Thermo-stabilized lignin fibers from pH-fractionated softwood kraft lignin were carbonized to various temperatures during thermomechanical analysis (TMA) under static and increasing load and different rates of heating. The aim was to optimize the carbonization process to obtain suitable carbon fiber material with good mechanical strength potential (high tensile strength and high E-modulus). The carbon fibers were therefore mainly evaluated of mechanical strength in Dia-Stron uniaxial tensile testing. In addition, chemical composition, in terms of functional groups, and elemental (atomic) composition was studied in Fourier transform infrared spectroscopy (FTIR) and in energy-dispersive X-ray spectroscopy (EDS), respectively. The structure of carbon fibers was imaged in scanning electron microscope (SEM) and light microscopy. Thermogravimetrical analysis was performed on thermo-stabilized lignin fibers to evaluate the loss of mass and to calculate the stress-changes and diameter-changes that occur during carbonization. The TMA-analysis of the deformation showed, for thermo-stabilized lignin fibers, a characteristic behavior of contraction during carbonization. Carbonization temperatures above 1000°C seemed most efficient in terms of E-modulus and tensile strength whereas rate of heating did not matter considerably. The E-modulus for the fibers was improved significantly by slowly increasing the load during the carbonization. The tensile strength remained however unchanged. The FTIR-analysis indicated that many functional groups, mainly oxygen containing, dissociate from the lignin polymers during carbonization. The EDS supported this by showing that the oxygen content decreased. Accordingly, the relative carbon content increased passively to around 90% at 1000°C. Aromatic structures in the carbon fibers are thought to contribute to the mechanical strength and are likely formed during the carbonization. However, the FTIR result showed no evident signs that aromatic structures had been formed, possible due to some difficulties with the KBr-method. In the SEM and light microscopy imaging one could observe that porous formations on the surface of the fibers increased as the temperature increased in the carbonization. These formations may have affected the mechanical strength of the carbon fibers, mainly tensile strength. The carbonization process was optimized in the sense that any heating rate can be used. No restriction in production speed exists. The carbonization should be run to at least 1000°C to achieve maximum mechanical strength, both in E-modulus and tensile strength. To improve the E-modulus further, a slowly increasing load can be applied to the lignin fibers during carbonization. The earlier the force is applied, to counteract the lignin fiber contraction that occurs (namely around 300°C), the better. However, in terms of mechanical performance, the lignin carbon fibers are still far from practical use in the industry.

In der vorliegenden Arbeit wurden Untersuchungen zum Initiierungs- und Ausbreitungsverhalten kurzer Ermüdungsrisse in einem austenitischen sowie einem austenitisch-ferritischen Edelstahl durchgeführt. Dazu erfolgten zyklische Verformungsexperimente sowohl ex situ als auch in situ im Rasterelektronenmikroskop. Die Auswertung der Experimente erfolgte im Rasterelektronenmikroskop sowohl abbildend in verschiedenen Modi als auch über Rückstreuelektronenbeugungsmessungen. Bezüglich der Rissinitiierung wurde eine Häufigkeitsverteilung der Rissinitiierungsorte für beide Stähle erstellt. Die dabei ermittelte stark unterschiedliche Häufigkeit für die transkristalline Rissinitiierung in der austenitischen Phase konnte mit der unterschiedlichen Textur und Mikrostruktur der beiden Stähle in Zusammenwirken mit den elastischen Eigenschaften der beiden Phasen erklärt werden. Für die Rissausbreitung wurde gezeigt, dass eine Korrelation zwischen der Risslänge und der Rissausbreitungsrate besteht, aus der hervorgeht, dass die Übergangsrisslänge zwischen den Bereichen der mikrostrukturell und mechanisch kurzen Risse etwa einen Korndurchmesser beträgt. Anhand der in situ Messung der (plastischen) Rissöffnung und -scherung wurden die Unterschiede im Rissausbreitungsverhalten in den verschiedenen Phasen herausgearbeitet. Für die austenitische Phase ergibt sich dabei ein öffnungsdominierter und für die ferritische Phase ein scherungsdominierter Mechanismus. Die im Ferrit auftretenden zwei unterschiedlichen Ausprägungen der Oberflächenrisspfade („rau“ und „glatt“) konnten mit der Orientierung der jeweils risstragenden Körner korreliert werden. In Zusammenwirken mit der beobachteten Systematik der Anordnung der Gleitspuren um kurze Risse im Ferrit sowie einer Analyse der Spannungsverteilung um die Rissspitze wurde ein Modell des Rissausbreitungsmechanismus\' erstellt sowie die bisher in der Literatur vorherrschende These des Einfachgleitens widerlegt. Schließlich konnte die Barrierenwirkung von Korn- und Phasengrenzen sowohl anhand der Messung der Rissausbreitungsrate als auch der plastischen Rissöffnung bzw. -scherung gezeigt und daraus Rückschlüsse auf die Ausdehnung der plastischen Zone vor der Rissspitze gezogen werden. Gleichzeitig wurde dabei die Korrelation zwischen Rissausbreitungsrate und plastischer Rissöffnung bzw. -scherung nachgewiesen.

A ação do instrumento endodôntico nas paredes do canal leva à formação de debris dentinários. Sua remoção é principalmente função das manobras de irrigação. Entretanto, a ação do instrumento pode facilitar ou não o acúmulo dos debris dentinários, principalmente em função da sua cinemática. O sistema Twisted File (TF) Adaptive (SybronEndo, Orange, CA) combina o movimento rotatório contínuo e reciprocante e o sistema Reciproc (VDW, Munique, Alemanha) realiza o preparo do canal radicular pelo movimento reciprocante puro. Os objetivos deste estudo foram, utilizando a microtomografia computadorizada (micro-CT): avaliar, ex vivo, o preparo (aumento de volume e superficies não preparadas) e quantificar o acúmulo de debris dentinários em canais ovais longos comparando os sistemas TF Adaptive e Reciproc; avaliar o efeito da irrigação ultrassônica ativada intermitente (IUAT) após o preparo químico-cirúrgico com os sistemas propostos, na redução de debris dentinários; e relacionar a presença de debris dentinários com o magma dentinário avaliado por meio do microscópio eletrônico de varredura. Canais distais de trinta e oito molares inferiores foram selecionados e divididos em dois grupos: G1 - TFA (n=19) e G2 - RC (n=19). Cada espécime foi submetido a três escaneamentos: prée pós-operatório e pós-irrigação ultrassônica passiva final. Após a reconstrução das imagens resultantes dos três escaneamentos, foi feito o corregistro das mesmas com o programa DataViewer. Os programas CTAn e CTvol foram utilizados para binarização dos objetos de interesse, avaliações morfométricas e reconstrução dos modelos tridimensionais. Foram mensurados o aumento de volume do canal, as superfícies não preparadas e os debris dentinários após o preparo químico-cirúrgico. Após a irrigação final, cinco raízes de cada grupo foram clivadas longitudinalmente ao meio no terço apical e analisadas no microscópio eletrônico de varredura (MEV) quanto à presença de magma dentinário. O sistema de pontuação utilizado foi o de Hülsmann et al. (1997). Os resultados foram analisados pelo programa Bioestat e mostraram uma distribuição não-paramétrica pelo teste D\'Agostino. Por esta razão, para a análise dois a dois entre os grupos foi utilizado o teste de Mann-Whitney. Na análise intra-grupo, o teste de Kruskal-Wallis foi o escolhido, com complementação do teste de Dunn quando necessário. Os dados obtidos mostraram que o sistema TF Adaptive removeu mais dentina quando todo canal foi considerado (p<0,05). Entretanto, não houve diferença estatisticamente significante quanto à porcentagem de superfície não preparada em ambos os sistemas (p>0.05). Em relação ao acúmulo de debris dentinários e redução de debris dentinários pós-irrigação ultrassônica passiva, também não houve diferença entre os grupos (p>0.05). A IUAI promoveu redução significativa de debris dentinários, à exceção do terço apical. Qualitativamente, no MEV, observou-se magma dentinário não-homogêneo cobrindo a parede do canal, especialmente no grupo Reciproc. Conclui-se que nenhum sistema conseguiu preparar completamente as paredes de canal radicular oval longo e que a IUAI reduz os debris dentinários na ordem de 60-70%. Na análise do MEV, pode-se observar que não houve correlação entre a redução de debris dentinários e o magma dentinário. / The action of the endodontic instrument leads to hard-tissue debris. The main goal of the irrigation procedures is its removal. Nevertheless, depending on its kinematics the rotary file can contribute to the removal of hard-tissue debris. The TF Adaptive system (SybronEndo, Orange, CA) combines the rotary and reciprocating movement and the Reciproc system (VDW< Munique, Alemanha) with pure reciprocating movement, removes significant quantities of dentin of the canal wall with more difficulties of pulling out hard-tissue debris. The aims of this study were, using microcomputed tomography: evaluate preparation and quantify hard-tissue debris reduction in long-oval canals comparing TF Adaptive and Reciproc systems; evaluate the effect of passive ultrassonic irrigation (PUI) after preparation with the proposed groups in the accumulation of hard-tissue debris; and correlate the presence of hardtissue debris with smear layer evaluated by scanning eléctron microscope (SEM). Distal canals of thirty-eight lower molars were selected and divided in two groups: G1 - TFA (n=19) and G2 - RC (n=19). Each specimen was scanned three times: preand post-instrumentation of the root canal; and post-passive ultrassonic irrigation. After reconstruction of the scanned images, a co-registration was done with DataViewer. The softwares CTan and CTvol were used for binarization of the objects of interest, morphometrics alterations and reconstruction of tridimensional models and hard-tissue debris models. Volume increasing, non-prepared surfaces and hardtissue debris after instrumentation were measured. After final irrigation, the root canals were clived in halves at the apical third and analyzed by scanning eléctron microscope related to smear layer. The score system described by Hülsmann et al. (1997) was used. The results showed a non-parametric distribution by D\'Agostino test. For that reason, Mann-Whitney test was used to compare the experimental groups and the Kruskall-Wallis test to compare intra-group performance. Dunn test determined which sample was different. Data shows that TF Adaptive removed more dentin in the whole root canal (p<0,05). There was no significant statistic difference comparing non-prepared surfaces between the systems (p>0,05). Related to hardtissue debris and reduction of hard-tissue debris after passive ultrassonic irrigation, there was no significant difference between TF Adaptive and Reciproc. The PUI reduced significantly hard-tissue debris, except for the apical third. The scanning electron microscope (SEM) showed a non-homogeneous smear layer covering the canal dentin walls, specially the Reciproc group. It was concluded that no system completely prepared the dentin walls of long-oval root canals and the passive ultrassonic irrigation decreased hard-tissue debris about 60-70% in the evaluated systems. SEM analysis reported no correlation between hard-tissue reduction and smear layer.

O presente estudo in vitro analisou o efeito de 3 sucos de fruta com baixo pH (suco de cupuaçu, taperebá e laranja), e saliva artificial (controle) sobre materiais restauradores indicados em lesões cervicais não cariosas: resina composta nanoparticulada (Filtek Z350 XT), cimento de ionômero de vidro resino modificado (Vitremer) e um cimento de ionômero de vidro convencional (Fuji II). Os materiais foram avaliados, quantitativamente, quanto à alteração de: peso, rugosidade superficial e microdureza superficial, e qualitativamente, por microscopia eletrônica de varredura (MEV). Foram confeccionados 144 corpos de prova para cada teste quantitativo (n=12) e 45 para o MEV (n=3), de (8mm de diâmetro x 2mm de altura). Os corpos de prova foram preparados, mantidos em saliva artificial por 24 h à 37º C, receberam acabamento em politriz, e em seguida foram realizadas as leituras iniciais. Durante um período de 10 dias consecutivos, os corpos de prova foram submetidos ao desafio erosivo (nos respectivos sucos de frutas) durante 30 minutos três vezes ao dia, totalizando 90 minutos/dia e mantidos em saliva artificial entre os intervalos. Após o período de ciclagem erosiva, foram realizadas as leituras finais. Os resultados obtidos foram submetidos ao teste t, ANOVA e Tukey. As médias de alteração entre os valores de peso finais e iniciais demonstraram diferença significativa (p<0,01) nos materiais estudados e em todos os sucos estudados, com exceção do Vitremer quando imerso no suco de taperebá (p>0,01). As médias de alteração entre os valores de rugosidade superficial final e inicial demonstraram diferença significativa (p<0,01) para todos os materiais estudados em todos os sucos, exceto a Filtek Z350 XT no grupo controle que não apresentou diferença significativa (p>0,01). A comparação entre os valores de microdureza final e inicial demonstrou diferença significativa (p<0,01) na microdureza dos materiais estudados em todos os meios de imersão, inclusive no grupo controle. De um modo geral o suco de taperebá foi o que provocou a maior alteração na superfície dos materiais restauradores quanto ao peso, rugosidade, microdureza e na microscopia eletrônica de varredura. A resina composta Filtek Z350 XT foi o material restaurador que menos sofreu alterações de superfície. Concluiu-se que os sucos das frutas estudados são capazes de alterar os materiais restauradores, sendo que a resina composta foi o material que sofreu menor alteração. / This in vitro study examined the effects of 3 fruit juices with low pH (cupuaçu, taperebá and orange) and artificial saliva (control) upon restorative materials indicated in noncarious cervical lesions: nanoparticle composite resin (Filtek Z350 XT), resin-modified glass ionomer cement (Vitremer) and a glass ionomer cement (Fuji II). The materials were evaluated quantitatively as for alterations in weight, surface roughness and surface microhardness, and qualitatively by scanning electronic microscopy (SEM). 144 specimens were prepared for each quantitative test (n = 12) and 45 for the SEM (n = 3), of (8mm diameter x 2mm height). The specimens were prepared, stored in artificial saliva for 24 hours at 37º C, were finished in a polishing machine, and then the initial readings were performed. During a period of 10 consecutive days, the specimens were subjected to erosive challenge (in the respective juices) for 30 minutes, three times a day, and totaling 90 minutes/day and kept in artificial saliva between intervals. After the erosive cycling period, the final readings were taken. The data were analyzed using t test, ANOVA and Tukey.Test The average alterations between the values of initial and final weight showed significant difference (p < 0.01) in the material studied and all the juices studied, except for Vitremer when immersed in taperebá juice (p > 0.01). The average alterations between the values of initial and final surface roughness showed a significant difference (p < 0.01) for all materials studied in all juices, except for Filtek Z350 XT, in the control group, that showed no significant differences (p > 0.01). The comparison between the values of initial and final microhardness showed a significant difference (p < 0.01) in microhardness of the materials studied in all immersion means, including the control group. In general, taperebá juice was the one that caused the biggest alterations in the surface of restorative materials with respect to weight, roughness, hardness and scanning electronic microscopy. The composite resin Filtek Z350 XT was the restorative material that suffered less surface alterations. It was concluded that the fruit juices studied are capable of altering the restorative materials, and composite resin was the material that has undergone minor changes.

Introdução - A malária é uma das principais doenças humanas do mundo e afeta principalmente as populações pobres em regiões tropicais e subtropicais onde as condições ambientais são favoráveis tanto para a proliferação dos agentes etiológicos como dos mosquitos vetores. No Brasil, An. darlingi é considerado vetor primário de plasmódios humanos. Devido à importância médica, esse inseto tem sido objeto de campanhas de controle populacional. No entanto, não foi considerada a ocorrência de microevolução em An. darlingi e consequentemente, a possibilidade de populações diferentes apresentarem características biológicas distintas. Objetivo Verificar a presença de variabilidade genética e morfológica em populações de An. darlingi no Brasil. Metodologia - Foram analisados e comparados 26 atributos da morfologia externa de ovos de nove populações, bem como a morfometria geométrica da forma alar de espécimes de 10 localidades diferentes de Anopheles darlingi. Além disso, foram empregadas sequências do gene mitocondrial citocromo oxidase subunidade I (COI) para analisar a estrutura populacional de An. darlingi. Resultados e Conclusão Apesar dos atributos dos ovos apresentarem variação, somente as amostras de Tocantins e Pará foram diferenciadas das demais populações. As variações nas estruturas externas dos ovos são provavelmente adaptativas, com influência de fatores ambientais, como temperatura, umidade e disponibilidade de alimento para as fêmeas. A comparação da morfometria geométrica da asa demonstrou que existe maior similaridade entre as populações da costa (estados do Espírito Santo , do cerrado (estados de Goiás e Tocantins), do norte do rio Amazonas (estados do Amazonas e Amapá), e do sul do rio Amazonas (estados de Mato Grosso e Pará). As análises de COI demonstraram diferenciação das populações da costa da Mata Atlântica em relação às demais populações do Brasil central, Amazônia e Mata Atlântica do Interior. O padrão da diversidade de haplótipos de COI, os testes de neutralidade e a distribuição de diferenças pareadas indicaram recente expansão demográfica. A distância geográfica, as ecorregiões e fatores ambietais podem provavelmente limitar a dispersão da espécie, tendo alguma influência sobre a estrutura populacional de An. darlingi / Introduction Malaria is a major human disease that primarily affects poor persons in tropical and subtropical regions where environmental conditions are favorable to the proliferation of the etiological agent as well as vector mosquitoes. In Brazil, Anopheles darlingi is considered a primary vector of human plasmodia and has been the target of control campaigns because of its medical importance. However, the occurrence of microevolution in An. darlingi was not considered and, consequently, the possibility of different populations exhibit distinct biological characteristics. Objective Verify the presence of morphological and genetic variability in Brazilian Anopheles darlingi populations. Methods Twenty six attributes of external egg morphology were analyzed and compared in nine populations. Similarly, the geometric morphometry of wing shape was evaluated in ten An. darlingi localities. In addition, the mitochondrial gene cytochrome oxidase subunit I (COI) was employed to analyze the population structure of An. darlingi. Results and Conclusion - Although, egg attributes showed variation, only samples from Tocantins and Pará were differentiated from other populations. Variation in external egg structure is arguably adaptive in light of environmental factors such as temperature, humidity and food availability for females. Comparisons of wing geometric morphometry indicated that there is greater similarity between Coastal (Espírito Santo and Rio de Janeiro states) and Inner (São Paulo and Paraná states) populations of the Atlantic Forest, and differentiation of those from (Goiás and Tocantins states) and regions both north (Amazonas and Amapá states) and south (Pará and Mato Grosso states) of the Amazon Region. Cytochrome oxidase I analyses indicated differentiation between coastal Atlantic Forest populations (Espírito Santo and Rio de Janeiro states) and those from the cerrado, the Amazon and the interior Atlantic Forest. The pattern of COI haplotype diversity, neutrality tests and distribution of pairwise differences suggest a recent demographic expansion. Geographical distance, ecoregions and potentially environmental constraints may limit the species´ dispersal and influence the population structure of An. darlingi

Esta pesquisa apresenta os resultados obtidos com o emprego de um método físico para aumento da resistência de concretos projetados a pequenas idades. O método consiste na aplicação de gradientes elétricos ao material logo após a projeção, sendo mantido nas primeiras 5:30 h de hidratação. O comportamento mecânico do concreto projetado submetido a gradientes elétricos foi analisado em termos da resistência à compressão e módulo de elasticidade a partir da resposta de modelos estruturais e de amostras extraídas de estruturas projetadas em diferentes idades. Os modelos estruturais foram desenvolvidos para simular esforços ao concreto projetado semelhantes àqueles resultantes da interação solo-suporte em obras subterrâneas. A projeção do concreto nestes modelos ocorreu diretamente sobre o solo, permitindo assim a análise da eficiência do método sob condições de fuga de corrente elétrica para o maciço em diferentes tipos de solos. A instrumentação destes modelos permitiu analisar a eficiência do método sobre a deformabilidade do concreto projetado, sendo medidas as evoluções de deformações elásticas e deformações de fluência ao longo do tempo bem como deformações independentes de tensões desde as primeiras horas de hidratação. Constataram-se acréscimos na resistência nas primeiras 8 h de idade do concreto projetado em projeção sobre placas de madeira e diretamente sobre o solo. O módulo de elasticidade obtido a partir da instrumentação da resposta instantânea ao carregamento também constatou melhorias pela aplicação do gradiente elétrico. A reologia do concreto projetado, a partir das parcelas de deformações instantânea, retardada e lenta foi analisada utilizando-se o modelo proposto por SCHUBERT (1988). Melhorias foram observadas na resposta em termos de deformações do concreto projetado quando submetidos ao gradiente elétrico, apresentando menores taxas de evolução de deformações lentas em resposta a carregamentos iniciados em idades inferiores a 10 h e redução da parcela de deformação permanente frente ao descarregamento. A investigação dos fatores que provocam acréscimos na resistência a pequenas idades pela aplicação de gradientes elétricos a pastas e argamassas foi realizada utilizando-se técnicas de Microscopia Eletrônica de Varredura e Difratometria de Raio X. Constataram-se alterações na microestrutura de argamassas submetidas a gradiente elétrico, sem alteração nos compostos hidratados. Alterações na taxa de hidratação foram evidenciadas pela comparação de padrões difratométricos entre pastas submetidas a gradientes elétricos e pastas de referência. / This work presents the results obtained by employing a physical method for the strength increase of shotcrete at early age. The method consists of applying electric gradient to the material during the first 5 hours and 30 minutes of hydration, starting immediately after spraying. The mechanical behavior of shotcrete subjected to electric gradient was evaluated at different ages in terms of unconfined compressive strength and elastic modulus obtained from the response of structural models and on samples cored from the structural models. Shotcrete structural models were constructed in order to simulate internal forces resulting from ground mass - support interaction in underground works. Shotcrete in these models was sprayed directly on soil. It was thus possible to analyse the efficiency of the method when leakage currents occur through the soil. Model instrumentation alloed to evaluate the method efficiency in terms of shotcrete deformability. The evolution of elastic and creep strains were evaluated, as well as stress-independent strains since the beginning of hydration. Strength increase during the first 8 hours of age were observed both on panels shotcreted on wooden forms and directly on soil. The elastic modulus was also obtained from the analysis of the instantaneous strain reponse to the applied load. Improvement due to electric gradient was also found this way. Shotcrete rheology in terms instantaneous, delayed and creep strains was analyzed adopting the model proposed by SCHUBERT (1988). Improvement due to the electric gradient was found with respect to each of those strain components resulting from load applied at ages lower that 10h. Permanent strain after unloading was also reduced. The investigation of the phenomena responsible for the strength increase at early age due to the application of electric gradient to cement paste and mortar was carried out with the techniques of scanning electron microscope and X-ray diffraction. Microstructure changes were found in mortar speciments subjected to electric gradient, however without any change of hydrated products. Hydration rate changes were detected from diffractometric patterns of cement pastes subjected to electric gradient.

Master´s thesis is focused on diagnostics of semiconductor materials by EBIC method (measuring of currents induced beam), determination of the lifetime of minority carriers, or their diffusion length. The theoretical part is aimed at the principle of scanning electron microscopy, the characteristic properties of the microscope and the signals generated by the interaction of the primary electron beam with the sample. The thesis describes a structure of semiconducting silicon, band models, types of lattice defects and doped of semiconductor structures. After that it is described the theory of calculation of the diffusion length of minority carriers in semiconductors of type N and P. The aim of the experiment part of the thesis is to measure the properties of the semiconductor structure by EBIC and determination of diffusion length and lifetime of minority charge carriers based on the measured data The aim of the experiment part of the thesis is to measure the properties of the semiconductor structure by EBIC and determination of diffusion length and lifetime of minority charge carriers on the basis of the measured data.

The dissertation thesis deals with optimization of the scintillation detector for efficient detection of low energy signal electrons in a specimen chamber of a scanning electron microscope. The solution was based on the study of signal electron energy loss mechanisms during their interaction with a conductive layer and a scintillator that can be studied using simulations based on the stochastics Monte Carlo methods. Based on test simulations and their comparison with experimental data, the ideal Monte Carlo software was chosen and used for the study of signal electron energy losses during their transport through the conductive layer as well as following interaction with scintillator, in dependency on the signal electron energy. Simulation results allowed to define criteria for the optimization of the conductive layer. According to these parameters, the optimized layers were deposited on the surface of different scintillators and experimentally tested in the scintillation detector of the scanning electron microscope. Experimental measurements allowed to verify accomplished simulations and provide new information about impact of materials and thicknesses of conductive layers in combination with materials of scintillators and light guides. The increase of the detection efficiency of the scintillation detector equipped with optimised conductive layers and its capability to detect low energy signal electrons were experimentally proved.

In this master’s thesis, a mechanical design of an in-column secondary electrons (SE) detector is presented. It is an ultravacuum compatible fibre-scintillation detector designed for use in an ultrahigh vacuum scanning electron microscope (UHV SEM). The designed in-column SE detector was manufactured and tested upon overcoming R&D challenges. The first section of this thesis deals with theoretical basis needed for understanding of functional principles of UHV SEM system and means of SE’s detection. In the second section, mechanical design of the in-column SE detector is described. The last section describes functionality of the designed detector. Effectiveness of light shielding of the detector was tested and the detective quantum efficiency was measured. Finally, images created by the designed in-column detector and an in-chamber SE detector were evaluated and compared.

This thesis deals with the influence of process parameters on the contamination level of powder materials produced by mechanical alloying (MA) technology. For this purpose austenitic stainless steel 316 L and equiatomic CoCrFeNi high-entropy alloy (HEA) were prepared by high-energy ball milling. Both materials were milled in argon and nitrogen atmospheres from 5 to 30 hours. Spark plasma sintering method (SPS) was then used for consolidation of chosen powder samples. Chemical analysis of contamination within MA was carried out using combustion analysers for determination of carbon, oxygen, and nitrogen contents after different lengths of milling. Also differences in chemical composition of powder and corresponding bulk samples were measured. The microstructure analysis using scanning electron microscopy (SEM) of both powder and bulk materials was executed with focus on oxide and carbide presence and dispersion. Increasing content of carbon with increasing milling time was observed across all measured samples. This contamination is attributed to using milling vial made of tool steel AISI D2 (containing 1,55 wt. % of carbon). Increase of carbon content within consolidation using SPS was also observed. Milling of specimens using N2 as milling atmosphere caused higher contamination level in both AISI 316 L and HEA compared to milling in argon.