Along with many other solar energy conversion processes, research on photocatalytic water splitting to generate hydrogen and oxygen has experienced rapid major development over the past years. Developing an efficient visible-light-responsive photocatalyst has been one of the targets of such research efforts. In this regard, nitride materials, particularly Ta3N5, have been the subject of investigation due to their promising properties. This dissertation focuses on the fundamental parameters involved in the photocatalytic processes targeting overall water splitting using Ta3N5 as a model photocatalyst. The discussion primarily focuses on relevant parameters that are involved in photon absorption, exciton separation, carrier diffusion, carrier transport, and catalytic efficiency. A collection of theoretical and experimental studies of properties associated with Ta3N5 have been utilized to obtain a comprehensive understanding of this material. The fundamental structural and optoelectronic properties of Ta3N5 have been addressed. From the electronic properties, the dielectric constant and effective masses have been calculated. Because of its high dielectric constant and relatively low effective masses, Ta3N5 is promising for photocatalytic reaction applications. Studies of lattice dynamics, optical properties, and band positions have been able to clearly show that the synthesized Ta3N5 is essentially non-stoichiometric and that a truly pure phase of Ta3N5 has never been achieved, even though XRD has shown a pure phase sample. The photophysical properties of Ta3N5, such as the absorption coefficient, carrier mobility, and carrier lifetime, have been experimentally measured by synthesizing Ta3N5 thin films. Very low kinetic properties with very low transport properties and fast carrier recombination explained why overall water splitting has never been achieved with Ta3N5 as a photocatalyst to date. The extent to which the surface states of Ta3N5 photocatalysts affect photocatalytic performance has been investigated. The surface topmost layer is demonstrated to play a critical role in the photocatalytic activity of Ta3N5; further research on the surface properties of Ta3N5 should be conducted to understand and improve charge separation and the resulting photocatalytic activity. Finally, a remarkable improvement in the photocatalytic OER has been achieved with the addition of cobalt as a cocatalyst. There is a trade-off between the optimum contact of hole transfer from bulk Ta3N5 to the surface of the cobalt cocatalyst and providing active sites for the electrochemical reaction. Knowing the characteristics of cobalt on the Ta3N5 surface, further improvement was attempted by adding a noble metal to the CoOx/Ta3N5 photocatalyst system, where a synergetic effect of CoOx and noble metals was observed.

Visible light-driven photocatalysis has shown considerable potential in the area of clean and renewable energy, as well as in wastewater treatment. This thesis describes the synthesis, characterization and applicability of a visible-light active photocatalyst, bismuth oxybromide (BiOBr). The photocatalytic activity of BiOBr was investigated through its preparation via hydrothermal and solvothermal synthesis routes under various conditions. Hydrothermal catalyst was prepared using non template based method while for solvothermal synthesis CTAB was used as a template. Parameters of temperature and time of thermal treatment were optimized for each synthesis method and overall tests for catalyst dosage and recyclability were performed. An overall optimal route leading to high photocatalytic performance was also proposed based on the obtained results. Studies were also conducted to examine the applicability of optimally synthesized BiOBr in drinking water applications by studying catalyst-mediated disinfection of E. coli and degradation of phenol. Favourable results were obtained, confirming the prospective application of BiOBr as a viable photocatalyst for disinfection. Furthermore, the potential of enhancing BiOBr to further improve its performance is described through synthesis of a novel PdCl2/BiOBr based photocatalyst. Overall, the performance of BiOBr under various conditions in this study establishes its potential as a holistic photocatalyst and merits further development.

Visible light-driven photocatalysis has shown considerable potential in the area of clean and renewable energy, as well as in wastewater treatment. This thesis describes the synthesis, characterization and applicability of a visible-light active photocatalyst, bismuth oxybromide (BiOBr). The photocatalytic activity of BiOBr was investigated through its preparation via hydrothermal and solvothermal synthesis routes under various conditions. Hydrothermal catalyst was prepared using non template based method while for solvothermal synthesis CTAB was used as a template. Parameters of temperature and time of thermal treatment were optimized for each synthesis method and overall tests for catalyst dosage and recyclability were performed. An overall optimal route leading to high photocatalytic performance was also proposed based on the obtained results. Studies were also conducted to examine the applicability of optimally synthesized BiOBr in drinking water applications by studying catalyst-mediated disinfection of E. coli and degradation of phenol. Favourable results were obtained, confirming the prospective application of BiOBr as a viable photocatalyst for disinfection. Furthermore, the potential of enhancing BiOBr to further improve its performance is described through synthesis of a novel PdCl2/BiOBr based photocatalyst. Overall, the performance of BiOBr under various conditions in this study establishes its potential as a holistic photocatalyst and merits further development.

A aplicação de semicondutores no tratamento de água e efluentes líquidos é uma tecnologia de remediação ambiental promissora, em especial para poluentes orgânicos. Entre os vários semicondutores que também são fotocatalisadores, o TiO2 é amplamente usado em aplicações ambientais, por ser inerte biológica e quimicamente, ter elevado potencial de oxidação, baixo custo e estabilidade frente à corrosão. Entretanto, o TiO2 também tem algumas desvantagens, tais como: ele é excitado apenas por luz UV e requer uma operação unitária adicional (por exemplo, filtração ou centrifugação) para o reuso do catalisador. Para contornar estas limitações, usou-se um procedimento simples para a síntese de um fotocatalisador magnético (Fe3O4/TiO2) com alta área superficial específica e atividade catalítica, quando comparado com o TiO2 P25 da Evonik. O fotocatalisador foi sintetizado através de um procedimento em três etapas: (1) Partículas α-Fe2O3 foram obtidas por precipitação de uma solução de FeCl3.6H2O 0.01 mol L-1, que foi submetida a uma hidrólise forçada à 100°C por 48 h; (2) Partículas de α-Fe2O3/TiO2 foram obtidas por heterocoagulação de oxi-hidróxidos de Ti(IV) sobre as partículas de α-Fe2O3, as quais foram calcinada a 500°C por 2 h; e (3) As partículas \"casaca/caroço\" do fotocatalisador foram obtidas por calcinação a 400°C por 1 h sob atmosfera redutora (H2). A atividade fotocatalítica do material sintetizado foi avaliada aplicando-o no descoramento de uma solução do corante Azul Ácido 9 (C.I. 42090). Os efeitos do pH e da concentração de catalisador foram estimados por meio de um planejamento fatorial 22. Foi obtido um fotocatalisador com área superficial específica de 202 m2 g-1, facilmente separável do meio reacional em aproximadamente 2 min com o auxílio de um ímã. O fotocatalisador apresentou absorção em toda a região do visível. A maior remoção de cor (54%) foi obtida com pH 3,0, 1,0 g L-1 de catalisador e 2 horas de reação. / The use of semiconductors for treating polluted waters and wastewaters is a promising environmental remediation technology, especially for organic pollutants. Among the several semiconductors that are also photocatalysts, TiO2 is extensively used for environmental application, due to its biological and chemical inertness, high oxidation power, low cost, and stability regarding corrosion. However, TiO2 also has some disadvantages, such as: it is only UV-excited and requires an additional unit operation (e.g. filtration or centrifugation) for reuse purposes. In order to work around those limitations, a simple procedure for synthesizing a magnetic photocatalyst (Fe3O4/TiO2), with high specific surface area and good photocatalytic activity when compared to Evonik\'s TiO2 P25, was used. The photocatalyst was synthesized in a three-step procedure: (1) α-Fe2O3 particles were obtained, by precipitation, from FeCl3.6H2O 0.01 mol L-1, which underwent a forced acid hydrolysis at 100°C for 48 h; (2) α-Fe2O3/TiO2 particles were obtained, by heterocoagulation, of Ti(IV) oxide species on the α-Fe2O3, followed by calcination at 500°C for 2 h; and (3) The core/shell photocatalyst particles were obtained by calcination the α-Fe2O3/TiO2 particles at 400°C for 1 h under reducing atmosphere (H2). The photocatalytic activity of the synthesized material was assessed by the color removal of an Acid Blue 9 (C.I. 42090) dye solution. pH and catalyst dosage effects were estimated by a 22 factorial design. Fe3O4/TiO2 core/shell particles with specific surface area of 202 m2 g-1were obtained. They were easily separated from the reaction medium, in approximately 2 min, with the aid of a magnet. The photocatalyst absorbed radiation throughout the visible spectrum. The greatest color removal (54%) was achieved with pH 3.0, 1.0 g L-1 of photocatalyst, and 2 h of reaction.

Nanostructured molybdenum trioxide (MoO3) was synthesized and used as a precursor in a comparative study, along with commercial MoO3, to synthesize molybdenum dioxide (MoO2) nanoparticles. Scanning electron microscope (SEM) images revealed the particles to be approximately 30-50 nm in diameter. X-ray diffraction (XRD) confirmed MoO3 was fully reduced to MoO2 in all cases. Time dependent experiments showed that within two hours no traces of MoO3 are present. All of the experiments showed the materials were excellent absorbent materials, as well as photocatalysts. Both MoO2 materials performed almost exactly the same, with both samples being able to remove 100% of the methylene blue (MB) in one minute with light, and in two minutes without light. The morphology of MoO2 was controlled in a comparative study by varying the concentration of cetyltrimethylammonium bromide (CTAB) present during the hydrothermal reaction. As the concentration of CTAB increased, the morphology of the material changed from nanoparticles, to nanospheres, to microspheres, to hollow microspheres, and finally a highly agglomerated version of microspheres and particles combined, as confirmed by SEM images. A formation mechanism for the formation of the various sized spheres was proposed with a combination of aggregation and Ostwald ripening. XRD confirmed that all of the MoO3 was reduced to MoO2, along with no residual peaks from the CTAB that was present during the reaction. Upon trying to mix some of the materials into the MB solutions, it became obvious that some of the materials were hydrophobic. The decontamination results once again showed that the synthesized MoO2 materials were not only photocatalysts, but adsorbents as well. Samples synthesized with 0.1-5 mM CTAB were able to remove 100% of the MB in 10 minutes or less. Samples synthesized with 10 mM CTAB were able to remove 54.4% and 35% of the MB in 10 minutes, with and without light, respectively. Samples synthesized with 15 mM CTAB were able to remove 29.4% and 26.3% of the MB in 10 minutes, with and without light, respectively. The apparent decrease in decontamination performance was proposed to be caused by surface morphology induced hydrophobicity. A mechanism to describe why the hydrophobic particles were still able to decontaminate the water was proposed to be caused by coming into direct contact with the magnetic stirrer as the water level dropped due to sample collection. MoO2 nanoparticles were successfully synthesized onto a copper substrate, in a single step, via a hydrothermal synthesis technique. It is believed to be the first report of such a synthesis method. XRD confirmed all of the MoO3 had been reduced to MoO2, and also confirmed that no other compounds had formed between the molybdenum and copper. SEM images of the MoO2 coated copper substrate showed uniform nanoparticles ranging from 30-50 nm. The MoO2 coated copper substrate was able to decontaminate 57.5% of the MB from water in 10 minutes without exposure to light, while it was able to decontaminate 71.7% of the MB from water in 10 minutes with exposure to light.

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/ line-height:115% / } @page Section1 {size:8.5in 11.0in / margin:1.0in 1.0in 1.0in 1.0in / mso-header-margin:.5in / mso-footer-margin:.5in / mso-paper-source:0 / } div.Section1 {page:Section1 / } --> </style><!--[if gte mso 10]> <style> /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal" / mso-tstyle-rowband-size:0 / mso-tstyle-colband-size:0 / mso-style-noshow:yes / mso-style-priority:99 / mso-style-qformat:yes / mso-style-parent:"" / mso-padding-alt:0in 5.4pt 0in 5.4pt / mso-para-margin-top:0in / mso-para-margin-right:0in / mso-para-margin-bottom:10.0pt / mso-para-margin-left:0in / line-height:115% / mso-pagination:widow-orphan / font-size:11.0pt / font-family:"Calibri","sans-serif" / mso-ascii-font-family:Calibri / mso-ascii-theme-font:minor-latin / mso-fareast-font-family:"Times New Roman" / mso-fareast-theme-font:minor-fareast / mso-hansi-font-family:Calibri / mso-hansi-theme-font:minor-latin / mso-bidi-font-family:"Times New Roman" / mso-bidi-theme-font:minor-bidi / } </style> <![endif]--> <p class="MsoNormal"><span style="font-size: 12pt / line-height: 115% / font-family: &quot / Times New Roman&quot / ,&quot / serif&quot / ">The heterogeneous photocatalytic oxidation of dinitrogen to nitrate, NO3 and/or nitrite, no2 using peroxy species of titanium (IV) in aqueous suspensions has been investigated. The photocatalysts used were titanium peroxide and Degussa p25 TiO2 pretreated with H2O2. These photocatalysts were investigated by SEM and FTIR spectroscopy. <span style="">&nbsp / </span><o:p></o:p></span></p> <span style="font-size: 12pt / font-family: &quot / Times New Roman&quot / ,&quot / serif&quot / "><o:p></o:p></span></p> </p>

In This study a thin film of nanometric TiO2 was sol-gel prepared and used for heterogeneous photocatalytic reaction to treat chlorobenzene in testing solution and to evaluate its removal efficiency. Conventionally, the material of photocatalyst was mainly fabricated in form of powder used in the suspension system. Although TiO2 powder has a high specific surface area for heterogeneous photocatalysis, it still leaves a great number of suspended solids in solution awaiting proper handling after the treatment is completed. Also, such suspended solids would pose ¡§shielding¡¨ effect from UV light, and thus affected the efficiency of photocatalytic degradation. To overcome this drawback, a proper mesh size of stainless steel webnet was first selected as a treatment substrate and TiO2 dip-coated, followed by calcination at 500¢J. The end product was used as the TiO2 photocatalytic film for this study. The film of TiO2, verified as anatase type of crystal lattice by XRD and SEM, contained particle sizes ranging from 10 to 20 nm. A solution containing chlorobenzene was used in the study to assess the extent of photocatalytic degradation by UV/TiO2 film. The test was to evaluate the effects of the number of dip-coating and calcining (thickness), initial pH, UV light intensity (@365 nm), and applied electric voltage on photocatalytic removal of chlorobenzene in the solution. The test results indicated that TiO2 film was capable of degrading chlorobenzene; however, enhancement of the degradation efficiency was found to be needed. It was also found that the degradation rate of chlorobezene increased with an increasing thickness of the film and UV light intensity. The pH of test solution was found to be insensitive to degradation of chlorobenzene, probably due to its non-dissociation nature. It was found that electric voltage exerted was unable to prevent electrons and holes from re-combining, and a negative effect of external voltage was even observed. Therefore, it was believed that voltage exertion was not beneficial to phtocatalysis in this study. Kinetics of the tests in this study assumed a pseudo-first-order reaction, which resulted in a rate constant k' = 1.3¡Ñ10-5¡]min-1¡^. The reaction rate was found to be proportional to the 0.7507 order of UV light intensity.

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(工学) / 甲第19000号 / 工博第4042号 / 新制||工||1622 / 31951 / 京都大学大学院工学研究科分子工学専攻 / (主査)教授 田中 庸裕, 教授 今堀 博, 教授 阿部 竜 / 学位規則第4条第1項該当

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/ line-height:115% / } @page Section1 {size:8.5in 11.0in / margin:1.0in 1.0in 1.0in 1.0in / mso-header-margin:.5in / mso-footer-margin:.5in / mso-paper-source:0 / } div.Section1 {page:Section1 / } --> </style><!--[if gte mso 10]> <style> /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal" / mso-tstyle-rowband-size:0 / mso-tstyle-colband-size:0 / mso-style-noshow:yes / mso-style-priority:99 / mso-style-qformat:yes / mso-style-parent:"" / mso-padding-alt:0in 5.4pt 0in 5.4pt / mso-para-margin-top:0in / mso-para-margin-right:0in / mso-para-margin-bottom:10.0pt / mso-para-margin-left:0in / line-height:115% / mso-pagination:widow-orphan / font-size:11.0pt / font-family:"Calibri","sans-serif" / mso-ascii-font-family:Calibri / mso-ascii-theme-font:minor-latin / mso-fareast-font-family:"Times New Roman" / mso-fareast-theme-font:minor-fareast / mso-hansi-font-family:Calibri / mso-hansi-theme-font:minor-latin / mso-bidi-font-family:"Times New Roman" / mso-bidi-theme-font:minor-bidi / } </style> <![endif]--> <p class="MsoNormal"><span style="font-size: 12pt / line-height: 115% / font-family: &quot / Times New Roman&quot / ,&quot / serif&quot / ">The heterogeneous photocatalytic oxidation of dinitrogen to nitrate, NO3 and/or nitrite, no2 using peroxy species of titanium (IV) in aqueous suspensions has been investigated. The photocatalysts used were titanium peroxide and Degussa p25 TiO2 pretreated with H2O2. These photocatalysts were investigated by SEM and FTIR spectroscopy. <span style="">&nbsp / </span><o:p></o:p></span></p> <span style="font-size: 12pt / font-family: &quot / Times New Roman&quot / ,&quot / serif&quot / "><o:p></o:p></span></p> </p>

京都大学 / 新制・課程博士 / 博士(工学) / 甲第23911号 / 工博第4998号 / 新制||工||1780(附属図書館) / 京都大学大学院工学研究科物質エネルギー化学専攻 / (主査)教授 阿部 竜, 教授 陰山 洋, 教授 藤田 晃司 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM