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Strategies Toward Functional Transparent P-type Layers: Epitaxy of Copper Iodide by Pulsed Laser DepositionStorm, Philipp 11 October 2022 (has links)
In der vorliegenden kumulativen Arbeit werden Untersuchungen am transparenten p-Typ Halbleiter Kupferiodid (CuI) beschrieben. Die Dünnschichtherstellung erfolgte mittels gepulster Laserabscheidung (PLD). Der Einfluss der Wachstumsbedingungen auf die strukturellen, morphologischen und elektrischen Eigenschaften wird dargelegt hinsichtlich des Ziels der Fabrikation funktioneller Schichten auf Basis von CuI. Dazu wird im ersten Teil der Arbeit der generelle Einfluss der PLD-Parameter auf das Schichtwachstum beschrieben. Ein dominierender Einfluss der Wachstumstemperatur auf die kristalline Qualität, Oberflächenrauhigkeit sowie Ladungsträgerdichte und Mobilität wurde beobachtet. Die 250nm dicken Dünnschichten zeigen im sichtbaren Bereich eine Transmittanz von bis zu 90%. Exzitonische Absorptions- und Lumineszenzcharakteristika konnten an solchen Schichten nachgewiesen werden. Eine schützende Deckschicht aus Al2O3 erwies sich als elementar zur Stabilisierung der elektrischen Eigenschaften und erlaubte die Fabrikation nicht-degenerierten Kupferiodids. Im zweiten Teil werden detail- lierte Untersuchungen des elektrischen Langzeitverhaltens von CuI in Abhängigkeit des Wachstums der Al2O3 Deckschichten diskutiert. Für Sauerstoff-defizientes Al2O3 zeigte das CuI komplexe elektrische Degradationsmechanismen, welche auf die Diffusion von Sauerstoff innerhalb der Heterostruktur zurückgeführt wurden. Die Ergebnisse beweisen einen dominierenden Einfluss extrinsischer Akzeptoren auf die elektrischen Eigenschaften von PLD gewachsenem CuI. Im Kontrast zum bisherigen Stand der Literatur spielen intrinsische Defekte für die Erklärung eine untergeordnete Rolle. Um eine Stabilisierung der Ladungsträgerdichten im Zusammenspiel mit Sauerstoff-defizientem Al2O3 zu er- reichen, wurden die CuI Dünnfilme mit Selen dotiert. Die Grenze zwischen Dotierung und Legierung, welche sich durch reduzierte Bandkantenenergien und eine einsetzende Phasenseparation definiert, wurde bestimmt. Weiterhin konnte die Bindungsenergie des Selen-Akzeptors in CuI bestimmt werden. Der finale Teil der Arbeit fokussierte sich auf die Unterdrückung der Bildung von Rotationsdomänen als dominierende Defekte von PLD gewachsenem CuI. Dieses Ziel wurde mittels PLD gewachsenen Natriumbromid (NaBr) Zwischenschichten auf kommerziellen Strontiumfluorid Substraten erreicht. Die Oberflächenrauigkeit von entsprechenden Dünnschichten ist deutlich reduziert. Unter Ausnutzung der hohen Wasserlöslichkeit von NaBr wurde ein epitaktischer Ablöseprozess entwickelt, der zur Herstellung frei stehender CuI Schichten geeignet ist. Das Wachstum von einkristallinen Volumenkristallen ist jedoch beschränkt, da bei Schichtdicken > 2 μm Defekthäufungen beobachtet werden und Rotationsdomänen auftreten.:1 Introduction
2 Theoretical Descriptions
2.1 Copper Iodide
2.1.1 Conductivity and Defect Chemistry
2.2 Epitaxy of Crystalline Thin Films
2.2.1 Stress and Strain
2.2.2 Heteroepitaxy of Copper Iodide
2.3 Electronic Defect States in Semiconductors
3 Experimental Methods
3.1 Sample Preparation by Pulsed Laser Deposition-PLD
3.1.1 Combinatorial and Eclipse PLD
3.2 Characterization Techniques
3.2.1 X-ray Diffraction-XRD
3.2.2 Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray Spectrometry(EDX)
3.2.3 Atomic Force Microscopy-AFM
3.2.4 Laser Scanning Microscopy-LSM
3.2.5 Time-of-Flight Secondary Ion Mass Spectrometry - ToF-SIMS
3.2.6 Rutherford Backscattering-RBS
3.2.7 Hall-Effect
3.2.8 Spectroscopic Ellipsometry
3.2.9 Photoluminsescence Spectroscopy-PL
3.2.10 Transmission Spectroscopy
4 Cumulative Part
4.1 Optimization of Copper Iodide Thin Film Growth by Pulsed Laser Deposition
4.2 Origin of Free Charge Carriers and p-Doping of PLD Copper Iodide
4.3 Suppression of Rotational Domains, Volume Crystals and Epitaxial Lift-Off
5 Summary and Outlook
Bibliography
List of Abbreviations
List of Publications
Author Contributions
Zusammenfassung nach Promotionsordnung §11(4)
Selbstständigkeitserklärung
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Reactivity and photochemistry of copper halide complexes / Reaktivitet och fotokemi hos kopparhalidkomplexWicksell Chuainukun, Needa Athitaya January 2021 (has links)
This paper deals with 3-picoline, 4-picoline, 3,4-lutidine and 3,5-lutidine complexes of copper(I) iodide (CuI(3-pic), CuI(4-pic), CuI(3,4-lut) and (CuI(3,5-lut)). The experimental investigation was divided into several parts. Firstly, the synthesis and characterization of the compounds both as powder and as thin films. Secondly, the photoluminescence study. Thirdly, the observation of ligand exchange reaction by vapor diffusion, and lastly, the determination of the lifetime by time-resolved photoluminescence of respective compound. All studied copper(I)-iodide-substituted pyridine compounds were emissive both as powders and thin films. The synthesis of the tetranuclear cluster powders yields both cluster and polymeric forms of structure. The pXRD of the powders CuI(3-pic), CuI(4-pic), and CuI(3,5- lut) confirmed to be as polymeric structures, hence the CuI(3-pic) showed thermochromism behavior. The structure of CuI(3,4-lut) is still unconfirmed. The most effective method for the synthesis of the thin films was the SILAR method. The photoluminescence spectra of respective thin films differ from their corresponding powders, and the structure of the compounds as thin films is yet unexplored. The emission of CuI(3-pic), CuI(4-pic), and CuI(3,4-lut) as thin films were similar 480nm, hence the emission of CuI(3,5-lut) thin film lays on 518 nm. Therefore, the ligand exchange reaction was performed on the CuI(3-pic) thin film with 3,5-lutidine as the exchanging ligand. The ligand exchange reaction of CuI(3-pic) thin film by vapor diffusion of 3,5-lutidine results in a spectrum shift from the emission spectrum of CuI(3-pic) to the spectrum of CuI(3,5-lut). This indicates a successful ligand exchange reaction by vapor diffusion. The lifetimes of the investigated compounds which have their best fit of mono-exponential function were between 2,2 μs and 9,52 μs. The lifetimes were determined on the thin films with time-resolved photoluminescence. The ligand exchange reaction was also observed by time- resolved photoluminescence which reveals some stable lifetimes during the reaction that can indicate the formation of intermediates. In contrast, the measured lifetimes during the ligand exchange reaction have their best fit of bi-exponential function which can be due to reaction conditions during the measurement or the homogeneity of the thin films. / Denna uppsats behandlar 3-pikolin, 4-pikolin, 3,4-lutidin och 3,5-lutidin komplex av koppar(I) jodid (CuI(3-pic), CuI(4-pic), CuI(3,4-lut) och (CuI(3,5-lut)). Den experimentella undersökningen delades in i olika delar. Först, syntesen och karakteriseringen av föreningarna både som pulver och som tunn film. Sedan studerades fotoluminiscensen av respektive förening. Därefter genomförde en ligand-utbytes-reaktion genom förgasning och slutligen bestämde livstiden av föreningarnas exciterade tillstånd. Alla koppar(I) jodid föreningar som studerade gav upphov till emission både som pulver och som tunn film. Syntesen av tetranukleära kluster i pulverform resulterade i både kluster och polymer struktur. pXRD av pulvren CuI(3-pic), CuI(4-pic) och CuI(3,5-lut) bekräftade dess struktur som polymera strukturer. Däremot visade CuI(3-pic) termokromism. Strukturen för CuI (3,4-lut) kunde inte obekräftas. Den mest effektiva metoden för syntes av tunn film i det här fallet är med SILAR-metoden. Fotoluminescensspektra för respektive tunn film skiljer sig från deras motsvarande pulverform och strukturen på tunn film är fortfarande outforskat. Emission av CuI(3-pic), CuI(4-pic) och CuI(3,4-lut) som tunn film var ungefär lika ~480 nm medan för CuI(3,5-lut) så var det på 518 nm. Med denna kontrast utfördes ligand-utbyte-reaktionen på tunn film av CuI(3-pic) med 3,5- lutidin. Ligand-utbyte-reaktionen av CuI(3-pic) på tunn film via förgasning av 3,5-lutidin resulterar i en spektrumförskjutning från spektrumet av CuI(3-pic) till spektrumet av CuI(3,5-lut). Detta indikerar i en lyckad ligand-utbyte-reaktion. Livslängderna för de undersökta föreningarna vilket har sin bästa passning i mono- exponentiell funktion var mellan 2,2 μs och 9,52 μs. Livstiderna bestämdes på de tunn film med ”time-resolved photoluminescence”. Ligand-utbyte-reaktionen observerades också med ”time- resolved photoluminescence” som avslöjar några stabila livstider under reaktionen vilket kan indikera bildning av intermedianer. De uppmätta livstiderna under ligand-utbyte-reaktionen har däremot sin bästa passning av bi-exponentiell funktion vilket kan bero på reaktionsförhållanden under mätningen och tunn filmernas homogenitet.
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Robust Capillary Electrophoresis Methods for Biomarker Discovery and Routine Measurements in Clinical and Epidemiological ApplicationsNori de Macedo, Adriana January 2017 (has links)
Biochemical markers (i.e., biomarkers) are of key importance to guide clinical decisions and public health policies by enabling early detection, accurate diagnosis and/or prevention of human diseases. However, major challenges remain due to the limited clinical utility of many biomarkers and the lack of robust analytical methods for their reliable measurements in a routine clinical setting that is also suitable to large-scale epidemiological studies. This thesis includes two major research themes involving the analysis of known biomarkers that lack appropriate methods, and the discovery of new biomarkers for complex disease conditions. In particular, this thesis describes the (1) development and validation of robust analytical methods based on capillary electrophoresis (CE) with photometric detection for the measurement of inorganic anions in volume-restricted biofluids; and (2) characterization of the sweat metabolome in infants and identification of sweat biomarkers in asymptomatic cystic fibrosis (CF) infants using multisegment injection-capillary electrophoresis-mass spectrometry (MSI-CE-MS). Chapter II introduces a simple CE assay that is remarkably selective for the analysis of sulfate, sulfite and chloride, which was applied in a pilot study to investigate the role of urinary sulfate as a biomarker for kidney stone risk assessment in children. Chapter III introduces a novel CE method for assessing iodine nutrition, which is followed by an inter-method comparison with inductively coupled plasma-mass spectrometry as described in Chapter IV. This led to the development of a fully validated CE method for monitoring the prevalence of iodine deficiency on a population level as required for global health initiatives. Chapter V demonstrates that more than 64 endogenous and exogenous compounds are present in the sweat of screen-positive CF infants, including a panel of differentiating metabolites that are associated with CF status, as well as treatment responsivity to nutritional and/or drug intervention. In summary, this thesis has contributed novel analytical methods suitable for routine biomarker analysis, in addition to the first non-targeted characterization of the sweat metabolome from infants, which require further studies to evaluate their clinical utility as biomarkers that allow for improved diagnosis, prognosis and treatment monitoring of the highly variable CF disease spectrum. / Thesis / Doctor of Philosophy (PhD)
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Haloethane Reactions over the Chromia Cr₂O₃ (1012) SurfaceMa, Qiang 01 September 2005 (has links)
Ethyl iodide and ethyl chloride have been used as reactants to produce ethyl fragments on the stoichiometric α-Cr₂O₃ (1012) surface by means of thermal dissociation. Ethyl iodide is dissociated giving iodine adatoms and ethyl fragments bound to surface Cr cation sites, while ethyl chloride is dissociated giving chlorine adatoms and ethyl fragments. No oxygenated products are observed in thermal desorption, suggesting the 3-coordinate lattice oxygen on the stoichiometric α-Cr₂O₃ (1012) surface is very stable, and no nucleophilic attack occurs at the carbon atoms on surface ethyl fragments.
For both reactants, the only reaction products observed are ethylene gas (CH₂=CH₂), ethane gas (CH₃-CH₃), hydrogen gas (H₂) and halogen adatoms (Cl<sub>ads</sub> or I<sub>ads</sub>). In thermal desorption experiments, all the gas phase products from ethyl chloride are produced in a reaction-limited, high temperature desorption feature attributed to a rate limiting β-hydride elimination from surface ethyl fragments. Similar product desorption features are observed for the reaction of ethyl iodide. However, the reaction of ethyl iodide also produces ethylene and ethane via a low temperature, desorption-limited reaction channel. It is postulated that I adatoms produced in the reaction of ethyl iodide thermal desorption might somehow promote a low temperature route to products that Cl adatoms do not. / Master of Science
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Automated radiosynthesis of 2-['1'1C]thymidine and ['1'1C]methyl halides for use in Positron Emission TomographySteel, Colin James January 2000 (has links)
No description available.
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Trace chemical analysis and molecular dynamics utilising ultraintense femtosecond lasersGraham, Paul January 2000 (has links)
No description available.
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Electronic Structure and Stability of Ligated Superatoms and Bimetallic ClustersBlades, William H 01 January 2016 (has links)
Quantum confinement in small metal clusters leads to a bunching of states into electronic shells reminiscent of shells in atoms. The addition of ligands can tune the valence electron count and electron distribution in metal clusters. A combined experimental and theoretical study of the reactivity of methanol with AlnIm− clusters reveals that ligands can enhance the stability of clusters. In some cases the electronegative ligand may perturb the charge density of the metallic core generating active sites that can lead to the etching of the cluster. Also, an investigation is conducted to understand how the bonding scheme of a magnetic dopant evolves as the electronic structure of the host material is varied. By considering VCun+, VAgn+, and VAun+ clusters, we find that the electronic and atomic structure of the cluster plays a major role in determining how an impurity will couple to its surroundings.
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Hipotireoidismo congênito: rastreamento e identificação de mutações no gene TPO em pacientes com defeito parcial ou total de incorporação de iodeto / Screening and identification of TPO gene mutations in patients with partial or total iodide organification defectNeves, Solange Caires 06 February 2009 (has links)
Introdução: O hipotireoidismo congênito é a causa mais frequente de retardo mental evitável, cuja prevalência é de 1/3000 crianças nascidas vivas. Pode ser causado por disgenesia tireoideana (80% dos casos) ou por defeitos de síntese hormonal (20% restantes). As disormonogêneses tem sido associadas a mutações nos genes da tireoperoxidase (TPO), tireoglobulina, dual oxidase 2, pendrina, desalogenase e do simportador sódio/iodo. A tireoperoxidase (TPO) é uma glicoproteína de 105 KDa, localizada na membrana apical do tireócito, responsável pela organificação do iodeto. Até o momento 54 mutações, associadas ao hipotireoidismo congênito foram identificadas no gene TPO. Objetivos: Este estudo visou rastrear mutações no gene TPO em pacientes com hipotireoidismo congênito, com defeito total ou parcial de incorporação de iodeto, e associar o defeito genético com o fenótipo do paciente. Casuística e Métodos: Foram estudados 34 pacientes com hipotireoidismo congênito, 13 com DIIT (descarga de iodeto >50%) e 21 com DIIP (descarga de iodeto entre 25 e 50%) por possível defeito no gene TPO. Os métodos empregados foram: extração do DNA genômico de sangue periférico, amplificação por PCR do promotor e dos 17 exons do gene TPO e dos 33 exons do gene DUOX2 , eletroforese em gel de gradiente denaturante (DGGE) e seqüenciamento. Resultados: Foram identificadas 8 novas alterações de seqüências que levam a troca de aminoácidos: Leu68Ile, Gly319Glu, Ala426Gly, Arg584Gln, Val618Met, Pro883Leu, Ala909Thr, A909fsX49; e 4 já descritas na literatura: 396fsX76, Gln660Gly, Arg665Trp, Cys838Ser. Dois pacientes com DTII apresentaram mutações em homozigose, e dois pacientes (um com DTII e um com DPII) eram portadores de alterações em heterozigose composta. Seis pacientes eram portadores de um único alelo da TPO afetado (três com DPII e três com DTII). Foram identificados também 33 polimorfismos (10 novos). Apenas polimorfismos foram identifiados no gene DUOX2. Conclusão: Foi verificada alta freqüência de mutações monoalélicas em pacientes com DIIT e DIIP. Em ambos os grupos as mutações se localizaram ao longo de todo o gene, tanto no domínio extracelular como no intracelular da proteína. Somente duas mutações foram identificadas em mais de um paciente, mostrando a heterogeneidade genotípica da doença nesta população / I ntroduction: Congenital Hypothyroidism affects 1/3000 birth, is caused by thyroid gland dysgenesis (80%) or inborn errors of the thyroid hormone biosynthesis (20%). Genetics defects of the genes for thyroid peroxidase, (TPO), thyroglobulin, sodium/iodine simporter, dual oxidase 2, and pendrine have been associated to dyshormonogenesis. TPO is a glycoprotein of 105 KDa situated in the apical membrane of the thyroid cell, responsible for iodide organification. At least 54 mutations have been identified in patients with dyshormonogenesis. Objectives: The aim of the study was to identify TPO gene mutations in patients with congenital hypothyroidism with total (DIIT) and partial (DIIP) iodide organification defects and to associate the genetic defect with the phenotype of the patient. Patients and Methods: Thirty four patients with congenital hypothyroidism, 13 with DIIT (iodide discharge >50%) and 21 patients with DIIP (iodide discharge between 25- 50%) due to possible TPO gene defect. Extraction of genomic DNA from peripheral blood, PCR amplification of the promoter, 17 exons of TPO gene and of the 33 exons of DUOX2 gene, denaturant gradient gel electrophoreses (DGGE) and sequencement were performed. Results: Eight new sequence alterations were identified: Leu68Ile, Gly319Glu, Ala426Gly, Arg584Gln, Val618Met, Pro883Leu, Ala909Thr, A909fsX49; and four previously described mutations: 396fsX76, Gln660Gly, Arg665Trp, Cys838Ser. Homozygous mutations were identified in two patients with DTII. Ttwo patients (one with DTII and one with DPII) were carrying compound heterozygous mutations. TPO monoallelic mutations were identified in six patients (3 with DPII and 3 with DTII). Thirty three polymorphisms had also been identified (10 news). Conclusion: High frequency of TPO monoallelic mutations was detected in patients with DIIT and DIIP. In both groups of patients the mutations were located all throughout the gene, in the extracellular as well as in the intracellular domain. Only two mutations have been identified in more than one patient, indicating the genotypic heterogeneity of the illness in this population
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Análise microscópica e histométrica comparativa da aplicação de uma pasta à base de metronidazol e da irrigação com iodeto de sódio e peróxido de hidrogênio para o tratamento de alvéolos dentários infectados de ratos / Microscopic and histometric comparative analysis of a metronidazole ointment application and sodium iodide plus hydrogen peroxide irrigation in the treatment of infected tooth sockets of ratsRodrigues, Moacyr Tadeu Vicente 06 July 2007 (has links)
O processo de reparo em alvéolo infectado de ratos foi avaliado após a utilização de três tipos de tratamento: (1) curetagem e irrigação com soro fisiológico seguida do preenchimento com uma pasta à base de metronidazol a 10%, lidocaína a 2%, menta e carboximetilcelulose, (2) irrigação única com solução de iodeto de sódio a 2% e peróxido de hidrogênio a 3% na proporção 1:1 e (3) irrigação diária, por 3 dias, com solução de iodeto sódio a 2% e peróxido de hidrogênio a 3% na proporção 1:1. Foram utilizados 75 ratos que constituíram os seguintes grupos: Grupo I: alvéolo não infectado (grupo controle positivo); Grupo II: alvéolo infectado sem nenhum tratamento; Grupo III: alvéolo infectado tratado com irrigação única de solução de iodeto de sódio a 2 % e peróxido de hidrogênio a 3% na proporção 1:1; Grupo IV: alvéolo infectado tratado com irrigação diária, por 3 dias, de solução de iodeto de sódio a 2 % e peróxido de hidrogênio a 3% na proporção 1:1; Grupo V: alvéolo infectado submetido à curetagem, irrigação com soro fisiológico e preenchimento com pasta à base de metronidazol a 10% e lidocaína a 2%, carboximetilcelulose e menta. Os animais, em número de 5 em cada grupo foram sacrificados aos 6, 15 e 28 dias após a exodontia do incisivo superior e as peças obtidas analisadas em microscopia óptica. Os resultados foram submetidos à análise qualitativa e quantitativa e evidenciaram melhor reparo nos grupos tratados em relação ao grupo sem tratamento. Com base nos resultados foi possível concluir que: os grupos III, IV e V apresentaram melhores condições de reparo frente ao grupo II, porém diferentes significantemente ao grupo I; o grupo V apresentou os melhores resultados quanto à neoformação óssea nos períodos de 15 e 28 dias, sendo uma opção interessante a ser considerada para o tratamento da alveolite. / The healing process in infected tooth sockets was evaluated after application of three types of treatment.: (1) surgical cleaning of the socket with alveolar curettes, saline solution irrigation and complete filling of the socket with a 10% metronidazole, 2% lidocaine, carboxymethylcelullose and mint as flavoring, (2) Single irrigation with 2% sodium iodide and 3% hydrogen peroxide solution (1:1) and (3) Daily irrigation, for three days, with 2% sodium iodide and 3% hydrogen peroxide solution (1:1). Seventy-five rats were randomly assigned to the following groups: Group I: Non-infected tooth socket (positive control group); Group II: Infected tooth socket without treatment; Group III: Infected tooth socket treated with single irrigation of 2% sodium iodide and 3% hydrogen peroxide solution (1:1); Group IV: Infected tooth socket treated daily, for three days, with irrigation of 2% sodium iodide and 3% hydrogen peroxide solution (1:1); Group V: Infected tooth socket treated with surgical cleaning of the socket with alveolar curettes, saline solution irrigation and complete filling of the socket with a 10% metronidazole, 2% lidocaine, carboxymethylcelullose and mint as flavoring. The rats were killed in number of five at each group after 6, 15 e 28 days of superior incisor extraction. The histological findings were measured by qualitative and quantitative methods. The results demostrated better results of tooth socket healing in treated groups. Based on the results it was possible to conclude that groups III, IV and V exhibited better conditions of alveolar healing, compared to group II, although significant difference was observed with group I. Group V showed the best results in bone formation at 15 and 28 days, consisting in an interesting option for dry socket treatment.
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Filmes finos de iodeto de chumbo (PbI2)produzidos por spray pyrolysis / Thin films of lead iodide (PbI2) produced by spray pyrolysisCondeles, José Fernando 31 October 2003 (has links)
Pesquisadores em todo o mundo buscam métodos alternativos que minimizem o tempo de deposição de filmes finos semicondutores cotados como promissores candidatos em aplicações médicas como detectores de raios-X em radiografias digitais. O iodeto de chumbo (PbI2) é considerado, entre outros, como um bom candidato para a fabricação de detectores usados à temperatura ambiente. Outros pesquisadores fabricaram protótipos de detectores usando esse material. Seus experimentos mostraram alta resolução e sensibilidade para imagens em tempo real, mostrando que o material possui potencialidade para aplicações médicas futuramente. Não obstante, uma das desvantagens de seus métodos é o longo tempo necessário para a deposição na fabricação de filmes finos. Este trabalho apresenta uma nova metodologia usada para a deposição de filmes finos de iodeto de chumbo (PbI2). O método alternativo de crescimento dos filmes é chamado de spray pyrolysis. A técnica possui uma vantagem intrínseca pelo fato de a deposição ser facilmente expandida para grandes áreas de substrato que é desejado nas linhas de produção industrial. O pó de iodeto de chumbo foi dissolvido em água deionizada a 100ºC (água em ebulição) onde a solubilidade é maior que à temperatura ambiente. Após a dissolução do pó, a solução foi resfriada até a temperatura ambiente e filtrada para a remoção do excesso de cristais formados. Os filmes foram depositados a partir de solução aquosa sobre substrato de vidro em diferentes temperaturas (de 150 a 270ºC). O tempo total de deposição foi de 2,5 horas levando a uma espessura de . Em adição foram investigadas as propriedades estruturais (Difração de raios-X e espalhamento Raman), eletrônicas (condutividade elétrica no escuro em função da temperatura) e da superfície (por AFM) obtidas com os filmes produzidos. Com o intuito de aumentar o tamanho dos grãos cristalinos após a deposição dos filmes, as amostras originais foram submetidas a tratamento térmico a 350ºC durante 3 horas em atmosfera ambiente e posteriormente em atmosfera controlada (N2). No primeiro caso foi observada a influência do oxigênio com dopante da amostra. Foram analisadas as dimensões dos grãos cristalinos (relativo ao pico principal 001) para diferentes temperaturas de deposição e de tratamento térmico, bem como a energia de ativação no transporte elétrico. Obteve-se um valor de energia de ativação de aproximadamente 0,50 eV para filmes depositados a 200ºC. Para outras temperaturas de deposição entre 150 e 250ºC foi obtido um mínimo e máximo de energia de ativação de 0,45 e 0,66 eV, respectivamente. Em resumo, as propriedades estruturais e eletrônicas são discutidas e relacionadas com o método de deposição e tratamento térmico. Acreditamos que filmes finos com interessantes propriedades estruturais e eletrônicas podem ser produzidos por spray pyrolysis com baixo tempo de deposição. / Researchers in the whole world search alternative methods that minimize the time of deposition of thin films of promising semiconductor candidates for medical applications, such as X-rays detectors for digital radiography. Lead iodide (PbI2) has been among those as a good candidate for the fabrication of room temperature detectors. Other authors have fabricated prototype detectors using this material. Their experiments show high resolution and sensitivity for real time imaging, thus showing the material potentiality for medical applications in the future. Nevertheless, one of the drawbacks of their methods is the long deposition time needed for the fabrication of the thin films. In this work we present a new experimental methodology used for the deposition of thin films of lead iodide (PbI2). The alternative growth method is called spray pyrolysis. Note that an intrinsic advantage of the technique is the fact that it can be easily expanded for large area substrates as desired by the industrial fabrication line. Lead iodide powder was dissolved in deionized water at 100ºC (boiling water) where its solubility is higher than at room temperature. After the dissolution of the powder, the solution is cooled down to ambient temperature and filtered for the removal of the excess of formed crystals. The films were deposited from aqueous solutions on glass substrates sitting at different temperatures (from 150 to 270ºC). The total deposition time is about 2.5 hours leading to a film thickness of . In addition we also investigate the structural (X-ray diffraction and Raman scattering), electronic (dark conductivity as a function of temperature) and atomic force microscopy (AFM) properties of the obtained films. In order to induce crystalline grain growth after the deposition of the films, the original samples were also submitted to thermal treatment at 350ºC during 3 hours either in ambient or under controlled atmosphere (N2). The influence of oxygen doping was only observed in the first case. We analyze the variation of the size of the crystals (relative to the main peak - 001) and the activation energies for electric transport. The activation energy for films deposited at 200ºC is about 0.50 eV. For other deposition temperatures, varying from 150 to 250ºC, it was experimentally measured a minimum and maximum value of activation energy of 0.45 and 0.66 eV, respectively. In summary, the electronic and structural properties are correlated and discussed based on the deposition method, and thermal treatments. It is the present authors belief that thin films with interesting structural and electronic properties can be produced by spray pyrolysis with short deposition time.
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