Electrical resistivity is an important indicator of metal thin film quality. In this study, the influence of argon working pressure on the properties of metal thin films was evaluated, and the thickness effect on the resistivity of metal thin films was investigated. The sputtered thin film resistivity performances of seven metals as a function of argon pressure were measured, and the results turned out that the argon pressure was vital to film quality. Further investigation on sputtered chromium thin films using XRD, SEM and XPS revealed that the argon pressure influences the microstructure of sputtered metal thin films. Different microstructure is the reason for different resistivity performances, and John Thornton's "Zone Model" explains all these behaviours well. The resistivity of aluminum and chromium thin films with thickness from 15 to 150 nm were compared, the resistivity change significantly. The scaling trends are different for different metals. / Materials Engineering

Nanowires of Zinc oxide and bismuth oxide were grown on silicon substrates using vapor-liquid-solid (VLS) and unbalanced magnetron sputtering. Characterization using x-ray diffraction (XRD) and scanning electron microscopy (SEM) was conducted to investigate how growth conditions influence the structural and morphological properties of the materials. Optical properties were investigated using photoluminescence (PL), direct absorption spectra and cyclic voltammetry. The physical properties of sputtered ZnO were found to be dependent on oxygen flow rate, temperature, and the initial foreign metal catalysis seed layer. Nanowires were grown using a two-step process whereby an initial Au layer was deposited followed by Zn with oxygen. Doped ZnO-TiO2 nanostructures were created by sputtering Ti and Zn simultaneously. Homo- and hetero-structured ZnO-ZnO and ZnO-TiO2 were created using additional sputtering cycles. A systematic approach was taken to produce nanoarrays of Bi2O3 by adjusting initial seed layer thickness and oxygen flow rates. A two step process involving variable oxygen flow rates was found to create the highest density of Bi2O3 nanowires in the array. Top-view and cross-sectional SEM micrographs suggested that the resulting Bi2O3 nanowires were approximately 300 nm in length with diameters of 100 nm at the base and 30 nm at the top. Investigation into the growth method suggests a self-catalytic VLS-like process. Degradation tests using rhodamine 6G dye were compared to SEM images. Samples of ZnO and Bi2O3 displayed a direct correlation between nanowire density and photocatalytic efficiency.

It is well known that ion bombardment of growing films can strongly influence their microstructure and consequently their physical properties. The available technology for ion assisted deposition, particularly where separate sources are used for the deposition flux and the ion flux, is difficult to implement in many production situations. The planar magnetron provides a controllable ion flux while retaining the many other desirable features of simplicity, high deposition rate, geometric versatility and tolerance of reactive gases. This assists in the implementation of ion beam assisted deposition in both research and production.

No description available.

This thesis investigates low-energy xenon-molybdenum (Xe+-Mo) sputtering yields for ion energies of 100 eV and less. Sputtering yield data at these energies are important for ion thruster design and lifetime prediction. The basic principles of sputtering phenomena are discussed. An overview of various popular types of experimental sputtering yield methods is presented with an emphasis on the techniques that have been used to find Xe+-Mo sputtering yields in the past. Sputtering yields in this study are found through both models and experiments. Sputtering yields are calculated using the Sigmund, Bohdansky, Yamamura, and Wilhelm formulas. The computed sputtering yields for these models varied widely at low-energy. TRIM (The TRansport of Ions in Matter), a Monte-Carlo simulation program, was adapted to study sputtering yields, and energy and angular distributions of sputtered atoms. Simulations were run at various combinations of ion energy and ion incidence angle. TRIM did not prove to be an adequate model for low-energy sputtering. Experimental measurements of sputtering were made using both Rutherford backscattering spectrometry (RBS) and mass-loss methods. Sputtering was performed in a small vacuum facility using an ion gun. For the RBS technique, sputtered material was collected on aluminum foil substrates. The area density of the deposited Mo film on the substrates was measured using RBS. These measurements enabled calculation of differential sputtering yields, which were integrated to find the total sputtering yield. Sputtering yield was found by the mass-loss technique by simply comparing the mass of the sample both before and after sputtering using a microbalance. Sputtering yields at 100 eV, 90 eV, 80 eV, 70 eV, and 60 eV were found using the RBS technique. The mass-loss technique was only successful in the 80 eV experiment. The experimental results were unexpected. The measured sputtering yields were significantly higher than those reported by other researchers. Also, sputtering yields were found to increase with decreasing ion energy from 90 eV down to 60 eV. / Master of Science

Energy distribution measurements of sputtered neutral particles contribute to the general knowledge of sputtering, a common technique for surface analysis. In this work emphasis was placed on the measurement of energy distribution of sputtered neutral atoms from different depths. The liquid Ga-In eutectic alloy as a sample target for this study was ideal due to an extreme concentration ratio gradient between the top two monolayers. In pursuing this study, the method of sputter-initiated resonance ionization spectroscopy (SIRIS) was utilized. SIRIS employs a pulsed ion beam to initiate sputtering and tunable dye lasers for resonance ionization. Observation of the energy distribution was achieved with a position-sensitive detector. The principle behind the detector's energy resolution is time of flight (TOF) spectroscopy. For this specific detector, programmed time intervals between the sputtering pulse at the target and the ionizing laser pulse provided information leading to the energy distribution of the secondary neutral particles. This experiment contributes data for energy distributions of sputtered neutral particles to the experimental database, required by theoretical models and computer simulations for the sputtering phenomenon.

Atualmente, nanopartículas (NPs) são utilizadas em todos os ramos da tecnologia. Suas promissoras aplicações envolvem entre outros, o campo dos sensores e transdutores, mídia de gravação magnética, carreadores magnéticos de drogas medicinais. Com o objetivo de produzir NPs pelo método físico, um gerador de nanopartículas foi adaptado usando um dos canhões do sistema de magnetron sputtering, baseando-se no método de agregação gasosa. Com o gerador somos capazes de produzir NPs de diversos materiais e codepositá-las em matrizes dielétricas ou metálicas. Neste trabalho apresentamos o desenvolvimento da metodologia para a produção de nanopartículas de materiais magnéticos duros, usando alvos de SmCo5, Sm2Co17, Nd2Fe17B, FePt e CoPt. Investigamos a influência dos parâmetros de deposição (pressão, fluxo de gás e potência de sputtering), tipo de substrato e a existência de buffer e/ou codeposição, na obtenção das propriedades estruturais e magnéticas desejadas para esses materiais. As NPs produzidas são analisadas magneticamente pelo VSM e SQUID, sua morfologia e tamanho por TEM e SEM, a sua estequiometria pelo RBS, e a sua estrutura cristalina por XRD, a fim de obter nano-ímãs de alta anisotropia magnética. Da caracterização morfológica, através de microscopia eletrônica, encontramos para as NPs produzidas e estudadas diâmetros entre 5 e 17 nm. Através de análises de RBS obtemos para composição das NPs que as mesmas possuem estequiometria diferente dos alvos usados. Estudos estruturais e magnéticos mostram que para Sm-Co, Fe-Pt e Co-Pt é possível obter NPs cristalinas e com coercividade da ordem de 1 kOe. / In the recent years, nanoparticles (NPs) are being in all fields of technology. Their promising applications involve among others, the field of sensors and transducers, magnetic recording media, magnetic carriers of medicinal drugs. Aiming to produce NPs by physical method, a generator of nanoparticles was adapted using a system of guns \"magnetron sputtering\", based on the aggregation gas method. With the generator we are able to produce NPs with different types of material. In this work, we present the development of the methodology for the production of nanoparticles of hard magnetic materials, using targets of SmCo5, Sm2Co17, Nd2Fe17B, FePt and CoPt. We investigated the influence of the deposition parameters (pressure, gas flux and sputtering power), substrate type and the existence of the buffer and/or codeposition layers, to obtain the desired structural and magnetic properties for the nanoparticles. The produced NPs were magnetically analyzed by VSM and SQUID, the morphology and size by TEM and SEM, the stoichiometry by RBS and the crystal structure by XRD. The main objective of this work is to obtain nano-magnet with high magnetic anisotropy. Through the morphological characterization by electron microscopy, we found for NPs produced and studied have diameters between 5 and 17 nm. Through RBS analysis we have obtained the composition of the NPs, and also that they have different stoichiometry in relation to the used targets. Structural and magnetic studies have show that for Sm-Co, Fe-Pt and Co-Pt it is possible to obtain crystalline NPs with coercive field around 1 kOe.

Filmes finos de óxido de nióbio têm sido usados em muitas aplicações tecnológicas. Existem pelo menos três óxidos estáveis de nióbio: NbO, NbO2 e Nb2O5 e cada um deles tem propriedades específicas. O Nb2O5 é a forma termodinamicamente mais estável e apresenta propriedades físicas e químicas únicas, como alto índice de refração, band gap largo, excelente estabilidade química e resistência à corrosão, baixa absorção óptica no campo da luz visível até regiões próximas ao infra-vermelho, sendo amplamente utilizados como filtros de interferência óptica de alta qualidade. Neste trabalho foram depositados filmes de óxido de nióbio por meio da técnica de sputtering reativo sobre substratos de silício e borossilicato. Os filmes finos foram obtidos com vazão de oxigênio variando entre 15 e zero sccm. O objetivo deste trabalho foi a caracterização das propriedades ópticas dos filmes. Foram avaliados o índice de refração e a espessura pela técnica de elipsometria, o band gap pelo método de Tauc e a razão atômica e a densidade superficial por meio de Espectrometria de Retroespalhamento Rutherford (RBS). Foram obtidos espectros de transmitância e refletância por Espectrofotometria UV/Vis/NIR e o coeficiente de extinção foi calculado pelo método de Hong. Todos estes parâmetros são importantes para aplicação em dispositivos ópticos. Nos filmes depositados com vazão de oxigênio de 15 sccm foi observado que o índice de refração aumenta com o aumento da espessura dos filmes e que o composto formado foi Nb2O5. Para uma vazão de 2,0 sccm foi encontrado o composto NbO2 e o filme apresentou alta absorção ótica. Os resultados sugerem que outros óxidos de nióbio ou nióbio metálico foram incorporados nos filmes conforme o fluxo de oxigênio foi diminuído. Foi observada uma relação direta entre a diminuição da vazão de oxigênio durante a deposição e um aumento da quantidade de nióbio nos filmes, acompanhados de um aumento do índice de refração e da densidade superficial. / Niobium oxide thin films have been used in many technological applications. There are at least three stable niobium oxides: NbO, NbO2 and Nb2O5 and each one has specific properties. The Nb2O5 is the most stable thermodynamically form having unique physical and chemical properties such as high refractive index, wide band gap, excellent chemical stability and corrosion resistance, low optical absorption in the field of visible light to near the infrared regions, being widely used as high quality optical interference filters. In this work niobium oxide thin films were deposited by reactive sputtering technique on silicon and borosilicate substrates. The films were obtained by using oxygen flow rates varying from 15 up to zero sccm. The objective of this work was the optical characterization of niobium oxide films. The refractive index and the thickness were evaluated by ellipsometry technique, the band gap by TAUC method and the atomic ratio and the surface density by means of Rutherford backscattering spectrometry (RBS). Spectral transmittance and reflectance spectrophotometry by UV / Vis / NIR curves were obtained and the extinction coefficient was calculated by the method of Hong. All of these parameters are important for application in optical devices. In the films deposited with oxygen flow of 15 sccm it was observed that the refractive index increases with increasing thickness of the films and analyzes indicated that Nb2O5 forms for when a flow rate of 15 sccm is used. For a flow rate of 2.0 sccm it was found NbO2 and a high optical absorption. As the flow of oxygen used in the deposition of the films was decreased, there were signs that were incorporated in the films other oxides of niobium or niobium metal itself. A direct relationship between decreased of oxygen flow during deposition and a increase in niobium quantity in the films, accompanied by an increase in the refractive index and surface density was observed.

New restrictions and regulations regarding internal combustion engines introduced severe mechanical and thermo-mechanical loads on engine parts, mostly on piston rings, leading to high wear and premature damage, thus causing oil leakage into the combustion chamber and increasing emissions. One of the most viable solutions to overcome these issues is the use of coatings to change surface properties. Coatings produced by High Power Impulse Magnetron Sputtering (HiPIMS) and Direct Current Magnetron Sputtering (dcMS) have shown promising results to form dense coatings with high hardness and high wear resistance. Those properties can be further enhanced by using a periodic structure in the form of multilayers of different materials. In this study, we proposed a hybrid process with HiPIMS and dcMS to produce multilayer coatings of CrN and CrAlN. Different target combinations and negative substrate bias were studied. Furthermore, the base layer influence and an evaluation of the periodicity effects were presented. Structure and morphology of the coatings were characterized with X-Ray Diffraction, Scanning Electron Microscopy and Atomic Force Microscopy. Meanwhile, instrumented nanohardness, corrosion and wear tests were performed to characterize mechanical, electrochemical and tribological properties. Results showed that the choice of target combination and bias values are fundamental for enhancing mechanical and tribological properties. On the other hand, we found no evidence of superlattice hardening when changing periodicity but an increase in corrosion resistance when reducing periodicity was found. The combination of targets, substrate bias, base layer and periodicity presented here showed promising results on wear tests, especially when compared with the current coating under the same engine conditions. / Novas restrições e regulamentações de motores de combustão interna introduziram severas cargas mecânicas e termomecânicas no motor, principalmente nos anéis de pistão, o que leva a um alto desgaste e ao dano prematuro dos mesmos e causa vazamentos de óleo na câmara, aumentando as emissões de poluentes. Uma das soluções mais viáveis para solucionar este problema é o uso de recobrimentos para alterar as propriedades da superfície. Recobrimentos produzidos pelas técnicas High Power Impulse Magnetron Sputtering (HiPIMS) e Direct Current Magnetron Sputtering (dcMS) mostraram resultados promissores na formação de filmes densos com elevada dureza e resistência ao desgaste. Essas propriedades podem ser melhoradas com a utilização de estruturas periódicas na forma de multicamadas. Nesse estudo, foi proposto um processo híbrido de HiPIMS e dcMS para produzir recobrimentos multicamadas de CrN/CrAlN. Diferentes combinações de alvos e de valores de polarização negativa do substrato (bias) foram estudadas. Além disso, foram apresentadas a influência da camada base e a avaliação dos efeitos da mudança de periodicidade. Estrutura e morfologia dos recobrimentos foram caracterizadas por Difração de Raios-X, Microscopia Eletrônica de Varredura e Microscopia de Força Atômica. As caracterizações mecânica, eletroquímica e tribológica foram realizadas com ensaios de Nanodureza Instrumentada, Corrosão e Desgaste. Os resultados mostram que a escolha da combinação de alvos e de valores de bias são fundamentais para a melhoria das propriedades mecânicas e tribológicas. Por outro lado, não foram encontradas evidências de endurecimento devido ao efeito de super-redes com a variação de periodicidade, mas um aumento da resistência à corrosão foi evidenciado. A combinação de alvos, bias, camada base e periodicidade apresentadas aqui mostraram resultados promissores em testes de desgaste, principalmente quando comparadas com os recobrimentos utilizados comercialmente nas mesmas condições de trabalho do motor.

O uso de magnetismo em sensores, transdutores e, principalmente, em mídias de gravação magnética, atinge uma escala de investimento no mercado global de bilhões de dólares anualmente. Essas aplicações tecnologicas, atualmente, apontam para usos do magnetismo na escala nanoscópica, por meio da miniaturização de dispositivos magnéticos sensores e transdutores; em gravação magnética através da nanoestruturação das unidades básicas de armazenamento; ou, ainda, na medicina pelo uso de nanopartículas magnéticas como carregadores de drogas medicinais ou como elementos aquecedores por meio da radiação em radiofrequência. Neste trabalho, adotamos uma abordagem top-down. Partimos de objetos magnéticos microscópicos e buscamos progressivamente reduzir a sua escala espacial visando atingir a escala nanoscópica. Produzindo objetos com formato regular e simples, como quadrados, discos e triângulos produzidos por litografia de feixe de elétrons e método lift-off, a partir de filmes finos produzidos por Magnetron Sputtering. Utilizando como elemento de estudo Metais de Transição (MT) e Terras Raras (TR). A estequiometria e espessura dos filmes finos de Tb-Fe foram obtidas com análise de RBS. Já a análise magnética dos filmes finos de Tb-Fe foram obtidas por técnicas de VSM e SQUID. O que possibilitou averiguar que as amostra com a proporção de Tb variando entre 22% e 36% possuem uma anisotropia magnética perpendicular bem definida e possuem um ordenamento sperimagnético. Através do microscópio de força magnética observamos a formação de domínios magnéticos do tipo bolha irregular nos filmes finos de Tb-Fe. Utilizando o microscópio eletrônico de varredura e o SNOM-MO foi possível analisar a morfologia dos micro-objetos produzidos. Os resultados mostram uma eficácia na preparação de estruturas com dimensões maiores que 2 µm, com altura de aproximadamente 50 nm. Fazendo-se necessário um estudo mais preciso para obtenção de amostra com dimensões abaixo desta dimensão. / The use of magnetism in sensors, transducers and, mainy, in magnetic recordable media reaches a total investment of billions of dollars annually in the markets worldwide. These applications in technology are currently being focused toward the uses of magnetism in the nanoscopic scale, by shrinking the magnetic sensor devices and transducers. Also, in magnetic recordings by the nanostructuration of basic storage units or - going even further - in the use of nanomagnetic particles in Medicine such as drug delivery or heating elements by radiofrequency radiation. In this paper, we take a \"top-down\" approach. We start with microscopic magnetic objects and seek progressively reduce its spatial scale in order to reach the nanoscale. Producing objects with regular and simple format, such as squares, triangles and discs produced by electron beam lithography and lift-off method, The thin films were based on transition metal and rare earth elements. The thickness and stoichiometry of thin films of Tb-Fe were meadured with RBS analysis. The analysis of the Tb-Fe magnetic thin films were obtained by techniques VSM and SQUID. The sample with the ratio of Tb ranging between 22% and 36% have a well-defined perpendicular magnetic anisotropy and have a sperimagnetic behavior. Through the magnetic force microscopy we observed the formation of magnetic domain structure of the \"irregular bubble\" type. Using scanning electron microscope and the SNOM-MO was possible to analyze the morphology of the produced micro-objects. The results show that efficiency in the preparation of structures with dimensions larger than 2 microns, and a height of approximately 50 nm. This result exposes the need for a more investigation in order to produce samples with smaller dimension.