rede cristalina do material, composi??o qu?mica e espessura, sendo, portanto, uma boa ferramenta para verifica??o do controle do processo. De maneira geral, os filmes obtidos com fluxo de 0 sccm de H2 possuem uma maior transmit?ncia atribu?da ao menor cristalinidade decorrente da maior quantidade de nitrog?nio na rede cristalina do TiN. Os filmes obtidos nos fluxos de 1 e 2 sccm de H2 obtiveram um aspecto dourado e o difratograma apresentou picos caracter?sticos do TiN com maior intensidade e menor largura a meia altura, sugerindo que com a presen?a de hidrog?nio na atmosfera do plasma os filmes s?o mais estequiom?tricos e com maior cristalinidade. Quanto ? configura??o da gaiola observou-se que com maior quantidade de furos na tampa, maior a proximidade da tampa com a amostra e menor o di?metro do furo, maior ? a espessura do filme, o que ? justificado pela maior probabilidade das esp?cies do plasma atingirem efetivamente o substrato e promoverem o crescimento do filme

Made available in DSpace on 2014-12-17T14:07:06Z (GMT). No. of bitstreams: 1 PolianaRFS_DISSERT.pdf: 3998823 bytes, checksum: e0480a4a5d6b04450e748434898535a9 (MD5) Previous issue date: 2013-03-01 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The technique of plasma nitriding by the cathode cage mainly stands out for its ability to produce uniform layers, even on parts with complex geometries. In this study, it was investigated the efficiency of this technique for obtaining duplex surface, when used, simultaneously, to nitriding treatment and thin film deposition at temperatures below 500?C. For this, were used samples of AISI 41 0 Martensitic Stainless Steel and performed plasma treatment, combining nitriding and deposition of thin films of Ti and/or TiN in a plasma atmosphere containing N2-H2. It was used a cathodic cage of titanium pure grade II, cylindrical with 70 mm diameter and 34 mm height. Samples were treated at temperature 420?C for 2 and 12 hours in different working pressures. Optical Microscopy (OM), Scanning Electron Microscopy (SEM) with micro-analysis by Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and analysis of Vickers Microhardness were used to investigate coating properties such as homogeneity and surface topography, chemical composition, layer thickness, crystalline phase, roughness and surface microhardness. The results showed there is a direct proportionality between the presence of H2 in plasma atmosphere and the quantity of titanium in surface chemical composition. It was also observed that the plasma treatment at lowpressure is more effective in formation of TiN thin film / A t?cnica de nitreta??o a plasma por gaiola cat?dica vem se destacando, principalmente, pela sua capacidade de produzir camadas uniformes mesmo em pe?as com geometria complexa. Neste trabalho, investigou-se a efici?ncia desta t?cnica para obten??o de superf?cie duplex, quando utilizada, simultaneamente, para tratamento de nitreta??o e deposi??o de filmes finos em temperaturas inferiores a 500?C. Para tal, foram utilizadas amostras do a?o inoxid?vel martens?tico AISI 410 e realizados tratamentos a plasma, combinando a nitreta??o e deposi??o de filmes finos de Ti e/ou TiN, em uma atmosfera contendo N2-H2. Foi utilizada uma gaiola cat?dica de tit?nio puro grau II em forma cil?ndrica, com 70 mm de di?metro e 34 mm de altura. As amostras foram tratadas numa temperatura de 420?C, com dura??o de 2 e 12 horas e em diferentes press?es de trabalho. Microscopia ?ptica (MO), Microscopia Eletr?nica de Varredura (MEV) com microan?lise por Espectroscopia de Energia Dispersiva (EDS), Difra??o de Raios-X (DRX), Microscopia de For?a At?mica (MFA) e ensaio de Microdureza Vickers foram empregados para investigar as propriedades do revestimento, tais como homogeneidade e topografia superficial, composi??o qu?mica, espessura da camada, fases cristalinas, rugosidade e microdureza superficial. Os resultados mostraram existir uma proporcionalidade direta entre a presen?a de H2 na atmosfera do plasma e a quantidade do elemento qu?mico tit?nio na composi??o qu?mica superficial. Observou-se, tamb?m, que o tratamento a plasma em baixa press?o ? mais eficaz na forma??o do filme fino de nitreto de tit?nio