Thesis (Ph. D.)--West Virginia University, 2006. / Title from document title page. Document formatted into pages; contains xxi, 227 p. : ill. (some col.), col. maps. Includes abstract. Includes bibliographical references (p. 152-157).

Made available in DSpace on 2015-03-03T11:52:49Z (GMT). No. of bitstreams: 0 Previous issue date: 2014-08-15Bitstream added on 2015-03-03T12:07:00Z : No. of bitstreams: 1 000808295.pdf: 1454675 bytes, checksum: dfd00c1da776e021a570aaa2c9380541 (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Filmes de óxido de cobalto apresentam interesses para aplicações em catálise, sensores de gás e para estudos do efeito de exchange bias em multicamadas de CoO/Co/CoO. Neste trabalho, filmes de óxido de cobalto foram depositados usando a técnica de DC sputtering, nas potências 80,120 e 240W. A superfície dos filmes preparados a potências menores não apresentaram trincas. Medidas de difração de raios X indicaram a presença da fase Co3O4 nas deposições de 80 e 120 W. Para deposição com 240 W, observa-se apenas a presença da fase CoO. Os espectros de espalhamento Raman dos filmes apresentaram bandas referentes aos modos do Co3O4 para todas as amostras crescidas, já a análise de transmitância no infravermelho apresentou bandas de absorção relacionadas à fase CO3O4 nos filmes depositados com baixa potência, e uma mistura de bandas do CoO e Co3O4 na deposição a 240 W. O espectro de transmitância no UV/VIS/NIR apresentou absorções relacionadas a transições eletrônicas do óxido de cobalto em em 0,8,0,9,1,7 e 3eV na amostra crescida em 80 W. Com o objetivo de criar camadas nanométricas de cobalto puro, intercaladas com filmes de óxido de cobalto, foram depositados filmes nos quais o fluxo de oxigênio foi interrompido. A potência utilizada foi 120 W e os tempos de interrupção foram 120 e 12s. Imagens de microscopia eletrônica de varredura indicaram que não houve rachaduras na superfície dos filmes e medidas na seção transversal das amostras indicaram formaram das camadas metálicas no interior do filme depositado com interrupção de oxigênio por 120s. Análise de difração de raios X das multicamadas mostrou um favorecimento da fase CoO em relaçãoao tetraóxido, porém o espectro Raman dos filmes apresentaram picos claros da fase Co3O4. Utilizando uma simulação computacional baseada no método de Monte Carlo (Stopping and Range of lons in Matter-SRIM) estimou-se a energia com que os átomos e íons... / Cobalt oxide films have interest for application in catalysis, gas sensors, and for studies of the exchange bias effect in CoO/Co/CoO multilayers. In this work, cobalt oxide films were deposited using DC sputtering technique. The deposition powers tested were 80,120 and 240 W. The surfaces of the films prepared at 240 W have cracked, while films prepared at lower powers showed no cracks. X-ray diffraction measurements indicated that films prepared at lower powers are deminated by the Co3O4 with spinel strucuture while at higher powers the CoO rocksalt phase is favored. Raman scattering measurements of the films showed bands related to Co3O4 spinel modes for all samples, while the infrared transmittance analysis showed absorption bands related to the Co3O4 phase on films deposited at low power and a mixture of CoO and Co3O4 bands deposition to 240 W. In the UV/VIS/NIR spectrum, absorption bands related to electronic transitions of cobalt oxide at 0.8, 0.9, 1.7 and 3 eV were observed in the sample grown at 80 W. Aiming to create nanometric layers of pure cobalt interspersed cobalt oxide films, depositions in which the oxygen flow was periodically stopped were made. In these experiments, the power was kept at 120W and interrupetion periods of 120 and 12 s were used. Scanning electron microscopy image indicated that there were no cracks on the surfaces of the films and cross section measurements idicated the formation of metal layers inside the film deposited with interruption of oxygen for 120 s. Analysis of X-ray diffraction of multilayers showed a favoring of the CoO phase, but the Raman spectra of the films showed clear peaks of Co3O4 phase. Using a computer simulation based on the Monte Carlo method (Stopping and Range of Ions in Matter, SRIM) the energies of the atoms and ions that reach the substrate were estimated. The estimations were performed when deposition is taken with outputs of 120 and 240 W. An increase of the average...

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Thesis (Master of Engineering in Chemical Engineering)--Cape Peninsula University of Technology, 2018. / Electrochemical and non-enzymatic fructose detection has evoked keen interest in the scientific literature. Several authors have reported on different methods of electrode preparation for fructose sensors. However, little systematic study has been conducted to design a cheap, efficient method of depositing metal oxides to detect fructose. To address the challenge, a Co3O4 thin film was fabricated using a simple solution step deposition on Fluorine doped Tin oxide (FTO) glass electrode. In this study, a report on the selective oxidation of fructose on Co3O4 thin film electrode surface is presented. Electrode characterization was done using X-ray diffraction (XRD), High Resolution Transmission Electron Microscopy (HR-TEM), Scanning Electron Microscope (SEM), Atomic Fluorescence Microscopy (AFM), and Electrochemical Impedance Spectroscopy (EIS). All cyclic voltammetry (CVs) and chronoamperometry tests were carried out by the use of an AUTOLAB POTENTIOSTAT 302 N, controlled by Nova 2.0 software instrumentation using a customized 50 cm3 electrochemical cell. The cell consisted of a graphite rod as the counter electrode (CE), 3 M Ag/AgCl reference electrode (RE) and the fabricated Co3O4/FTO as the working electrode (WE). All experiments were carried out at 25±2 ⁰C. From the results, the constructed sensor exhibited two distinctive linear ranges in the ranges of 0.021 – 1.74 mM and from 1.74 - ~15 mM, covering a wide linear range of up to ~15 mM at an applied potential of +0.6V vs. Ag/AgCl in 0.1M NaOH solution. The sensor demonstrated a high, reproducible and repeatable sensitivity of 495 (lower concentration range) & 53 (higher concentration range) μA cm-2 mM-1 for a low R.S.D of 5 %. The Co3O4 thin film produced a low detection limit of ~1.7 μM for a signal to noise ratio of 3 (S/N = 3); a fast response time of 6s and long term stability. The repeatability and stability of the electrode resulted from the chemical stability of Co3O4 thin film. The study showed that the sensor was highly selective towards fructose compared to the presence of other key interferences i.e. AA, AC, and UA. Because of such a favourable electrocatalysis of the Co3O4 sensor towards fructose, the ease of the electrode fabrication and reproducibility makes it a future candidate for commercial applications in the food and beverages sector.

Orientador: José Roberto Ribeiro Bortoleto / Banca: José Humberto da Silva / Banca: Johnny Vilcari Romero Lopez / Resumo: O avanço das técnicas de deposição de filmes finos sobre as superfícies dos materiais tem permitido agregar valor e dar novas funcionalidades aos produtos. Atualmente, os filmes finos de óxido de estanho dopado com índio (ITO) têm encontrado grande aplicação no mercado. Entretanto, devido à pouca disponibilidade do índio na natureza e aos altos custos envolvidos na sua aquisição, elementos alternativos estão sendo estudados para sua substituição. Nesse contexto, destaca-se o óxido de zinco dopado com alumínio (AZO) como um promissor substituto, devido às características de elevada transmissividade, baixa resistividade e band gap da ordem de 3,37 eV, que permitem sua aplicação na síntese de filmes finos semicondutores. Com base no exposto, neste trabalho, foi projetado e desenvolvido o protótipo de uma fonte amplificadora de potência (FAP) de corrente alternada (AC) em baixa frequência, operando entre 15 a 40 kHz, responsável por iniciar e sustentar o campo elétrico utilizado para a geração do plasma. Esta FAP foi utilizada para a deposição de filmes finos de (AZO) por meio da técnica de magnetron sputtering. A análise das características morfológicas, ópticas e elétricas dos filmes de AZO produzidos neste estudo resultaram em uma transmitância superior a 80%, energia de band gap de 3,82 eV, e resistividade de 1,46.10-3 .cm, permitindo concluir que o filme produzido se comporta como um TCO (óxido transparente condutivo). A comparação desses resultados com trabalhos disponívei... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The development of thin films deposition techniques allows to increase value and give new features to the materials. Currently, indium doped zinc oxide (ITO) is widely used in the market. However, due to the low availability of the indium in the nature and the high costs involved on its acquisition, alternative elements are being studied for its replacement. Aluminum doped zinc oxide (AZO) stands out as a promising substitute, mainly because of its characteristics, such as high transmissivity, low resistivity and band gap value of 3.37 eV. That allow the application of AZO in the synthesis of thin films semiconductors. In this work, it was developed a prototype of a plasma power source amplifier (FAP) to operate in alternating current (AC) and low frequency (15 - 40 kHz), responsible for initiating and sustaining the electric field used for plasma generation. This FAP was used to deposit AZO thin films by the technique of magnetron sputtering. The analysis of the morphological, optical and electrical characteristics of the AZO films produced in this study resulted in more than 80% transmittance, band gap energy value of 3,82eV, and resistivity of 1,46.10-3 .cm. The thin films synthetized was classified as transparent conductive oxide (TCO). The comparison of these results with the characteristics of similar films avaiable in the bibliography, allows to conclude that the power amplifier source developed in this dissertation makes it possible to obtain thin films of AZO with c... (Complete abstract click electronic access below) / Mestre

Complex lanthanide oxide systems are known to host novel phases of matter, while also providing functionality for practical applications. In this dissertation, the structural, magnetic and magnetocaloric properties of three families of lanthanide oxides have been studied with the dual aims of investigating the magnetic behaviour and identifying promising magnetic refrigerants for cooling to temperatures currently accessible using non-renewable liquid He. The thesis presents a two-part study of the magnetic and magnetocaloric properties of the geometrically frustrated lanthanide garnets, where the magnetic $Ln^{3+}$ form corner-sharing triangles. First, the family of garnets $Ln_3A_2X_3$O$_{12}$, $Ln$ = Gd, Tb, Dy, Ho, $A$ = Ga, Sc, In, Te, $X$ = Ga, Al, Li are investigated. Changes to the single-ion anisotropy of the magnetic ion as well as variations in the chemical pressure radically alters the nature of magnetic ordering, the degree of frustration and the magnetocaloric performance. In the second part, the garnets $Ln_3A$Ga$_4$O$_{12}$, $Ln$ = Gd, Tb, Dy, Ho, $A$ = Cr, Mn, are studied. Introducing additional spins significantly reduces the frustration in the garnet lattice. Low temperature powder neutron diffraction of Ho$_3$MnGa$_4$O$_{12}$ reveals concomitant ordering of Ho$^{3+}$ and Mn$^{3+}$ moments below the ordering temperature, $T_N$ = 5.8 K. The magnetocaloric performance of $Ln$_3CrGa$_4$O$_{12}$, $Ln$ = Gd, Dy, Ho, greatly surpasses that of the parent $Ln_3$Ga$_5$O$_{12}$ at $T$ = 2 K. The final results chapters in the thesis describe the magnetism and magnetocaloric effect in the lanthanide orthoborates, $Ln$BO$_3$ , $Ln$ = Eu, Gd, Tb, Dy, Ho, Er, Yb and the lanthanide metaborates, $Ln$(BO$_2$)$_3$, $Ln$ = Pr, Nd, Gd, Tb. The magnetic $Ln^{3+}$ form slightly distorted edge-sharing triangular layers in $Ln$BO$_3$. Unique magnetic features are observed, including short-range ordering and spin reorientation transitions depending on the single-ion anisotropy of the $Ln^{3+}$. The $Ln$BO$_3$ are also efficient magnetocalorics in the liquid helium temperature range. The lanthanide metaborates contain one-dimensional chains of magnetic lanthanide ions. Bulk magnetic measurements show features consistent with low-dimensional magnetism, such as magnetisation plateaux at one-third of the saturation magnetisation for Nd(BO$_2$)$_3$ and Tb(BO$_2$)$_3$ in a field of 14 T. This thesis provides insight into the fundamental magnetic properties of complex lanthanide oxide systems and also demonstrates strategies for identifying new magnetocaloric materials: both through chemical control of the structure of well-known magnetocalorics and by studying materials that have not been explored previously. The results pave the way for further in-depth investigations and finding new magnetic coolants based on complex lanthanide oxide systems.

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(工学) / 甲第13781号 / 工博第2885号 / 新制||工||1426(附属図書館) / 25997 / UT51-2008-C697 / 京都大学大学院工学研究科機械理工学専攻 / (主査)教授 井手 亜里, 教授 木村 健二, 教授 河合 潤 / 学位規則第4条第1項該当

Orientador: José Humberto Dias da Silva / Banca: Paulo Noronha Lisboa Filho / Banca: Fernando Rogerio de Paula / Resumo: Filmes de óxido de cobalto apresentam interesses para aplicações em catálise, sensores de gás e para estudos do efeito de exchange bias em multicamadas de CoO/Co/CoO. Neste trabalho, filmes de óxido de cobalto foram depositados usando a técnica de DC sputtering, nas potências 80,120 e 240W. A superfície dos filmes preparados a potências menores não apresentaram trincas. Medidas de difração de raios X indicaram a presença da fase Co3O4 nas deposições de 80 e 120 W. Para deposição com 240 W, observa-se apenas a presença da fase CoO. Os espectros de espalhamento Raman dos filmes apresentaram bandas referentes aos modos do Co3O4 para todas as amostras crescidas, já a análise de transmitância no infravermelho apresentou bandas de absorção relacionadas à fase CO3O4 nos filmes depositados com baixa potência, e uma mistura de bandas do CoO e Co3O4 na deposição a 240 W. O espectro de transmitância no UV/VIS/NIR apresentou absorções relacionadas a transições eletrônicas do óxido de cobalto em em 0,8,0,9,1,7 e 3eV na amostra crescida em 80 W. Com o objetivo de criar camadas nanométricas de cobalto puro, intercaladas com filmes de óxido de cobalto, foram depositados filmes nos quais o fluxo de oxigênio foi interrompido. A potência utilizada foi 120 W e os tempos de interrupção foram 120 e 12s. Imagens de microscopia eletrônica de varredura indicaram que não houve rachaduras na superfície dos filmes e medidas na seção transversal das amostras indicaram formaram das camadas metálicas no interior do filme depositado com interrupção de oxigênio por 120s. Análise de difração de raios X das multicamadas mostrou um favorecimento da fase CoO em relaçãoao tetraóxido, porém o espectro Raman dos filmes apresentaram picos claros da fase Co3O4. Utilizando uma simulação computacional baseada no método de Monte Carlo (Stopping and Range of lons in Matter-SRIM) estimou-se a energia com que os átomos e íons... / Abstract: Cobalt oxide films have interest for application in catalysis, gas sensors, and for studies of the exchange bias effect in CoO/Co/CoO multilayers. In this work, cobalt oxide films were deposited using DC sputtering technique. The deposition powers tested were 80,120 and 240 W. The surfaces of the films prepared at 240 W have cracked, while films prepared at lower powers showed no cracks. X-ray diffraction measurements indicated that films prepared at lower powers are deminated by the Co3O4 with spinel strucuture while at higher powers the CoO rocksalt phase is favored. Raman scattering measurements of the films showed bands related to Co3O4 spinel modes for all samples, while the infrared transmittance analysis showed absorption bands related to the Co3O4 phase on films deposited at low power and a mixture of CoO and Co3O4 bands deposition to 240 W. In the UV/VIS/NIR spectrum, absorption bands related to electronic transitions of cobalt oxide at 0.8, 0.9, 1.7 and 3 eV were observed in the sample grown at 80 W. Aiming to create nanometric layers of pure cobalt interspersed cobalt oxide films, depositions in which the oxygen flow was periodically stopped were made. In these experiments, the power was kept at 120W and interrupetion periods of 120 and 12 s were used. Scanning electron microscopy image indicated that there were no cracks on the surfaces of the films and cross section measurements idicated the formation of metal layers inside the film deposited with interruption of oxygen for 120 s. Analysis of X-ray diffraction of multilayers showed a favoring of the CoO phase, but the Raman spectra of the films showed clear peaks of Co3O4 phase. Using a computer simulation based on the Monte Carlo method (Stopping and Range of Ions in Matter, SRIM) the energies of the atoms and ions that reach the substrate were estimated. The estimations were performed when deposition is taken with outputs of 120 and 240 W. An increase of the average... / Mestre