Submitted by Mateus Gallucci Masteghin (mgmasteghin@gmail.com) on 2018-06-26T11:25:57Z No. of bitstreams: 1 masteghin_mg_me_araiq_int.pdf: 9325879 bytes, checksum: ad179c16b4a7ebea4933249a05a03ba1 (MD5) / Approved for entry into archive by Ana Carolina Gonçalves Bet null (abet@iq.unesp.br) on 2018-06-28T17:19:59Z (GMT) No. of bitstreams: 1 masteghin_mg_me_araiq_int.pdf: 9325879 bytes, checksum: ad179c16b4a7ebea4933249a05a03ba1 (MD5) / Made available in DSpace on 2018-06-28T17:19:59Z (GMT). No. of bitstreams: 1 masteghin_mg_me_araiq_int.pdf: 9325879 bytes, checksum: ad179c16b4a7ebea4933249a05a03ba1 (MD5) Previous issue date: 2018-06-06 / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Nesse trabalho, realizou-se um estudo a fim de compreender os mecanismos de transporte e as interações gás-sólido que ocorrem na superfície de nanoestruturas de SnO, Sn3O4 e SnO2, preparadas em diferentes dispositivos. Com o objetivo de se obter uma melhor compreensão dos fenômenos envolvidos, optou-se por estudar, individualmente e coletivamente (única e mútiplas), as nanofitas de cada uma das três composições, sendo que o primeiro método permite descartar interferências extrínsecas, analisando-se apenas os mecanismos intrínsecos de condução nas nanoestruturas, sem a presença de barreiras de potencias geradas pelo contato semicondutor/semicondutor e, na maioria dos casos, sem o possível contato não-ôhmico metal/semicondutor. Para isso, os materiais foram sintetizados pelo método de redução carbotérmica e, posteriormente, foram caracterizados por DRX, Raman, UV-Vis e MEV-FEG para confirmar a eficácia da síntese, parte fundamental para a obtenção de resultados confiáveis. Os materiais também foram caracterizados em relação à sua resposta como sensor de gás na presença de gases oxidantes e redutores (por exemplo, NO2 e CO) em baixas concentrações (na escala de ppm) e em temperaturas de trabalho entre 100 °C e 350°C, sendo que para atingir tais temperaturas utilizou-se o método convencional de aquecimento e o método de self-heating, sendo o último promissor por não necessitar de fonte externa para realizar o aquecimento, gerando economia de energia e possibilitando maior mobilidade na detecção de vazamentos. As principais novidades deste trabalho são a caracterização individual de nanofitas de Sn3O4 e des micro-discos de SnO como sensor de gás, o estudo da resposta sensora de nanofitas de mesma composição química com diferentes diâmetros (em nano escala), permitindo o cálculo da camada de depleção (comprimento de Debye) para cada estequiometria, e na escolha do método self-heating de aquecimento para o estudo sensor das estruturas de SnO e Sn3O4. Para realizar esses estudos, fabricou-se dispositivos individuais utilizando trilhas interdigitais e eletrodos específicos em um equipamento de feixe duplo (Focused Ion Beam - FIB) equipado para realizar litografia eletrônica. Deste modo, a principal contribuição do trabalho para a literatura será o estudo das interações sólido-gás em materiais termodinamicamente instáveis (SnO e Sn3O4), no estudo de como o gás analito influencia na espessura da camada de depressão (indiretamente, nas propriedades sensoras) e na utilização de um novo método de sensoriamento de gás (self-heating) para estes materiais. Ao final, espera-se que todo este estudo permita o desenvolvimento de materiais sensores com elevada sensibilidade, seletividade, rápido tempo de resposta e capacidade de miniaturização, sendo essa última característica muito importante quando almeja-se futuras aplicações práticas desse material em dispositivos eletrônicos portáteis. / In the following work, it was carried out a study in order to understand the transport mechanisms and the gas-solid interactions that occur on the surface of SnO, Sn3O4, and SnO2 nanostructures, made-up over different devices. As the main goal of a better understanding regarding involved interaction phenomena, it was chosen to study the nanostructures individually (single-element devices) and as multiple structures (carpet mode devices), in which the former allows to discard extrinsic interferences, such as potential Schottky-type barriers as a result of the semiconductor/semiconductor contact, and in the most of the cases when dealing with single-element devices, without the possible metal/semiconductor non-ohmic contact. Thus, the materials were synthesized by the carbothermal reduction method and characterized by XRD, Raman Spectroscopy, UV-Vis light measurements, and SEM-FEG. The materials were investigated as gas sensors, using oxidizing and reducing gases (such as NO2 and CO) in low concentration levels (ppm), and with working temperatures ranging from 100 °C to 300 °C. These working temperatures were reached using the conventional heating and the self-heating methods, the latter being advantageous for not requiring an external source to the heating, resulting in low dissipated power and allowing higher mobility when seeking for in-situ leakage detections. The highlighted contributions from this work are the Sn3O4 nanobelts and SnO micro-disks characterization as single-element gas sensor devices and the study of different diameters of the same material (nanobelts with same oxidation state), that allowed to calculate the depletion layer length (Debye length) for each stoichiometry; besides the use of the self-heating method in the gas sensor study of SnO and Sn3O4. In the end, the author wishes that all the study performed allows the development of gas sensor devices with high sensitivity, selectivity, fast response and recovery times, and the miniaturization capability. / FAPESP: 2015/21033-0 & BEPE-FAPESP: 2017/12870-0

abstract: With the high demand for faster and smaller wireless communication devices, manufacturers have been pushed to explore new materials for smaller and faster transistors. One promising class of transistors is high electron mobility transistors (HEMT). AlGaAs/GaAs HEMTs have been shown to perform well at high power and high frequencies. However, AlGaN/GaN HEMTs have been gaining more attention recently due to their comparatively higher power densities and better high frequency performance. Nevertheless, these devices have experienced truncated lifetimes. It is assumed that reducing defect densities in these materials will enable a more direct study of the failure mechanisms in these devices. In this work we present studies done to reduce interfacial oxygen at N-polar GaN/GaN interfaces, growth conditions for InAlN barrier layer, and microanalysis of a partial InAlN-based HEMT. Additionally, the depth of oxidation of an InAlN layer on a gate-less InAlN/GaN metal oxide semiconductor HEMT (MOSHEMT) was investigated. Measurements of electric fields in AlGaN/GaN HEMTs with and without field plates are also presented. / Dissertation/Thesis / Doctoral Dissertation Physics 2018

Proteomic studies at the single molecular level could provide better understanding of the protein’s behaviour and the effects of its interactions with other biomolecules. This could have an impact on drug development methods, disease diagnosis, and targeted therapy. Aperture assisted optical trapping is a proven technique for isolating single proteins in solution without the use of tethers or labels, and without denaturing them. Thus enabling studies of protein-protein interactions, protein-small molecule interactions, and protein-DNA interactions. In this work, double nanohole (DNH) optical tweezers were used to analyze the protein composition of heterogeneous mixtures. The trapped proteins were grouped by molecular mass based on two metrics: standard deviation of the trapping laser intensity fluctuations, and the time constant of the autocorrelation function of these fluctuations. The quantitative analysis is demonstrated first for two separate standard-size proteins, then for a mixed solution of both. Finally, the approach is applied to real unprocessed egg white solution. The results correspond well with the known protein composition of egg white found in the literature. The DNH optical tweezers’ ability to distinguish proteins in unpurified heterogeneous mixtures, can progress this technique to the next level, allowing for single biomolecular studies of unprocessed physiological solutions like blood, urine, or saliva. / Graduate

The purpouse of the master's thesis is study problematic of focused ion beams and their material influence. In this thesis are described interactions in the sample after impact of ion beam, use and applications of FIB systems. Second part of thesis are simulations of ion influence on different kinds of materials by the help of SRIM program.

Abstract In this work the LCVD of copper and nickel from the precursor gases Cu(hfac)tmvs and Ni(CO)4 has been investigated. The in-house constructed LCVD system and processes and the practical utilisation of these in prototype integrated circuit edit work are described. The investigated process parameters include laser power, laser scan speed, precursor partial pressure and the effect of H2 and He carrier gases. The deposited metal conductor lines have been examined by LIMA, AFM, FIB secondary electron/ion micrography, and by electrical measurements. Furthermore, the study of experimental FIB circuit edit processes is carried out and discussed with particular emphasis on ion beam induced ESD damages. It is shown how the LCVD and FIB methods can be combined to create a novel method to carry out successfully circuit edit cases where both methods alone will fail. The combined FIB/LCVD- method is shown to be highly complementary and effective in practical circuit edit work in terms of reduced process time and improved yield. Circuit edit cases where both technologies are successfully used in a complementary way are presented. Selected examples of some special circuit edit cases include RF- circuit editing, a high resolution method for FIB-deposited tungsten conductor line resistance reduction and large area EMI shielding of IC surfaces. Based on the research it was possible for a formal workflow for the combined process to be developed and this approach was applied to 132 circuit edit cases with 85% yield. The combined method was applied to 30% of the total number of edit cases. Finally, the developed process and constructed system was commercialized.

Une étude cinétique de l’hydrofluoration du dioxyde d’uranium a été menée entre 375 et 475°C sous des pressions partielles d’HF comprises entre 42 et 720 mbar. La réaction a été suivie par thermogravimétrie isotherme et isobare. Les données cinétiques obtenues, couplées à une caractérisation de la poudre avant, pendant et après réaction par MEB, EDS, DRX et BET, ont montré que les grains de poudre d’UO2 se transforment selon un modèle de germination instantané, croissance anisotropre et développement interne. L’étape limitant la vitesse de croissance est la diffusion d’HF dans la couche d’UF4. Un mécanisme de croissance de la couche d’UF4 a été proposé. Dans le domaine de température et de pression étudié, la réaction est d’ordre 1 par rapport à HF et suit une loi d’Arrhénius. Une équation de vitesse a été déterminée et a servi à effectuer des simulations cinétiques qui ont toutes montré une très bonne corrélation avec l’expérience.Le couplage de cette équation de vitesse avec les phénomènes de transport de chaleur et de matière a permis d’effectuer des simulations à l’échelle d’un agglomérat de poudre. Elles ont montré que certaines structures d’agglomérats influencent la vitesse de diffusion des gaz dans le milieu poreux et par conséquent influencent la vitesse de réaction. Enfin des simulations de vitesse de transformation de tas de poudre et de pastilles ont été réalisées et comparées aux vitesses expérimentales. Les courbes cinétiques expérimentales et simulées ont même allure, mais des améliorations dans les simulations sont nécessaires pour pouvoir prédire avec précision des vitesses : le couplage entre les trois échelles (grain, agglomérat, four) en est un exemple. / A kinetic study of hydrofluorination of uranium dioxide was performed between 375 and 475°C under partial pressures of HF between 42 and 720 mbar. The reaction was followed by thermogravimetry in isothermal and isobaric conditions. The kinetic data obtained coupled with a characterization of the powder before, during and after reaction by SEM, EDS, BET and XRD showed that the powder grains of UO2 are transformed according a model of instantaneous germination, anisotropic growth and internal development. The rate limiting step of the growth process is the diffusion of HF in the UF4 layer. A mechanism of growth of the UF4 layer has been proposed. In the temperature and pressure range studied, the reaction is of first order with respect to HF and follows an Arrhenius law. A rate equation was determined and used to perform kinetic simulations which have shown a very good correlation with experience. Coupling of this rate equation with heat and mass transport phenomena allowed to perform simulations at the scale of a powder’s agglomerate. They have shown that some structures of agglomerates influence the rate of diffusion of the gases in the porous medium and thereby influence the reaction rate. Finally kinetic simulations on powder’s beds and pellets were carried out and compared with experimental rates. The experimental and simulated kinetic curves have the same paces, but improvements in the simulations are needed to accurately predict rates: the coupling between the three scales (grain, agglomerate, oven) would be a good example.

Microtubules play a major role in intracellular trafficking of vesicles in endocrine cells. Detailed knowledge of microtubule organization and their relation to other cell constituents is crucial for understanding cell function. However, their role in insulin transport and secretion is currently under debate. Here, we use Fib-Sem to image islet beta cells in their entirety with unprecedented resolution. We reconstruct mitochondria, Golgi apparati, centrioles, insulin secretory granules and micro-tubules of seven beta cells, and generate a comprehensive spatial map of microtubule-organelle interactions. We find that micro-tubules form non-radial networks that are predominantly not connected to either centrioles or endomembranes. Microtubule number and length, but not microtubule polymer density, vary with glucose stimulation. Furthermore, insulin secretory granules are enriched near the plasma membrane where they associate with microtubules. In summary, we provide the first 3D reconstructions of complete microtubule networks in primary mammalian cells together with evidence regarding their importance for insulin secretory granule positioning and thus supportive role in insulin secretion.

Tato práce se zabývá charakterizací nanovláken na bázi polyvinylidenfluoridu. Zaměření práce je na piezoelektrické vlastnosti vlákna, které jsou studovány metodou piezoelektrické silové mikroskopie. Takto byly měřeny dva typy odlišných vzorků, které se lišily v parametrech výroby. Odlišnosti vláken v jejich fázovém složení byly také zkoumány za využití Ramanovy spektroskopie a infračervené spektroskopie s Fourierovou transformací. Chemická analýza povrchu a jeho stavu proběhla pomocí rentgenové fotoelektronové spektroskopie. Různé uspořádání nanovláken spolu s jejich průřezem bylo pozorováno rastrovacím elektronovým mikroskopem za využití fokusovaného iontového svazku. Rovněž byla zkoumána smáčivost a kontaktní úhel povrchu vzorků s demineralizovanou vodou. Bylo zjištěno, že vyšší rychlost otáček válce během procesu elektrostatického zvlákňování má velmi významný vliv na jejich uspořádání a tím i na parametry ovlivňující tvorbu piezoelektrického jevu a dalších materiálových vlastností.

The main goal of this work is to find a methodology of the fabrication of microcompressive specimens (pillars) from thin metallic film prepared by means of PVD. The studied film was prepared by the ON Semiconductor company, Roznov pod Radhostem. Its chemical composition was Al-1.5 wt.% Cu; such films are used for electric connections on integrated circuits. At first, a thin intermediate layer of W-10 wt.% Ti was deposited on the Si single crystalline substrate with the purpose of improving adhesion properties of the studied film. The geometry of the microcompressive specimen should be as close to the cylindrical shape as possible. The height of the cylinder is given by the film thickness, its diameter is approximately 1 m. Such specimens were prepared in Quanta 3D FEG Dual BeamTM facility using focused ion beams technology. Experiments were done at FEI Company in Brno. In total, 39 microcompressive specimens were prepared at various ion milling conditions. The required geometry was finally attained by the optimization of processing parameters, in particular the parallelism of lateral faces was improved, the bottom of the removed zone in the vicinity of the pillar was almost flat and the transition pillar – flat bottom was regular. The prepared pillars are suitable for the microcompression tests; the first of them have been already performed within the cooperation with the Institut of Physics, Academy of Sciences of the Czech Republic, Praha.

This diploma thesis is focused on the application of Kelvin probe microscopy on graphene fabricated by the chemical vapour deposition. The theoretical part of the thesis deals with basic principles of Kelvin force microscopy and focus ion beam. Further, basic properties of graphene and its possible fabrication methods are discussed. The experimental part is focused on the surface potential measurements on graphene membranes fabricated on the substrate modified by focus ion beam. Finally, atomic force microscope lithography was used for nanopatterning of graphene sheets.