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Semiconductor nanocrystals are interesting candidates as new light-absorbing materials for photovoltaic (PV) devices. They can be dispersed in solvents and cheaply deposited at low-temperature on various substrates. Also, the nanocrystals have unique optical properties depending on their size due to the quantum size effect and moreover it is easy to uniformly control their stoichiometry. CdTe/CdSe/CdTe heterostructure nanorods and I-III-VI₂ nanocrystals were selected to synthesize and investigate in order to utilize the benefits of colloidal nanocrystals described above. Colloidal nanorods with linear CdTe/CdSe/CdTe heterojunctions were synthesized by sequential reactant injection. After CdTe deposition at the ends of initially formed CdSe nanorods, continued heating in solution leads to Se-Te interdiffusion across the heterojunctions and coalescence to decreased aspect ratio. The Se-Te interdiffusion rates were measured by mapping the composition profile using nanobeam energy dispersive X-ray spectroscopy (EDS). The rate of nanorod coalescence was also measured and compared to model predictions using a continuum viscous flow model. The synthetic method of monodisperse chalcopyrite (tetragonal) CuInSe₂ nanocrystals was also developed. The nanocrystals have trigonal pyramidal shape with one polar and three non-polar surface facets. When drop-cast onto carbon substrates, the nanocrystals self-assemble into close-packed monolayers with triangular (honeycomb) lattice structure. Moreover, the effect of excess Cu precursor (CuCl) was studied for the formation of monodisperse trigonal pyramidal CuInSe₂ nanocrystals. The formation mechanism of monodisperse trigonal pyramidal CuInSe₂ nanocrystals was suggested with regard to excess amount of CuCl precursor, based on the nucleationgrowth model of colloidal nanocrystal formation. A new wurtzite phase of CuInS₂, CuInSe₂, and Cu(InxGa1-x)Se₂ (CIGS) was observed in nanocrystals synthesized by heating metal precursors and Se-(or S-)urea in alkylamine. X-ray diffraction (XRD) showed the predominant phase to be wurtzite (hexagonal) instead of chalcopyrite (tetragonal). High resolution transmission electron microscopy (TEM), however, revealed polytypism in the nanocrystals, with the wurtzite phase interfaced with significant chalcopyrite domains. / text

Made available in DSpace on 2015-03-26T13:35:13Z (GMT). No. of bitstreams: 1 texto completo.pdf: 1486986 bytes, checksum: a086a712989295bff60986e7d0bcdd7e (MD5) Previous issue date: 2010-02-25 / Fundação de Amparo a Pesquisa do Estado de Minas Gerais / Cadmium telluride films grown on glass substrates covered by fluorine doped tin oxide (TCO) were studied by generic dynamical scaling theory proposed by L ópez et al. [Phys. Rev. Lett. 84, 2199 (2000)]. The samples were grown by Ferreira et al. [Appl. Phys. Lett. 88, 244102 (2006)] using hot wall epitaxy and the interface scaling properties were investigated in this work using the power spectrum, height-height correlation function, and interface width. The theory adopted has six scaling exponents, but only four of them are independent. However, in order to classify which growth regime the system follows one should analyze three of these exponents, namely, α, αloc and αs which are related to the global, local, and power spectrum fluctuations, respectively. The results show that the studied system exhibit anomalous scaling behavior characterized by global roughness exponent di fferent from the local one. Actually, in agreement with the adopted theory we have found a growth regime ruled by faceted interfaces, characterized by αloc = 1 and α ≠ αs > 1. This prediction of the anomalous scaling theory was corroborated by atomic force microscopy of the samples. We conjecture that non-local effects, caused by the initial disorder imposed by the amorphous substrate, rule the anomalous scaling. / Filmes de telureto de cádmio crescidos sobre substratos de vidro recobertos com oxido de estanho dopado com flúor (TCO) foram estudados usando a teoria de escala dinâmica proposta por Lopez et al. [Phys. Rev. Lett. 84, 2199 (2000)]. As amostras foram crescidas por Ferreira et al. [Appl. Phys. Lett. 88, 244102 (2006)] usando a técnica de epitaxia por paredes quentes e as propriedades de escala da interface foram investigadas neste trabalho através do espectro de potência, da função de correlação de alturas e da espessura da interface. A teoria usada possui seis expoentes de escala, sendo quatro independentes. Entretanto, para classificar qual regime de crescimento o sistema obedece deve-se analisar três desses expoentes, a saber, α, αloc e αs relacionados com as flutuações globais, locais e do espectro de potência da interface, respectivamente. Os resultados mostram que o sistema estudado apresenta comportamento de escala anômalo caracterizado pelo expoente de rugosidade global diferente da rugosidade local. Mais precisamente, em acordo com a teoria usada, encontramos um regime de crescimento com interfaces facetadas caracterizadas por α loc = 1 e α ≠ α s > 1. Essa previsão da teoria de escala anômala foi corroborada através de microscopia de força atômica das amostras. Conjecturamos que efeitos não-locais originados pela desordem inicial imposta pelo substrato amorfo são os fatores que originam o comportamento de escala anômalo.

Made available in DSpace on 2015-03-26T13:35:16Z (GMT). No. of bitstreams: 1 texto completo.pdf: 3403324 bytes, checksum: 2828289d9a42c60c7cb3b860cb3dca61 (MD5) Previous issue date: 2011-05-30 / Conselho Nacional de Desenvolvimento Científico e Tecnológico / In this work the techniques of hot wall epitaxy (HWE) and molecular beam epitaxy (MBE) on thin films of CdTe (cadmium telluride) were used in order to manufacture a prototype solar cell type Schottky barrier. The films were produced by evaporation of a solid alloy of CdTe, varying two parameters of deposition: the growth time and substrate temperature. In the manufacture the Schottky Barrier solar cells Al-CdTe, the CdTe film was grown on glass substrate coated with a layer of TO (tin oxide doped with fluorine - SnO2:F) and an evaporation system was used in the deposition of Al contacts. The films were characterized by several techniques including profilometry to measure the thickness, atomic force microscopy (AFM) for determining surface morphology and x-ray diffraction for crystalline properties. The prototypes of the solar cell were characterized by electrical measurements (IxV curve) with and without illumination. The results show a strong influence of substrate temperature and thickness on the properties of solar cells. It was observed that the increase of substrate temperature favors the increase of grain and the growth of films with better quality, resulting in devices with better features. In addition, thinner layers of CdTe cells also produce a higher short circuit current when illuminated. Although the cells produced showed very low efficiency, we believe that it is possible to improve manufacturing processes, achieving better efficiency. / Neste trabalho utilizou-se as técnicas de epitaxia por paredes quentes (HWE) e epitaxia por feixe molecular (MBE) na fabricação de filmes finos de CdTe (telureto de cádmio) com o objetivo de fabricar um protótipo de célula solar tipo barreira Schottky. Os filmes foram obtidos por evaporação de uma liga sólida de CdTe, fazendo-se variar dois parâmetros de deposição: o tempo de crescimento e a temperatura do substrato. Na fabricação das células solares tipo Barreira Schottky Al-CdTe, o filme de CdTe foi crescido sobre o substrato de vidro recoberto com uma camada de TO (óxido de estanho dopado com Flúor – SnO2:F) e uma metalizadora foi utilizada na deposição dos contatos de Al. Os filmes foram caracterizados por diversas técnicas, incluindo a perfilometria para medida da espessura, a microscopia de força atômica (AFM) para determinação das propriedades morfológicas e difração de raios-x para determinação das propriedades cristalinas. Os protótipos da célula solar foram caracterizados através de medidas elétricas da curva IxV com e sem iluminação. Os resultados obtidos mostram uma forte influência da temperatura do substrato e da espessura nas propriedades das células solares construídas. Observou-se que o aumento da temperatura do substrato favorece o aumento do grão e o crescimento de filmes com melhor qualidade resultando em dispositivos com melhores características. Além disso, camadas mais finas de CdTe também produzem células que apresentam maior corrente de curto-circuito, quando iluminadas. Apesar das células fabricadas apresentarem eficiência muita baixa, acreditamos que existe a possibilidade de melhorar os processos de fabricação, conseguindo melhorar a eficiência.

Submitted by Fabio Sobreira Campos da Costa (fabio.sobreira@ufpe.br) on 2016-07-14T16:14:49Z No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) DissertSergioPassos32abntCD.pdf: 3127165 bytes, checksum: e4b607e29cf477a0026a7c45e1d7d953 (MD5) / Made available in DSpace on 2016-07-14T16:14:49Z (GMT). No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) DissertSergioPassos32abntCD.pdf: 3127165 bytes, checksum: e4b607e29cf477a0026a7c45e1d7d953 (MD5) Previous issue date: 2015-01-16 / FACEPE / Neste trabalho foi desenvolvido um novo método eletroquímico de síntese de PQs de CdTe estabilizados por ácido mercaptopropiônico (AMP) e cisteamina (CYS). O método consiste na redução eletroquímica do telúrio metálico em pó em célula de cavidade. O Te0 foi misturado ao grafite em pó (material do cátodo) e submetido a uma corrente controlada (-30 mA), que permitiu a geração das espécies reduzidas Te2- e Te2 2-. As espécies reduzidas de telúrio migram para um compartimento intermediário da célula de cavidade e na presença de sal de cádmio e um agente estabilizante orgânico (AMP ou CYS) possibilitaram a formação do CdTe coloidal em única etapa; para posterior obtenção dos PQs através de tratamento térmico à 90°C. CdTe/CdS-AMP e CdTe/CdS-CYS foram obtidos em meio aquoso pH=12 e 5,5, respectivamente. Esse método mostrou ser de fácil aplicação, rápido, eficiente, reprodutível e dispensa o uso de agentes redutores químicos, podendo ser estendido para síntese de outros PQs. Os PQs sintetizados apresentaram nanocristais de alta qualidade, muito estáveis e com carga superficial negativa no caso do estabilizante AMP (potencial zeta = -30mV) e positiva na presença da CYS. Foi observado que o tamanho das partículas aumenta proporcionalmente com o tempo de aquecimento, apresentando fluorescência com emissão nas cores entre o verde (522 nm) e o vermelho (643 nm). Foi determinado um tamanho médio de partícula de 4,1 nm para o CdTe/CdS-AMP após 120 minutos de tratamento térmico, com rendimento quântico de 11%. / A new electrochemical method was developed for the CdTe quantum dots (QDs) synthesis, stabilized by mercaptopropionic acid (MPA) and cysteamine (CYS). The method comprises the electrochemical reduction of tellurium powder in a cavity cell. The Te0 was mixed to graphite powder (cathode material) and subjected to a controlled current (-30 mA) electrolysis, which allowed the generation of Te2- Te2 2-. These tellurium reduced species migrate to an intermediate compartment of the cavity cell containing Cd2+/organic stabilizer (AMP or CYS) aqueous solution pH 13, which enabled the formation of colloidal CdTe in one pot process. The QDs are retrieved after heat treatment at 90°C. CdTe/CdS-AMP e CdTe/CdS-CYS were obtained in aqueous medium adjusting the pH to 12 and 5.5, respectively. This method proved to be easy, fast, efficient, reproducible and avoids the use of chemical reducing agents. It can also be extended to the synthesis of other QDs. The synthesized QDs presented a good quality nanocrystals, with high stability and negative charge surface in the case of the AMP stabilizer (zeta potential = -30mV) and positive in the presence of CYS. It was observed that the particle size increases proportionately with the heating time, showing fluorescence emission in the colors between green (522 nm) and red (643 nm). It was determined an average size of 4.1 nm particle for CdTe / CdS-AMP after 120 minutes of heat treatment, with a quantum yield of 11%.

Aus CdTe- und Edelmetallnanopartikeln werden 3-dimensionale Netzwerkstrukturen aufgebaut, welche durch einen überkritischen Trocknungsprozess zu hochporösen, weitverzweigten Halbleiter-Metall-Nanokompositen, sogenannten Aerogelen, umgewandelt werden. Zunächst werden Thiol-stabilisierte CdTe- und Edelmetallnanopartikel im wässrigen Milieu hergestellt und deren Morphologie und optischen Eigenschaften umfangreich mittels UV-Vis-Spektroskopie, Fluoreszenzspektroskopie und -lebensdauermessung, ICP-OES, TEM, STEM-EDX und AFM charakterisiert. Als Metallkomponente kamen Gold-, Palladium- sowie bimetallisch gemischte Gold-Palladium-Nanopartikel zum Einsatz. Die Gelierung der Nanopartikellösungen erfolgt durch Vermischen der Kolloide und anschließender kontrollierter Destabilisierung mithilfe einer Xe-Dampflampe oder der Zugabe von Wasserstoffperoxid. Neben einer mechanistischen Beschreibung der Gelbildungsmethoden wurden die resultierenden Hydrogele und die aus der überkritischen Trocknung erhaltenen Aerogele bezüglich Zusammensetzung, Morphologie und optischen Eigenschaften mithilfe von TEM und REM jeweils gekoppelt mit EDX-Analyse, Stickstoff-Porosimetrie, diffuser Reflexionsspektroskopie, Fluoreszenzspektroskopie und Fluoreszenzlebensdauermessungen untersucht. Weiterhin wird die UV-Vis-Spektroskopie als Methode zur Konzentrationsbestimmung von Gold in Lösungen kolloidaler Gold-Nanopartikel validiert. Dabei wird die Absorption der Kolloide bei einer Wellenlänge von 400 nm als Maß verwendet. Die NP-Lösungen werden anhand der Parameter Partikelgröße, Oberflächenfunktionalität und der Oxidationsstufe des enthaltenen Goldes variiert. / 3-dimensional network structures are formed combining CdTe and noble metal nanoparticles. A supercritical drying process allows production of highly porous and widely branched semiconductor-metal nanohybrids, so-called aerogels. Primarily, thiol-capped CdTe and noble metal nanoparticles are synthesized in aqueous media and their morphology and optical properties are studied extensively using UV-Vis and fluorescence spectroscopy, time-resolved fluorescence spectroscopy, ICP-OES, TEM, STEM-EDX and AFM. The metal entity involves gold and palladium nanoparticles as well as bimetallic mixed Au/Pd nanoparticles. After mixing of the different colloids gelation is induced by a controlled destabilization process using a Xenon lamp irradiation or the addition of hydrogen peroxide. Gelation techniques are described mechanistically. Resulting hydrogels and aerogels which are obtained by supercritical drying approach are characterized concerning composition, morphology and optical properties using TEM and SEM each coupled with EDX, nitrogen porosimetry, diffuse reflection spectroscopy, fluorescence spectroscopy and time-resolved fluorescence spectroscopy. Moreover, the UV-Vis spectroscopy is validated as a method to determine the gold concentration in gold nanoparticle solutions using the colloids absorbance at 400 nm as a measure. Gold nanoparticle solutions are varied concerning the parameters particle size, surface functionality and oxidation state of contained gold.

L'apparition des détecteurs à comptage de photons X à base de CdTe avec des capacités de discrimination de l'énergie des photons ouvre de nouvelles perspectives pour l'imagerie radiographique. Les applications médicales et en contrôle de bagages X sont caractérisées par un flux de photons X très élevé, et exigent par conséquent une mise en forme très rapide du photo-courant mesuré pour limiter les empilements. Cependant, si cette mise en forme est plus courte que le temps de transit des électrons dans le semi-conducteur, la charge mesurée devient inférieure à la charge déposée : c’est le déficit balistique. Par ailleurs, la variation dans le temps du profil du champ électrique dans le volume du détecteur entraîne une augmentation du temps de transit des électrons. En conséquence, la charge mesurée diminue dans le temps, faussant la mesure de l’énergie des photons X. L’objectif de ce travail est de caractériser cette instabilité et de développer une méthode de correction de son effet sur les spectres en énergie. Nous avons proposé un algorithme de correction basé sur l'utilisation de deux Lignes à Retard (LAR). Une LAR rapide (50ns ?) permet de mesurer les spectres X à très fort flux sans compromis sur le taux de comptage. Une LAR lente (200ns ?) est utilisée pour mesurer intégralement la charge déposée sans déficit balistique. Un facteur de correction est évalué et utilisé pour stabiliser la mesure de l’énergie des X avec la LAR rapide. Une étape importante de cet algorithme consiste à trier les impulsions traitées pour rejeter celles qui peuvent dégrader la mesure de ce facteur de correction, notamment les empilements. La méthode proposée a été implémentée dans un FPGA pour fonctionner en temps réel et a été testée avec un détecteur CdTe de 3mm d'épaisseur avec 4×4 pixels au pas de 800 microns, capable de mesurer des spectres X dans la gamme d'énergie 20-160 keV avec 256 canaux d'énergie. La méthode développée a été initialement testée à faible taux de comptage avec des sources gamma Co-57 et Am-241, puis à fort taux de comptage jusqu'à ~2 Mc/s avec un tube à rayons X. Cet algorithme innovant a montré sa capacité de fournir une réponse stable du détecteur dans le temps sans affecter la résolution d'énergie (7 % à 122 keV) et le temps mort (~70 ns). / The emergence of CdTe Photon Counting Detectors (PCD) with energy discrimination capabilities, opens up new perspectives in X-ray imaging. Medical and security applications are characterized by very high X-ray fluxes and consequently require a very fast shaper in order to limit dead time losses due to pile-up. However, if the shaper is faster than the collection of the charges in the semiconductor, there is a loss of charge called ballistic deficit. Moreover, variations of the electric field profile in the detector over time cause a change in the collection time of the charges. As a result, the conversion gain of the detector will be affected by these variations. The instability of the response is visible over time as a channel shift of the spectra, resulting in a false information of the photon energy. The aim of this work is to characterize this instability in order to understand the mechanisms behind them and to develop a method to correct its effect. We proposed a correction algorithm based on the use of two Single Delay Line (SDL) shaping amplifiers. A fast SDL is used to measure the X-ray spectra at high count rates with limited count rate losses. A slow SDL is used to measure the full collected charge in order estimate a correction factor for the compensation of the ballistic deficit fluctuations of the fast SDL. An important step is to sort the processed pulses in order to reject pile-up and other undesirable effects that may degrade the measurement of the correction factor. The proposed method was implemented in an FPGA in order to correct the ballistic deficit in real-time and to give a stable response of the detector at very high fluxes. The method was tested with a 4x4 pixels detector (CdTe) of 3 mm thickness and 800 micron pitch, which is able to measure transmitted X-ray spectra in the energy range of 20-160 kV on 256 energy bins. The developed method was initially tested at low count rate with a Co-57 and an Am-241 gamma-ray sources, then at high count rates up to ~2 Mc/s with an X-ray source. With the characterization and the validation of this innovative algorithm we prove its ability in providing a stable response of the detector over time without affecting the energy resolution (~7% at 122 keV) and the dead time (~70 ns).