In the past few years, “green technologies and touch screen technologies for portable devices has came to hot topic in consumer market. The demand for transparent conducting oxides (TCO) is increasing continuously. Therefore, the potential replacement of indium tin oxide (ITO), which is the most widely used TCO in industry, by aluminum zinc oxide (AZO) draws much attention in order to solve the problem of shortage of ITO one day due to the consisting of rare-earth element. In this work, electrical and optical properties of AZO had been characterized according to different sputtering parameters such as oxygen contents, working pressures and gas flow ratios. Physics of electrical conduction and optical transparency of AZO films were revealed and analyzed in order to set up a more complete relationship between mechanism and performance. Meanwhile, a comparison of sensitivity between AZO and zinc oxide (ZnO) to sputtering environment had been made and behaviors of AZO at low temperature had been presented. Optimum sputtering conditions for AZO had been established as a function of sputtering time and the film resistivity reached down to 7 x 10-4 Ω·cm while film transmittance was above 85% when t = 140 mins having film thickness about 610 nm. Degradation of AZO had been investigated. Application of AZO in OLED fabrication had been carried out after film refinement and device performance had been given. Finally, simulation of OLED structure was done for better device performance

Submitted by Ranilson Angelo da Silva null (ranilsonangelo@yahoo.com.br) on 2016-10-03T13:42:06Z No. of bitstreams: 1 Tese Doutorado_Ranilson_Final.pdf: 16582757 bytes, checksum: de5b3924045b0020ea737e76aa06ee18 (MD5) / Approved for entry into archive by Ana Paula Grisoto (grisotoana@reitoria.unesp.br) on 2016-10-05T19:07:16Z (GMT) No. of bitstreams: 1 silva_ra_dr_araiq.pdf: 16582757 bytes, checksum: de5b3924045b0020ea737e76aa06ee18 (MD5) / Made available in DSpace on 2016-10-05T19:07:16Z (GMT). No. of bitstreams: 1 silva_ra_dr_araiq.pdf: 16582757 bytes, checksum: de5b3924045b0020ea737e76aa06ee18 (MD5) Previous issue date: 2016-06-29 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / A eficiência dos materiais semicondutores óxidos metálicos utilizados em dispositivos sensores, depende fortemente de parâmetros morfológicos e estruturais. É de grande interesse que os materiais apresentem um elevado grau nos parâmetros de medidas que definem um bom sensor, como: sinal, sensibilidade, seletividade. Devido a isso, métodos de sínteses adequados têm grande influência no desempenho dos dispositivos, já que interferem diretamente na morfologia e estrutura dos materiais semicondutores. Através dessa perspectiva, nesse trabalho, morfologias do composto semicondutor óxido metálico ZnO foram superficialmente modificadas com o intuito de realizar melhorias para aplicações em sensores de gás e de radiação luminosa (fotocondução) na faixa do ultravioleta. Dois métodos de sínteses foram utilizados: i) evaporação térmica por redução carbotérmica e ii) hidrotermal assistido por micro-ondas, responsáveis por obter morfologias tipo tetrapés e estrelas multipontas, respectivamente. Processos de evaporação térmica por redução carbotérmica tem a grande vantagem de obter estruturas com morfologias unidimensionais, em contrapartida, o método hidrotermal assistido por micro-ondas pode sintetizar uma enorme gama de diferentes morfologias com a vantagem de ser um processo rápido e de baixos custos energéticos. Técnicas como microscopia eletrônica de varredura, microscopia eletrônica de transmissão, difração de raios-X, espectroscopia ultravioleta visível e infravermelho, foram utilizadas para caracterizar o material em seu aspecto morfológico e estrutural. Análises em gases como NO2, CO e H2, e da radiação eletromagnética na região ultravioleta, foram realizadas com a finalidade de se obter parâmetros relevantes como, sinal do sensor (para aplicação em sensor de gás) e responsividade (para aplicação em fotocondução), e verificar a performance do ZnO puro e decorado nesses dois seguimentos de aplicação. Através dos resultados e possível observar que houve boa uniformidade das partículas metálicas aderidas à superfície do ZnO. Com relação as respostas do sensor de gás para os materiais puros e decorados houve um aumento do sinal para decoração com Ag na presença do gás H2. Na presença do gás NO2 o material puro obteve um maior sinal, para ambas morfologias. Já para o gás CO, somente é observado uma resposta do sensor para as estrelas multipontas decoradas com platina. A responsividade das amostras de tetrapés foram elevadas em comparação as amostras de estrelas multipontas com valor da ordem de 0,8 A/W. Os resultados obtidos são de fundamental importância para contribuição científica e levanta margem para um foco ainda mais profundo para o desenvolvimento de dispositivos sensores de alto desempenho. / Efficiency of the metal oxide semiconductor materials used in sensor devices, relies heavily on morphological and structural parameters. Is of great interest that the materials have a high degree in the measurement parameters that define a good sensor, such as signal sensitivity, selectivity. Methods suitable synthesis have great influence on the performance of the devices, since they directly affect the morphology and structure of the semiconductor materials. Therefore, in this work, morphologies of the compound semiconductor metal oxide ZnO were surface modified in order to make improvements for applications in gas sensors and light radiation (photoconduction) in the ultraviolet range. Two methods of synthesis were used: i) thermal evaporation by carbothermal reduction and ii) hydrothermal assisted by microwave, responsible for obtaining morphologies type tetrapods and stars multi-point, respectively. Thermal evaporation processes by reduction carbothermic, has the great advantage of obtaining structures with one-dimensional morphology, however, the hydrothermal method assisted by microwave can synthesize a wide range of different morphologies with the advantage of being a quick process and lower costs energy. Techniques such as scanning electron microscopy, transmission electron microscopy, X-ray diffraction, ultraviolet–visible spectroscopy and infrared, were used to characterize the material in its morphological and structural aspect. Analysis of gases such as NO2, CO and H2, and electromagnetic radiation in the ultraviolet region were performed in order to obtain relevant parameters as sensor signal (for use in gas sensor) and responsivity (for use in photoconduction) and check the performance of ZnO and decorated ZnO, in these two application segments. From the results it is observed that there was good uniformity of metal particles adhered to the surface of ZnO. In relation the responses of the gas sensor for pure and decorated material, there was an increase signal for decoration with Ag in the presence of H2 gas. In the presence of NO2 gas, there was a higher signal to both morphologies of pure ZnO. For CO gas, a response to the multi-point stars decorated with platinum is observed. The responsivity of the tripods samples was high compared with multi-point stars, with value of the order of 0.8 A / W. The results are of fundamental importance for scientific contribution and raises margin for an even deeper focus to developing high-performance sensor devices.

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Orientador: José Roberto Ribeiro Bortoleto / Co-orientador: Americo Sheitiro Tabata / Banca: Luis Vicente de Andrade Scalvi / Banca: Jose Humberto Dias da Silva / Banca: Julio Ricardo Sambrano / Banca: Maximo Siu Li / O Programa de Pós Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi / Resumo: Este trabalho apresenta um estudo das propriedades ópticas de filmes finos de ZnO puro e de ZnO dopado com Al; e um estudo da influência da variação de pressão do gás argônico durante a deposição dos filmes, nas propriedades ópticas e estruturais. Os filmes foram depositados em substrato de vidro e silício pela técnica RF magnetron sputtering com alvo de uma liga de Zn-Al, com uma concentração de 2% em peso de alumínio. As análises de DRX dos filmes apresentam um pico preferencial no plano (002) - eixo c, que mostra a formaão de uma estrutura de wurtzita correpondente ao ZnO, e que há um aumento do tamanho do cristalino com a dopagem de Al, em concordância com resultados de AFM. Medidas Raman mostram o modo de vibração característico do ZnO ao redor de 575 cm-1 e a melhora da cristalinidade do material com a dopagem de Al, sem a deterioração com a variação de pressão de argônio. Os filmes apresentam valores de transmitância óptica acima de 70% na faixa do visível do espectro (400 a 700 nm) e correlacionados com o espectro de refletância possibilitaram obter dados como o gap óptico na ordem de 3,5 - 3,6 eV, que estão acima dos valores esperados para o ZnO intrínseco (3,3 eV). Os resultados de gap óptico foram correlacionados com dados obtidos através de Modelagem Computacional (DFT). As medidas de fotoluminescência mostram uma larga faixa de emissão de luz na região visível e linhas de emissão em 3,32 e 3,37 eV que sugerem efeito de dopagem de Al. Os resultados de medidas ópticas correlacionadas com a modelagem computacional reforçam que o efeito Burstein-Moss é dominante para esse material / Abstract: This thesis presents a study of the optical properties of thin films of pure ZnO and ZnO doped with Al; and a study of the influence of argon gas pressure of argon gas pressure variation during synthesis of films on the optical and structural properties. The films were deposited on glass and silicon substrate by RF magnetron suputtering technique with a target Zn-Al alloy with a concentration of 2% by weight of aluminum. The XRD analysis of the film showed a preferential peak in the (002) - c axis, showing the formation of a wurtzite structure corresponding to the ZnO, and that there is an increase in crystalline size with. Al doping, in agreement with results AFM. Measurements showed the characteristic. Raman vibration mode ZnO around 575 cm-1 and the improvement of crystallinity of the material with the doping of Al, without impairment to the variation of argon pressure. The films exhibited optical transmittance above 70% in the visible spectrum range (400 to 700 nm) and correlated with the reflectance spectrum enabled to obtain data such as the optical band gap in the range 3.5 to 3.6 eV which are above the values obtained for the intrinsic ZnO (3.3 eV). The optical gap results were correlated data obtained through Computational Modeling. The photoluminescence measurements showed a large light emission range in the visible region and emission lines at 3.32 and 3.37 eV suggest that Al doping effect. The optical resuts correlated with the computational modeling reinforce the Burstein-Moss effect is dominant for that material / Doutor

Orientador: José Roberto Ribeiro Bortoleto / Banca: Marcio Peron Franco de Godoy / Banca: Elidiane Cipriano Rangel / O Programa de Pós Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi / Resumo: Devido ao avanço da tecnologia as pesquisas sobre filmes finos óxidos transparentes, depositados principalmente em subtratos poliméricos flexíveis, vem crescendo muito. Neste trabalho foram sintetizados filmes finos de óxido de zinco e de óxido de estanho, sobre substratos poliméricos de poliereftalato de etileno (PET). Os filmes foram sintetizados através da técnica de magnetron sputtering utilizando fonte utilizados para a síntese dos filmes: gás argônio para geral o plasma, gás oxigênio para a formação dos filmes, alvo de zinco metálico para o filme de ZnO e alvo de estanho metálico para o filme de SnO2. Os filmes foram depositados variando o tempo de deposição. Alguns filmes de ZnO foram sintetizados sobre substratos de PET tratados a plasma de gás argônico a fim de investigar a aderência no substrato. A caracterização composicional foi realizada por MEV-EDS, a caracterização óptica foi realizada por espectroscopia óptica, a morfologia superficial foi realizada através de microscopia de força atômica (AFM), a caracterização das estruturas químicas através do infravermelho e a espessura dos filmes através do perfilômetro. Os filmes de ZnO apresentaram-se transparentes e a análise química indicou que o filme é formado por zinco e oxigênio. A rugosidade da superfície e a espessura aumentaram com o tempo de deposição. Para os filmes de SnO2, observou-se uma transmitância menor que o filme de ZnO e também uma menor adesão na superfície do substrato / Abstract: Due to advancement in technology research on transparent oxide thin films, deposited mainly on flexible polymeric substrates, has been increasing. In this study were synthesized thin films of zinc oxide and tin oxide, on polymeric substrates of polyethylene terephthalate (PET). The films were synthesized by magnetron sputering technique using a source of RF (radio frequency) were used for the synthesis of films: argon gas to generate plasma, oxygen gas for the formation of films of metallic zinc target to film ZnO and metallic tin target for the film of SnO2. The films were deposited by varying the time of deposition. Some ZnO were synthesized on substrates of PET treated to argon gas plasma in order to investigate the adhesion to the substrate. The compositional characterization was perfomed by SEM-EDS, the optical characterization was carried out by optical spectroscopy, the surface morphology was carried out by atomic force microscopy (AFM) to characterize the chemical structure by infrared and through the thickness of the films profilometer. The ZnO showed is transparent and chemical analysis indicated that films is formed by zinc and oxygen. The surface roughness and the thickness increased with the time of deposition. For films of SnO2, was observed under a transmittance of the film of the films profilometer. The ZnO showed is transparent and chemical analysis indicated that the films is formed by zinc and oxygen. The surface roughness and the thickness increased with the time of deposition. For films of SnO2, was observed under a transmittance of the film of ZnO and also a lower adhesion on the substrate surface / Mestre

abstract: This thesis elaborates the application of carbon nanotubes (CNTs) and it is discussed in two parts. In the first part of the thesis, two types of CNTs inks for inkjet materials printer are prepared. They are both chemical stable and printable, effective and easily made. The sheet resistance of printed films decreases exponentially as the number of layers increases. In the second part of this study, CNTs/ZnO composite structures are fabricated to understand the electronic and optical properties. The materials were deposited by two different methods: drop-drying and RF magnetic sputtering system on flexible polymer substrates. To further increase the conductivity of the various layers of deposited CNTs films, electrical and optical characterizations are also done. This study establishes CNTs as a multi-functional semitransparent conductor, which can be deposited at room-temperature with other transparent conductive oxide (TCO) composites for application in flexible electronics and printed circuit and sensors. / Dissertation/Thesis / M.S. Materials Science and Engineering 2012

Three systems of electrospun composite membranes with piezoelectric polymer polyvinylidene fluoride (PVDF) as matrix incorporating: 1) Carbon based fillers: carbon nanotube (CNT) and graphene oxide (GO); 2) Ceramic based fillers-barium titanate (BT), zinc oxide (ZnO) and nanoclays (halloysite and bentonite); 3) Cellulosic fillers: microcrystalline cellulose (MCC) and nanocrystalline cellulose (NCC) at different loadings were prepared by electrospinning process. Influence of filler type and loading on total PVDF crystallinity (Xc), relative fraction of β phase (piezoelectric phase) in total crystalline PVDF (Fβ), volume fraction of β phase in the samples (vβ) and piezoelectric coefficient d33 were characterised and analysed. Correlation between vβ and piezoelectric performance (d33) will be focused by this work. A common situation was observed for the composites-d33 increased while vβ is reduced by the fillers, so it can be concluded that d33 of the composites is not totally up to their vβ, there are other factors that need to be taken into account. For example, for carbon based filler like CNT, it increased electric conductivity of sample during and after electrospinning process, making it easier for charges produced by β crystals from inside of sample to be transferred to surfaces of the sample, and possibly promoting orientation of β crystals in d33 direction, therefore enhanced d33 of the composites though β phase formation was significantly hindered by inclusion of CNT; For piezoelectric ceramic fillers like BT and ZnO, a possible combined piezoelectricity from filler and β phase PVDF might enhanced d33 though less β phase was formed; And for non-piezoelectric and non-conductive fillers, enhancement in orientation of β crystals might play a major role in promotion of d33. Keywords: electrospinning; polyvinylidene fluoride (PVDF); nanocomposites; piezoelectric coefficient d33; energy harvesting.

Zinc oxide (ZnO) is a II-VI semiconductor material that offers tremendous potential as a light emitter in the blue-to-UV range. It has a wurtzite structure, and a direct band gap that can be tuned from 3.0 to 4.0 eV by alloying with Cd or Mg, respectively. In this work, ZnO thin films were grown by metalorganic chemical vapor deposition (MOCVD) on n-Si 2 ° off (100), amorphous glass, n-GaAs (100), and c-plane sapphire substrates. Diethyl zinc (DEZn) and tert-butanol (TBOH) were chosen as precursors. For the first time, Second Harmonic Generation Imaging was applied to the mapping of ZnO epilayers. The images obtained highlighted the polycrystalline character of the thin films, and provided insight as to the growth mode of ZnO on Si. The influence of substrate temperature on the structural properties of the epilayers was investigated by X-ray diffraction and optical microscopy. Grain sizes as high as 54 nm were measured. The optimum temperature range for this system proved to be 450 – 500 °C. The influence of the VI:II ratio during growth on the optical properties of the epilayers was studied by UV-vis-near IR spectroscopy. The lowest Urbach tail E0 parameter was measured for material grown at a VI:II ratio of 18:1. The films’ free electron concentration was shown to decrease by over two orders of magnitude, from 1019 to 1017 cm-3, as the VI:II ratio increased from 10 to 60:1. This decrease in carrier concentration with rising VI:II ratio was paralleled to the surge at 12 K of a photoluminescence (PL) emission band characteristic of p-type ZnO. The band gap energies extracted from room temperature transmission spectra ranged between 3.35 and 3.38 eV, in agreement with the value of 3.35 eV measured by room temperature PL. Moreover, variable temperature PL spectra were recorded between 12 and 298 K on ZnO grown on Si. The 12 K spectrum was dominated by a donor-bound exciton (D°X) at 3.36 eV, while the 298 K scan displayed strong free exciton emission (FX) at 3.29 eV. The width of the D°X band proved to be as narrow as 7 meV. The intensity ratio between the room temperature near-band edge emission and the defect-related green band was as high as 28:1, highlighting the optical quality of the layers deposited in this work. The electrical properties of the thin films were studied by Hall measurements (van der Pauw configuration), and a maximum room temperature mobility of 11 cm2/Vs was recorded. Furthermore, a palladium (Pd) Schottky barrier diode on ZnO was fabricated. The barrier height and ideality factor were calculated from current–voltage measurements to be 0.83 eV and 1.6, respectively. The capacitance–voltage curve of the diode yielded a carrier concentration in the depletion region of 8·1017 cm-3. This study has shown that the optical and electrical properties of ZnO depend strongly on the growth conditions employed. A suitable choice of growth parameters can yield high quality ZnO that may be used for various devices. Keywords: Hall, MOCVD, optical spectroscopy, photoluminescence, Schottky barrier diode, SH Imaging, X-ray diffraction, ZnO.

M.Tech. (Chemical Engineering) / Please refer to full text to view abstract

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