A indústria cimenteira busca alternativas para economia de recursos no processo produtivo, em especial envolvendo o uso de materiais residuais no cimento, como escórias siderúrgicas. A escória de aciaria, em particular, apresenta composição desfavorável para aplicação in natura, porém há metodologias na literatura de modificação do material para aplicações cimentícias. No entanto, ainda não se encontram avaliações da corrosão de armaduras de aço em compósitos cimentícios com essa adição, seja em meio sólido ou líquido (água de poro). Esse estudo avaliou, através de curvas de polarização e da espectroscopia de impedância eletroquímica (EIE), a resistência à corrosão do aço CA-50 em soluções representativas de águas de poro extraídas por pressão de pastas de cimento com 25 % de escória de aciaria in natura ou modificada por processo pirometalúrgico. Para efeitos comparativos, foi feita também a avaliação do desempenho do aço em meios de águas de poro indicadas na literatura como representativas de cimento Portland comum e de escória de alto forno. O efeito da presença de espécies agressivas na resistência à corrosão do aço foi avaliado adicionando-se 1,0 % de NaCl em massa às soluções estudadas. Nas águas de poro sem 1,0 % de cloreto, o aço CA-50 apresentou-se passivo e não mostrou indícios de corrosão nos ensaios nem de polarização nem de EIE durante 120 h de imersão. Entretanto, os ajustes dos diagramas com circuito elétrico equivalente (CEE) apontaram que as características de proteção da camada passiva formada nas águas de poro de cimento com escória de aciaria foram superiores, resultando em maior resistência à corrosão do aço CA-50 nestes meios. Por sua vez, nos meios com 1,0 % de NaCl, após polarização e EIE até 120 h, o aço sofreu corrosão para as águas de poro de cimento comum e escória de alto forno, porém não corroeu nas águas de poro representativas de cimentos com escórias de aciaria, cujo melhor desempenho foi associado à maior alcalinidade destes meios. A caracterização microestrutural por microscopia eletrônica de varredura após os ensaios de polarização anódica e de imersão mostrou que o principal produto de corrosão formado foi a lepidocrocita (?-FeOOH), comum em ataque do aço por cloretos. / The cement industry seeks alternatives to save resources in production processes, especially involving the use of residual materials in cements, such as slags. Steel slags present unfavorable composition for application as cement additions in natura, but there are methodologies in the literature for modifying this material for commercial application. However, there are no evaluations of the corrosion of steel reinforcements in cementitious composites with steel slags, either in solid or liquid medium (pore water). The present study employed polarization curves and electrochemical impedance spectroscopy (EIS) to evaluate the corrosion resistance of CA-50 steel in pore water solutions representative of cement pastes with 25 % steel slag in natura or modified by a pyrometallurgical process. For comparison purposes, the performance of CA-50 steel in the pore waters indicated in the literature as representatives of Portland cement and blast furnace slag activated with cement were also evaluated. The effect of aggressive species on the corrosion resistance of the steel was assessed by adding 1.0 % NaCl by mass to the pore water solutions. Without 1.0 % chloride addition, CA-50 steel exhibited good performance and showed no evidences of corrosion in all of the investigated media, both in anodic polarization and in EIS tests performed up to 120 h immersion. However, the fitting of the EIS diagrams with equivalent electric circuit (EEC) revealed that the protectiveness of the passive layer formed in pore waters representative of cements with steel slags were superior, indicating better corrosion resistance of CA-50 steel in these media. Conversely, when 1.0 % chloride was added to the pore waters, CA-50 steel presented pitting corrosion, and impedance decreases with immersion in the pore waters representative of pure cement and blast furnace slag, whereas no corrosion was detected by both methodologies in pore waters representatives of cements with steel slags, which superior performance was ascribed to their higher alkalinity. Microstructural characterization by scanning electron microscopy (SEM) after anodic polarization and immersion tests showed that the main corrosion product formed was lepidocrocite (?-FeOOH), usual of chloride attack of steel.

A preocupação com o desenvolvimento sustentável tem levado a indústria e os órgãos controladores do meio ambiente a reavaliarem o emprego em larga escala de procedimentos industriais que, embora eficientes, são prejudiciais à saúde humana e ao meio ambiente. Em concordância com estas novas tendências, as indústrias de tratamento de superfícies de metais e instituições de pesquisa têm empregado grandes esforços no sentido de encontrar substitutos eficientes para procedimentos de proteção contra a corrosão que contenham íons de cromo hexavalente, os quais são muito eficientes, mas apresentam o inconveniente de não serem ambientalmente corretos devido ao caráter cancerígeno e poluente do íon Cr(VI) já reconhecido por diversas agências de proteção ambiental. Com a finalidade de aumentar a proteção contra a corrosão, em linhas industriais contínuas de eletrogalvanização por eletrodeposição, as peças produzidas são protegidas por uma camada de passivação obtida em banho de conversão contendo sais de Cr(VI) e, na maioria dos casos, não passa pelo processo de enxágue após sua produção. Neste trabalho o comportamento de corrosão do aço eletrogalvanizado protegido com camadas de passivação obtidas a partir de banhos de conversão contendo sais de Cr(III) e Co(II) ou uma emulsão de um copolímero de etileno, sem enxágue, foi avaliado por técnicas eletroquímicas, especificamente, acompanhamento do potencial de circuito aberto, curvas de polarização potenciodinâmica anódicas e catódicas, e espectroscopia de impedância eletroquímica (EIS), em soluções com diferentes concentrações de NaCl. Adicionalmente foi avaliado o comportamento de corrosão por ensaios em câmara de névoa salina, realizados de acordo com a norma ASTM B117-11. Como referência, os resultados foram comparados com aqueles apresentados por amostras protegidas por camada de passivação produzida a partir de banho contendo íons de Cr(VI). Para melhor compreender a influência da microestrutura sobre o mecanismo de corrosão, as amostras foram caracterizadas por microscopia eletrônica de varredura antes e após imersão nos diferentes eletrólitos. A análise microestrutural foi complementada por ensaios de difração de raios-X. 7 Os resultados dos ensaios eletroquímicos realizados após tempos curtos de imersão mostraram melhor desempenho para as amostras protegidas com a camada de passivação produzida a partir de banho contendo íons Cr(VI). Entretanto os ensaios de EIS após tempos mais longos de imersão nos diferentes eletrólitos ensaio, bem como os ensaios de névoa, evidenciaram que as amostras protegidas com a camada passiva obtida a partir do banho contendo íons de Cr(III) e Co(II) podem apresentar desempenho semelhante àquelas protegidas com camada de conversão de Cr(VI). Para esta condição, a análise microestrutural e o ajuste dos diagramas de EIS com circuitos equivalentes indicaram um papel importante dos produtos de corrosão no comportamento anticorrosivo das amostras protegidas com a camada de passivação de Cr(III) e Co(II). Em nenhuma das condições estudadas as amostras protegidas com o copolímero de etileno apresentaram desempenhos comparáveis aos das outras duas camadas de passivação estudadas. / Recent concerns with sustainable development have led industries and environment regulatory agencies to reassess the use at large scale of industrial procedures that, although efficient, are harmful to human health and the environment. In accordance with these new tendencies, surface treatment industries and research institutes have expended great efforts to find efficient substitutes for corrosion protection procedures that employ hexavalent chromium ions (Cr(VI)). They are very effective but have the drawback of not being environmentally friendly due to the carcinogenic and pollutant properties of Cr(VI) ions, already recognized by several environmental protection agencies. Aiming to increase the corrosion protection, in industrial continuous lines of galvanizing by electroplating, the parts produced are protected with a passivation layer obtained from a conversion bath containing Cr(VI). These parts are not rinsed after the final production step. In this work the corrosion behavior of electroplated galvanized steel protected with passivation layers from conversion baths containing Cr(III) and Co(II) ions or an ethylene copolymer emulsion was evaluated by means of electrochemical techniques, specifically, open circuit potential measurements, anodic and cathodic potentiodynamic polarization curves and electrochemical impedance spectroscopy (EIS). The tests were performed in sodium chloride solutions of different concentrations. Additionally, the corrosion behavior was evaluated by salt spray tests performed according the ASTM B117-11 standard. For reference, the results were compared with those presented by samples protected by passivation layers produced from conversion baths containing Cr (VI) ions. Aiming to better understand the influence of microstructure on the corrosion mechanism, the samples were characterized by scanning electron microscopy before and after immersion in the different electrolytes. Microstructure analysis was complemented by X-ray diffraction. The results of electrochemical tests performed after short immersion times showed better corrosion performance for samples protected with the passivation layer produced from conversion baths containing Cr(VI) ions. However, the EIS tests performed after longer immersion times in the different electrolytes, as well as the 9 salt spray tests, showed that samples protected with the passive layer obtained from the bath containing Cr (III) and Co (II) ions may present similar performance to those protected with the Cr (VI) conversion layer. The microstructural analysis and fitting of the EIS diagrams with equivalent circuits indicated an important role of corrosion products in the anti-corrosive performance of the samples protected with the passivation layer of Cr (III) and Co (II). In the studied conditions, the samples protected with the ethylene copolymer did not showed comparable performance to the other two passivation layers investigated in the present study.

O objetivo principal deste trabalho foi adicionar novos módulos (tanto eletrônicos quanto computacionais) necessários para efetuar medidas espectroscópicas com o microscópio de tunelamento construído há alguns anos no Laboratório de Novos Materiais Semicondutores do Instituto de Física da USP. Para checar a performance do novo sistema implementado, foram realizadas medidas sobre materiais condutores (grafite e ouro). Visando a análise topográfica e espectroscópica de amostras semicondutoras dos grupos III-V, estudamos alguns métodos para a preparação destas superfícies. Dentre eles, a passivação foi capaz de fornecer os resultados mais significativos. Finalmente, curvas da corrente de tunelamento em função da tensão aplicada à junção foram adquiridas sobre amostras de GaAs e pontos quânticos de InAs crescidos pela técnica de epitaxia por feixe molecular (MBE). / The goal of the present work was to upgrade the home-made Scanning Tunneling Microscope present in our group, adding the new hardware necessary to carry out spectroscopic measurements. A new software was also developed to control the new functions of the microscope. In order to check the performance of the whole system, several types of experiments where carried out on graphite and gold. A special care was taken to adequately prepare the samples of III-V semiconductors. The passivation of the sample yielded the best results both for topographic and spectroscopic measurements. Finally, I-V curves were taken on GaAs layers and InAs quantum dots grown by molecular beam epitaxy (MBE).

As estruturas metal-óxido-semicondutor (MOS) são o coração dos transistores de efeito de campo. O estudo e caracterização físico-química desses dispositivos foram a chave para o avanço da tecnologia do Si na indústria microeletrônica. Hoje, a ciência busca novos materiais para a produção de dispositivos de alta mobilidade. Um dos materiais visados é o Ge, pois apresenta mobilidade de cargas superior ao Si (duas vezes para elétrons e quatro vezes para lacunas). Porém, a interface Ge/GeO2 é de natureza reativa, limitando seu uso na construção de tais dispositivos. Muitos esforços têm sido feitos para superar as limitações. Entre eles, encontram-se a passivação da superfície do Ge a partir de solução aquosa de (NH4)2S, previamente a deposição do dielétrico. Outra etapa do processamento desse material na indústria a ser investigada são os tratamentos térmicos posteriores à deposição: a caracterização de estruturas MOS de Pt/HfO2/Ge submetidas a tratamentos térmicos levaram a melhoria das propriedades elétricas. Nesse sentido, o trabalho tem como objetivos investigar o papel da passivação sulfídrica em estruturas dielétrico/Ge e a influência do eletrodo de Pt nas estruturas Pt/HfO2/Ge quando submetidas a tratamentos térmicos. / The heart of field effect transistors is the metal-oxide-semiconductor (MOS) structure. Physico-chemical characterization of the materials employed in such structures enabled the development of Si technology. Nowadays, in order to build high mobility devices, new material are needed. Ge is an alternative material, since its carrier mobilities are higher than those of Si (almost two times for electrons and four times higher for holes). However, the GeO2/Ge interface is not thermally stable, which is a problem for its use on electronic devices. Many attempts to enhance this stability were already investigated. Among them, sulfur passivation of the Ge surface was employed using (NH4)2S aqueous solution prior to the deposition of dielectric layers. Another important step in the fabrication of MOS structures is post-deposition annealing. Pt/HfO2/Ge MOS structures presented improved electrical characteristics following post deposition annealing. The main objectives of this work are to investigate the role of sulfur passivation on dielectric/Ge structures and the influence of Pt electrode in Pt/HfO2/Ge structures submitted to post deposition annealing.

This thesis deals with pre-treatment of surface of aluminium alloys. The theoretical part focuses on the properties of aluminium and its alloys, on methods of surface treatment and the possibilities of quality assessment of pre-treated surface. The experimental part deals with finding of a proper method of pre-treatment. The quality of surface pre-treatment is assessed by observation by SEM with EDS and by single lap shear tests of adhesive joints. According to evaluated results, the optimalised methods are qualitatively and financially compared with the commercial method.

Diploma thesis deals with the technology of surface modifications of magnesium alloys. Basic knowledge from the field of the corrosion of metal materials. The division corrosion according to way of attack and corrosion environment, etc. There is an enumeration of ways of the corrosion defence. Questions of surface modifications with an emphasis on passivation by conversion coating and its analysis. Characteristics of magnesium and its alloys. Magnesium alloys with lithium, possibilities of its passivation and the verification of corrosion resistance. Enumeration of the used devices, chemicals and materials. characteristics of the used alloys. creation of the corrosion resistance standard. Research in passivation on the alloy containing 12 percent of lithium. The verification of the corrosion test usability based on the suggestion of the background research results. The test results for passivated as well as untreated samples and the reference material (steel). Aplication of chromate-free passivation and corrosion test on the alloy containing 12 percent of lithium.

The work deals with a comparison of existing and perspective types of passivation and anti-reflective coating for silicon solar cells. The theoretical part describes the appropriate methodology for the characterization of these layers and focuses on the passivation layers based on Al2O3. The practical part describes design and verification operations of the equipment for measuring of the amount of fixed charge in the passivation layers using corona discharge. It also describes the implementation of equipment and the results of indicative tests for positive and negative polarity of high voltage. The final part discusses the possibility of equipment improving.

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<p dir="ltr">Since before the Apollo era, the rocket propulsion sector has been a key player in developing standards of cleanliness and compatibility when designing, building, and operating systems with toxic propellants. The advent of hypergols and the widespread use of propellants like N₂O₄, Mixed Oxides of Nitrogen (MON), and hydrazine have forced new standards to be developed to meet the ever-growing need for safety when working with dangerous substances. These systems have only continued to grow more complex and many propellant combinations remain toxic and corrosive to most substances as the industry seeks the optimal methods for deriving the most efficient, highest performing, and generally more capable. ASTM International and other standards organizations carry on documenting standards for cleaning and passivation to ensure safe use today to meet the needs of the ever-expanding propulsion industry.</p><p dir="ltr">This thesis aims to determine the feasibility of using Raman spectroscopy as a method of characterizing interactions between metals and propellants. First, a background of knowledge regarding the spectroscopic method, propellants, and industry practices was researched and current areas of possible application were identified. The passivation and propellant storage phases of system lifecycles were determined to be the scope and target for experimentation. A multilevel passivation study consisting of exposing three metal types to different concentrations of nitric acid for various durations was conducted to begin developing a greater understanding of the applicability of and the techniques required to make Raman spectroscopy work as a complement to the ASTM passivation verification tests. Lessons learned from this and a short-duration compatibility study with MON and similar metal samples were documented and will be used for a larger scale and longer duration compatibility study in conjunction with NASA White Sands Test Facility (WSTF). The buildup of safe and adequate facilities for such a study was undertaken, completed, and documented in this work.</p><p dir="ltr">The results of testing in this thesis suggest the promising and desirable non-destructive and minimally invasive features of Raman spectroscopy have the potential to be used extensively in the propulsion sector. Suggestions for developing key techniques and methods for this application are developed and outlined as they were learned throughout the study's conduction.</p>