Thèses : « Nanostructured Oxide Semiconductors »

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Berhe, Seare Ahferom. « Acceptor-sensitizers for Nanostructured Oxide Semiconductor in Excitonic Solar Cells ». Thesis, University of North Texas, 2014. https://digital.library.unt.edu/ark:/67531/metadc699927/.

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Organic dyes are examined in photoelectrochemical systems wherein they engage in thermal (rather than photoexcited) electron donation into metal oxide semiconductors. These studies are intended to elucidate fundamental parameters of electron transfer in photoelectrochemical cells. Development of novel methods for the structure/property tuning of electroactive dyes and the preparation of nanostructured semiconductors have also been discovered in the course of the presented work. Acceptor sensitized polymer oxide solar cell devices were assembled and the impact of the acceptor dyes were studied. The optoelectronic tuning of boron-chelated azadipyrromethene dyes has been explored by the substitution of carbon substituents in place of fluoride atoms at boron. Stability of singlet exited state and level of reduction potential of these series of aza-BODIPY coumpounds were studied in order to employ them as electron-accepting sensitizers in solid state dye sensitized solar cells.

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Wang, Jinfeng. « Characterization and synthesis of nanoscale materials ». Diss., Rolla, Mo. : Missouri University of Science and Technology, 2008. http://scholarsmine.mst.edu/thesis/pdf/JinfengWang_09007dcc80564540.pdf.

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Thesis (Ph. D.)--Missouri University of Science and Technology and University of Missouri--St. Louis, 2008.
Vita. The entire thesis text is included in file. Title from title screen of thesis/dissertation PDF file (viewed August 28, 2008) Thesis completed as part of a cooperative degree program with Missouri University of Science & Technology and the University of Missouri--St. Louis. Includes bibliographical references (p. 129-142).

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Akande, Amos Adeleke. « Gas sensing properties of nanostructured vanadium oxide semiconductors by chemoresistive and optical methods ». Thesis, University of Pretoria, 2017. http://hdl.handle.net/2263/65892.

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The aims of this research thesis are to synthesise VO2, V2O5 and V6O13 nanostructures and apply the materials on sensor electrodes for gas and humidity sensing. These materials were synthesised and optimised using chemical vapour deposition (CVD), microwave assisted and pulse laser deposition (PLD) techniques. Analyses with thermogravimetric (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), high resolution transmission electron microscope (HRTEM), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometry (VSM), Raman and Fourier transform infrared (FTIR) spectroscopy showed VOx phases order as NH4VO3 ? VO2 + V2O5 (150 – 200 °C) ? V6O13 (300 °C) ? V2O5 (above 350 °C). This is when the precursor NH4VO3 was annealed in CVD between 100 – 350 °C in H2 atmosphere for 2 hrs. Adsorption analysis of VOx nanostructures showed a profile of Brunauer-Emmett-Teller (BET) surface areas which increased with the annealing temperature until 300 °C after which the transition occurred. Humidity (%) sensing response of VOx showed high response for V6O13 and V2O5 phase whereas, the Langmuir isotherm plot in the form of the response per BET surface area with respect to different levels of relative humidity showed high response for VO2. Phase evolution diagram based on these properties has been proposed. Thermal CVD annealing of NH4VO3 at 500 °C in N2 atmosphere for 2, 12 and 24 hours produced monoclinic V6O13 (at 2 hrs) and ?-orthorhombic V2O5 (at 12 and 24 hrs) nanorod structures using the above characterization techniques. Gas sensing application of these structures revealed that the H2S gas is selective in adsorption to V6O13 phase with 132 % response magnitude at 350 °C and 60 ppm, this response is 647.2 % higher than that of NH3, CH4, NO2, H2 and CO. The response and recovery times are 32 and 129 s respectively which is remarkably short compared with the data in literatures. This V6O13 sensor was ranked with its V2O5 counterpart and still found to be 238.5 % higher for H2S gas. Density functional theory (DFT) through ab initio molecular dynamics of (110) facet of monoclinic V6O13 and ?- orthorhombic V2O5 also showed high H2S adsorption energy for V6O13 than V2O5 with a profile which simulate the experimental findings. Low temperature microwave assisted synthesis of VOx from NH4VO3 without post-annealing treatment demonstrated small size homogeneous crystallite with high BET surface area and high adsorption and desorption pores. These properties translated to sub-ppm room temperature sensing of the flammable CH4 and odorant NH3 and toxic NO2 with high sensitivity. The VO2 (B) phase produced via the same microwave process applied for humidity sensing in the lateral gate metal oxide semiconductor field effect transistor (MOSFET) configuration for 0, 5, 8, 10, 12 and 15 V gate voltages. An optimum percentage humidity response observed at 5 V showed response and recovery times in the order of 60 – 70 s which is remarkably shorter than the ? 300 s response of the non-gated VO2 humidity sensor reported in this thesis. Statistical information extracted from the non-linear S-curve Hill Dose rate showed that the VO2 (B) sensor is very resilient to relative humidity by showing the humidity level of more than 100% where the response of the sensor could be reduced to 50%. In-situ Raman spectroscopy sensing of NH3 gas at the surface of PLD deposited V2O5 thin film was presented. The film crystal structure, depth profile and oxidation state was studied by cross section scanning electron microscope (SEM), time of flight secondary ion mass spectroscopy (TOF-SIMS), XPS and group theoretical analysis. Recoverable red shift of 194 cm-1 and blue shift of 996 cm-1phonons upon the interaction with the NH3 gas at 25 and 100 °C was observed. Decrease in the Raman scattered photons of the 145 cm-1 phonon was also observed for different levels of NH3 exposure. The responses of these phonon properties in NH3 environment compared to the chemoresistive sensing of the film at 40 ppm showed that the in-situ Raman spectroscopy techniques is not only more sensitive but also demonstrated possibility for selective gas detection via blue and red shift of phonon frequencies.
Thesis (PhD)--University of Pretoria, 2017.
Physics
PhD
Unrestricted

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Zhang, Shaolin. « Wide band gap nanomaterials and their applications ». Click to view the E-thesis via HKUTO, 2009. http://sunzi.lib.hku.hk/hkuto/record/B41758225.

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Zhang, Shaolin, et 張少林. « Wide band gap nanomaterials and their applications ». Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2009. http://hub.hku.hk/bib/B41758225.

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Lima, Francisco Anderson de Sousa. « Application of transition-metal-oxide-based nanostructured thin films on third generation solar cells ». reponame:Repositório Institucional da UFC, 2015. http://www.repositorio.ufc.br/handle/riufc/14584.

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LIMA, F. A. S. Application of transition-metal-oxide-based nanostructured thin films on third generation solar cells. 2015. 225 f. Tese (Doutorado em Ciência de Materiais) – Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2015.
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One of the greatest challenges of our time is to devise means to provide energy in a sustainable way to attend an exponentially growing demand. The energy demand is expected to grow 56% by 2040. In this context, the use of clean and sustainable sources of energy is imperative. Among these sources, solar energy is the only one which can meet the total world energy requirement even considering such large growth in demand. The solar power incident on the Earth's surface every second is equivalent to 4 trillion 100-watt light bulbs. Photovoltaic solar cells are one of several ways to harness solar energy. These cells convert solar energy directly into electricity. Commercial photovoltaic devices are already a reality, but their share of the world energy matrix is still quite small, mainly due to the high costs. Next generation photovoltaics open a number of new possibilities for photovoltaic energy applications that can potentially decrease the overall cost of energy production. Transition metal semiconductor oxides are promising materials that can be produced by low cost methods and o er interesting new features. The use of these materials in next generation photovoltaics is therefore a very promising and interesting application. In this thesis work zinc, titanium and vanadium oxides were used in next generation solar cells. Thin lms of zinc oxide were synthesized by the low cost and environmentally friendly techniques of electrodeposition and hydrothermal synthesis and applied as working electrodes in highly e cient dye sensitized solar cells (DSSCs). The lms were characterized by structural and optical techniques while the cells were tested by current vs: voltage and quantum e ciency measurements. The e ciencies of these cells were as high as 2.27% using ZnO thin lms without any post deposition treatment. Moreover, natural dyes extracted from plants of northeastern Brazil were applied as sensitizers in DSSCs assembled with commercial available TiO 2 as working electrode. The natural dyes were extracted employing very simple methods and were characterized by XPS and UPS techniques. Their band alignments were shown to be compatible with the TiO 2 as well as with the mediator electrolyte. The e ciency of DSSCs sensitized with natural dyes were as high as 1.33%. Finally, water based V 2 O 5 was used as hole transport medium (HTM) in conventional organic solar cells (OSCs) and ITO-free, plastic OSCs. The results obtained with V 2 O 5 were compared with the results obtained from cells assembled with PEDOT:PSS, which is the most used HTM. This comparison showed that the use of V 2 O 5 as HTM can lead to more e cient OSCs. The stability of these devices were evaluated by tests applying the ISOS standards ISOS-D-1, ISOS-L-1 and ISOS-O-1. A UV- lter and a protective graphene oxide (GO) layer were employed seeking to improve the stability of OSCs. The combination of both UV- lter and GO protective layer was shown to be the most e ective way to improve the stability of these devices
Um dos maiores desa os do nosso tempo e desenvolver formas para fornecer energia de forma sustent avel para atender uma demanda que cresce exponencialmente e que dever a crescer 56% at e 2040. Neste contexto, o uso de fontes limpas e sustent aveis de energia e um imperativo. Entre essas fontes, a energia solar e a unico que pode satisfazer a ne- cessidade total de energia do mundo, mesmo considerando o crescimento na demanda. A pot^encia solar incidente na superf cie da Terra a cada segundo e equivalente a 4 trilh~oes de l^ampadas de 100 watts. C elulas solares fotovoltaicas s~ao uma das v arias maneiras de aproveitar a energia solar, convertendo-a diretamente em eletricidade. Dispositivos com- erciais fotovoltaicos j a s~ao uma realidade, mas a sua participa c~ao na matriz energ etica mundial ainda e muito pequena, principalmente devido aos seus custos elevados. C elulas fotovoltaicas de nova gera c~ao abrem uma s erie de novas possibilidades para aplica c~oes de energia fotovoltaica que pode diminuir o custo total de produ c~ao de energia. Oxidos semicondutores de metais de transi c~ao s~ao materiais promissores que podem ser produzi- dos atrav es de m etodos de baixo custo e que possuem caracter sticas interessantes. Por conseguinte, o uso destes materiais em energia fotovoltaica de pr oxima gera c~ao se apre- senta com uma aplica c~ao promissora. Nesta tese de doutorado oxidos de zinco, tit^anio e van adio foram utilizados em c elulas solares de pr oxima gera c~ao. Filmes nos de oxido de zinco foram sintetizados por eletrodeposi c~ao e s ntese hidrot ermica. Os lmes foram apli- cados como eletrodos de trabalho em c elulas solares sensibilizadas por corante (DSSCS) altamente e cientes. Os lmes foram caracterizados por t ecnicas estruturais e oticas en- quanto que as c elulas foram testadas por medidas de corrente vs: voltagem e de e ci^encia qu^antica. A e ci^encia dessas c elulas atingiu 2,27% utilizando lmes nos de ZnO sem qualquer tratamento p os-deposi c~ao. Al em disso, corantes naturais extra dos de plan- tas do nordeste do Brasil foram aplicados como sensibilizadores em DSSCs montadas com TiO 2 comercial utilizado como eletrodo de trabalho. Os corantes naturais foram extra das empregando m etodos simples e foram caracterizados por espectroscopia de fotoel etrons excitados por raios X e por radia c~ao ultravioleta, XPS e UPS respectivamente. Seus alin- hamentos de banda se mostraram compat veis com o TiO 2 e com o eletrodo de regenera c~ao. A e ci^encia das DSSCs sensibilizadas com corantes naturais chegou a 1,33%. Finalmente, V 2 O 5 a base de agua foi usado como material transportador de buracos (HTM) em c elulas solares org^anicas (OSCs) convencionais e OSCs de pl astico constru das sem ITO. Os re- sultados obtidos com V 2 O 5 foram comparados com os resultados de c elulas constru das com PEDOT:PSS, que e o HTM mais utilizado. Esta compara c~ao revelou que o uso de V 2 O 5 como HTM pode levar a OSCs mais e cientes. A estabilidade destes dispositivos foi avaliada por testes aplicando os padr~oes ISOS-D-1, ISOS-L-1 e ISOS-O-1. O uso de ltros ultravioleta e de uma camada protetora de oxido de grafeno reduzido foi testado com o intuito de melhorar a estabilidade desses dispositivos. O uso de uma combina c~ao de ambos se mostrou a forma mais efetiva de melhorar a estabilidade das OSCs

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Chen, Xinyi, et 陈辛夷. « Wide band-gap nanostructure based devices ». Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2012. http://hub.hku.hk/bib/B49799290.

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Wide band gap based nanostructures have being attracting much research interest because of their promise for application in optoelectronic devices. Among those wide band gap semiconductors, gallium nitride (GaN) and zinc oxide (ZnO) are the most commonly studied and optoelectronic devices based on GaN and ZnO have been widely investigated. This thesis concentrates on the growth, optical and electrical properties of GaN and ZnO nanostructures, plus their application in solar cells and light emitting diodes (LEDs). GaN-nanowire based dye sensitized solar cells were studied. Different post-growth treatments such as annealing and coating with a TiOx shell were applied to enhance dye absorption. It was found that TiOx increased the dye absorption and the performance of the dye sensitized solar cell. ZnO nanorods were synthesized by vapor deposition and electrodeposition. Post-growth treatments such as annealing and hydrothermal processing were used to modify the defect chemistry and optical properties. LEDs based on GaN/ZnO heterojunctions were studied. The influence of ZnO seed layers on GaN/ZnO LEDs was investigated. GaN/ZnO LEDs based on ZnO nanorods with MgO and TiOx shells were also prepared in order to modify the LED performance. The coating condition of the shell was found to influence the current-voltage (I-V) characteristics and device performance. Moreover, high brightness LEDs based on GaN with InGaN multiple quantum wells were also fabricated. The origin of the emission from GaN/ZnO LEDs was studied using different kinds of GaN substrates. Direct metal contacts on bare GaN substrates were also employed to investigate the optical emission and electrical properties. It is found that the emission from the GaN/ZnO LEDs probably originated from the GaN substrate. GaN/ZnO LEDs with MgO as an interlayer were also fabricated. The MgO layer was expected to modify the band alignment between the GaN and the ZnO. It was shown that GaN/MgO/ZnO heterojunctions (using both ZnO nanorods and ZnO films) have quite different emission performance under forward bias compared to those that have no MgO interlayer. An emission peak was around 400 nm could originate from ZnO. Nitrogen doped ZnO nanorods on n-type GaN have been prepared by electrodeposition. Zinc nitrate and zinc acetate were used as ZnO precursors and NH4NO3 was used as a nitrogen precursor. Only the ZnO nanorods made using zinc nitrate showed obvious evidence of doping and coherent I-V characteristics. Cerium doped ZnO based LEDs were fabricated and showed an emission that depended on the cerium precursor that was employed. This indicates that the choice of precursor influences the growth, the materials properties and the optical properties of ZnO.
published_or_final_version
Physics
Doctoral
Doctor of Philosophy

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Hansson, (f d. Wadeasa) Amal. « Heterojunctions between zinc oxide nanostructures and organic semiconductor ». Doctoral thesis, Linköpings universitet, Fysik och elektroteknik, 2011. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-71843.

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Lighting is a big business, lighting consumes considerable amount of the electricity. These facts motivate for the search of new illumination technologies that are efficient. Semiconductor light emitting diodes (LEDs) have huge potential to replace the traditional primary incandescent lighting sources. They are two basic types of semiconductor LEDs being explored: inorganic and organic semiconductor light emitting diodes. While electroluminescence from p-n junctions was discovered more than a century ago, it is only from the 1960s that their development has accelerated as indicated by an exponential increase of their efficiency and light output, with a doubling occurring about every 36 months, in a similar way to Moore's law in electronics. These advances are generally attributed to the parallel development of semiconductor technologies, optics and material science. Organic light emitting diodes (OLEDs) have rapidly matured during the last 30 years driven by the possibility to create large area light-emitting diodes and displays. Another driving force to specifically use semiconducting polymers is the possibility to build the OLED on conventional flexible substrates via low-cost manufacturing techniques such as printing techniques, which open the way for large area productions. This thesis deals with the demonstration and investigation of heterojunction LEDs based on p-organic semiconductor and n-ZnO nanostructures. The ZnOorganic heterojunctions are fabricated using low cost and simple solution process without the need for sophisticated vacuum equipments. Both ZnO-nanostructures and the organic materials were grown on variety of substrates (i.e. silicon, glass and plastic substrates) using low temperature methods. The growth mechanism of the ZnO nanostructures has been systematically investigated with major focus in ZnO nanorods/nanowires. Different organic semiconductor materials and device configurations are explored starting with single polymer emissive layer ending up with separate emissive and blocking layers, or even blends. Interestingly, the photoluminescence and electroluminescence spectra of the hybrid LEDs provided a broad emission band covering entirely the visible spectrum [∼400-∼800nm]. The hybrid light emitting diode has a white emission attributed to ZnO intrinsic defects and impurities in combination with the electroluminescence from the conjugated polymers. The ZnO nanostructures in contact with a high workfunction electrode constitute an air stable electron injecting contact for the organic semiconductor. Hence, we have shown that a white light emission can be achieved in a ZnO-organic hybrid light emitting diode using cheap and low temperature growth techniques for both organic and inorganic materials.
The series number "1504" is incorrect and is changed in the electronic version to the correct number "1405".

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González, Zalba Miguel Fernando. « Single donor detection in silicon nanostructures ». Thesis, University of Cambridge, 2013. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.608181.

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Khunou, Ramotseng. « Gas sensing properties of Ceo2 nanostructures ». University of the Western Cape, 2020. http://hdl.handle.net/11394/7909.

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>Magister Scientiae - MSc
The industrial safety requirements and environmental pollution have created a high demand to develop gas sensors to monitor combustible and toxic gases. As per specifications of World Health Organization (WHO) and Occupational Safety and Health Administration (OSHA), lengthy exposure to these gases lead to death which can be avoided with early detection. Semiconductor metal oxide (SMO) has been utilized as sensor for several decades. In recent years, there have been extensive investigations of nanoscale semiconductor gas sensor.

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ZHANG, JIE. « INVESTIGATIONS OF OXIDE AND SULFIDE BASED LOW DIMENSIONAL NANO STRUCTURES FOR CONDUCTOMETRIC GAS SENSORS, MEMRISTORS AND PHOTODETECTORS ». OpenSIUC, 2015. https://opensiuc.lib.siu.edu/dissertations/1086.

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Low dimensional semiconductors are promising materials with diverse range of applications in a variety of fields. Specifically, in recent times low dimensional oxide and sulfide based semiconductors are regarded as materials that can have potential applications in chemical gas sensor, optoelectronic devices and memristor. How ever, in some cases it is envisioned that appropriate doping as well as phase stabilization is important in enhancing their material properties. This work presents the synthesis, characterization and application of various (pristine and doped) quasi-one dimensional metal oxides (TiO2, VO2) and two-dimensional materials (CuO thin film, MoS2). Some practical protocols for stabilization of specific phases at ambient conditions via a new method of doping in VO2 nanostructures with aluminum, is demonstrated. Similarly, a temperature-doping level phase diagram for the free-standing nanostructures in the temperature range close to the ambient conditions was presented. TiO2 nanowire was doped during growth and electrical measurements on individual TiO2 single crystal nanowires indicate that light in visible range can induce electron-hole pair formation. Furthermore, gas sensing (CO, H2) measurements taken under visible light irradiation imply that photo-activated chemical oxidization on the surface of TiO2 nanowires occurs, which is responsible for the observed measurements. Further, the effect of self heating in some nanostructures was also explored. Since self-heating is a prospective power-efficient energy delivery channel to the conductometric chemical sensors that require elevated temperatures for their operation, the unprecedentedly low power consumption can be achieved via minimizing the heat dissipation in the optimized device architecture. By investigating the heat dissipation in these devices we show that the thermal, electrical and chemical properties of the self-heated semiconducting nanowires appear to be strongly coupled with each other at nanoscale. This opens up unique opportunity to fabricate low power nanoscopic sensing leading to an ultra-small and power efficient single nanostructure gas recognition system. The CuO film based lateral devices were fabricated and studied for its resistive switching behavior. A good, stable and reproducible threshold RS performance of CuO film was obtained by electrical measurement. Finally, the micro-flake MoS2 based FET photoelectronic device was fabricated (using mechanically exfoliated MoS2) and its electronic and photoelectronic properties were investigated. We show that though the FET mobility values of MoS2 microflake is in the average range, but the photo-responsivity is much higher compared to most of others similar sulfide based 2D layered materials.

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Simo, Aline. « Physical properties of vanadium dioxide nanoparticles : application as 1-d nanobelts room temperature for hydrogen gas sensing ». Thesis, University of the Western Cape, 2013. http://hdl.handle.net/11394/4581.

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Philosophiae Doctor - PhD
Transition metal oxides magneli phases present crystallographic shear structure which is of great interest in multiple applications because of their wide range of valence, which is exhibited by the transition metals. The latter affect chemical and physical properties of the oxides. Amongst them we have nanostructures VO2 system of V and O components which are studied including chemical and physical reactions based on non-equilibrium thermodynamics. Due to their structural classes of corundum, rocksalt, wurtzite, spinel, perovskite, rutile, and layer structure, these oxides are generally used as catalytic materials which are prepared by common methods under mild conditions presenting distortion or defects in the case of VO2. Existence of an intermediate phase is proved using an x-ray thermodiffraction experiment providing structural information as the nanoparticles are heated. Potential application as gas sensing device has been the first time obtained due to the high surface to volume ratio, and good crystallinity, purity of the material and presence of suitable nucleating defects sites due to its n-type semiconductor behavior. In addition, annealing effect on nanostructures VO2 nanobelts shows a preferential gas reductant of Ar comparing to the N2 gas. Also, the hysteresis loop shows that there is strong size dependence to annealing treatment on our samples. This is of great interest in the need of obtaining high stable and durable material for Mott insulator transistor and Gas sensor device at room temperature.

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Chunder, Anindarupa. « FABRICATION OF FUNCTIONAL NANOSTRUCTURES USING POLYELECTROLYTE NANOCOMPOSITES AND REDUCED GRAPHENE OXIDE ASSEMBLIES ». Doctoral diss., University of Central Florida, 2010. http://digital.library.ucf.edu/cdm/ref/collection/ETD/id/3082.

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A wide variety of nanomaterials ranging from polymer assemblies to organic and inorganic nanostructures (particles, wires, rods etc) have been actively pursued in recent years for various applications. The synthesis route of these nanomaterials had been driven through two fundamental approaches - Â Top downÂ and Â Bottom upÂ . The key aspect of their application remained in the ability to make the nanomaterials suitable for targeted location by manipulating their structure and functionalizing with active target groups. Functional nanomaterials like polyelectrolyte based multilayered thin films, nanofibres and graphene based composite materials are highlighted in the current research. Multilayer thin films were fabricated by conventional dip coating and newly developed spray coating techniques. Spray coating technique has an advantage of being applied for large scale production as compared to the dip coating technique. Conformal hydrophobic/hydrophilic and superhydrophobic/hydrophilic thermal switchable surfaces were fabricated with multilayer films of poly(allylaminehydrochloride) (PAH) and silica nanoparticles by the dip coating technique, followed by the functionalization with thermosensitive polymer-poly(N-isopropylacrylamide)(PNIPAAM) and perfluorosilane. The thermally switchable superhydrophobic/ hydrophilic polymer patch was integrated in a microfluidic channel to act as a stop valve. At 70 degree centigrade, the valve was superhydrophobic and stopped the water flow (close status) while at room temperature, the patch became hydrophilic, and allowed the flow (open status). Spray-coated multilayered film of poly(allylaminehydrochloride) (PAH) and silica nanoparticles was fabricated on polycarbonate substrate as an anti-reflection (AR) coating. The adhesion between the substrate and the coating was enhanced by treating the polycarbonate surface with aminopropyltrimethoxylsilane (APTS) and sol-gel. The coating was finally made abrasion-resistant with a further sol-gel treatment on top of AR coating, which formed a hard thin scratch-resistant film on the coating. The resultant AR coating could reduce the reflection from 5 to 0.3% on plastic. Besides multilayered films, the fabrication of polyelectrolyte based electrospun nanofibers was also explored. Ultrathin nanofibers comprising 2-weak polyelectrolytes, poly(acrylic acid) (PAA) and poly(allylaminehydrochloride) (PAH) were fabricated using the electrospinning technique and methylene blue (MB) was used as a model drug to evaluate the potential application of the fibers for drug delivery. The release of MB was controlled in a nonbuffered medium by changing the pH of the solution. Temperature controlled release of MB was obtained by depositing temperature sensitive PAA/poly(N-isopropylacrylamide) (PNIPAAM) multilayers onto the fiber surfaces. The sustained release of MB in a phosphate buffered saline (PBS) solution was achieved by constructing perfluorosilane networks on the fiber surfaces as capping layers. The fiber was also loaded with a real life anti-depressant drug (2,3-tertbutyl-4-methoxyphenol) and fiber surface was made superhydrophobic. The drug loaded superhydrophobic nanofiber mat was immersed under water, phosphate buffer saline and surfactant solutions in three separated experiments. The rate of release of durg was monitored from the fiber surface as a result of wetting with different solutions. Time dependent wetting of the superhydrophobic surface and consequently the release of drug was studied with different concentrations of surfactant solutions. The results provided important information about the underwater superhydrophobicity and retention time of drug in the nanofibers. The nanostructured polymers like nanowires, nanoribbons and nanorods had several other applications too, based on their structure. Different self-assembled structures of semiconducting polymers showed improved properties based on their architectures. Poly(3-hexylthiophene) (P3HT) supramolecular structures were fabricated on P3HT-dispersed reduced graphene oxide (RGO) nanosheets. P3HT was used to disperse RGO in hot anisole/N, N-dimethylformamide solvents, and the polymer formed nanowires on RGO surfaces through a RGO induced crystallization process. The Raman spectroscopy confirmed the interaction between P3HT and RGO, which allowed the manipulation of the composite's electrical properties. Such a bottom-up approach provided interesting information about graphene-based composites and inspired to study the interaction between RGO and the molecular semiconductor-tetrasulphonate salt of copper phthalocyanine (TSCuPc) for nanometer-scale electronics. The reduction of graphene oxide in presence of TSCuPc produced a highly stabilized aqueous composite ink with monodispersed graphene sheets. To demonstrate the potential application of the donor (TSCuPc)Â acceptor (graphene) composite, the RGO/TSCuPc suspension was successfully incorporated in a thin film device and the optoelectronic property was measured. The conductivity (dark current) of the composite film decreased compared to that of pure graphene due to the donor molecule incorporation, but the photoconductivity and photoresponsivity increased to an appreciable extent. The property of the composite film overall improved with thermal annealing and optimum loading of TSCuPc molecules.
Ph.D.
Department of Chemistry
Sciences
Chemistry PhD

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Yang, Li Li. « Synthesis and Characterization of ZnO Nanostructures ». Doctoral thesis, Linköpings universitet, Institutionen för teknik och naturvetenskap, 2010. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-60815.

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One-dimensional ZnO nanostructures have great potential applications in the fields of optoelectronic and sensor devices. Therefore, it is very important to realize the controllable growth of one-dimensional ZnO nanostructures and investigate their properties. The main points for this thesis are not only to successfully realize the controllable growth of ZnO nanorods (ZNRs), ZnO nanotubes (ZNTs) and ZnMgO/ZnO heterostructures, but also investigate the structure and optical properties in detail by means of scanning electron microscope (SEM), transmission electron microscope (TEM), resonant Raman spectroscopy (RRS), photoluminescence (PL), time resolved PL (TRPL), X-ray photoelectron spectroscopy (XPS) and Secondary ion mass spectrometry (SIMS). For ZNRs, on one hand, ZNRs have been successfully synthesized by a two-step chemical bath deposition method on Si substrates. The diameter of ZNRs can be well controlled from 150 nm to 40 nm through adjusting the diameter and density of the ZnO nanoparticles pretreated on the Si substrates. The experimental results indicated that both diameter and density of ZnO nanoparticles on the substrates determined the diameter of ZNRs. But when the density is higher than the critical value of 2.3×108cm-2, the density will become the dominant factor to determine the diameter of ZNRs. One the other hand, the surface recombination of ZNRs has been investigated in detail. Raman, RRS and PL results help us reveal that the surface defects play a significant role in the as-grown sample. It is the first time to the best of our knowledge that the Raman measurements can be used to monitor the change of surface defects and deep level defects in the CBD grown ZNRs. Then we utilized TRPL technique, for the first time, to investigate the CBD grown ZNRs with different diameters. The results show that the decay time of the excitons in ZNRs strongly depends on the diameter. The altered decay time is mainly due to the surface recombination process. A thermal treatment under 500°C can strongly suppress the surface recombination channel. A simple carrier and exciton diffusion equation is also used to determine the surface recombination velocity, which results in a value between 1.5 and 4.5 nm/ps. Subsequently, we utilized XPS technique to investigate the surface composition of as-grown and annealed ZNRs so that we can identify the surface recombination centers. The experimental results indicated that the OH and H bonds play the dominant role in facilitating surface recombination but specific chemisorbed oxygen also likely affect the surface recombination. Finally, on the basis of results above, we explored an effective way, i.e. sealing the beaker during the growth process, to effectively suppress the surface recombination of ZNRs and the suppression effect is even better than a 500oC post-thermal treatment. For ZNTs, the structural and optical properties have been studied in detail. ZNTs have been successfully evolved from ZNRs by a simple chemical etching process. Both temperature-dependent PL and TRPL results not only further testify the coexistence of spatially indirect and direct transitions due to the surface band bending, but also reveal that less nonradiative contribution to the emission process in ZNTs finally causes their strong enhancement of luminescence intensity. For ZnMgO/ZnO heterostructures, the Zn0.94Mg0.06O/ZnO heterostructures have been deposited on 2 inch sapphire wafer by metal organic chemical vapor deposition (MOCVD) equipment. PL mapping demonstrates that Mg distribution in the entire wafer is quite uniform with average concentration of ~6%. The annealing effects on the Mg diffusion behaviors in Zn0.94Mg0.06O/ZnO heterostructures have been investigated by SIMS in detail. All the SIMS depth profiles of Mg element have been fitted by three Gaussian distribution functions. The Mg diffusion coefficient in the as-grown Zn0.94Mg0.06O layer deposited at 700 oC is two orders of magnitude lower than that of annealing samples, which clearly testifies that the deposited temperature of 700 oC is much more beneficial to grow ZnMgO/ZnO heterostructures or quantum wells. This thesis not only provides the effective way to fabricate ZNRs, ZNTs and ZnMgO/ZnO heterostructures, but also obtains some beneficial results in aspects of their optical properties, which builds theoretical and experimental foundation for much better understanding fundamental physics and broader applications of low-dimensional ZnO and related structures.
Endimensionella nanostrukturer av ZnO har stora potentiella tillämpningar för optoelektroniska komponenter och sensorer. Huvudresultaten för denna avhandling är inte bara att vi framgångsrikt har realiserat med en kontrollerbar metod ZnO nanotrådar (ZNRs), ZnO nanotuber (ZNTs) och ZnMgO/ZnO heterostrukturer, utan vi har också undersökt deras struktur och optiska egenskaper i detalj. För ZNRs har diametern blivit välkontrollerad från 150 nm ner till 40 nm. Den storlekskontrollerande mekanismen är i huvudsak relaterad till tätheten av ZnO partiklarna som är fördeponerade på substratet. De optiska mätningarna ger upplysning om att ytrekombinationsprocessen spelar en betydande roll för tillväxten av ZNR. En värmebehandling i efterhand vid 500 grader Celsius eller användande av en förseglad glasbägare under tillväxtprocessen kan starkt hålla nere kanalerna för ytrekombinationen.För ZNT, dokumenterar vi inte bara samexistensen av rumsliga indirekta och direkta övergångar på grund av bandböjning, men vi konstaterar också att vi har mindre icke-strålande bidrag till den optiska emissionsprocessen i ZNT. För ZnMgO/ZnO heterostrukturer konstaterar vi med hjälp av analys av Mg diffusionen i den växta och den i efterhand uppvärmda Zn(0.94)Mg(0.06)O filmen, att en tillväxt vid 700 grader Celsius är den mest lämpliga för att växa ZnMgO/ZnO heterostrukturer eller kvantbrunnar. Denna avhandling ger en teoretisk och experimentell grund för bättre förståelse av grundläggande fysik och för tillämpningar av lågdimensionella strukturer.
SSF, VR

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Clavijo, William Paul. « Low-temperature Fabrication Process for Integrated High-Aspect Ratio Metal Oxide Nanostructure Semiconductor Gas Sensors ». VCU Scholars Compass, 2017. http://scholarscompass.vcu.edu/etd/4781.

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This work presents a new low-temperature fabrication process of metal oxide nanostructures that allows high-aspect ratio zinc oxide (ZnO) and titanium dioxide (TiO2) nanowires and nanotubes to be readily integrated with microelectronic devices for sensor applications. This process relies on a new method of forming a close-packed array of self-assembled high-aspect-ratio nanopores in an anodized aluminum oxide (AAO) template in a thin (2.5 µm) aluminum film deposited on a silicon and lithium niobate substrate (LiNbO3). This technique is in sharp contrast to traditional free-standing thick film methods and the use of an integrated thin aluminum film greatly enhances the utility of such methods. We have demonstrated the method by integrating ZnO nanowires, TiO2 nanowires, and multiwall TiO2 nanotubes onto the metal gate of a MOSFET (Metal-Oxide-Semiconductor Field-Effect Transistor), and the delay line of a surface acoustic wave (SAW) device to form an integrated ChemFET (Chemical Field-Effect Transistor) and a orthogonal frequency coded (OFC) SAW gas sensor. The resulting metal oxide nanostructures of 1-1.7 µm in height and 40-100 nm in diameter offer an increase of up to 220X the surface area over a standard flat metal oxide film for sensing applications. The metal oxide nanostructures were characterized by SEM, EDX, TEM and Hall measurements to verify stoichiometry, crystal structure and electrical properties. Additionally, the electrical response of ChemFETs and OFC SAW gas sensors with ZnO nanowires, TiO2 nanowires, and multiwall TiO2 nanotubes were measured using 5-200 ppm ammonia as a target gas at room temperature (24ºC) showing high sensitivity and reproducible testing results.

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Wang, Dake Park Minseo. « Optical spectroscopy of wide-band-gap semiconductors raman and photoluminescence of gallium nitride, zinc oxide and their nanostructures / ». Auburn, Ala., 2006. http://repo.lib.auburn.edu/2006%20Fall/Dissertations/WANG_DAKE_24.pdf.

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Prades, García Juan Daniel. « Modelling of the Chemical and Light Interactions in Individual Metal Oxide Nanowires for Sensing Applications ». Doctoral thesis, Universitat de Barcelona, 2009. http://hdl.handle.net/10803/663486.

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En la presente tesis se analizan desde el punto de vista de la modelización teórica los mecanismos de interacción de gases y luz con nanohilos individuales de óxidos metálicos. Desde este enfoque novedoso, se pretende alcanzar una mayor compresión de los mecanismos de transducción que dan lugar a la utilidad de dichos materiales en aplicaciones de sensado químico y de luz. Los resultados que aquí se presentan permiten comprender los detalles de las interacciones de gases, tanto oxidantes como reductores, sobre superficies de óxidos metálicos; siendo especialmente remarcable el descubrimiento del papel clave que juegan las vacantes de oxígeno en superficie en este proceso. Así mismo, se proponen técnicas experimentales tanto para la generación controlada de dichas vacantes como para su posterior detección. De este modo se das las herramientas necesarias para controlar a voluntad la respuesta a gases de estos materiales. Des de el punto de vista de la detección de luz, se demuestra que la gran relevancia de los efectos de superficie en los nanohilos permite obtener fotorespuestas muy por encima de las conseguidas con otras tecnologías pero, como contrapartida, la respuesta dinámica se ve severamente penalizada. Por ello se proponen y demuestran diversos métodos para modificar la influencia de la superficie en la respuesta total de los nanohilos. Finalmente, en base al conocimiento adquirido, se demuestra que es posible acoplar ambas interacciones (gas-óxido metálico y luz-óxido metálico) para ampliar las aplicaciones de estos materiales. En particular, no sólo se demuestra que es posible activar la respuesta a gases por medio de la iluminación, sino que también se presenta un modelo que describe cuantitativamente este fenómeno, abriendo las puertas a un gran número de aplicaciones de detección de gas a temperatura ambiente.

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Vabbina, Phani Kiran. « Sonochemical Synthesis of Zinc Oxide Nanostructures for Sensing and Energy Harvesting ». FIU Digital Commons, 2016. http://digitalcommons.fiu.edu/etd/2534.

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Semiconductor nanostructures have attracted considerable research interest due to their unique physical and chemical properties at nanoscale which open new frontiers for applications in electronics and sensing. Zinc oxide nanostructures with a wide range of applications, especially in optoelectronic devices and bio sensing, have been the focus of research over the past few decades. However ZnO nanostructures have failed to penetrate the market as they were expected to, a few years ago. The two main reasons widely recognized as bottleneck for ZnO nanostructures are (1) Synthesis technique which is fast, economical, and environmentally benign which would allow the growth on arbitrary substrates and (2) Difficulty in producing stable p-type doping. The main objective of this research work is to address these two bottlenecks and find a solution that is inexpensive, environmentally benign and CMOS compatible. To achieve this, we developed a Sonochemical method to synthesize 1D ZnO Nanorods, core-shell nanorods, 2D nanowalls and nanoflakes on arbitrary substrates which is a rapid, inexpensive, CMOS compatible and environmentally benign method and allows us to grow ZnO nanostructures on any arbitrary substrate at ambient conditions while most other popular methods used are either very slow or involve extreme conditions such as high temperatures and low pressure. A stable, reproducible p-type doping in ZnO is one of the most sought out application in the field of optoelectronics. Here in this project, we doped ZnO nanostructures using sonochemical method to achieve a stable and reproducible doping in ZnO. We have fabricated a homogeneous ZnO radial p-n junction by growing a p-type shell around an n-type core in a controlled way using the sonochemical synthesis method to realize ZnO homogeneous core-shell radial p-n junction for UV detection. ZnO has a wide range of applications from sensing to energy harvesting. In this work, we demonstrate the successful fabrication of an electrochemical immunosensor using ZnO nanoflakes to detect Cortisol and compare their performance with that of ZnO nanorods. We have explored the use of ZnO nanorods in energy harvesting in the form of Dye Sensitized Solar Cells (DSSC) and Perovskite Solar Cells.

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Yu, Zexin. « Development and characterization of metal oxide semiconductor films deposited by solution precursor thermal spray process ». Thesis, Bourgogne Franche-Comté, 2018. http://www.theses.fr/2018UBFCA036.

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Les procédés de photodégradation, de conversion photocatalytique du CO2 et la technologie des supercondensateurs représentent des options intéressantes pour palier aux problèmes environnementaux et pour apporter des réponses à la crise énergétique. Dans ces trois domaines, les matériaux à base d'oxydes métalliques sont très prometteurs. Cependant, les voies classiques (c'est-à-dire par voies hydrothermales ou de sol-gels) présentent un certain nombre d’inconvénients tels que leur longues durées de préparation et leurs rendements limités. En outre, la mise en oeuvre de nanopoudres suppose une opération de post-filtration dans les procédés de photodégradation et l’utilisation supplémentaire d’un liant dans la confection d’électrodes de supercondensateurs, ce qui non seulement réduit les performances respectives de ces deux procédés mais entrave également leur développement au niveau industriel. Dans cette thèse, les technologies SPPS (Solution Precursor Plasma Spray) et SPFS (Solution Precursor Flame Spray) ont été introduites pour préparer des films d'oxydes métalliques à base de ZnO, en bénéficiant des avantages de rapidité et simplicité de ces techniques de formation de dépôts. Les films ainsi obtenues ont ensuite été testés dans des expériences de photodégradation, de conversion photocatalytique du CO2 et sous forme de supercondensateurs. Tout d'abord, à notre connaissance, c'est la première fois que l'on synthétise directement des nanostructures de ZnO (par exemple des nanotubes ou des nanofils) par des procédés SPPS. Ces films nanostructurés et hiérarchisés présentent non seulement une croissance préférentielle le long du plan cristallin (002), mais contiennent aussi des lacunes d'oxygène dans leurs réseaux. La mise en œuvre de simulations DFT a permis de proposer un mécanisme possible de croissance des nanostructures de ZnO lors de leur synthèse par la voie SPPS. Deuxièmement, divers films “composites”, constitués de ZnO et d’un second oxide “MO” ont également été préparés par SPPS afin de réduire les bandes d'énergie interdites. Dans cette partie de la thèse, nous avons étudié l’effet du rapport molaire MO/ZnO sur la structure des films MO/ZnO obtenus (M = Mn et Cu); nous avons aussi préparé, par cette nouvelle méthode, des films fins CuO/ZnO et CeO2/ZnO ainsi que des films de ZnO “décorés”. Troisièmement, des films mettant en œuvre des structures du type spinelle (tels que les oxydes mixtes ZnFe2O4, NiCo2O4, ZnCo2O4 et Co3O4) ont également été synthétisés et déposés à l’aide des techniques SPPS et SPFS, ceci en raison de leur grand intérêt pour les applications susmentionnées. Il a été constaté que les structures obtenues sont très sensibles aux rapports MO/ZnO et que les morphologies de surface dépendent davantage des paramètres d'injection des solutions. En outre, la puissance de la torche joue un rôle plus critique dans la synthèse in situ de la phase spinelle binaire que la température de préchauffage du substrat. Enfin, la voie de préparation par SPPS favorise la formation de dépôts de textures floconneuses, notamment dans le cas des films de NiCo2O4 et Co3O4, tandis que des particules de formes sphériques ont été plutôt observées dans les échantillons préparés par la voie SPFS
The fields of research dealing with photodegradation, photocatalytic conversion of CO2 and supercapacitors are important to address environmental problems and respond to the energy crisis. Metal oxides are promising materials in these three domains. However, the conventional routes (i.e. hydrothermal, sol-gel) suffer from major deficiencies, namely their multi-step natures, their long preparation duration and small-scaled yields. Moreover, the usage of nanopowders implies a post-filtration operation at the end of the photodegradation processes and requires an additional binder in supercapacitor electrodes. In this thesis, “Solution Precursor Plasma Spray” (SPPS) and “Solution Precursor Flame Spray” (SPFS) technologies have been introduced to develop metal oxide films in view of the three aforementioned applications, benefiting from the facility and rapidity advantages of this one-step process.Firstly, to our best knowledge, it is the first time that films composed by ZnO nanostructures (e.g. nanorods, nanowires) are directly synthesized via a SPPS process. These hierarchical ZnO nanostructured films not only exhibit preferential orientation growth along the (002) crystal plane, but also feature in-situ oxygen vacancies. As a result, a possible growth mechanism of ZnO nanostructures via SPPS route was proposed.Secondly, various metal oxides composite films containing ZnO and a second metal oxide were also prepared by SPPS in an effort to narrow the energy bandgaps. In this work, not only the effect of the molar CuO/ZnO and MnO/ZnO ratio was investigated, but also laminated CuO/ZnO and CeO2/ZnO films and CuO, Co3O4 and Fe2O3 decorated ZnO nanorods films were pioneeringly deposited via this novel route.Thirdly, films involving spinel-type materials (including ZnFe2O4, NiCo2O4, ZnCo2O4 and Co3O4) were also synthesized and deposited by the SPPS and SPFS technologies, owing to their high-interest in the aforementioned applications. We found that the phase compositions are more sensitive to the Fe/Zn and Ni/Co ratios and that the surface morphologies are more dependent on the patterns of the solution injection. In addition, the power of the torch plays a more critical role on the in-situ synthesis of binary spinel phase. Besides, the SPPS route promotes the formation of flake-like particles both in the NiCo2O4 and Co3O4 films, while sphere-like particles were observed in the SPFS-prepared samples.Finally, some as-prepared films were selected to evaluate their performances within the three applications. On the one hand, Orange II was successfully (100%) degraded within 2h under UV irradiation and about 85% was removed within 6h under visible light irradiation. On the other hand, Co3O4 samples exhibited specific capacitances up to 1190 F g−1 with a retention capacity of 136% after 2500 cycles at a 20 mV/s scanning rate in 2 M KOH electrolyte. Finally, when using ZnCo2O4 as photocatalyst, CO2 was converted into CO by visible light irradiation with a maximum turnover number as high as 61.38 and a selectivity as high as 90.5 %.Overall, this work not only improves the performances of the three studied processes thanks to the use of novel, fast preparation methods, but also suggests that “Solution Precursor Thermal Spray” should be a highly promising technology for further, alternative functional applications that involve finely structured metal oxides film

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Zhang, Kelvin Hongliang. « Structural and electronic investigations of In₂O₃ nanostructures and thin films grown by molecular beam epitaxy ». Thesis, University of Oxford, 2011. http://ora.ox.ac.uk/objects/uuid:de125918-b36f-47cc-b72d-2f3a27a96488.

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Transparent conducting oxides (TCOs) combine optical transparency in the visible region with a high electrical conductivity. In2O3 doped with Sn (widely, but somewhat misleadingly, known as indium tin oxide or ITO) is at present the most important TCO, with applications in liquid crystal displays, touch screen displays, organic photovoltaics and other optoelectronic devices. Surprisingly, many of its fundamental properties have been the subject of controversy or have until recently remained unknown, including even the nature and magnitude of the bandgap. The technological importance of the material and the renewed interest in its basic physics prompted the research described in this thesis. This thesis aims (i) to establish conditions for the growth of high-quality In2O3 nanostructures and thin films by oxygen plasma assisted molecular beam epitaxy and (ii) to conduct comprehensive investigations on both the surface physics of this material and its structural and electronic properties. It was demonstrated that highly ordered In2O3 nanoislands, nanorods and thin films can be grown epitaxially on (100), (110) and (111) oriented Y-stabilized ZrO2 substrates respectively. The mismatch with this substrate is -1.7%, with the epilayer under tensile strain. On the basis of ab initio density functional theory calculations, it was concluded that the striking influence of substrate orientation on the distinctive growth modes was linked to the fact that the surface energy for the (111) surface is much lower than for either polar (100) or non-polar (110) surfaces. The growth of In2O3(111) thin films was further explored on Y-ZrO2(111) substrates by optimizing the growth temperature and film thickness. Very thin In2O3 epilayers (35 nm) grew pseudomorphically under high tensile strain, caused by the 1.7% lattice mismatch with the substrate. The strain was gradually relaxed with increasing film thickness. High-quality films with a low carrier concentration (5.0  1017 cm-3) and high mobility (73 cm2V-1s-1) were obtained in the thickest films (420 nm) after strain relaxation. The bandgap of the thinnest In2O3 films was around 0.1 eV smaller than that of the bulk material, due to reduction of bonding-antibonding interactions associated with lattice expansion. The high-quality surfaces of the (111) films allowed us to investigate various aspects of the surface structural and electronic properties. The atomic structure of In2O3 (111) surface was determined using a combination of scanning tunnelling microscopy, analysis of intensity/voltage curves in low energy electron diffraction and first-principles ab initio calculations. The (111) termination has an essentially bulk terminated (1 × 1) surface structure, with minor relaxations normal to the surface. Good agreement was found between the experimental surface structure and that derived from ab initio density functional theory calculations. This work emphasises the benefits of a multi-technique approach to determination of surface structure. The electronic properties of In2O3(111) surfaces were probed by synchrotron-based photoemission spectroscopy using photons with energies ranging from the ultraviolet (6 eV) to the hard X-ray regime (6000 eV) to excite the spectra. It has been shown that In2O3 is a highly covalent material, with significant hybridization between O and In orbitals in both the valence and the conduction bands. A pronounced electron accumulation layer presents itself at the surfaces of undoped In2O3 films with very low carrier concentrations, which results from the fact the charge neutrality level of In2O3 lies well above the conduction band minimum. The pronounced electron accumulation associated with a downward band bending in the near surface region creates a confining potential well, which causes the electrons in the conduction band become quantized into two subband states, as observed by angle resolved photoemission spectra (ARPES) Fermi surface mapping. The accumulation of high density of electrons near to the surface region was found to shrink the surface band gap through many body interactions. Finally epitaxial growth of In2O3 thin films on α-Al2O3(0001) substrates was investigated. Both the stable body centred cubic phase and the metastable hexagonal corundum In2O3 phase can be stabilized as epitaxial thin films, despite large mismatches with the substrate. The growth mode involves matching small but different integral multiples of lattice planes of the In2O3 and the substrate in a domain matching epitaxial growth mode.

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Falyouni, Farid. « Croissance et propriétés de nanostructures à base de ZnO ». Versailles-St Quentin en Yvelines, 2011. http://www.theses.fr/2011VERS0017.

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Ce travail a pour objectif d'étudier la croissance et les propriétés des nanostructures unidimensionnelles (nanofils) à base de ZnO. Ces nanostructures ont été réalisées par approche bottom-up selon deux mécanismes de croissance : Vapeur-Solide (VS, non catalysé) et Vapeur-Liquide-Solide (VLS, catalysé via une gouttelette d'or). Les matériaux étudiés sont élaborés par MOCVD. Les nanofils ont été caractérisés par différentes techniques, notamment en microscopie électronique à balayage (MEB), microscopie électronique en transmission TEM, spectroscopie Raman, spectroscopie de Photoluminescence (PL) et spectroscopie de Cathodoluminescence (CL). Dans un premier temps, nous portons notre attention à la croissance des nanostructures de ZnO selon le mécanisme VS. D’abord, une étude expérimentale nous a permis déterminer une condition nécessaire à la croissance spontanée de nanofils et de nanoaiguilles. En suite, nous présentons une étude comparative entre TEM et CL sur ces aiguilles de ZnO. Dans un second temps, nous étudions la croissance des nanostructures de ZnO selon le mécanisme catalysé VLS, pour lequel les fils de ZnO poussent sous une bille d'or. Nous nous intéressons plus particulièrement à l’impact des paramètres de croissance (température, rapport VI/II, pression et substrat) sur la morphologie des nanostructures et la cinétique de croissance. L’analyse structurale de nanostructures variées, nano -fils, -aiguilles, -rubans de ZnO, est réalisée par MEB et TEM. Enfin, un dernier volet concerne la possibilité de dopage des nanofils ZnO. L'incorporation d'impuretés d'azote, dopant potentiel en vue du type p, a été étudiée. Les analyses Raman et PL sur des nanofils dopés à l’azote montrent que l’azote est bien incorporé dans les fils mais que cette incorporation n’est pas homogène le long des fils
The objective of this work is to study the growth and properties of ZnO nanostructures. These nanostructures were made by bottom-up approach using two mechanisms : vapor-solid (VS) and Vapor-Liquid-Solid (VLS). The materials were prepared by MOCVD. The samples were characterized by different techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, photoluminescence spectroscopy (PL) and cathodoluminescence spectroscopy (CL). First of all, we focused on the growth of ZnO nanostructures according to the VS mechanism. An experimental study has enabled us to determine the necessary conditions to the spontaneous growth of nanowires and needles. Then we have presented a comparative study with TEM and CL of ZnO needles. Subsequently, we investigated the growth of ZnO nanostructures according to the VLS mechanism which refers to "catalysed" growth. We were particularly interested in the impact of the growth parameters (temperature, rapport VI/II, pressure and substrate) on the nanostructures morphologies and their growth kinetics. The structural properties of ZnO nanostructures has been studied by SEM and TEM; this study showed the different morphologies of nanowires, needles and rubans. Finally, in this work we investigated the possibility of incorporating dopant impurities in ZnO nanowires. The case of nitrogen for a potential p-type conduction was studied. Raman and PL analysis on the nanowires doped with nitrogen shows that nitrogen is incorporated into the nanowires and that incorporation is not homogeneous along the nanowires

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El, Zein Basma. « Growth and characterization of zinc oxide (ZnO) nanostructures for photovotaic applications ». Thesis, Lille 1, 2012. http://www.theses.fr/2012LIL10141/document.

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Le développement des nanotechnologies offre de nouvelles perspectives pour la conception des cellules solaire à fort rendement de conversion. Jusqu’à présent les efforts se sont portés principalement sur des structures à base de semi-conducteurs, de métaux et de polymères. Dans nos travaux, nous avons considéré des nanoparticules de Sulfure de Plomb (PbS) pour lesquelles l'énergie de bande interdite et les propriétés optiques sont fonction de la taille de la particule afin de tirer parti de l'ensemble du spectre optique couvert par l'énergie solaire. Nous avons également considéré des nanofils d'oxyde de zinc (ZnO) pour la séparation et le transport des charges photo-crées. Nous pensons que l'association des nanoparticules de PbS avec des nanofils de ZnO devrait pouvoir augmenter considérablement le rendement des cellules solaires. Dans ce but, nous avons démontré la croissance auto-ordonné des nanofils de ZnO sur substrats silicium et verre par dépôt laser pulsé (pulsed laser deposition ) utilisant le réseau de nanoparois de ZnO en forme de nid d'abeille comme couche germe. Nous avons démontré que les conditions de croissance sont essentielles pour contrôler la cristallinité, la morphologie des nanofils de ZnO , ainsi que la densité de défauts de croissance. Les analyses MEB, DRX, TEM, et HR-TEM montrent que nous avons obtenu des nanostructures très cristallines et orientées verticalement. Nous avons également démontré la croissance in-situ de nanoparticules de PbS sans ligand sur la surface des nanofils de ZnO verticaux à l'aide de la technique SILAR (Successive Ionic Layer Adsoprtion and Reaction) .Nous avons constaté que les nanoparticules de PbS sont fortement accrochées à la surface des nanofils de ZnO avec différentes dimensions et des densités variables .Ces résultats ont été obtenus sans introduire de matière organique (Ligand) qui pourrait perturber à la fois la structure électronique à l'interface ZnO/PbS et le transfert des électrons du PbS au ZnO. Les analyses MEB, TEM et HR-TEM confirment le bon accrochage des nanoparticules de PbS sur les nanofils de ZnO . Leur forme est sphérique et elles sont poly-cristallines. A la fin de ce travail de thèse nous proposons une hétérojonction p-PbS/n-ZnO constituée de nanoparticules de PbS dopées P et de nanofils de ZnO dopés n pour de futures applications en photovoltaïque
To date, the development of nanotechnology has launched new ways to design efficient solar cells. Strategies have been employed to develop nanostructure architectures of semiconductors, metals, and polymers for solar cells. In this research we have considered the Lead sulfide (PbS) nanoparticles with their tunable band gap and optical properties to harvest the entire solar spectrum which can improve the optical absorption, and charge generation. On the other hand, Zinc oxide (ZnO) nanowires will provide the charge separation and transportation. The ZnO Nanowires sensitized with PbS nanoparticles might significantly impact power conversion efficiency of the solar cells Driven by these unique properties, we demonstrate the successful growth of self catalyzed ZnO nanowires on silicon and glass substrates, by pulsed laser deposition (PLD) using ZnO nanowall network with honeycomb structure as seed layer. We identified that the growth parameters are vital to control the crystallinity, morphology and the defect levels in the synthesized ZnO nanowires. SEM, XRD, TEM, HRTEM analysis show that the nanostructures are highly crystalline and are vertically oriented. We also report the in-situ growth of PbS nanoparticles without linker on the surface of well –oriented ZnO NWs by (SILAR) technique. The PbS Nanoparticles are packed tightly on the surface of the ZnO Nanowires with different sizes and densities, without insulating nature organic ligands, which might affect both the electronic structure at the interface and the electron - transfer rate. The SEM, TEM, HRTEM, PL and XRD analysis, confirm the attachment of the spherical shape polycrystalline PbS nanoparticles. We propose at the end of the thesis the p-PbS /n-ZnO hetero-junction with its future applications in solar cells

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Renault, Christophe. « Spectroélectrochimie résolue en temps de biomolécules sur électrode poreuse transparente nanostructurée ». Paris 7, 2011. http://www.theses.fr/2011PA077173.

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Des molécules comme les enzymes et certains complexes biomimétiques sont capables de catalyser des réactions chimiques avec une grande efficacité grâce à des mécanismes relativement complexes. Pour étudier ces derniers, nous avons développé une nouvelle technique de spectroélectrochimie résolue en temps où la sonde redox est immobilisée dans un film inorganique poreux plus ou moins conducteur et transparent dans le visible. Dans un premier temps, nous avons utilisé un film semiconducteur de TiO₂ déposé par voie sol gel (EISA) et caractérisé par une mésoporosité hautement structurée. Des expériences de voltamétrie cyclique et de chronampérométrie suivies en temps réel par spectroscopie d'absorption UV-visible nous ont permis de mettre en évidence les modes de transport et de transfert de charges à l'origine de la conversion électrochimique de deux porphyrines de fer et d'une protéine hémique, adsorbées dans l'électrode poreuse de TiO₂. Grâce à la technique de dépôt physique GLAD, nous avons aussi pu disposer d'une électrode conductrice transparente d'oxyde d'indium dopé à l'étain (ITO) caractérisée par une macroporosité structurée. Nous avons étudié la conduction de cette électrode ainsi que la thermodynamique et la cinétique du transfert électronique avec une porphyrine de fer, une flavine et deux protéines hémiques, adsorbées dans l'électrode poreuse d'ITO. Nous avons par ailleurs vérifié qu'il est parfaitement possible d'utiliser d'autres spectroscopies dans le domaine visible, comme par exemple le Raman résonant sur les systèmes hémiques. Enfin nous avons montré qu'il est possible d'atteindre avec les électrodes poreuses d'ITO une résolution temporelle d'environ 10 ms
Enzymes and biomimetic complexes are able to catalyze efficiently a large variety of chemical reactions nevertheless they generally involve complicated mechanisms. To study these latter we developed a new time-resolved spectroelectrochemical technique where the redox probe is immobilized in a more or less conductive porous inorganic film but still transparent in the visible range. First we used TiO₂ semiconductive films deposited by sol gel chemistry (EISA) and characterized by a highly organized mesoporsity. By the mean of chronoamperometric and cyclic voltamétrie experiments coupled to real time UV-visible absorbance monitoring, we evidenced and characterized the different charge transport and charge transfer process that cause the oxidation/reduction of two iron porphyrines and one hemoprotein adsorbed in the porous TiO₂electrode. Thanks to a physical deposition technique we also disposed of conductive transparent electrodes of indium tin oxide characterized by a well structured macroporosity. We studied the conduction of this second type of electrode and the thermodynamic/kinetic of electron transfer with an iron porphyrin, a flavin and two hemoprotein adsorbed in the porous ITO electrode. We also confirmed the possibility to perform other types of spectroscopies in the visible range such as resonant Raman for hemes. Finally we demonstrated a time resolution of about 10 ms for the porous ITO electrodes

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Amirifar, Nooshin. « Métrologie des dopants dans les nanostructures ZnO par sonde atomique tomographique ». Rouen, 2015. http://www.theses.fr/2015ROUES030.

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Ces dernières années, un nombre accru de travaux de recherche ont été menés pour le développement de dispositifs optoélectroniques et électroniques à base de ZnO. La conception de ces dispositifs nécessite une maîtrise totale des processus de synthèse et de dopage car ils en déterminent les propriétés électriques et optiques finales. Aujourd’hui encore, l'un des obstacles majeur à la réalisation de tels dispositifs réside dans la difficulté d’obtenir un dopage de type-p dans le ZnO. Il faut pour cela des techniques de caractérisation pouvant fournir des informations directes sur la distribution des dopants. Dans ce travail de thèse, la sonde atomique tomographique (SAT), a été utilisée afin d’étudier l’incorporation de dopants dans des films minces et des nanofils de ZnO. Deux types de dopage ont été étudiés. Des dopages de type-p de nanofils de ZnO ont été entrepris par deux techniques différentes : l’une ex-situ, par diffusion thermique après élaboration des nanofils et l’autre, in-situ, par incorporation durant la croissance. Bien qu’une incorporation homogène des dopants ait été obtenue, les nanofils présentent une conductivité de type-n. Des dopages avec des éléments de terres rares (TR) ont également été étudiés pour améliorer les propriétés optiques des couches minces de ZnO. Il a été montré que les traitements thermiques influencent fortement les propriétés optiques des ZnO:TR. L’analyse en SAT a montré que les recuits ont peu d’influence sur la distribution des dopants. Cette étude montre que les propriétés électriques et optiques du ZnO sont très sensibles aux paramètres d’élaboration et de post-traitement mais que les plus pertinents sont encore à découvrir
In recent years, an increasing number of research studies has been conducted for the development of optoelectronic and electronic devices based on ZnO. The design of these devices requires a total control of synthesis and doping process as they determine the final electrical and optical properties. Today, one major obstacle in achieving such devices is the difficulties of obtaining a p-type ZnO. Achieving this requires proper characterization techniques that can provide direct information about the distribution of dopants. In this thesis, atom probe tomography (APT) has been used to study the incorporation of dopants in ZnO thin films and nanowires. Two types of doping were studied. P-type doping of ZnO nanowires were attempted by two different techniques: one ex-situ process through thermal diffusion into undoped nanowire and the other one through an in-situ incorporation during the wire growth. It was shown that despite the fact that a homogeneous incorporation of dopants was achieved, the doped nanowires showed n-type conductivity. Doping with rare earth elements (RE) was also studied in order to improve the optical properties of ZnO thin films. It has been shown that heat treatments strongly influence the optical properties of the doped thin layers. Analysis by APT has revealed a slight influence of heat treatments on the distribution of dopants. This study shows that the electrical and optical properties of ZnO are strongly dependent on the elaboration and annealing parameters but the most relevant parameter are yet to be discovered

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Merupo, Victor Ishrayelu. « Synthèse et caractérisation de matériaux nanostructurés BiVO4 dopés par des métaux pour des applications en Photocatalyse ». Thesis, Le Mans, 2016. http://www.theses.fr/2016LEMA1006/document.

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Le travail de thèse est consacré à la synthèse, l’élaboration et à l’étude des propriétés physiques d’une famille d’oxydes semi-conducteurs BiVO4 sous formes de nanostructures et de films minces incluant un dopage métallique (Metal = Cu, Mo et Ag) dans le but de réaliser des photocatalyseurs efficaces sous irradiation en lumière visible. La synthèse de nanopoudres dopées a ainsi été effectuée par la technique de broyage planétaire à haute énergie ainsi que par la méthode sol-gel. Les matériaux obtenus et les effets de dopage ont été étudiés sur les caractéristiques structurales, électroniques et optiques. En conjuguant des études par XPS, Raman et RPE, nous avons montré que le dopage substitutionnel est effectivement réalisé pour les ions (Cu, Mo) localisés dans les sites cristallins des ions vanadium alors que le dopage par l’élément Ag contribue à former des clusters métalliques localisés à la surface de nanoparticules de BiVO4 formant ainsi des nanocomposites. Les réactions photocatalytiques ont été étudiées par la dégradation de colorants organiques (Acide bleu 113, méthyle orange (MO)) dans des solutions faiblement concentrées. Parmi les ions dopants substitués dans les matrices hôtes, le dopage au cuivre (Cu2+) a montré de meilleures performances en raison d'une augmentation de la densité de charges photo-générées et de la conductivité électrique par rapport au cas du dopage au molybdène. Pour le dopage à l’argent, la formation de clusters métalliques donnent lieu à des effets de résonances plasmoniques qui améliorent l'efficacité photocatlytique à un niveau équivalent à celui du dopage substitutionnel au cuivre. La deuxième contribution de ce travail a porté sur la réalisation par pulvérisation cathodique rf-magnétron de films minces BiVO4 dopés par des éléments Mo et Cu dans des conditions définies par l'atmosphère de dépôt à base de pressions partielles d’un gaz Ar ou d’un mélange Ar / O2 et des températures de substrats variables jusqu'à 450 ° C. Les paramètres optimaux de dépôt ont été identifiés pour réaliser des films cristallins à faible rugosité de surfaces ou à morphologies en nano-îlots. Des études photocatalytiques utilisant des films minces dopés ont été effectuées par la dégradation des colorants organiques (MO) sous rayonnement visible. Ces études montrent que la morphologie des films avec des surfaces spécifiques importante est aussi un facteur d’amplification des performances photocatalytiques des films minces dopés Me-BiVO4
The thesis work is devoted to the synthesis and investigations of the physical properties of a family of semiconducting oxides based on BiVO4 as nanostructures or thin films including a metal doping (Metal = Cu, Mo and Ag) in order to achieve effective photocatalysts under visible light irradiation. The synthesis of doped nanopowders was carried out by the techniques of high-energy ball milling and sol-gel. The resulting materials and doping effects were characterized on the structural, electronic and optical properties. By combining XPS, Raman and EPR studies, it was shown that the substitutional doping is achieved for the doping ions (Cu, Mo) being located in the lattice sites of the vanadium ions. Oppositely, Ag doping contributes to form Ag metal clusters located on the surface of nanoparticles of BiVO4 thereby forming nanocomposites. Photocatalytic reactions were studied by the degradation of organic dyes (Acid Blue 113, methyl orange (MO)) in low concentrated solutions. Among the doping ions substituted in the host matrices, Cu2+ showed better photocatalytic performances because of an increase in the density of photo-generated charges and similar effect on the electrical conductivity compared to the case of Mo doping. In the Ag based nanocomposites, the formation of metal clusters seems to induce surface resonance plasmonic effects that improve the efficiency of photocatalytic reactions with respect to the activity demonstrated for substitutional doping. The second contribution of the thesis work was devoted to BiVO4 thin films deposition by rf sputtering process with Mo and Cu doping under defined synthesis conditions such as the partial pressures of Ar gas or an Ar / O2 mixture and varying the substrate temperatures up to 450 ° C. The optimal deposition parameters have been identified to achieve crystalline films with low roughness surface or alternatively with nano-islands morphologies. Photocatalytic studies using doped thin films were carried out through the degradation of organic dyes (MO) under visible light irradiation. The performed measurements show that the film morphology with high specific surface is also a key factor in the amplification of photocatalytic reactions in metal doped thin films

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Koussi-Daoud, Sana. « Préparation électrochimique et caractérisation de couches nanostructurées de semi-conducteurs de type p pour cellules photovoltaïques hybrides ». Thesis, Paris 6, 2016. http://www.theses.fr/2016PA066505/document.

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Cette thèse visait à développer des techniques de croissance électrochimiques d'oxydes pour obtenir des semi-conducteurs de type p utilisables comme photocathodes dans les cellules solaires à colorant (p-DSSC). Dans la littérature, la méthode d'électrodépôt n'a pas été explorée pour l'application p-DSSC. Les conditions de synthèse de films de NiO avec une épaisseur contrôlée ont été définies. Des couches de NiO ont été obtenues par électrodépôt en milieu aqueux, en milieu éthanol, en milieu diméthylsulfoxide DMSO et en milieu mixte DMSO/eau. Ces couches ont été caractérisées par DRX, spectroscopie Raman, MEB, mesures optiques, etc¿ puis testées comme photocathode dans des p-DSSC. L'électrodépôt de l'oxyde cuivreux Cu2O en milieu aqueux a été également étudié. Les rendements de conversion photovoltaïques des dispositifs ont été déterminés. Une nanostructuration des couches d'oxyde de nickel et d'oxyde cuivreux a aussi été réalisée en utilisant comme agent structurant des sphères de polystyrène fonctionnalisées par des groupements carboxyls. Enfin, nous avons exploré l'électrodépôt de la delafossite de cuivre CuFeO2 en milieu DMSO
The objective of this thesis was the electrochemical deposition (ECD) of p-type semiconductors forthe fabrication of p-Dye Sensitized Solar Cells (p-DSSCs). The electrodeposition method remained unexploredfor the p-DSSC applications. The best conditions for ECD of nickel oxide layers with a controlled thickness havebeen defined. Nickel oxide has been deposited in water medium, in ethanol, in dimethyl sulfoxide (DMSO)medium and in a mixture of DMSO/water solvent. The layers have been characterized by XRD, Ramanspectroscopy, SEM, optical measurements… then have been tested as a photocathode in p-DSSCs. The cuprousoxide (Cu2O) electrodeposition in an aqueous bath has also been investigated. The photovoltaic efficiency of thevarious prepared layers has been evaluated in p-DSSCs. We have also prepared inverse opal organized structureswith a perfectly defined macropore organization and size using a macrosphere polystyrene template. Finally, wehave explored the ECD of a copper delafossite CuFeO2 in DMSO medium

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Sandana, Eric Vinod. « Synthèse et maîtrise de la croissance de nanocristaux : applications aux composants à base de semi-conducteurs à grande bande interdite ». Palaiseau, Ecole polytechnique, 2011. http://pastel.archives-ouvertes.fr/docs/00/64/06/52/PDF/Eric_Vinod_SANDANA_Ecole_Polytechnique_EDX_447.pdf.

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Ce travail a pour objectif la maitrise de la croissance et l'analyse des propriétés des nanostructures d'oxyde de zinc (ZnO). Trois procédés de fabrication de nanostructures de ZnO ont été étudiés : dépôt chimique en phase vapeur de composés organométalliques (MOCVD), dépôt par ablation laser (PLD) et dépôt par transport physique en phase vapeur (PVT). Les substrats utilisés pour cette étude sont : saphir, silicium, ZnO massif, acier austénitique, mylar et papier. Les nanostructures ont été caractérisées par différentes techniques, notamment la microscopie électronique à balayage, la photoluminescence, la cathodoluminescence, la diffraction de rayon X et des mesures de réflectivité. Une grande variété de formes de structures a été obtenue par les trois procédés de croissance : nanofiles, nanocolonnes, nanocônes, nanopeignes. Mais par PLD on obtient des réseaux de nanocolonnes et nanocônes autoformées, alignées, verticales, homogènes dont les qualités structurales sont excellentes y compris sur des substrats avec lesquels ZnO n'a pas un bon accord paramétrique. Ces nanostructures sont obtenues sans utiliser de catalyseur. Leurs propriétés d'émission sont aussi excellentes avec des bandes de défauts, observables en PL, relativement faibles. La faisabilité de composants à base de nano ZnO a été démontrée grâce à la réalisation d'une nanoLED de type n-nanoZnO/ p-Si, mais aussi par la reprise de croissance de GaN sur des nanocônes de ZnO/Si qui agissent comme une couche antireflet (~95% d'absorption de la lumière visible). L'étude a aussi porté sur la fabrication d'un composant transistor couche mince dont les caractéristiques de transfert rectifiante ont été obtenues
The objective of this work was to grow, study & control the properties of ZnO thin films & nanostructures. Three growth processes were studied: Metal-Organic Chemical Vapour Deposition (MOCVD), Pulsed Laser Deposition (PLD) & Physical Vapour Transport (PVT). The substrates used were: c-Al2O3; Si, ZnO, steel, mylar & paper. The ZnO was characterized using scanning electron microscopy, photoluminescence , cathodoluminescence , X-ray diffraction & optical reflectivity. A very wide range of ZnO nanostructures was observed, including nanorods, nanoneedles, nanocombs & some novel structures. Self-forming arrays of vertically aligned nanostructures (moth-eye nanocones & nanocolumns (vertical & broadening)) could be obtained by PLD without the use of a catalyst. The various characterisation techniques indicated that these arrays were significantly better crystallized & more highly oriented than those grown by PVT/MOCVD. The feasibility of devices was also demonstrated. A nanoLED (n-nanoZnO/p-Si) had a rectifying I/V characteristic & gave blue/white electroluminescence. Moth-eye coatings on Si, resembling black-silicon, were used as templates for the growth of GaN by MOCVD. Angular-dependent specular reflection indicated that the GaN/ZnO nanostructures were broadband antireflection coatings with < 1% reflection over the visible spectrum for incidence angles < 60°. A back-gate geometry ZnO/Si3N4/SiO2/Si transparent thin film transistor was fabricated. It demonstrated a rectifying transfer characteristic, hard saturation & enhancement mode operation. Id was in the mA range & the VON was ~ 0V. Finally, conductive Amorphous Oxide Semiconductor ZnO was grown at RT on paper & mylar

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Bouhjar, Feriel. « Preparation et performance d'une cellule photocatalytique à base d'hématite pour la génération d'hydrogène ». Doctoral thesis, Universitat Politècnica de València, 2018. http://hdl.handle.net/10251/106345.

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El hidrógeno es un portador de energía que ya ha demostrado su capacidad para reemplazar el petróleo como combustible. Sin embargo, los medios de producción actualmente en uso siguen siendo altamente emisores de gases de efecto invernadero. La foto-electrólisis del agua es un proceso que, a partir de la energía solar, separa los compuestos elementales del agua como el hidrógeno y el oxígeno utilizando un semiconductor con propiedades físicas adecuadas. La hematita (¿-Fe2O3) es un material prometedor para esta aplicación debido a su estabilidad química y su capacidad para absorber una porción significativa de la luz (con una banda prohibida entre 2.0 - 2.2 eV). A pesar de estas propiedades ventajosas, existen limitaciones intrínsecas al uso de óxido de hierro para la descomposición fotoelectroquímica del agua. La primera restricción es la posición de su banda de conducción que es menor que el potencial de reducción de agua. Esta limitación se puede superar mediante la adición en serie de un segundo material, en tándem, que absorberá una parte complementaria del espectro solar y llevar a los electrones a un nivel de energía más alto que el potencial para la liberación de hidrógeno. El segundo obstáculo proviene del desacuerdo entre la corta longitud de difusión de los portadores de carga y la profundidad de penetración larga de la luz. Por lo tanto, es necesario controlar la morfología de los electrodos de hematita en una escala de tamaño similar a la longitud de transporte del orificio. En esta tesis, se introduce un nuevo concepto para mejorar el rendimiento fotoelectroquímico de la hematita. Usando el método hidrotermal depositamos capas delgadas de hematita dopada con Cr en sustratos de vidrio conductivo. También se ha preparado por medios electroquímicos una heterounión del tipo p-CuSCN/n-Fe2O3 depositando secuencialmente una capa de ¿-Fe2O3 y una película de CuSCNsobre sustratos de FTO (SnO2: F).Finalmente, se ha preparado células solares de perovskitas y óxido de hierro. Para ello se depositó una capa delgada, densa y uniformede óxido de hierro (¿-Fe2O3) como capa de transporte de electrones (ETL) en lugar de dióxido de titanio (TiO2) que se utiliza convencionalmente en las células fotovoltaicas perovskitastipoCH3NH3PbI3 (SGP). Este último dispositivo mostró un aumento en la fotocorriente del 20% y un IPCE30 veces mayor que la hematita simple, lo que sugiere una mejor conversión de las longitudes de onda por encima de 500 nm. Palabras clave: Fotoelectroquímica, división de agua, producción de hidrógeno, evolución de oxígeno, semiconductores de óxido de metal, hematita, óxido de hierro, nanoestructuras
Hydrogen is an energy carrier that has already demonstrated its ability to replace oil as a fuel. However, the means of production currently used remain highly emitting greenhouse gases. Photo-electrolysis of water is a process that uses solar energy to separate the elemental compounds of water such as hydrogen and oxygen using a semiconductor with adequate physical properties. Hematite (¿-Fe2O3) is a promising material for this application because of its chemical stability and ability to absorb a significant portion of light (with a band-gap between 2.0 - 2.2 eV). Despite these advantageous properties, there are intrinsic limitations to the use of iron oxide for the photoelectrochemical cracking of water. The first constraint is the position of its conduction band, which is lower than the water reduction potential. This constraint can be overcome by the addition in series of a second material, in tandem, which will absorb a complementary part of the solar spectrum and bring the electrons to a higher energy level than the potential of hydrogen release. The second obstacle comes from the disagreement between the short diffusion length of the charge carriers and the long light penetration depth. It is therefore necessary to control the morphology of the hematite electrodes on a scale of similar size to the transport length of the hole. In this thesis a new concept is introduced to improve the photoelectrochemical performances. Using the hydrothermal method we deposited thin layers of Cr-doped hematite on conductive glass substrates. We also electrochemically prepared a p-CuSCN / n-Fe2O3 heterojunction by sequentially depositing ¿-Fe2O3 and CuSCN films on FTO (SnO2: F) substrates. Finally, we have used uniform and dense thin layers of iron oxide (¿-Fe2O3) as an electron transport layer (ETL) in place of titanium dioxide (TiO2) conventionally used in photovoltaic cells based on perovskites CH3NH3PbI3 (PSC). This latter concept showed a 20% increase of the photocurrent and an IPCE 30 times greater than the simple hematite, suggesting better conversion of high wavelengths (> 500 nm). Keywords: Photoelectrochemistry, Water Splitting, Hydrogen Production, Oxygen Evolution, MetalOxide Semiconductors, Hematite, Iron Oxide, Nanostructures, Surface.
L'hidrogen és un proveïdor d'energia que ja ha demostrat la seva capacitat per reemplaçar el petroli com a combustible, però els mitjans de producció actuals continuen essent fortament emissors dels gasos responsables d'efecte hivernacle. La fotoelectròlisi de l'aigua és un procés que, a partir de l'energia solar, separa els compostos elementals d'aigua com l'hidrogen i l'oxigen utilitzant un semiconductor amb propietats físiques adequades. La hematita (¿-Fe2O3) és un material prometedor per a aquesta aplicació a causa de la seva estabilitat química i capacitat d'absorbir una porció significativa de la llum (amb un gap entre 2,0 i 2,2 eV). Malgrat aquestes propietats avantatjoses, hi ha limitacions intrínseques per a l'ús d'òxid de ferro per a la descomposició fotoelectroquímica de l'aigua. La primera restricció és la posició de la seva banda de conducció que és inferior al potencial de reducció d'aigua. Aquesta limitació es pot superar mitjançant l'addició en sèrie d'un segon material, en tàndem, que absorbirà una part complementària de l'espectre solar i portar els electrons a un nivell d'energia més alt que el potencial per a l'alliberament d'hidrogen. El segon obstacle prové del desacord entre la curta durada de la difusió dels portadors de càrrega i la llarga profunditat de penetració de la llum. Per tant, és necessari controlar la morfologia dels elèctrodes d'hematita en una escala de mida similar a la longitud del forat del transport. En aquesta tesi, es presenta un nou concepte per millorar el rendiment fotoelectroquímic. Mitjançant el mètode hidrotermal es van dipositar capes primes de hematita Cr-doped sobre substrats de vidre conductor. També s'han preparat electroquímicamentheterounions de tipus p-CuSCN/n-Fe2O3 dipositant seqüencialment una capa de ¿-Fe2O3 i altra de CuSCN sobre substrats FTO (SnO2: F).Finalment, s'han produït cél·lules solars de perovskitesi óxid de ferro. Per això es va depositaruna capa prima,densai uniforme d'òxid de ferro (¿-Fe2O3) com a capa de transport d'electrons (ETL) en lloc de diòxid de titani (TiO2) que s'utilitza convencionalment en les cèl·lules fotovoltaiques de perovskita híbrida del tipus CH3NH3PbI3 (SGP). Aquest últim dispositiu va mostrar un augment del fotocorrent del 20% i una IPCE30 vegades superior a la hematita simple, la qual cosa suggereix una millor conversió a longitud d'ones per sobre de 500 nm. Paraules clau:Fotoelectroquímica, divisió d'aigua, producció d'hidrogen, evolució d'oxigen, semiconductors d'òxids metàl·lics, hematita, òxid de ferro, nanoestructures.
Bouhjar, F. (2018). Preparation et performance d'une cellule photocatalytique à base d'hématite pour la génération d'hydrogène [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/106345
TESIS

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Haneche, Nadia. « Etudes optiques de ZnO et des solutions solides Zn[1-x]MgxO et Zn[1-x]CdxO : conception de nanostructures et dopage de type p ». Versailles-St Quentin en Yvelines, 2011. http://www.theses.fr/2011VERS0037.

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L’oxyde de zinc (ZnO) est un semi conducteurs à grand gap actuellement très étudié pour les applications en optoélectronique. Les verrous actuels pour ces applications sont liés à la conception de structures à puits quantiques, et surtout à la réalisation du dopage type p de ZnO. Dans cette perspective, nous avons étudié les propriétés optiques des couches élaborées par MOCVD principalement à l’aide de la photoluminescence (PL). Les alliages Zn1-xMgxO et Zn1-xCdxO ont montré de très bons taux d’incorporation du Mg et de Cd. Les hétérostructures à puits quantiques de ZnO/Zn1-XMgXO polaires, et non polaires (sans champ électrique interne), sont de bonne qualité optique et structurale. Concernant le dopage type p de ZnO, le dopage azote des fils est plus efficace avec le précurseur NH3. Les couches dopées antimoine sont fortement dopées. Par ailleurs, il semble que deux types d’accepteurs différents évoluent dans les couches réalisées sur substrat ZnO et saphir-R
Zinc oxide (ZnO) is a wide band gap semiconductor, and receives actually a considerable attention for the realization of optoelectronics devices. The current problems for these applications are related to the growth of quantum well structures, but especially to the successful of the p-type doping of ZnO. From this point of view, we studied the optical properties of layers and nanowires prepared by MOCVD using mainly the photoluminescence spectroscopy (PL). MgxZN1-xO and the CdxZn1-xO alloys show a very good incorporation of Mg and Cd. ZnO/MgXZn1-XO quantum well heterostructures on polar, and non-polar orientations (without an internal electric field) are obtained with a good structural and optical quality. Regarding to the p-type doping of ZnO, nitrogen doping seems to be more efficient with the NH3 precursor. The antimony doped layers are heavily doped. Moreover, it seems that two types of acceptors are observed into the layers made on C-oriented ZnO and R-sapphire substrates

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González, Fernández Alfredo A. « Studies and integration of Silicon-based light emitting systems ». Doctoral thesis, Universitat de Barcelona, 2014. http://hdl.handle.net/10803/285863.

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This project presents the study of luminescent devices and materials based on silicon for its use in the fabrication of an optical system that integrates light emitter, waveguide, and light sensor in a single chip obtained by the use of standard CMOS techniques and materials. The atomic and structural characteristics of the materials are analysed and related to its luminescent response. Taking into account the results from the active material characterization, the design, fabrication, and characterization of electroluminescent devices based on such materials is presented. Finally, the design, fabrication and characterization of a complete CMOS compatible Integrated Optical System consisting of a transceiver, is discussed and analysed. The active materials used for light emission were different Silicon Rich Silicon Dioxide(SRO) and SRO-Si3 N4 bi-layers, obtained by a variety of CMOS compatible techniques and fabrication parameters. Two contributing mechanisms to photoluminescence in SRO were identified in all cases, respectively linked to the presence of radiative defects, and to Quantum Confinement phenomena. It is proposed and tested a model to describe the latter, based on the effective mass approximation, and the relation between the amount of Si-Si links and the volume of nano-agglomerates present in the material. In bi-layer samples, an additional luminescence band was observed, found to be generated in the transition material between silicon nitride and dioxide, and related to energy states introduced by defects. Samples with SRO thickness ten times higher than that of nitride, presented a clear dominance of the photoluminescence related to the dioxide. The centres responsible for electroluminescence in the electronicd evices were found to be fundamentally the same as those for photoluminescence despite the differences in measured spectra, and it was concluded that the influence of the architecture on the light output is of significant importance. It was shown that bi-layered devices delivered better results in terms of efficiency, light emission control, distribution and stability. The carrier transport mechanisms observed in the devices were dominated by material breakdown in single-layered devices, and Trap-assisted Tunnelling in the bi-layers. The Optical System integrating the light emitter, a waveguide, and a light detector, was designed and fabricated based on the results from the fabrication and analysis of the stand alone light emitting devices. During the design stage, it was corroborated by computer simulations that the characteristics of thelight emittedby thedevices thatpresented thehighest e.ciency and reliability, were suitable for its transmission trough the proposed waveguide architecture. The detection capabilities of the designed light sensors were also theoretically corroborated to be appropriated for the detection of the emitted light type. The proper functioning of the elements conforming the finally fabricated system was probed. Differences were found in the operation of the stand alone light emitting devices and those integrated, but the resulting luminescence was within the boundaries of the transmittable spectrum. The operation of the Integrated Optical System was tested and preliminarily studied, obtaining positive results in its stimulus-detection response, fulfilling the main objective of the work, and opening the door for further studies which can lead to the optimization of the design for particular applications.
Este proyecto aborda el estudio de dispositivos y materiales luminiscentes basados en silicio para su uso en la fabricación de un sistema óptico que integre emisor de luz, guía de ondas, y sensor en un solo chip obtenido mediante el uso de técnicas y materiales estándar para la fabricación CMOS. Las características atómicas y estructurales de los materiales son analizados y relacionados con su respuesta luminiscente. Considerando los resultados de la caracterización del material activo, se presenta el diseño, fabricación, y caracterización de dispositivos electroluminiscentes basados en dichos materiales. Finalmente, se discute y analizan el diseño, fabricación, y caracterización de un transceptor como Sistema Óptico Integrado. Los materiales activos para la emisión de luz fueron distintos Dióxidos de Silicio enriquecidos con Silicio (SRO por sus siglas en inglés) y bi-capas SRO-Si3 N4, obtenidos mediante una variedad de técnicas compatibles con los procesos CMOS y distintos parámetros para los mismos. Se identificaron dos mecanismos que contribuyen a la fotoluminiscencia del SRO en todos los casos, relacionados con defectos radiativos y fenómenos de Confinamiento Cuántico, respectivamente. Se sugiere y pone a prueba un modelo para describir este último, basado en la aproximación de la masa efectiva y la relación entre la cantidad de enlaces Si-Si y el volumen de nano-aglomerados. En muestras bi-capa, se observó una banda adicional de luminiscencia, cuya generación fue identificada en el material de transición entre el nitruro de silicio y el óxido, y relacionada con estados de energía introducidos por defectos. Muestras con un espesor de SRO diez veces mayores a aquel del nitruro presentaron una clara dominación de la luminiscencia relacionada con el óxido. Se halló que los centros responsables por la electroluminiscencia en los dispositivos electrónicos son fundamentalmente los mismos que los responsables de la fotoluminiscencia a pesar de las diferencias en los espectros medidos, y se concluyó que la influencia de la arquitectura sobre el espectro de salida es de importancia significativa. Se mostró que dispositivos bi-capa entregan mejores resultados en términos de eficiencia, control sobre la luz emitida, distribución de la misma, y estabilidad en el funcionamiento. Se observó que los mecanismos de transporte de carga hallados en los dispositivos están dominados por ruptura del material en el caso de dispositivos de una sola capa, y Tuneleo Asistido por Trampas en el caso de dispositivos bi-capa. El Sistema Óptico que integra el emisor, una guía de ondas, y el detector de luz, fue diseñado y fabricado con base en los resultados de la fabricación y análisis de los dispositivos emisores de luz aislados. Durante la etapa de diseño, se corroboró mediante simulaciones por computadora que las características de la luz emitida por los dispositivos que presentaron la máxima eficiencia y fiabilidad fueran apropiadas para su transmisión a través de la guía de ondas propuesta. También se corroboró teóricamente que las capacidades de detección de los sensores diseñados fuera la adecuada para el tipo de luz emitida. Se exploró el apropiado funcionamiento de los elementos del sistema finalmente fabricado. Se encontraron diferencias en la operación de los dispositivos emisores de luz aislados y aquellos integrados, pero la luminiscencia resultante se halló dentro de los límites del espectro transmisible. La operación del Sistema Óptico Integrado fue probada y estudiada de manera preliminar, con la obtención de resultados positivos en su respuesta estímulo-detección, cumpliendo así con el objetivo principal del trabajo, y abriendo la puerta para estudios posteriores que pueden guiar a la optimización del diseño del sistema para aplicaciones particulares.

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Altomare, M. « TOWARDS THE PHOTOCATALYTIC PRODUCTION OF SOLAR FUELS - NANOSTRUCTURED TITANIUM DIOXIDE FOR PHOTOCATALYSIS & ; PHOTO-ELECTROCHEMISTRY ». Doctoral thesis, Università degli Studi di Milano, 2014. http://hdl.handle.net/2434/229553.

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In spite of many efforts given during the last decades to find new alternative photocatalytic materials, titanium dioxide (TiO2) still represents the most widely employed semiconductor for photocatalytic applications, being photoactive, cheap, easily available, non-toxic, inert and, most of all, chemically stable. However, although exhibiting a powerful combination of extraordinary and attractive physico-chemical properties, it suffers from some issues, common to all semiconductors, related to the dynamic of the charge carriers. Precisely, trapping and recombination of valence band holes and conduction band electrons occur at a certain extent, anyway resulting in a drop of the process efficiency. Therefore, in view of limiting these detrimental phenomena, the charge transfer and the electric conductivity of a semiconductor can be enhanced, thus leading to an overall improvement of the photocatalyst performance. In the first part of the work, homemade and commercial TiO2 powders were studied as photocatalysts for different applications, including the liquid-phase photocatalytic oxidation of ammonia and formic acid, and the H2 production through photocatalytic reforming of water-methanol vapors. In this context, a dopant (NH4F) was used during the sol-gel synthesis of the semiconductor to stabilize the formation of the TiO2 anatase phase (typically more active than rutile TiO2 because of its higher electron mobility), especially when crystallization of the amorphous oxides was performed at high temperature (700 ˚C). Furthermore, the effects induced by noble metal nanoparticles deposition on TiO2 anatase powders were also investigated. In situ electron spin resonance spectroscopy was employed to determine the amount of electrons and holes trapping centers formed under irradiation, in the absence and in the presence of noble metal co-catalysts at the surface of TiO2, hence assessing also the ability of Au and Pt nanoparticles in trapping conduction band electrons. The results were of great usefulness not only to interpret the different H2 production rates but also to understand some mechanistic aspects concerning the selectivity towards the different oxidation products in the methanol photo-steam reforming reaction. In the second part of the work, the nanostructuring of the semiconductor was explored by fabricating TiO2 nanotube arrays through electrochemical anodization. The anodic oxides were employed for both photocatalytic and photo-electrochemical H2 production. In view of large-scale application, the anodization approach was studied on wide Ti substrate surfaces, in order to assess the feasibility of the scale up. Moreover, TiO2 nanotubes were also grown on Ti-based alloys. When fabricating the nanotubes under optimized conditions on Ti-Ta alloys, highly photoactive Ta-doped TiO2 nanotubes were obtained, exhibiting superior water splitting ability. When anodizing Ti-Au alloys, the TiO2 nanotubes resulted decorated with Au nanoclusters. These Au-decorated TiO2 nanotube arrays were used as efficient photocatalyst for H2 production from ethanol-water solutions. Finally, the fabrication of short TiO2 nanotube layers exhibiting an unprecedented level of self-ordering was achieved through an innovative anodization approach. The highly ordered topography allowed the subsequent self-ordering dewetting of Au, leading to Au nanoparticles of controllable size and distribution. These short, Au nanoparticles-filled TiO2 nanotubes exhibited advanced photoactivity ascribed to their reaction vessel-like geometry, fulfilling the requirements in terms of solid state charge carriers diffusion and liquid phase diffusion of oxidizing radicals.

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Al-Saadi, Ali. « Preparation and characterisation of encapsulation magnetic metal iron oxide nanoparticles ». Thesis, University of Oxford, 2012. http://ora.ox.ac.uk/objects/uuid:57bdcf38-9d45-48ab-a971-a2d60e2e4391.

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One of the most challenging goals in nanoparticle research is to develop successful protocols for the large-scale, simple and possibly low-cost preparation of morphologically pure nanoparticles with enhanced properties. The work presented in this thesis was focused on the synthesis, characterisation and testing of magnetic nanoparticles and their potential applications. There are a number of magnetic nano-materials prepared for specific applications such as metal oxide nanoparticles encapsulated with various porous materials including Fe₃O₄/Fe₂O₃ coated with soft bio-organic materials such as glycol chitosan and bovine serum albumin and hard materials such as silica (SiO₂) and zinc sulphide (ZnS). The preparation of these materials was achieved principally by bottom-up methods with different approaches including micro-emulsion, precipitation, electrostatic and thermolysis processes. The thesis also presents the uses of various analytical techniques for characterising different types of nano-materials including Attenuated Total Reflection Fourier Transformer Infrared Vibrational Spectroscopy (ATR-FTIR), Ultraviolet Visible- Near Infrared (UV-Vis-NIR) Spectroscopy, Zeta Potentiometric Surface Charge Analysis, Superconducting Quantum Interference Device (SQUID) and Vibration Sample Magnetometry (VSM) for magnetic analysis and powder X-Ray Diffraction (XRD) for crystallographic pattern analysis. There are many applications of magnetic nanoparticles, including nano-carriers for biological and catalytic reagents. The magnetic nanoparticles can facilitate separation in order to isolate the carriers from solution mixtures as compared to many inefficient and expensive classic methods, which include dialysis membrane, electrophoresis, ultracentrifugation, precipitation and column separation methods. There are six key chapters in this thesis: the first chapter introduces the up-to-date literature regarding magnetic nano-materials. The uses of magnetic nano-materials in drug binding and for protein separation are discussed in the second and third chapters. The fourth chapter presents the use of magnetic nanoparticle in conjunction with a photo-catalytic porous overlayer for the photo-catalytic reduction of organic molecules. The fifth chapter describes different analytical techniques used for the characterisation of nanoparticles and the underlying principles and the experimental details are also given. The sixth chapter summarises the results and provides an overview of the work in a wider context of future applications of magnetic nanoparticles.

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Demoulin, Rémi. « Etude structurale et cartographie du dopage dans des oxydes nanostructurés à base de sillicium ». Thesis, Normandie, 2019. http://www.theses.fr/2019NORMR086/document.

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La modification des propriétés optiques et électriques du silicium apportée par la réduction en taille, notamment due aux effets de confinement quantique des porteurs de charges, est aujourd'hui bien connue et a permis le développement de nouveaux systèmes en optoélectronique. Comme dans le cas du silicium massif, le dopage devrait permettre d'optimiser les propriétés du silicium nanostructuré. Cependant, les caractéristiques du dopage dans le silicium nanostructuré sont encore mal comprises et de nombreux questionnements, concernant la localisation des impuretés ainsi que leur état d'activation, restent en suspens. De plus, l'environnement des impuretés semble avoir une influence majeure sur l'ensemble des propriétés. Cette thèse vise à mieux comprendre les caractéristiques structurales du dopage à l'échelle atomique en fonction de la nature de l'impureté, de la matrice hôte et de la technique d'élaboration. Pour cela, nous avons étudié deux types de système en sonde atomique tomographique. Le premier concerne un dopage aux ions de terres rares dans les silicates d'hafnium. Nous avons mis en évidence que la formation de nano-grains de HfO2 cristallisés sous la forme cubique permet un transfert d'énergie efficace vers les ions praséodyme. Le second porte sur les dopages de type n et p de nanocristaux de silicium insérés dans la silice. Nous avons démontré l'introduction des impuretés de type n (As, P) au cœur des nanocristaux, indépendamment de la technique d'élaboration, permettant de réaliser des forts dopages. Un comportement différent a été mis en évidence pour les impuretés de type p, avec l'accumulation de Bore aux interfaces entre les nanocristaux et la matrice
The change of silicon optical and electrical properties induced by size reduction, due to the quantum confinement of charged carriers, is a well-known effect and allowed to develop new optoelectronic devices. As in bulk silicon, doping should allow to optimize these properties in nanostructured silicon. However, the characteristics of doping of nanostructured silicon still misunderstood and many questions, concerning the location of impurities and their activation state, remain unanswered. Moreover, in these materials, the environment of impurities seems to inuence strongly all of their properties. The purpose of this thesis is to get a better understanding of structural characteristics of doping at the atomic scale in function of the nature of the impurity, the host matrix, and the elaboration technic. In this way, we have investigated two di_erent systems using atom probe tomography. The first concerns a rare earth doping of hafnium silicates. We have evidenced that the clustering of HfO2 nano-grains crystallized in their cubic form induced an efficient energy transfer with praseodymium ions. The second system concern the n and p type doping of silicon nanocrystals embedded in silica. We have demonstrated the important introduction of n type impurities (As, P) in the core of every nanocrystals, independently of the elaboration technic. This introduction of impurities should allow the formation of highly doped silicon nanocrystals. A different behavior has been observed in the case of p type doping, represented by the aggregation of Boron at the interface between the nanocrystals and the silica matrix

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Schlur, Laurent. « Elaboration de cellules photovoltaïques hybrides solides à base d'oxyde de zinc nanostructuré ». Phd thesis, Université de Strasbourg, 2012. http://tel.archives-ouvertes.fr/tel-00864794.

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Cette thèse est consacrée à l'élaboration de cellules photovoltaïques hybrides solides sensibilisées à colorant, composées d'une couche dense de germes de ZnO recouverte de nanobâtonnets de ZnO sensibilisés par un colorant et infiltrés par du spiro-OMeTAD. La couche dense de germes de ZnO a été optimisée, afin qu'elle soit compacte, homogène et bien orientée. Les nanobâtonnets sont synthétisés par voie hydrothermale. L'influence de différents paramètres de synthèse sur la morphologie des nanobâtonnets a été testée. Deux méthodes permettant de modifier l'écart entre les nanobâtonnets ont également été mises au point. Les performances des cellules photovoltaïques varient en fonction de la longueur des nanobâtonnets, du colorant utilisé, de la durée de vieillissement des cellules à l'air, l'atmosphère, la température... Enfin, nous avons réussi à obtenir un rendement dépassant 1%, ce qui est supérieur à la meilleure performance publiée actuellement (0,25%) pour le même type de dispositif.

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Rauscher, Michael D. « Strain mediated self-assembly of ceramic nano islands ». Columbus, Ohio : Ohio State University, 2007. http://rave.ohiolink.edu/etdc/view?acc%5Fnum=osu1196195105.

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Mahato, Prabir. « Study and development of resistive memories for flexible electronic applications ». Thesis, Lyon, 2020. http://www.theses.fr/2020LYSEI134.

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L’avènement de l’électronique flexible a entraîné des recherches rapides sur des capteurs, des dispositifs bio-implantables et portables pour l’évaluation de maladies telles que l’épilepsie, la maladie de Parkinson et les crises cardiaques. Les dispositifs de mémoire sont des composants majeurs dans tous les circuits électroniques, uniquement secondaires aux transistors, par conséquent de nombreux efforts de recherche sont consacrés au développement de dispositifs de mémoire flexibles. Les mémoires à accès aléatoire à pont conducteur (CBRAM) basées sur la création / dissolution d'un filament métallique dans un électrolyte solide sont d'un grand intérêt pour la recherche en raison de leur architecture métallique isolante métallique simple, de leurs capacités basse tension et de leur compatibilité avec les substrats flexibles. Dans ce travail, au lieu d'un oxyde métallique conventionnel ou d'une couche de chalcogénure, un polymère biocompatible - l'oxyde de polyéthylène (PEO) - est utilisé comme couche d'électrolyte solide en utilisant l'eau comme solvant. Des dispositifs de mémoire, constitués d'empilements tri-couches Ag / PEO / Pt, ont été fabriqués à la fois sur du silicium et des substrats flexibles en utilisant un processus hétérogène combinant un dépôt physique en phase vapeur et un revêtement par rotation. Pour cela, une étude systématique de l'effet de la concentration de la solution et de la vitesse de dépôt sur l'épaisseur du PEO est présentée. Des mesures SEM / EDX et AFM ont ensuite été effectuées sur des structures planes dédiées à «nano-gap» et ont révélé la formation de précipités métalliques d'Ag ainsi que des changements morphologiques de la couche de polymère après commutation de résistance. Les performances des dispositifs de mémoire résistive sont ensuite évaluées sur silicium et substrats flexibles. En particulier, la programmation des statistiques de tension, le rapport de résistance OFF / ON, les cycles d'endurance et les tests de rétention sont effectués et l'effet de la conformité du courant est analysé. Le mécanisme de conduction dans le HRS / LRS est étudié sur les appareils de référence Ag / PEO / Pt et Pt / PEO / Pt. Enfin, la caractérisation électrique des dispositifs sur substrat souple est réalisée sous contrainte mécanique, donnant des résultats prometteurs. Les dispositifs CBRAM à base de polymères sont donc proposés comme candidats potentiels pour le développement durable de dispositifs de mémoire flexibles
The advent of flexible electronics has brought about rapid research towards sensors, bio implantable and wearable devices for assessment of diseases such as epilepsy, Parkinson’s and heart attacks. Memory devices are major component in any electronic circuits, only secondary to transistors, therefore many research efforts are devoted to the development of flexible memory devices. Conductive Bridge Random Access Memories (CBRAMs) based on creation/dissolution of a metallic filament within a solid electrolyte are of great research interest because of their simple Metal Insulator Metal architecture, low-voltage capabilities, and compatibility with flexible substrates. In this work, instead of a conventional metallic oxide or a chalcogenide layer, a biocompatible polymer - Polyethylene Oxide (PEO) – is employed as the solid electrolyte layer using water as solvent. Memory devices, consisting in Ag/PEO/Pt tri-layer stacks, were fabricated on both silicon and flexible substrates using a heterogeneous process combining physical vapour deposition and spin coating. To aim this, a systematic study on the effect of solution concentration and deposition speed on the PEO thickness is presented. SEM/EDX and AFM measurements were then conducted on devoted “nano-gap” planar structures and have revealed the formation of metallic Ag precipitates together with morphological changes of the polymer layer after resistance switching. The performance of the resistive memory devices is then assessed on silicon and flexible substrates. In particular programming voltage statistics, OFF/ON resistance ratio, endurance cycles and retention tests are performed and the effect of current compliance is analysed. The conduction mechanism in the HRS/LRS is studied on the Ag/PEO/Pt and Pt/PEO/Pt reference devices. Finally, the electrical characterization of devices on flexible substrate is performed under mechanical stress, showing promising results. Polymer-based CBRAM devices are therefore suggested as potential candidates for sustainable development of flexible memory devices

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Holder, Jenna Ka Ling. « Quantum structures in photovoltaic devices ». Thesis, University of Oxford, 2013. http://ora.ox.ac.uk/objects/uuid:d23c2660-bdba-4a4f-9d43-9860b9aabdb8.

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A study of three novel solar cells is presented, all of which incorporate a low-dimensional quantum confined component in a bid to enhance device performance. Firstly, intermediate band solar cells (IBSCs) based on InAs quantum dots (QDs) in a GaAs p-i-n structure are studied. The aim is to isolate the InAs QDs from the GaAs conduction band by surrounding them with wider band gap aluminium arsenide. An increase in open circuit voltage (V_OC) and decrease in short circuit current (J_sc) is observed, causing no overall change in power conversion efficiency. Dark current - voltage measurements show that the increase in V_OC is due to reduced recombination. Electroreflectance and external quantum efficiency measurements attribute the decrease in J_sc primarily to a reduction in InGaAs states between the InAs QD and GaAs which act as an extraction pathway for charges in the control device. A colloidal quantum dot (CQD) bulk heterojunction (BHJ) solar cell composed of a blend of PbS CQDs and ZnO nanoparticles is examined next. The aim of the BHJ is to increase charge separation by increasing the heterojunction interface. Different concentration ratios of each phase are tested and show no change in J_sc, due primarily to poor overall charge transport in the blend. V_OC increases for a 30 wt% ZnO blend, and this is attributed largely to a reduction in shunt resistance in the BHJ devices. Finally, graphene is compared to indium tin oxide (ITO) as an alternative transparent electrode in squaraine/ C₇₀ solar cells. Due to graphene’s high transparency, graphene devices have enhanced J_sc, however, its poor sheet resistance increases the series resistance through the device, leading to a poorer fill factor. V_OC is raised by using MoO₃ as a hole blocking layer. Absorption in the squaraine layer is found to be more conducive to current extraction than in the C₇₀ layer. This is due to better matching of exciton diffusion length and layer thickness in the squaraine and to the minority carrier blocking layer adjacent to the squaraine being more effective than the one adjacent to the C₇₀.

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Ruiz, Preciado Marco Alejandro. « Synthèse, caractérisation et réponse photocatalytique des oxydes semi-conducteurs à base de NiTiO3 ». Thesis, Le Mans, 2016. http://www.theses.fr/2016LEMA1037/document.

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Structures semi-conductrices à base de NiTiO3, et l'étude de leurs propriétés dans le but de les appliquer en photocatalyse. Une étude théorique et des simulations numériques ont été effectuées pour analyser les propriétés électroniques, vibrationnelles et optiques de NiTiO3 massif ou sous forme de clusters nanométriques. Les poudres NiTiO3 ont été synthétisées par sol-gel par réaction en phase solide, tandis que les films minces ont été obtenus par pulvérisation cathodique rf-magnétron. Les caractérisations de leurs propriétés physiques confirment l'obtention de NiTiO3 polycristallin dans sa phase ilménite. La détermination du gap électronique à 2,25 eV suggère la faisabilité de mise en oeuvre des matériaux synthétisés comme photocatalyseurs actifs sous irradiation en lumière visible. Cette fonctionnalité a été testée par la dégradation du bleu de méthylène en solution aqueuse en utilisant les couches minces de NiTiO3 sous irradiation visible, atteignant la dégradation de 60% de la concentration initiale du colorant en 300 minutes. En outre, l'électro-oxydation du méthanol a été réalisée en appliquant une tension externe sur une électrode contenant des poudres NiTiO3 dans des milieux alcalins. Les ions de Ni présents dans le catalyseur ont été identifiés comme des espèces actives et que l'oxydation des molécules organiques se produit sur la surface des sites de Ni3+. En résumé, NiTiO3 a été synthétisé sous forme de poudres et de films minces ayant des caractéristiques appropriées pour la photocatalyse hétérogène efficace et les capacités catalytiques de NiTiO3 ont été démontrées sur la photodégradation du bleu de méthylène et l'électrooxydation de méthanol
The thesis work is devoted to the synthesis of NiTiO3-based semiconductive structures, i.e. powders and thin films, and the investigation of their related properties with the aim of their applications in photocatalysis. Theoretical approach and numerical simulations of the electronic, vibrational and optical properties of bulk and nanosized NiTiO3 structures have been carried out in order to deepen the understanding of the experimental results. The synthesis of NiTiO3 powders has been achieved by sol-gel and solid state reaction, while NiTiO3 thin films have been grown by rf-sputtering.Characterizations on their structural, vibrational and optical properties confirm the stabilization of polycrystalline NiTiO3 in its ilmenite phase in both powders and thin films as well. The determination of a band gap at 2.25 eV suggests the feasibility to implement the synthesized materials as visible-light-active photocatalysts. This feature has been tested in thedegradation of methylene blue in aqueous solution using rf-sputtered NiTiO3 thin films irradiated with visible light,achieving the degradation of 60% of the initial concentration of the colorant in 300 minutes. In addition, the electro-oxidation of methanol has been accomplished by applying an external voltage on an electrode containing NiTiO3 powders in alkaline media. The Ni ions present in the catalyst have been identified as the active species with the oxidation of the organic molecules on the surface of Ni3+ sites. As a main achievement, NiTiO3 has been synthesized as powders and thin films with suitable characteristics for efficient heterogeneous photocatalysis and the catalytic capabilities of NiTiO3 have beendemonstrated on the photodegradation of Methylene Blue and the electro-oxidation of methanol

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Vargas, Hernandez Jesus. « Structural and Morphological modification of TiO2 doped metal ions and investigation of photo-induced charge transfer processes ». Thesis, Le Mans, 2017. http://www.theses.fr/2017LEMA1018/document.

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Le travail de thèse porte sur les méthodes de synthèse de nanostructures de dioxyde de titane et de leurs études physicochimiques afin de préciser les corrélations entre la morphologie, le dopage métallique, les caractéristiques structurales avec l'efficacité photocatalytique. Le grand intérêt pour les nanomatériaux TiO2 réside dans la mise au point de nouvelles sources d'énergie ou la conservation de l’environnement par des processus photocatalytiques. Cependant, la limitation principale de TiO2 est du au large gap électronique (eV ~3,2) du polymorphe Anatase. Ainsi, un des objectifs importants pour l'amélioration de l’efficacité des nanomatériaux TiO2 est d'augmenter leur photoactivité en décalantla création de paires d'électron-trou de l’UV à la gamme du visible. D'ailleurs, on a montré que l'utilisation de nanostructures 1D de TiO2 (nanotubes) a amélioré la collection de charges, en favorisant leur transport dans les structures 1D, qui par conséquent réduit au minimum la recombinaison et prolonge les durées de vie des électrons.La première partie de ce travail est dédiée à la synthèse des nanopoudres TiO2 dopées par des ions métalliques (Ag, Cu, Eu) préparés par sol-gel. Même avec différents éléments de dopage qui apparemment peuvent adopter le même état de valence (2+) (Cu2+, Ag2+, Eu2+), différents comportements ont été démontrés pour l'incorporation efficace de ces ions dans la structure de TiO2. L'anomalie entre les rayons ioniques des différents éléments utilisés module le rapport du dopage substitutionnel. Ceci est en effet réalisé pour Cu2+ mais dans moins d'ampleur pour Ag2+ tandis que les ions d'europium forment une ségrégation de phase Eu2Ti2O7. La dégradation de colorants de bleu de méthylène (MB) a étéaméliorée légèrement avec les échantillons dopés Ag. La raison a été attribuée aux clusters métalliques Ag qui ont été en effet mis en évidence à travers leur bande d’absorption plasmonique. La deuxième partie porte sur des couches minces de TiO2 dopés (Cu, Ag, et Eu) qui ont été élaborés par sol-gel et spin-coating et dipcoating. Les paramètres optimaux ont été obtenus pour réaliser les films cristallins mais présentant une organisation mésoporeuse qui dépend également du processus de dopage. Des études de Photocatalyse ont été également réalisées et l'efficacité des films ont été comparées en fonction des éléments dopants. La troisième partie de la thèse est liée à la modification morphologique des nanoparticules pour former des nanotubes à l'aide de la méthode hydrothermale sous pression contrôlée. Un plan d'expérience basé sur la méthode Taguchi a été utilisé pour la détermination des paramètres optimaux.Les nanotubes TiO2 augmentent la surface spécifique en comparaison avec les nanoparticules. La dégradation de bleu deméthylène par les nanotubes a montré une efficacité photocatalytique plus élevée qu’avec les nanopoudres TiO2 pures etdopés Ag
The thesis work is focused on the synthesis methods of titanium dioxide nanostructures and their physico-chemical studies in order to point out the correlations between the morphology, metal doping, structural features with the photocatalytic efficiency. The great interest on TiO2 nanomaterials deals with new sources of energy or in the environment preservation through the photocatalytic properties. However, the main limitations is due to the wide band gap (~3.2 eV) of the anatase polymorph. Thus, a major objective for improvement of the performance of TiO2 nanomaterials is to increase theirphotoactivity by shifting the onset of the electron-hole pairs creation from UV to the visible range. Moreover, it was found that using onedimensional (1-D) TiO2 (nanotubes) improved the charge collection by 1D nanostructures which consequently minimizes the recombination and prolongate the electron lifetimes. The first part of this work is focused on the synthesis of TiO2 nanopowders doped with metallic ions (Ag, Cu, Eu) prepared by Solgel. Even with different doping elements which apparently can adopt the same valence state (2+) such as (Cu2+, Ag2+,Eu2+), different behaviors were demonstrated for the effective incorporation of these ions in the host structure of TiO2. The discrepancy between ionic radii of the different used elements modulates the ratio of the substitutional doping. This is indeed achieved for Cu2+ but in less extent for Ag2+ while Europium ions form segregated phase as Eu2Ti2O7. The experiments on the degradation of methylene blue (MB)dyes have shown slight improvement with Ag-doped samples. The reason was tentatively attributed to the Ag clusters which were indeed demonstrated through their plasmon optical band. The second part of the work concerns thin films of TiO2 doped (Cu, Ag, and Eu) which were elaborated by spin coating and dip coating. The optimal parameters were obtained to achieve crystalline films but presenting mesoporous organisation which also depends on the doping process. Photocatalysis investigations were also realized and the efficiency of the films compared as function of the doping elements.The third part of the thesis is related to the morphological modification from nanoparticles to nanotubes by using the hydrothermal method with controlled pressure. An experimental design based on Taguchi Method was employed for the determination of the optimal parameters. TiO2 nanotubes increase the surface area in comparison with TiO2nanoparticles. TiO2 nanotubes were tested for the methylene blue degradation and show a higher photocatalytic efficiency than TiO2 nanopowders and TIO2 doped with Ag

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40

Yuvaraj, D. « Studies On The Growth And Characterization Of II-VI Semiconductor Nanostructures By Evaporation Methods ». Thesis, 2009. https://etd.iisc.ac.in/handle/2005/1037.

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In recent years, there has been growing interests on II-VI semiconductor nanostructures, which are suitable for applications in electronics and optoelectronic devices such as solar cells, UV lasers, sensors, light emitting diodes and field emission displays. II-VI semiconductor nanostructures with different morphologies such as wires, belts, rods, tubes, needles, springs, tetrapods, plates, hierarchical structures and so on, have been widely grown by vapor transport methods. However the process conditions used for the growth of nanostructures still remains incompatible for device fabrication. The realization of practical nanoscale devices using nanostructured film depends mainly on the availability of low cost and lower processing temperatures to manufacture high purity nanostructures on a variety of substrates including glass and polymer. In this thesis work, studies have been made on the growth and characterization of II-VI semiconductor nanostructures prepared at room temperature, under high vacuum, without employing catalysts or templates. (i) ZnO nanostructured films with different morphology such as flowers, needles and shrubs were deposited at room temperature on glass and polymer substrates by plasma assisted reactive process. (ii) Zn/ZnO core/shell nanowires were grown on Si substrates under optimized oxygen partial pressure. Annealing of this core shell nanowire in high vacuum resulted in the formation of ZnO nanocanals. (iii) ZnS and ZnSe nano and microstructures were grown on Si substrates under high vacuum by thermal evaporation. The morphology, structural, optical properties and composition of these nano and microstructures were investigated by XRD, SEM, TEM, Raman, PL and XPS. The growth mechanism behind the formation of the different nanostructures has been explained on the basis of vapour-solid (VS) mechanism.

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41

Yuvaraj, D. « Studies On The Growth And Characterization Of II-VI Semiconductor Nanostructures By Evaporation Methods ». Thesis, 2009. http://hdl.handle.net/2005/1037.

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In recent years, there has been growing interests on II-VI semiconductor nanostructures, which are suitable for applications in electronics and optoelectronic devices such as solar cells, UV lasers, sensors, light emitting diodes and field emission displays. II-VI semiconductor nanostructures with different morphologies such as wires, belts, rods, tubes, needles, springs, tetrapods, plates, hierarchical structures and so on, have been widely grown by vapor transport methods. However the process conditions used for the growth of nanostructures still remains incompatible for device fabrication. The realization of practical nanoscale devices using nanostructured film depends mainly on the availability of low cost and lower processing temperatures to manufacture high purity nanostructures on a variety of substrates including glass and polymer. In this thesis work, studies have been made on the growth and characterization of II-VI semiconductor nanostructures prepared at room temperature, under high vacuum, without employing catalysts or templates. (i) ZnO nanostructured films with different morphology such as flowers, needles and shrubs were deposited at room temperature on glass and polymer substrates by plasma assisted reactive process. (ii) Zn/ZnO core/shell nanowires were grown on Si substrates under optimized oxygen partial pressure. Annealing of this core shell nanowire in high vacuum resulted in the formation of ZnO nanocanals. (iii) ZnS and ZnSe nano and microstructures were grown on Si substrates under high vacuum by thermal evaporation. The morphology, structural, optical properties and composition of these nano and microstructures were investigated by XRD, SEM, TEM, Raman, PL and XPS. The growth mechanism behind the formation of the different nanostructures has been explained on the basis of vapour-solid (VS) mechanism.

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42

Triska, Joshua B. « Atomic layer deposition of nanolaminate high-κ gate dielectrics for amorphous-oxide semiconductor thin film transistors ». Thesis, 2011. http://hdl.handle.net/1957/21720.

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Nanolaminate dielectrics combine two or more insulating materials in a many-layered film. These structures can be made to significantly outperform films composed of a single one of their constituent materials by adjusting the composition ratio, arrangement, and size of the component layers. In this work, atomic layer deposition (ALD) is used to fabricate pure-oxide and nanolaminate dielectrics based upon Al₂O₃ and ZrO₂. The relative performance of these dielectrics is investigated with respect to application as gate dielectrics for ZnSnO (ZTO) and InGaZnO (IGZO) amorphous-oxide-semiconductor (AOS) thin-film transistors (TFTs). AOS TFTs are promising candidates for commercial use in applications such as active-matrix displays and e-paper. It was found that the layer thickness, relative composition, and interfacial material all had an effect on TFT performance. Several variants of the Al₂O₃/ZrO₂ nanolaminate were found to exhibit superior properties to either Al₂O₃ or ZrO₂ alone.
Graduation date: 2011

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43

Leelavati, A. « Nanostructured Hybrids with Engineered Interfaces for Efficient Electro, Photo and Gas Phase Catalytic Reactions ». Thesis, 2015. http://etd.iisc.ac.in/handle/2005/3849.

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Catalysis using nanostructures has been a topic of substantial interest for fundamental studies and for practical applications in energy and environmental sectors. The growing demand for production of energy and in the cleaning of polluting hazardous vehicles/industrial wastes has led to several studies in catalysis. Despite the substantial growth of heterogeneous catalytic technologies in last decade, they are still far from reaching their full potential in terms of efficiency, selectivity as well as durability. It is often difficult to simultaneously tackle all the mentioned issues with single component catalysts. Most of these challenges are being overcome with heterostructures/supported hybrid catalysts by modifying their interfaces. The properties of heterostructures hybrids arises not only from the individual contributions of the individual components but also from strong synergetic effect arising from the interface. Engineering the interfaces provides pathways to promote the catalytic performance and hence has been explored. In this regard, we have focused on the progress in investigating the active interfaces that affect the performance of metal oxide-metal, semiconductor-metal and coupled semiconductor nanocatalyst hybrids. We explored a wide spectrum of their applications in photo catalytic, electrocatalytic as well as gas-phase reactions and highlighted the importance of the interface for overall performance. The entire study reported in the thesis is organized as follows: Chapter 1 is a general introduction of hybrid nanocatalyst and their role in wide spectra of catalytic reactions in photo/electro catalysis as well as gas-phase reactions. This chapter describes the motivation behind modulating the interface between two or more nanostructures to obtain multifunctional nanocatalysts. Nan catalysts to achieve high throughput with active interfaces are elaborated while indicating the role of morphology, internal induced state, charge transfer, geometric, support, as well as electronic effect for enhanced performance. Motivation behind specific nanocatalyst hybrid, synthesis routes as well as characterization techniques are detailed in the respective chapters. Specific details for different hybrids are described in the following chapters. Chapter 2 describes the synthesis of high dense ultrathin Au wires on ZnO nanorods for electrocatalytic oxidation of ethanol, where the prerequisite step is the formation of amine-modified support. Oleylamine modification not only serves to anchor Au nanowires on ZnO but also passivates surface defects of ZnO, which in turn enhances the photocurrent. In addition to the stability, the support induces electronic eﬀect on Au nanowires, which facilitates redox process at low potential. Most importantly, the support promotes the activity of Au nanowires upon photoirradiation, and thus leading to synergy between electro and photooxidation current. This is of immense importance for photofuel cell technologies. Moreover, the method enabled the first time electrocatalysis on these nanowires that revealed ultrathin nanowires are potentially interesting systems for catalysis applications provided they are stabilized by a suitable support. Chapter 3 deals with the growth of ultrathin Au nanowires on metal oxide (TiO2) coupled with graphene hybrid support in order to overcome the low conductivity of metal oxide. Oleylamine, used for growth of Au nanowires simultaneously functionalizes the support and leads to room temperature GO reduction. With respect to catalytic activity, we also synthesized the binary counterparts (rGO/Au, TiO2/Au ultrathin nanowires) to delineate the contribution of each of the components to the overall electrocatalytic oxidation of ethanol. Comparative analysis of photo and electrocatalytic activity between the diﬀerent binary and ternary hybrids provides interesting information. Both, electronic effect of TiO2 and electrical conductivity of rGO add their specific beneficial to the nanowires, leading to superior ternary system. Chapter 4 rGO supported ultrathin Au nanowires exhibits high electrocatalytic performance for oxidation of borohydride with a lower onset potential compared to rGO/Au nanoparticles. Electrochemical impedance spectroscopy measurements display abnormal inductive behavior of the synthesized hybrids, indicative of Au surface reactivation. DFT calculations indicate that the origin of the high activity stems from the shift in the position of the Au d-band center. Chapter 5 Different aspect ratio ZnO nanostructures are obtained by varying the solvothermal reaction time. We observed a direct correlation between observed photocatalytic activity, measured photocurrent and length of the ZnO nanorods. Furthermore, photoresponse of the high aspect ratio ZnO nanorods are improved by attaching Au nanoparticles, intimate contact of two components leads to band bending. Thus, the synthesized ZnO/Au heterostructure favors for prominent separation of photogenerated charge carriers. Chapter 6 TiO2 and PbO/TiO2 hybrids are synthesized via non–hydrolytic sol–gel combustion method. Hybrid exhibits higher photocatalytic activity for the degradation of dye than TiO2. The estimated photogenerated species reveals that the origin of enhanced activity stems from the direct oxidization of dye via photogenerated hole rather than radicals. The semiconductors are matched based on their band edge positions, for the formation of energetic radicals to degrade the pollutants. Based on this study, we infer that semiconductors should not neglected (for example Si) based on calculated mismatch of their valence band edges position for photooxidation reaction via radicals. Chapter 7 describes the Pd dopant associated band engineering, a strategy for tuning the optoelectronic properties of ZnO towards enhanced photocatalytic activity. Incorporated Pd heterocation induces internal energy states within the ZnO band gap. The created energy level leads to trends mismatch between photocatalytic activity and measured photocurrent. Formed energy level arrests the photogenerated electrons, which make them not contribute for the photocurrent generation. Hence, the isolated photogenerated hole efficiently oxidizes the pollutants through hydroxyl radicals, and thus leads to enhanced photocatalytic activity. Chapter 8 employed Pd-substituted zinc stannate for CO oxidation as heterogeneous catalyst for the first time. Compared with SnO2 support, zinc stannate based materials exhibits abnormal sudden light-off profiles at selective temperatures. On the basis of DRIFT studies under relevant conditions, we find that the initially formed product gets adsorbed over the catalyst surface. It leads to the accumulation of carbonates as a consequence, both lattice oxygen mobility and further CO interactions are disabled. As soon as Sn redox nature dominates over the accumulated carbonates, this leads to sudden release of lattice oxygen, and thus leads to a sudden full conversion. Therefore, choosing the suitable support material greatly influences the nature of the light-off CO oxidation profile. Chapter 9 Although, reducible oxide supported gold nanostructures exhibits the highest CO oxidation activity; they still suffer from problems such as limited selectivity towards CO in the presence of H2. Both ex-situ and in-situ experiments demonstrate that, Au nanoparticles supported on Zn2SnO4 matrix selectively oxidizes CO. DRIFT experiments revealed that the involvement of OH groups leads to the formation of hydroxycarbonyl under PROX conditions. Chapter 10 This chapter discusses the conclusions for the previous chapters and highlights the possibilities for future scope for the developed nanocatalysts hybrids for energy and environmental applications.

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44

Leelavati, A. « Nanostructured Hybrids with Engineered Interfaces for Efficient Electro, Photo and Gas Phase Catalytic Reactions ». Thesis, 2015. http://etd.iisc.ernet.in/2005/3849.

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Résumé :

Catalysis using nanostructures has been a topic of substantial interest for fundamental studies and for practical applications in energy and environmental sectors. The growing demand for production of energy and in the cleaning of polluting hazardous vehicles/industrial wastes has led to several studies in catalysis. Despite the substantial growth of heterogeneous catalytic technologies in last decade, they are still far from reaching their full potential in terms of efficiency, selectivity as well as durability. It is often difficult to simultaneously tackle all the mentioned issues with single component catalysts. Most of these challenges are being overcome with heterostructures/supported hybrid catalysts by modifying their interfaces. The properties of heterostructures hybrids arises not only from the individual contributions of the individual components but also from strong synergetic effect arising from the interface. Engineering the interfaces provides pathways to promote the catalytic performance and hence has been explored. In this regard, we have focused on the progress in investigating the active interfaces that affect the performance of metal oxide-metal, semiconductor-metal and coupled semiconductor nanocatalyst hybrids. We explored a wide spectrum of their applications in photo catalytic, electrocatalytic as well as gas-phase reactions and highlighted the importance of the interface for overall performance. The entire study reported in the thesis is organized as follows: Chapter 1 is a general introduction of hybrid nanocatalyst and their role in wide spectra of catalytic reactions in photo/electro catalysis as well as gas-phase reactions. This chapter describes the motivation behind modulating the interface between two or more nanostructures to obtain multifunctional nanocatalysts. Nan catalysts to achieve high throughput with active interfaces are elaborated while indicating the role of morphology, internal induced state, charge transfer, geometric, support, as well as electronic effect for enhanced performance. Motivation behind specific nanocatalyst hybrid, synthesis routes as well as characterization techniques are detailed in the respective chapters. Specific details for different hybrids are described in the following chapters. Chapter 2 describes the synthesis of high dense ultrathin Au wires on ZnO nanorods for electrocatalytic oxidation of ethanol, where the prerequisite step is the formation of amine-modified support. Oleylamine modification not only serves to anchor Au nanowires on ZnO but also passivates surface defects of ZnO, which in turn enhances the photocurrent. In addition to the stability, the support induces electronic eﬀect on Au nanowires, which facilitates redox process at low potential. Most importantly, the support promotes the activity of Au nanowires upon photoirradiation, and thus leading to synergy between electro and photooxidation current. This is of immense importance for photofuel cell technologies. Moreover, the method enabled the first time electrocatalysis on these nanowires that revealed ultrathin nanowires are potentially interesting systems for catalysis applications provided they are stabilized by a suitable support. Chapter 3 deals with the growth of ultrathin Au nanowires on metal oxide (TiO2) coupled with graphene hybrid support in order to overcome the low conductivity of metal oxide. Oleylamine, used for growth of Au nanowires simultaneously functionalizes the support and leads to room temperature GO reduction. With respect to catalytic activity, we also synthesized the binary counterparts (rGO/Au, TiO2/Au ultrathin nanowires) to delineate the contribution of each of the components to the overall electrocatalytic oxidation of ethanol. Comparative analysis of photo and electrocatalytic activity between the diﬀerent binary and ternary hybrids provides interesting information. Both, electronic effect of TiO2 and electrical conductivity of rGO add their specific beneficial to the nanowires, leading to superior ternary system. Chapter 4 rGO supported ultrathin Au nanowires exhibits high electrocatalytic performance for oxidation of borohydride with a lower onset potential compared to rGO/Au nanoparticles. Electrochemical impedance spectroscopy measurements display abnormal inductive behavior of the synthesized hybrids, indicative of Au surface reactivation. DFT calculations indicate that the origin of the high activity stems from the shift in the position of the Au d-band center. Chapter 5 Different aspect ratio ZnO nanostructures are obtained by varying the solvothermal reaction time. We observed a direct correlation between observed photocatalytic activity, measured photocurrent and length of the ZnO nanorods. Furthermore, photoresponse of the high aspect ratio ZnO nanorods are improved by attaching Au nanoparticles, intimate contact of two components leads to band bending. Thus, the synthesized ZnO/Au heterostructure favors for prominent separation of photogenerated charge carriers. Chapter 6 TiO2 and PbO/TiO2 hybrids are synthesized via non–hydrolytic sol–gel combustion method. Hybrid exhibits higher photocatalytic activity for the degradation of dye than TiO2. The estimated photogenerated species reveals that the origin of enhanced activity stems from the direct oxidization of dye via photogenerated hole rather than radicals. The semiconductors are matched based on their band edge positions, for the formation of energetic radicals to degrade the pollutants. Based on this study, we infer that semiconductors should not neglected (for example Si) based on calculated mismatch of their valence band edges position for photooxidation reaction via radicals. Chapter 7 describes the Pd dopant associated band engineering, a strategy for tuning the optoelectronic properties of ZnO towards enhanced photocatalytic activity. Incorporated Pd heterocation induces internal energy states within the ZnO band gap. The created energy level leads to trends mismatch between photocatalytic activity and measured photocurrent. Formed energy level arrests the photogenerated electrons, which make them not contribute for the photocurrent generation. Hence, the isolated photogenerated hole efficiently oxidizes the pollutants through hydroxyl radicals, and thus leads to enhanced photocatalytic activity. Chapter 8 employed Pd-substituted zinc stannate for CO oxidation as heterogeneous catalyst for the first time. Compared with SnO2 support, zinc stannate based materials exhibits abnormal sudden light-off profiles at selective temperatures. On the basis of DRIFT studies under relevant conditions, we find that the initially formed product gets adsorbed over the catalyst surface. It leads to the accumulation of carbonates as a consequence, both lattice oxygen mobility and further CO interactions are disabled. As soon as Sn redox nature dominates over the accumulated carbonates, this leads to sudden release of lattice oxygen, and thus leads to a sudden full conversion. Therefore, choosing the suitable support material greatly influences the nature of the light-off CO oxidation profile. Chapter 9 Although, reducible oxide supported gold nanostructures exhibits the highest CO oxidation activity; they still suffer from problems such as limited selectivity towards CO in the presence of H2. Both ex-situ and in-situ experiments demonstrate that, Au nanoparticles supported on Zn2SnO4 matrix selectively oxidizes CO. DRIFT experiments revealed that the involvement of OH groups leads to the formation of hydroxycarbonyl under PROX conditions. Chapter 10 This chapter discusses the conclusions for the previous chapters and highlights the possibilities for future scope for the developed nanocatalysts hybrids for energy and environmental applications.

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Nubi, Olatunbosun Owolabi. « Single and double doping of nanostructured titanium dioxide with silver and copper : structural, optical and gas-sensing properties ». Thesis, 2016. http://hdl.handle.net/10386/1749.

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Thesis (Ph. D. (Physics)) -- University of Limpopo, 2016.
Single and double doped nanometric powders of Single and double doped nanometric powders of titanium dioxide (TiO2) were synthesised by the sol-gel process using titanium isopropoxide (TTIP) as the precursor. For comparison, an undoped sample was also prepared. The metal dopants, Ag and Cu, were used at doping levels of 5% molar weight. The samples were dried at 100°C in air and post annealing was done at 300°C, 600°C, 900°C and 1100°C. Structural characterisation of the samples was carried out by X-ray Diffraction (XRD), Raman Spectroscopy, Scanning Electron Microscopy (SEM) and Energy dispersive X-ray Spectrometry (EDS) techniques. Most samples annealed at the 300°C temperature (and lower) revealed the predominantly-anatase phase, while those annealed at 900°C and above were rutile-only. The double-doped powder that was annealed at 300°C was found to be constituted by anatase and brookite phases (with the dopants incorporated into the TiO2 matrix), and the one annealed at 600°C was a mixture of brookite and rutile. The results suggest that multiple doping of titania may favour a two-phase structure at lower temperatures than singly-doped powders. The co-existence of brookite with anatase is believed to be responsible for the enhancement of anatase to rutile transformation in the double-doped sample. UV-visible (UV-vis) and Photoluminescence (PL) measurements were also carried out to study the optical properties of the TiO2 nanoparticles. This revealed the active PL band at around 440 nm. By narrowing the band gap, the double-doped powders that exhibited the brookite phase, again showed improved visible light photo absorption over the other samples, with a significant shift of the absorption edge to shorter wavelengths. Further, PL spectra revealed a change in PL intensity with phase change, as well as the presence of exciton energy levels at the base of the conduction band. The changes in the electrical conductivities of representative anatase and rutile TiO2 nanopowders upon exposure to water-vapour, ammonia (NH3) and hydrogen (H2) were also investigated. Sensing measurements for water-vapour was done at room temperature for various humidity levels ranging from 5.4% RH to 88.4% RH. The detection of NH3 and H2 gases were carried out at temperatures extending from room temperature to 350°C and over concentration ranges of 25 sccm to 500 sccm and 15 v sccm to 200 sccm respectively. The gas-sensing results show that the sol-gel fabricated TiO2 nanoparticles (particularly in anatase form), has excellent fast and stable dynamic responses to humidity, NH3 and H2. They feature good sensitivities, even at a low operating temperatures. However, acceptor behaviour, for which there was a conductivity switch from n-type to p-type, was recorded for the Ag-doped rutile powders at operating temperatures of 300ºC and 350ºC. Overall, the double-doped sample annealed at 300ºC was deemed the most promising candidate for gassensing. (TiO2) were synthesised by the sol-gel process using titanium isopropoxide (TTIP) as the precursor. For comparison, an undoped sample was also prepared. The metal dopants, Ag and Cu, were used at doping levels of 5% molar weight. The samples were dried at 100°C in air and post annealing was done at 300°C, 600°C, 900°C and 1100°C. Structural characterisation of the samples was carried out by X-ray Diffraction (XRD), Raman Spectroscopy, Scanning Electron Microscopy (SEM) and Energy dispersive X-ray Spectrometry (EDS) techniques. Most samples annealed at the 300°C temperature (and lower) revealed the predominantly-anatase phase, while those annealed at 900°C and above were rutile-only. The double-doped powder that was annealed at 300°C was found to be constituted by anatase and brookite phases (with the dopants incorporated into the TiO2 matrix), and the one annealed at 600°C was a mixture of brookite and rutile. The results suggest that multiple doping of titania may favour a two-phase structure at lower temperatures than singly-doped powders. The co-existence of brookite with anatase is believed to be responsible for the enhancement of anatase to rutile transformation in the double-doped sample. UV-visible (UV-vis) and Photoluminescence (PL) measurements were also carried out to study the optical properties of the TiO2 nanoparticles. This revealed the active PL band at around 440 nm. By narrowing the band gap, the double-doped powders that exhibited the brookite phase, again showed improved visible light photo absorption over the other samples, with a significant shift of the absorption edge to shorter wavelengths. Further, PL spectra revealed a change in PL intensity with phase change, as well as the presence of exciton energy levels at the base of the conduction band. The changes in the electrical conductivities of representative anatase and rutile TiO2 nanopowders upon exposure to water-vapour, ammonia (NH3) and hydrogen (H2) were also investigated. Sensing measurements for water-vapour was done at room temperature for various humidity levels ranging from 5.4% RH to 88.4% RH. The detection of NH3 and H2 gases were carried out at temperatures extending from room temperature to 350°C and over concentration ranges of 25 sccm to 500 sccm and 15 v sccm to 200 sccm respectively. The gas-sensing results show that the sol-gel fabricated TiO2 nanoparticles (particularly in anatase form), has excellent fast and stable dynamic responses to humidity, NH3 and H2. They feature good sensitivities, even at a low operating temperatures. However, acceptor behaviour, for which there was a conductivity switch from n-type to p-type, was recorded for the Ag-doped rutile powders at operating temperatures of 300ºC and 350ºC. Overall, the double-doped sample annealed at 300ºC was deemed the most promising candidate for gassensing.

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46

Sai, Ranajit. « Development of CMOS-Compatible, Microwave-Assisted Solution Processing of Nanostructured Zine Ferrite Films for Gigahertz Circuits ». Thesis, 2013. http://etd.iisc.ac.in/handle/2005/3412.

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The development of radio frequency integrated circuits (RFICs), especially the dream of integrating analog, digital and radio frequency (RF) components on the same chip that is commonly known as System-on-a-Chip (SoC), is crucial to mobile communications of the future. Such SoC approach offers enhanced performance, greater reliability, and substantially less power consumption of integrated circuits while reducing overall physical size and thus manufacturing cost. However, the progress has been stalled by the lack of miniaturized inductor elements. Rise of unwanted parasitic effects limits down-scaling of the inductor structures and leaves the use of magnetic coating as a viable and attractive option to enhance the inductance and thus inductance density. It is also essential to shift from perm alloy and other amorphous alloys to ferrites and hex ferrites as the core material because of their very high electrical resistivity so as to keep losses in check, a criterion that cannot be compromised on in GHz frequency applications. This is viable, however, only if the integration of the magnetic core (film), particularly a ferrite film, is fully compatible with the CMOS fabrication process. Various approaches have been taken to meet this requirement, including investigations of employing layers of ferrite materials to envelop the inductor loop. However, the deposition of thin films of ferrites, whether by PVD or CVD, usually calls for the deposited ferrite layer to be annealed at an elevated temperature to crystallize the layer so that its magnetic characteristics are appropriate for the optimum performance of the circuit element. Such annealing is incompatible with CMOS process flow required for aggressive device geometries, as the inductor element is added after the active semiconductor circuit is processed, and any exposure of the processed circuit to elevated temperatures risks disturbing precise doping profiles employed and the integrity of the inter-layer dielectrics. What is called for is a low-temperature process for the deposition of a ferrite layer on top of the patterned inductor element – a layer of thickness such that most of the fringe field is encapsulated – while ensuring that the layer comprises crystallites of uniform size that leads to uniform magnetic behaviour. Recognizing the difficulty of meeting the various stringent requirements, it has recently been remarked that such a goal is a formidable challenge. In an attempt to address this challenge, in this work, we have adopted a counter-intuitive approach - the deposition of the desired ferrite composition on a processed die (that contains the inductor structures along with active semiconductor circuits) by immersing it into a chemical (reactant) solution, followed by a brief irradiation of microwave frequency. However, to identify the desired ferrite composition and the appropriate recipe to deposit them, a systematic effort had to be made first, to understand the inter-relationship between synthesis process, structure of resulting material, and its physical and chemical properties. Therefore, at the beginning, a general introduction in which key concepts related to the magnetic-core inductors, the microwave-irradiation-assisted synthesis of nanostructures, the ‗state of the art‘ in the field of integration of appropriate magnetic material to the RFICs, are all outlined. As a proof of concept, microwave-irradiation-assisted solution-based deposition of zinc ferrite thin films on the technologically important Si (100) substrate is demonstrated. The highlight of the process is the use of only non-toxic metal organic precursors and aqua-alcoholic solvents for the synthesis, which is complete in 10 minutes @< 100 °C, without any poisonous by-products. Effects of various process parameters such as solute concentrations, surfactant types, and their concentrations are investigated. A wide range of deposition rates (10 - 2000 nm/min) has been achieved by tweaking the process parameters. The simultaneous formation of zinc ferrite nanocrystallites (ZFNC) along with deposition of thin film is the hallmark of this synthesis technique. Unlike its bulk counterpart, both film and powder are found upon investigation to be rich in magnetic behavior– owing to plausible cationic distribution in the crystal lattice, induced by the inherently quick and far-from-equilibrium nature of the process. The accurate estimation of magnetic characteristics in film is, however, found to be difficult due to the high substrate-to-film mass ratio. The simultaneously prepared ZFNC is examined to arrive at the optimized process recipe that imparts the desired magnetic properties to the zinc ferrite system. The crystallographic cationic distribution in zinc ferrite powder is, however, difficult to study due to the nanoscale dimension of the as prepared material. To enable crystal growth, slow and rapid annealing in air at two different temperatures are employed. The effects of these annealing schemes on various attributes (magnetic properties in particular) are studied. Rapid annealing turns out to be an interesting pathway to promote rapid grain-growth without disturbing the crystallographic site occupancies. The presence of inversion, i.e., the amount of Fe3+ in the ‗A‘-sites in the spinel structure that ideally is zero in normal spinel structure of zinc ferrite, is evident in all annealed ZFNC, as determined by Riveted analysis. Such partially inverted ZFNC exhibits soft magnetic behavior with high saturation magnetization, which can easily be ―tuned‖ by choosing appropriate annealing conditions. However, a few unique strategic modifications to the same microwave-irradiation-assisted solution-based synthesis technique are tried for the formation of nanocrystalline powder with desired sizes and properties without the necessity of anneal. The approach eventually appears to pave a way for the formation of oriented structures of zinc ferrite. The effects of anneal, nevertheless, are studied with the help of neutron powder diffractometry and magnetic measurements. The magnetic ordering at various temperatures is analyzed and connected to the magnetic measurements. The study shows that long-range magnetic ordering, present even at room temperate, originates from the distribution of cations in the partially inverted spinel structures, induced by the rapid and kinetically driven microwave synthesis. Keeping the mild nature (<200 °C) of the processing in mind, a large degree of inversion (~0.5) is a surprise and results in a very high saturation magnetization, as much as 30 emu/g at room temperature (paramagnetic in bulk), in the ZFNC system. Based on the knowledge of process-structure-property interrelationship, a recipe for the deposition of ferrite thin films by the microwave-assisted deposition technique is optimized. Successful deposition of smooth and uniform zinc ferrite thin films on various substrates is, then, demonstrated. The mystery behind the strong adherence of the film to the substrate - an unexpected outcome of a low-temperature process - is probed by XPS and the formation of silicates at the interface is identified as the probable reason. The uniformity and consistency of film composition is also examined in this chapter. Another salient feature of the process is its capability to coat any complex geometry conformally, allowing the possibility of depositing the material in a way to ―wrap around‖ the three-dimensional inductor structures of RF-CMOS. Integration of nanostructure zinc ferrite thin films onto on-chip spiral inductor structures has been demonstrated successfully. The magnetic-core inductors so obtained exhibit the highest inductance density (700 nH/mm2) and the highest Q factor (~20), reported to date, operate at 5 GHz and above, by far the highest reported to date. An increase in inductance density of as much as 20% was achieved with the use of just 1 µm thick film of zinc ferrite covering only the ―top‖ of the spiral structure, i.e., up to 20% of chip real estate can potentially be freed to provide additional functionality. The microwave-assisted solution-based deposition process described in this thesis is meant for ‗post-CMOS‘ processing, wherein the film deposited on some specific electronic components can add desired functionality to or improve the performance of a component (circuit) underneath. However, the effect of such ‗post-CMOS‘ processing on the active MOS devices, interconnects, and even inter-layer-dielectrics fabricated prior to the deposition has to be mild enough to leave the performance of delicate MOS characteristics intact. Such CMOS-compatibility of the present deposition process has been tested with a satisfactorily positive result.

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47

Sai, Ranajit. « Development of CMOS-Compatible, Microwave-Assisted Solution Processing of Nanostructured Zine Ferrite Films for Gigahertz Circuits ». Thesis, 2013. http://etd.iisc.ernet.in/2005/3412.

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The development of radio frequency integrated circuits (RFICs), especially the dream of integrating analog, digital and radio frequency (RF) components on the same chip that is commonly known as System-on-a-Chip (SoC), is crucial to mobile communications of the future. Such SoC approach offers enhanced performance, greater reliability, and substantially less power consumption of integrated circuits while reducing overall physical size and thus manufacturing cost. However, the progress has been stalled by the lack of miniaturized inductor elements. Rise of unwanted parasitic effects limits down-scaling of the inductor structures and leaves the use of magnetic coating as a viable and attractive option to enhance the inductance and thus inductance density. It is also essential to shift from perm alloy and other amorphous alloys to ferrites and hex ferrites as the core material because of their very high electrical resistivity so as to keep losses in check, a criterion that cannot be compromised on in GHz frequency applications. This is viable, however, only if the integration of the magnetic core (film), particularly a ferrite film, is fully compatible with the CMOS fabrication process. Various approaches have been taken to meet this requirement, including investigations of employing layers of ferrite materials to envelop the inductor loop. However, the deposition of thin films of ferrites, whether by PVD or CVD, usually calls for the deposited ferrite layer to be annealed at an elevated temperature to crystallize the layer so that its magnetic characteristics are appropriate for the optimum performance of the circuit element. Such annealing is incompatible with CMOS process flow required for aggressive device geometries, as the inductor element is added after the active semiconductor circuit is processed, and any exposure of the processed circuit to elevated temperatures risks disturbing precise doping profiles employed and the integrity of the inter-layer dielectrics. What is called for is a low-temperature process for the deposition of a ferrite layer on top of the patterned inductor element – a layer of thickness such that most of the fringe field is encapsulated – while ensuring that the layer comprises crystallites of uniform size that leads to uniform magnetic behaviour. Recognizing the difficulty of meeting the various stringent requirements, it has recently been remarked that such a goal is a formidable challenge. In an attempt to address this challenge, in this work, we have adopted a counter-intuitive approach - the deposition of the desired ferrite composition on a processed die (that contains the inductor structures along with active semiconductor circuits) by immersing it into a chemical (reactant) solution, followed by a brief irradiation of microwave frequency. However, to identify the desired ferrite composition and the appropriate recipe to deposit them, a systematic effort had to be made first, to understand the inter-relationship between synthesis process, structure of resulting material, and its physical and chemical properties. Therefore, at the beginning, a general introduction in which key concepts related to the magnetic-core inductors, the microwave-irradiation-assisted synthesis of nanostructures, the ‗state of the art‘ in the field of integration of appropriate magnetic material to the RFICs, are all outlined. As a proof of concept, microwave-irradiation-assisted solution-based deposition of zinc ferrite thin films on the technologically important Si (100) substrate is demonstrated. The highlight of the process is the use of only non-toxic metal organic precursors and aqua-alcoholic solvents for the synthesis, which is complete in 10 minutes @< 100 °C, without any poisonous by-products. Effects of various process parameters such as solute concentrations, surfactant types, and their concentrations are investigated. A wide range of deposition rates (10 - 2000 nm/min) has been achieved by tweaking the process parameters. The simultaneous formation of zinc ferrite nanocrystallites (ZFNC) along with deposition of thin film is the hallmark of this synthesis technique. Unlike its bulk counterpart, both film and powder are found upon investigation to be rich in magnetic behavior– owing to plausible cationic distribution in the crystal lattice, induced by the inherently quick and far-from-equilibrium nature of the process. The accurate estimation of magnetic characteristics in film is, however, found to be difficult due to the high substrate-to-film mass ratio. The simultaneously prepared ZFNC is examined to arrive at the optimized process recipe that imparts the desired magnetic properties to the zinc ferrite system. The crystallographic cationic distribution in zinc ferrite powder is, however, difficult to study due to the nanoscale dimension of the as prepared material. To enable crystal growth, slow and rapid annealing in air at two different temperatures are employed. The effects of these annealing schemes on various attributes (magnetic properties in particular) are studied. Rapid annealing turns out to be an interesting pathway to promote rapid grain-growth without disturbing the crystallographic site occupancies. The presence of inversion, i.e., the amount of Fe3+ in the ‗A‘-sites in the spinel structure that ideally is zero in normal spinel structure of zinc ferrite, is evident in all annealed ZFNC, as determined by Riveted analysis. Such partially inverted ZFNC exhibits soft magnetic behavior with high saturation magnetization, which can easily be ―tuned‖ by choosing appropriate annealing conditions. However, a few unique strategic modifications to the same microwave-irradiation-assisted solution-based synthesis technique are tried for the formation of nanocrystalline powder with desired sizes and properties without the necessity of anneal. The approach eventually appears to pave a way for the formation of oriented structures of zinc ferrite. The effects of anneal, nevertheless, are studied with the help of neutron powder diffractometry and magnetic measurements. The magnetic ordering at various temperatures is analyzed and connected to the magnetic measurements. The study shows that long-range magnetic ordering, present even at room temperate, originates from the distribution of cations in the partially inverted spinel structures, induced by the rapid and kinetically driven microwave synthesis. Keeping the mild nature (<200 °C) of the processing in mind, a large degree of inversion (~0.5) is a surprise and results in a very high saturation magnetization, as much as 30 emu/g at room temperature (paramagnetic in bulk), in the ZFNC system. Based on the knowledge of process-structure-property interrelationship, a recipe for the deposition of ferrite thin films by the microwave-assisted deposition technique is optimized. Successful deposition of smooth and uniform zinc ferrite thin films on various substrates is, then, demonstrated. The mystery behind the strong adherence of the film to the substrate - an unexpected outcome of a low-temperature process - is probed by XPS and the formation of silicates at the interface is identified as the probable reason. The uniformity and consistency of film composition is also examined in this chapter. Another salient feature of the process is its capability to coat any complex geometry conformally, allowing the possibility of depositing the material in a way to ―wrap around‖ the three-dimensional inductor structures of RF-CMOS. Integration of nanostructure zinc ferrite thin films onto on-chip spiral inductor structures has been demonstrated successfully. The magnetic-core inductors so obtained exhibit the highest inductance density (700 nH/mm2) and the highest Q factor (~20), reported to date, operate at 5 GHz and above, by far the highest reported to date. An increase in inductance density of as much as 20% was achieved with the use of just 1 µm thick film of zinc ferrite covering only the ―top‖ of the spiral structure, i.e., up to 20% of chip real estate can potentially be freed to provide additional functionality. The microwave-assisted solution-based deposition process described in this thesis is meant for ‗post-CMOS‘ processing, wherein the film deposited on some specific electronic components can add desired functionality to or improve the performance of a component (circuit) underneath. However, the effect of such ‗post-CMOS‘ processing on the active MOS devices, interconnects, and even inter-layer-dielectrics fabricated prior to the deposition has to be mild enough to leave the performance of delicate MOS characteristics intact. Such CMOS-compatibility of the present deposition process has been tested with a satisfactorily positive result.

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48

Benedict, Samatha. « Nanostructured Metal Oxide Semiconductor Gas Sensor ». Thesis, 2018. https://etd.iisc.ac.in/handle/2005/5366.

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Gas sensors play a vital role in today’s world; be it in pollution monitoring, breath analysis, food quality monitoring or in agriculture. A variety of methods are being explored to develop reliable gas sensor systems such as optical, acoustic, electrochemical and chemical. Among these methods of gas detection, the chemical gas sensors based on conductometric change of the sensing materials; mainly semiconducting metal oxides, are gaining much attention due to their simplicity, easy fabrication and low cost. However, the metal-oxide based gas sensors still pose issues in terms of cross-sensitivity, reproducibility, and sensor life. Researchers have explored many avenues including processing methods, nanostructuring and doping to develop reliable metal oxide gas sensors. Gas sensors based on nanostructures of metal oxides have shown a lot of promise due to their high surface to volume ratio; high surface energies and specificity of crystallographic planes. The scope of this thesis is to explore different fabrication methods for developing nanodimensional gas sensors which meet the figures of merit namely sensitivity, selectivity and stability. Furthermore, an effort is also made to develop a low cost and low power sensor array platform on a flexible substrate, using CMOS processes, to enable the application of these gas sensors in wearable electronics. In this thesis, plasma oxidation of different metallic structures to form metal-metal oxide core-shell type sensors is investigated for achieving the best hydrogen sulfide sensor. Platinum, widely known for its catalytic nature, is plasma oxidized at optimum conditions to fabricate Pt-PtOx core-shell nanowire sensor. The Pt-PtOx sensor shows degradation in response when used for H2S sensing, which is due to surface contamination by the sulphur species. To recover the sensor, deep ultra-violet light (UV) treatment is studied as a promising recovery method for sulphur contaminated sensor surfaces. Further, plasma oxidation of tungsten nanodiscs decorated W nanowire is carried out to achieve high sensitive H2S sensor with fast response and recovery times and good response repeatability over a study span of 6 months. The nanostructured W-WOx nanowire sensor is highly selective towards H2S with low order of detection of 10 ppb which is one of the lowest values reported in literature. The tungsten nanodiscs are patterned using electron beam lithography process which is known to be expensive and time consuming. Thus, an effort is also made to integrate the inexpensive process such as colloidal lithography to pattern the nanostructures on the metal nanowires, later plasma oxidized to form the core shell sensor. Colloidal lithography assisted nanostructure-based palladium-palladium oxide sensor is fabricated and tested for sensing of H2S gas. The fabricated sensor shows a detection limit of 10 ppb but lacks its performance in terms of high response and high selectivity when compared to nanostructured W-WOx sensor. In summary, plasma oxidation of metallic structures is explored to fabricate H2S gas sensors, with low order of gas detection of 10 ppb. The surface poisoning during H2S sensing is tackled through UV exposure to recover the sulphur poisoned sensors. Colloidal lithography is investigated for fabricating nanostructures as an inexpensive alternate for electron beam lithography. Thus, we believe that plasma oxidation of metallic structures and nanostructuring using colloidal lithography are two important methods which need to be explored further to develop gas sensors which meet the SSS figure of merit with low cost fabrication methodology. We also explored a low cost and low temperature process for synthesizing nanostructured metal oxide through microwave radiation. Microwave synthesis of NiO is optimized for detection of NO2 resulting in room temperature response all the way down to 200 ppb. In sensor community the manufacturing cost of gas sensors which is a big concern has led to the exploration of new substrates to fabricate sensors. Motivated by this we developed a sensor array platform with integrated microheater on flexible and low-cost plastic substrate using CMOS compatible fabrication processes. The sensor array consisted of four sensors with individually controlled microheater deposited on nanogap created using electromigration process. Due to flexible nature of substrate, the bending angle dependent microheater characteristics and sensing performance show the potential of the sensor platform in low power wearable electronics.

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49

Vanithakumari, S. C. « Synthesis And Characterization Of One-Dimensional Oxide Nanostructures ». Thesis, 2009. https://etd.iisc.ac.in/handle/2005/962.

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Nanostructured materials especially, one-dimensional (1D) nanostructures have unique physical, chemical, mechanical properties and are the building blocks for a range of nanoscale devices. The procedure employed for the synthesis of nanostructures involves the use of sophisticated instruments or rigorous chemical reactions. The motivation of our work is to develop a strategy that is simple, cost effective and applicable to a host of oxide materials. Nanostructures of various oxides have been grown from the metal as the source material. 1D ZnO nanostructures have been obtained by simply heating Zn metal in ambient air at temperatures below 600 °C. The nanostructures grow on the surface of the source material and the morphology is controlled by monitoring the curvature of the source material. This technique has an added advantage that neither any catalyst nor any gas flow is required. Tetrapods of ZnO are obtained when Zn is heated above 700 °C in ambient air. It has been shown that the morphology and the aspect ratio (length-to-diameter ratio) of the tetrapods depend on the temperature and the temperature gradient. Photoluminescence studies reveal good optical quality ZnO nanostructures. The technique employed to synthesize 1D ZnO nanostructures has been checked for other oxides. The temperature required for the synthesis of Ga2O3 nanostructures is 1200 °C. Many researchers have shown that Ga2O3 emits in the blue-green region. A red emission is required to get the impression of white light which has been seen for nitrogen doped Ga2O3. As the temperature is very high and Ga is heated in ambient air, unintentional nitrogen doping of 1D Ga2O3 nanostructures is obtained which is the reason for white light emission. The morphology of Ga2O3 nanostructures has been controlled by monitoring the curvature of the starting material as is the case of ZnO. Similar technique has also been employed for the synthesis of CuO nanostructures. The morphology is temperature dependent and 1D CuO nanostructures are obtained when the synthesis temperature is between 400 and 600 C. Possible growth mechanisms have been proposed for all these oxide materials. The entire thesis is based on the results discussed above. It has been organized as follows: Chapter 1 deals with the introduction to nanostructures, importance of 1D nanostructures, the specific applications of different morphologies, materials that are widely explored in the synthesis of nanostructures and different approaches to the synthesis of nanostructures. Growth mechanisms like VLS, VS and SLS are briefly discussed. A brief review on the basic physical properties, applications and different morphologies of ZnO, Ga2O3 and CuO is outlined with emphasis to the various synthesis techniques. Finally the aim and scope of the present work is discussed. Chapter 2 describes the experimental setup used for the synthesis and the basic principles of characterization techniques like x-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), energy dispersive spectrum (EDS), electron energy loss spectroscopy (EELS), photoluminescence (PL), Raman spectroscopy, x-ray photoelectron spectroscopy (XPS), UV-Visible spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR) and thermogravimetric analysis (TGA). Chapter 3 deals with the synthesis of 1D ZnO nanostructures with different morphologies such as nanoneedles, nanorods, nanobelts from Zn powder/granule. The growth process is found to be different from the conventional VS mechanism. The advantage and the versatility of the method is emphasized. In this method, neither a catalyst nor any gas flow is required for the synthesis of oxide nanostructures. Depending upon the Zn powder or Zn granules as the starting material different nanostructures of ZnO have been synthesized. The as-synthesized materials are characterized by XRD, SEM, HRTEM, EDS, TGA and Raman spectroscopy and the results are discussed. Chapter 4 describes the controlled growth of ZnO tetrapods and the influence of temperature and temperature gradient on the growth process. Though there are several methods to synthesize ZnO tetrapods and it has been established that ZnO tetrapods can be synthesized by heating Zn in air, it is advantageous to grow tetrapods of different morphologies with different lengths. The large scale synthesis of ZnO tetrapods by heating Zn in air ambient is discussed in this chapter. The key parameters that control the diameter, length, and morphology of tetrapods are identified. It is shown that the morphology and dimensions of the tetrapods depend not only on the vaporization temperature but also on the temperature gradient of the furnace. The influence of vaporization temperature and growth temperature on the morphology of the tetrapods is discussed elaborately. Chapter 5 explains the one-step synthesis of nitrogen doped Ga2O3 nanostructures of different morphologies and the different growth mechanisms. The experimental method employed for the synthesis of nanostructures is simple and is different from the other reported methods. Neither any catalyst/substrate preparation nor any gas flow is required for the synthesis of Ga2O3 nanostructures. The synthesis involves the heating of molten Ga at high temperatures. Single crystalline monoclinic phase of nitrogen-doped Ga2O3 nanorods, nanobelts and nanoneedles are obtained by this method. The morphology is controlled by monitoring the curvature of the Ga droplet which is achieved by using different substrates. Possible growth processes of different morphology have been proposed. Chapter 6 includes some surprising results on the white light emission of Ga2O3 nanorods. High synthesis temperature generates a high vapor pressure suitable for the growth of Ga2O3 nanorods, creates oxygen vacancy and incorporates nitrogen from the ambient. The oxygen vacancy is responsible for the bluish-green emission, while nitrogen is responsible for the red emission. As a consequence, white light emission is observed from Ga2O3 nanorods when irradiated with UV light. The interesting point is that neither post-treatment of the nanorods nor size control is required for white light emission. Chapter 7 describes the synthesis of CuO nanostructures by heating Cu foil in air ambient. This is an attempt to check whether the synthesis technique employed for ZnO and Ga2O3 is applicable to other oxides. The as-synthesized CuO nanostructures are characterized by XRD, SEM, HRTEM, EDS, TGA, UV-visible, FTIR and the results are discussed. Chapter 8 gives the conclusions and the overall summary of the thesis.

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50

Vanithakumari, S. C. « Synthesis And Characterization Of One-Dimensional Oxide Nanostructures ». Thesis, 2009. http://hdl.handle.net/2005/962.

Texte intégral

Résumé :

Nanostructured materials especially, one-dimensional (1D) nanostructures have unique physical, chemical, mechanical properties and are the building blocks for a range of nanoscale devices. The procedure employed for the synthesis of nanostructures involves the use of sophisticated instruments or rigorous chemical reactions. The motivation of our work is to develop a strategy that is simple, cost effective and applicable to a host of oxide materials. Nanostructures of various oxides have been grown from the metal as the source material. 1D ZnO nanostructures have been obtained by simply heating Zn metal in ambient air at temperatures below 600 °C. The nanostructures grow on the surface of the source material and the morphology is controlled by monitoring the curvature of the source material. This technique has an added advantage that neither any catalyst nor any gas flow is required. Tetrapods of ZnO are obtained when Zn is heated above 700 °C in ambient air. It has been shown that the morphology and the aspect ratio (length-to-diameter ratio) of the tetrapods depend on the temperature and the temperature gradient. Photoluminescence studies reveal good optical quality ZnO nanostructures. The technique employed to synthesize 1D ZnO nanostructures has been checked for other oxides. The temperature required for the synthesis of Ga2O3 nanostructures is 1200 °C. Many researchers have shown that Ga2O3 emits in the blue-green region. A red emission is required to get the impression of white light which has been seen for nitrogen doped Ga2O3. As the temperature is very high and Ga is heated in ambient air, unintentional nitrogen doping of 1D Ga2O3 nanostructures is obtained which is the reason for white light emission. The morphology of Ga2O3 nanostructures has been controlled by monitoring the curvature of the starting material as is the case of ZnO. Similar technique has also been employed for the synthesis of CuO nanostructures. The morphology is temperature dependent and 1D CuO nanostructures are obtained when the synthesis temperature is between 400 and 600 C. Possible growth mechanisms have been proposed for all these oxide materials. The entire thesis is based on the results discussed above. It has been organized as follows: Chapter 1 deals with the introduction to nanostructures, importance of 1D nanostructures, the specific applications of different morphologies, materials that are widely explored in the synthesis of nanostructures and different approaches to the synthesis of nanostructures. Growth mechanisms like VLS, VS and SLS are briefly discussed. A brief review on the basic physical properties, applications and different morphologies of ZnO, Ga2O3 and CuO is outlined with emphasis to the various synthesis techniques. Finally the aim and scope of the present work is discussed. Chapter 2 describes the experimental setup used for the synthesis and the basic principles of characterization techniques like x-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), energy dispersive spectrum (EDS), electron energy loss spectroscopy (EELS), photoluminescence (PL), Raman spectroscopy, x-ray photoelectron spectroscopy (XPS), UV-Visible spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR) and thermogravimetric analysis (TGA). Chapter 3 deals with the synthesis of 1D ZnO nanostructures with different morphologies such as nanoneedles, nanorods, nanobelts from Zn powder/granule. The growth process is found to be different from the conventional VS mechanism. The advantage and the versatility of the method is emphasized. In this method, neither a catalyst nor any gas flow is required for the synthesis of oxide nanostructures. Depending upon the Zn powder or Zn granules as the starting material different nanostructures of ZnO have been synthesized. The as-synthesized materials are characterized by XRD, SEM, HRTEM, EDS, TGA and Raman spectroscopy and the results are discussed. Chapter 4 describes the controlled growth of ZnO tetrapods and the influence of temperature and temperature gradient on the growth process. Though there are several methods to synthesize ZnO tetrapods and it has been established that ZnO tetrapods can be synthesized by heating Zn in air, it is advantageous to grow tetrapods of different morphologies with different lengths. The large scale synthesis of ZnO tetrapods by heating Zn in air ambient is discussed in this chapter. The key parameters that control the diameter, length, and morphology of tetrapods are identified. It is shown that the morphology and dimensions of the tetrapods depend not only on the vaporization temperature but also on the temperature gradient of the furnace. The influence of vaporization temperature and growth temperature on the morphology of the tetrapods is discussed elaborately. Chapter 5 explains the one-step synthesis of nitrogen doped Ga2O3 nanostructures of different morphologies and the different growth mechanisms. The experimental method employed for the synthesis of nanostructures is simple and is different from the other reported methods. Neither any catalyst/substrate preparation nor any gas flow is required for the synthesis of Ga2O3 nanostructures. The synthesis involves the heating of molten Ga at high temperatures. Single crystalline monoclinic phase of nitrogen-doped Ga2O3 nanorods, nanobelts and nanoneedles are obtained by this method. The morphology is controlled by monitoring the curvature of the Ga droplet which is achieved by using different substrates. Possible growth processes of different morphology have been proposed. Chapter 6 includes some surprising results on the white light emission of Ga2O3 nanorods. High synthesis temperature generates a high vapor pressure suitable for the growth of Ga2O3 nanorods, creates oxygen vacancy and incorporates nitrogen from the ambient. The oxygen vacancy is responsible for the bluish-green emission, while nitrogen is responsible for the red emission. As a consequence, white light emission is observed from Ga2O3 nanorods when irradiated with UV light. The interesting point is that neither post-treatment of the nanorods nor size control is required for white light emission. Chapter 7 describes the synthesis of CuO nanostructures by heating Cu foil in air ambient. This is an attempt to check whether the synthesis technique employed for ZnO and Ga2O3 is applicable to other oxides. The as-synthesized CuO nanostructures are characterized by XRD, SEM, HRTEM, EDS, TGA, UV-visible, FTIR and the results are discussed. Chapter 8 gives the conclusions and the overall summary of the thesis.

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