Thermal control in spacecraft will be increasingly important as the spacecraft grows smaller and more compact. Such spacecraft with low thermal mass will have to be designed to retain or reject heat more efficiently. The passive smart radiation device (SRD) is a new type of thermal control material for spacecraft. Current space thermal control systems require heaters with an additional power penalty to maintain spacecraft temperatures during cold swings. Because its emissivity can be changed without electrical instruments or mechanical part, the use of SRD decreases the request of spacecraft power budget. The (SRD) based on VO2 films is one of the most important structures of the functional thermal control surface, being lighter, more advanced and without a moving devices. A large portion of the heat exchange between an object in space and the environment is performed throughout radiation, which is in turn determined by the object surface properties. The modulation device is coated on the spacecraft surface and thus provides a thermal window that can adapt to the changing conditions in orbit. VO2 is well known to have a temperature driven metal to insulator transition ≈ 68ᴼC accompanying a transformation of crystallographic structure, from monoclinic (M-phase, semiconductor) at temperature below 68ᴼC to tetragonal (R-phase, metal) at temperature above 68ᴼC. This transition temperature is accompanied by an increase of infrared reflectivity and a decrease of infrared emissivity with increasing temperature. This flexibility makes VO2 potentially interesting for optical, electrical, and electro-optical switches devices, and as window for energy efficiency buildings applications. This study reports on effect of thickness on VO2 as well as the effect of proton irradiation on VO2 for active smart radiation device (SRD) application. VO2 was deposited on mica by Pulsed laser deposition techniques. The thickness of the film was varied by varying the deposition time. To characterize VO2 the following techniques were performed: XRD, AFM, SEM, TEM, XPS, RBS, RAMAN and transport measurements for optical properties. The effect of proton irradiation was observed using the SEM, where the change in structure, from crystal grains to rods, was observed. / Physics / M.Sc. (Physics)

O objetivo principal deste trabalho é o estudo de transistores MuGFETs de porta tripla de Corpo de canal tipo-n com e sem a aplicação da configuração DTMOS. Este estudo será realizado através de simulações numéricas tridimensionais e por caracterizações elétricas. A corrente de dreno, a transcondutância, a resistência, a tensão de limiar, a inclinação de sublimiar e a Redução da Barreira Induzida pelo Dreno (DIBL) serão analisadas em modo DTMOS e em configuração de polarização convencional. Importantes figuras de mérito para o desempenho analógico como transcondutância-sobre-corrente de dreno, a condutância de saída, a tensão Early e o ganho de tensão intrínseco serão estudados tanto experimentalmente como através de simulações numéricas tridimensionais para diferentes concentrações de dopantes no canal. Os resultados indicam que a configuração DTMOS apresenta as características elétricas superiores (4 e 10 %) e maior eficiência dos transistores. Além disso, os dispositivos DTMOS com alta concentração de dopantes no canal apresentaram um desempenho analógico muito melhor quando comparados ao transistor de porta tripla de Corpo em modo de operação convencional. O ruído de baixa frequência (LF) é pela primeira vez experimentalmente analisado na região linear e saturação. A origem do ruído é analisada de maneira a compreender os mecanismos físicos envolvidos neste tipo de ruído. As medições mostraram que os espectros do sinal dos dispositivos de porta tripla de Corpo e DTMOS são compostos por flutuações referentes ao número de portadores devido ao ruído flicker e por ondas de ruído de geração e recombinação no dielétrico de porta que se torna maior com o aumento da tensão de porta. No entanto, o principal fato desta análise é que o dispositivo DTMOS apresentou praticamente a mesma magnitude do ruído LF na região linear e de saturação que o dispositivo de Corpo. A energia de 60 MeV na fluência de p/1012 cm-2 de radiações de prótons é também estudada experimentalmente em termos das características elétricas, desempenho do analógico e ruído LF nos dispositivos de porta tripla de Corpo e DTMOS. Os resultados indicam que combinado com as suas melhores características elétricas e um ótimo desempenho analógico do DTMOS, faz o transistor de porta tripla de Corpo um candidato muito competitivo para aplicações analógicas em ruído de baixa frequência antes e depois da irradiação. A vantagem da técnica DTMOS em transistores de porta tripla em ambientes onde os dispositivos têm de suportar alta radiação é devido à menor penetração do campo de dreno que reduz o efeito das cargas induzidas pelo óxido de isolação (STI). Finalmente, o transistor de Corpo de porta tripla de canal tipo-n é experimentalmente estudado como célula de memória, isto é, como 1T-DRAM (Memória de Acesso Aleatório Dinâmico com 1 transistor). Para escrever e ler 1 é utilizado um modo de programação que utiliza o efeito do transistor bipolar parasitário (BJT) enquanto a polarização direta da junção do corpo e do dreno é usada para escrever 0. As correntes de leitura e escrita aumentam com o aumento da tensão do corpo (VB) porque as cargas induzidas pelo efeito BJT é armazenada dentro da aleta. Quando o corpo do transistor está flutuante, o dispositivo retém mais cargas dentro da sua aleta. Além disso, transistor de Corpo pode ser utilizado como 1T-DRAM com eletrodo de porta e substrato flutuando. Neste caso, o dispositivo funciona como um biristor (sem porta). / The main goal of this work is to investigate the n-channel MuGFETs (triple-gate) Bulk transistors with and without the application of DTMOS operation. This work will be done through three-dimensional numerical simulation and by electrical characterizations. The drain current, transconductance, resistance, threshold voltage, subthreshold swing and Drain Induced Barrier Lowering (DIBL) will be analyzed in the DTMOS mode and the standard biasing configuration. Important figures of merit for the analog performance such as transconductance-over-drain current, output conductance, Early voltage and intrinsic voltage gain will be studied experimentally and through three-dimensional numerical simulations for different channel doping concentrations. The results indicate that the DTMOS configuration has superior electrical characteristics (4 e 10 %) and higher transistor efficiency. In addition, DTMOS devices with a high channel doping concentration exhibit much better analog performance compared to the normal operation mode. Low-Frequency (LF) noise is for the first time experimentally investigated in linear and saturation region. The origin of the noise will be analyzed in order to understand the physical mechanisms involved in this type of noise. Measurements showed that the signal spectra for Bulk and DTMOS are composed of number fluctuations related flicker noise with on top generation and recombination noise humps, which become more pronounced at higher gate voltage. However, the most important finding is the fact that DTMOS devices showed practically the same LF noise magnitude in linear and saturation region than standard Bulk device. Proton irradiation with energy of 60 MeV and fluence of p/1012 cm-2 is also experimentally studied in terms of electric characteristic, analog performance and the LF noise in Bulk and DTMOS triple gate devices. The results indicate that the combined of the better electrical characteristics and an excellent analog performance of DTMOS devices, makes it a very competitive candidate for low-noise RF analog applications before and after irradiation. The advantage of dynamic threshold voltage in triple gate transistors in environments where the devices have to withstand high-energy radiation is due to its lower drain electric field penetration that lowers the effect of the radiation-induced charges in the STI (shallow trench isolation) regions adjacent to the fin. Finally, the n-channel triple gate Bulk device is used for memory application, that is, 1T-DRAM (Dynamic Random Access Memory with 1 Transistor). Bipolar junction transistor (BJT) programming mode is used to write and read 1 while the forward biasing of the body-drain junction is used to write 0. The reading and writing current increases with increasing body bias (VB) because the load induced by the BJT effect is stored within the fin. When the body of the transistor is floating, the device retains more charge within its fin. In addition, transistor could also operate as 1T-DRAM with both gate and bulk contacts floating, which is similar to the biristor (gateless) behavior.

<p>Bonding techniques intended for assembling space microsystems are studied in this work. One of the largest problems in bonding pre-processed semiconductor wafers are the severe process restrictions imposed by material compatibility issues. Plasma processes have shown to be good for sensitive materials integration why the influence of different plasma parameters on the bondability of wafers is particularly studied. Conventional wet chemical and field-assisted methods are also examined. The resulting bond quality is assessed in terms of mechanical strength, homogeneity, and yield.</p><p>The effect of spaceflight environment on the reliability of wafer bonds is also investigated. Both high and low temperature annealed bonds are found to be very robust. Effects observed are that low temperature bonds are reinforced by thermal cycling in vacuum and that high temperature bonds degrade slightly by low dose γ irradiation.</p><p>Adhesion quantification is important for all bonding. Development of accurate quantification methods is considered necessary since most methods at hand are limited. This work includes the development of the blister test method. Former test structures are improved to be more practical to work with and to yield low experimental scatter. A physical stress model for the improved structure is suggested with which successful predictions of fracture for different test specimen configurations are made. The blister test method is used throughout this work to assess the strength of wafer bonds. The physics background and modelling of other common test methods are also thoroughly analysed. The methods’ practical capabilities and limitations are commented; origin and mitigation of measurement errors are discussed. It is shown that all methods can be significantly improved by small means.</p><p>Weibull statistics is introduced as a tool to characterise wafer bonds. This method is suitable to use in brittle materials design as the inherent variability in strength can be properly accounted for.</p>

Bonding techniques intended for assembling space microsystems are studied in this work. One of the largest problems in bonding pre-processed semiconductor wafers are the severe process restrictions imposed by material compatibility issues. Plasma processes have shown to be good for sensitive materials integration why the influence of different plasma parameters on the bondability of wafers is particularly studied. Conventional wet chemical and field-assisted methods are also examined. The resulting bond quality is assessed in terms of mechanical strength, homogeneity, and yield. The effect of spaceflight environment on the reliability of wafer bonds is also investigated. Both high and low temperature annealed bonds are found to be very robust. Effects observed are that low temperature bonds are reinforced by thermal cycling in vacuum and that high temperature bonds degrade slightly by low dose γ irradiation. Adhesion quantification is important for all bonding. Development of accurate quantification methods is considered necessary since most methods at hand are limited. This work includes the development of the blister test method. Former test structures are improved to be more practical to work with and to yield low experimental scatter. A physical stress model for the improved structure is suggested with which successful predictions of fracture for different test specimen configurations are made. The blister test method is used throughout this work to assess the strength of wafer bonds. The physics background and modelling of other common test methods are also thoroughly analysed. The methods’ practical capabilities and limitations are commented; origin and mitigation of measurement errors are discussed. It is shown that all methods can be significantly improved by small means. Weibull statistics is introduced as a tool to characterise wafer bonds. This method is suitable to use in brittle materials design as the inherent variability in strength can be properly accounted for.

O objetivo principal deste trabalho é o estudo de transistores MuGFETs de porta tripla de Corpo de canal tipo-n com e sem a aplicação da configuração DTMOS. Este estudo será realizado através de simulações numéricas tridimensionais e por caracterizações elétricas. A corrente de dreno, a transcondutância, a resistência, a tensão de limiar, a inclinação de sublimiar e a Redução da Barreira Induzida pelo Dreno (DIBL) serão analisadas em modo DTMOS e em configuração de polarização convencional. Importantes figuras de mérito para o desempenho analógico como transcondutância-sobre-corrente de dreno, a condutância de saída, a tensão Early e o ganho de tensão intrínseco serão estudados tanto experimentalmente como através de simulações numéricas tridimensionais para diferentes concentrações de dopantes no canal. Os resultados indicam que a configuração DTMOS apresenta as características elétricas superiores (4 e 10 %) e maior eficiência dos transistores. Além disso, os dispositivos DTMOS com alta concentração de dopantes no canal apresentaram um desempenho analógico muito melhor quando comparados ao transistor de porta tripla de Corpo em modo de operação convencional. O ruído de baixa frequência (LF) é pela primeira vez experimentalmente analisado na região linear e saturação. A origem do ruído é analisada de maneira a compreender os mecanismos físicos envolvidos neste tipo de ruído. As medições mostraram que os espectros do sinal dos dispositivos de porta tripla de Corpo e DTMOS são compostos por flutuações referentes ao número de portadores devido ao ruído flicker e por ondas de ruído de geração e recombinação no dielétrico de porta que se torna maior com o aumento da tensão de porta. No entanto, o principal fato desta análise é que o dispositivo DTMOS apresentou praticamente a mesma magnitude do ruído LF na região linear e de saturação que o dispositivo de Corpo. A energia de 60 MeV na fluência de p/1012 cm-2 de radiações de prótons é também estudada experimentalmente em termos das características elétricas, desempenho do analógico e ruído LF nos dispositivos de porta tripla de Corpo e DTMOS. Os resultados indicam que combinado com as suas melhores características elétricas e um ótimo desempenho analógico do DTMOS, faz o transistor de porta tripla de Corpo um candidato muito competitivo para aplicações analógicas em ruído de baixa frequência antes e depois da irradiação. A vantagem da técnica DTMOS em transistores de porta tripla em ambientes onde os dispositivos têm de suportar alta radiação é devido à menor penetração do campo de dreno que reduz o efeito das cargas induzidas pelo óxido de isolação (STI). Finalmente, o transistor de Corpo de porta tripla de canal tipo-n é experimentalmente estudado como célula de memória, isto é, como 1T-DRAM (Memória de Acesso Aleatório Dinâmico com 1 transistor). Para escrever e ler 1 é utilizado um modo de programação que utiliza o efeito do transistor bipolar parasitário (BJT) enquanto a polarização direta da junção do corpo e do dreno é usada para escrever 0. As correntes de leitura e escrita aumentam com o aumento da tensão do corpo (VB) porque as cargas induzidas pelo efeito BJT é armazenada dentro da aleta. Quando o corpo do transistor está flutuante, o dispositivo retém mais cargas dentro da sua aleta. Além disso, transistor de Corpo pode ser utilizado como 1T-DRAM com eletrodo de porta e substrato flutuando. Neste caso, o dispositivo funciona como um biristor (sem porta). / The main goal of this work is to investigate the n-channel MuGFETs (triple-gate) Bulk transistors with and without the application of DTMOS operation. This work will be done through three-dimensional numerical simulation and by electrical characterizations. The drain current, transconductance, resistance, threshold voltage, subthreshold swing and Drain Induced Barrier Lowering (DIBL) will be analyzed in the DTMOS mode and the standard biasing configuration. Important figures of merit for the analog performance such as transconductance-over-drain current, output conductance, Early voltage and intrinsic voltage gain will be studied experimentally and through three-dimensional numerical simulations for different channel doping concentrations. The results indicate that the DTMOS configuration has superior electrical characteristics (4 e 10 %) and higher transistor efficiency. In addition, DTMOS devices with a high channel doping concentration exhibit much better analog performance compared to the normal operation mode. Low-Frequency (LF) noise is for the first time experimentally investigated in linear and saturation region. The origin of the noise will be analyzed in order to understand the physical mechanisms involved in this type of noise. Measurements showed that the signal spectra for Bulk and DTMOS are composed of number fluctuations related flicker noise with on top generation and recombination noise humps, which become more pronounced at higher gate voltage. However, the most important finding is the fact that DTMOS devices showed practically the same LF noise magnitude in linear and saturation region than standard Bulk device. Proton irradiation with energy of 60 MeV and fluence of p/1012 cm-2 is also experimentally studied in terms of electric characteristic, analog performance and the LF noise in Bulk and DTMOS triple gate devices. The results indicate that the combined of the better electrical characteristics and an excellent analog performance of DTMOS devices, makes it a very competitive candidate for low-noise RF analog applications before and after irradiation. The advantage of dynamic threshold voltage in triple gate transistors in environments where the devices have to withstand high-energy radiation is due to its lower drain electric field penetration that lowers the effect of the radiation-induced charges in the STI (shallow trench isolation) regions adjacent to the fin. Finally, the n-channel triple gate Bulk device is used for memory application, that is, 1T-DRAM (Dynamic Random Access Memory with 1 Transistor). Bipolar junction transistor (BJT) programming mode is used to write and read 1 while the forward biasing of the body-drain junction is used to write 0. The reading and writing current increases with increasing body bias (VB) because the load induced by the BJT effect is stored within the fin. When the body of the transistor is floating, the device retains more charge within its fin. In addition, transistor could also operate as 1T-DRAM with both gate and bulk contacts floating, which is similar to the biristor (gateless) behavior.

Die Arbeit befasst sich mit der Untersuchung von weitbandlückigen Halbleitern über raumladungszonenspektroskopische Methoden. Dabei liegt der Schwerpunkt auf der Detektion von elektronisch und optisch aktiven Defektzuständen in solchen Materialien. Die Experimente wurden exemplarisch an dem II-VI Halbleiter Zinkoxid (ZnO) durchgeführt, welcher inform von Volumenkristallen, Mikronadeln und Dünnfilmen zur Verfügung stand. Raumladungszonen wurden über Schottky-Kontakte realisiert. Nach einer Einführung in die Theorie der Raumladungszonenspektroskopie wird ein Überblick über Defekte in verschiedenartig gezüchteten ZnO gegeben. Dazu werden die Standardverfahren Strom-Spannungs-Messung, Kapazitäts-Spannungs-Messung, Thermische Admittanz- Spektroskopie (TAS) und Deep Level Transient Spectroscopy (DLTS) verwendet. Ergänzend wurden die auf weitbandlückige Halbleiter ausgelegten Verfahren Low Rate Deep Level Transient Spectroscopy (LR-DLTS) und Deep Level Optical Spectroscopy (DLOS) eingesetzt, mit welchen es möglich ist Defektzustände in der gesamten Bandlücke von ZnO nachzuweisen. Für die untersuchten Störstellenniveaus konnten somit die thermische Aktivierungsenergie, Einfangquerschnitte freier Ladungsträger und Photoionisationsquerschnitte bestimmt werden. Typischerweise werden tiefe Defekte durch die Bestrahlung mit hochenergetischen Protonen erzeugt. Derartige Behandlungen wurden an binären ZnO- und ternären (Mg,Zn)ODünnfilmen durchgeführt, wobei die Generationsrate eines Defektes über Variation der verwendeten Strahlungsdosis bestimmt wurde. Ionenimplantationen spielen eine große Rolle im Herstellungsprozess von Bauelementen, sind jedoch für ZnO nicht etabliert. Die Auswirkung der Implantation von inerten Argon-Ionen, sowie die nachträgliche thermische Behandlung auf die Konzentration intrinsischer Defekte wurde untersucht. Zink- und Sauerstoff-Implantationen bewirken, neben der Generation von Defekten, eine lokale Änderung der Stöchiometrie. Durch einen Vergleich der Defektkonzentrationen nach Zn-, O-, Ne- und Ar-Implantation können Rückschlüsse auf die chemische Natur intrinsischer Defekte geschlossen werden.:1 Einleitung I Grundlagen 2 Elektronische Eigenschaften von Defekten in Halbleitern 2.1 Typen und Klassifizierung von Defekten 2.2 Lokalisierte Zustände in Halbleitern 2.2.1 Donatoren und Akzeptoren 2.2.2 Flache Defekte und effektive Masse-Näherung 2.2.3 Tiefe Defekte 2.3 Besetzungsstatistik und Ratengleichungen 2.3.1 Thermische Emission 2.3.2 Optische Emission 2.3.3 Nichtstrahlender Einfang und Multiphononen Emission 2.3.4 Arrhenius Auswertung 2.3.5 Zeitentwicklung des Besetzungsgrades 3 Raumladungszonenspektroskopie 3.1 Metall-Halbleiter-Kontakte 3.2 Kapazitätstransienten 3.3 Kapazitäts-Spannungs-Messungen (C(U)) 3.4 Thermische Admittanz Spektroskopie (TAS) 3.5 Deep level transient spectroscopy (DLTS) 3.6 Konzentrationsbestimmung 3.7 Laplace-Deep level transient spectroscopy (LDLTS) 3.7.1 Entstehung des LDLTS-Signals 3.7.2 Einschränkungen der Methode 3.8 Deep level optical spectroscopy (DLOS) 4 Die Halbleiter ZnO und MgZnO 4.1 Kristallstruktur und Gitterparameter 4.2 Bandstruktur 4.3 ZnO als transparentes leitendes Oxid 4.4 Defekte in ZnO 5 Probenherstellung und Charakterisierung 5.1 ZnO-Züchtung 5.1.1 ZnO-Volumenkristalle 5.1.2 ZnO-Dünnfilme 5.2 Kathodenzerstäubung 5.3 Protonenbestrahlung und Ionenimplantation 5.3.1 Bremsquerschnitt 5.3.2 Protonenbestrahlung 5.3.3 Ionenimplantation 5.4 Probenaufbau und Schottky-Kontakte 5.5 Raumladungszonenspektroskopie-Messplatz 5.6 Rasterkraftmikroskopie 5.7 Kelvinsondenkraftmikroskopie 5.8 Röntgendiffraktometrie 5.9 Photolumineszenzspektroskopie II Charakterisierung züchtungsinduzierter Defekte 6 Defekte in ZnO-Volumenkristallen und -Dünnfilmen 6.1 Elektrische Eigenschaften 6.2 Thermische Admittanz-Spektroskopie 6.3 Deep-level transient spectroscopy 6.4 E3 und E3’ in ZnO Dünnfilmen 6.4.1 Low Rate – DLTS 6.4.2 Laplace-DLTS 6.4.3 thermisch aktivierter Einfang von E3’ 6.5 Einfluss thermischer Nachbehandlung 6.6 Einfluss der Züchtungstemperatur 6.7 Die Meyer-Neldel Regel 6.8 E7, TH1 und T4 in ZnO – DLOS 6.8.1 Raumtemperatur DLOS des ZnO-Volumenkristall 6.8.2 Raumtemperatur DLOS des ZnO-Dünnfilm 6.8.3 DLOS-Messungen bei tiefen Temperaturen 6.9 Optische Anregung von E3’ in ZnO-Dünnfilmen 7 Defekte in (Mg,Zn)O-Dünnfilmen 7.1 (Mg,Zn)O-Dünnfilme auf a-Saphir 7.2 Photolumineszenz 7.3 XRD 7.4 DLTS-Untersuchungen 7.5 E3 in verspannten (Mg,Zn)O-Filmen 7.6 DLOS – T4 und TH1 in (Mg,Zn)O-Dünnfilmen 7.7 Zusammenfassung 8 Einfluss der Wachtumsorientierung auf die Defektstruktur von ZnO-Dünnfilmen 8.1 ZnO-Dünnfilme auf a-, m- und r-Saphir 8.2 Strukturelle Eigenschaften 8.3 Photolumineszenz 8.4 Elektrische Eigenschaften 8.5 Defektsignaturen III Charakterisierung strahlungsinduzierter Defekte 9 Protonenbestrahlung an (Mg,Zn)O-Dünnfilmen 9.1 Der E4-Defekt in ZnO – Stand der Literatur 9.2 E4 in polaren (Mg,Zn)O-Dünnfilmen 9.2.1 Probenaufbau und Protonenbestrahlung 9.2.2 Elektrische Eigenschaften 9.2.3 DLTS-Untersuchungen 9.3 E4 in unpolaren ZnO-Dünnfilmen 9.4 Zusammenfassung 10 Defekte in Argon-implantierten ZnO-Dünnfilmen 10.1 Probenstruktur und Ionenimplantation 10.2 Thermische DLTS 10.3 DLTS mit monochromatischer Anregung 11 Defekte in Zn- und O-implantierten ZnO-Dünnfilmen 11.1 Proben und Ionenimplantation 11.2 Nettodotierkonzentration 11.3 Thermische DLTS 11.4 DLOS 11.5 Defekte mit geringen Konzentrationen – E470 und E390 12 Zusammenfassung und Ausblick

This thesis was most concerned with the mechanical response to irradiation of two in-house produced oxide dispersion strengthened (ODS) steels and two non-ODS coun- terparts. The steels, manufactured by Dr. M. J. Gorley (University of Oxford), were me- chanically alloyed from gas-atomised Fe-14Cr-3W-0.2Ti, with the addition of 0.25Y₂O₃ powder in the case of the ODS variants. The powders were hot isostatic pressed at consolidation temperatures of 950 &deg;C and 1150 &deg;C. The four steels were designated 14WT 950 (non-ODS), 14YWT 950 (ODS), 14WT 1150 (non-ODS) and 14YWT 1150 (ODS), and were used in the as-produced condition. Initially, the macroscale elastic modulus and yield stress were determined using a four-point flexure test, employing digital image correlation (DIC) as a strain gauge. The microcantilever size eects were then characterised, and it was determined that the yield stress signicantly diverged from macroscale values at microcantilever beam depths of &LT; 4.5 &mu;m. Using knowledge of this, the in-house produced alloys were irradiated with 2 MeV protons at the Surrey Ion Beam Centre (University of Surrey, UK) to a displacement damage of &Tilde; 0.02 dpa and 0.2 dpa (Bragg peak). This was to produce a deep irradiated layer for the fabrication of large microcantilevers with reduced size effects. The cross-sectional surface of the irradiated layer was then exposed and inclined linear arrays of 250 nm deep indents were placed across the damage prole. 14WT 1150 (non-ODS) revealed a clear proton damage prole in plots of hardness against irradiation depth, 14WT 950 (non-ODS) also showed modest hardening in the region of the Bragg peak. No appreciable hardening was observed in either 14YWT specimens, attributed to the fine dispersion of nanoscale oxides providing a high number density of defect sink sites. However, a large bimodal variation in hardness was measured in both ODS variants. This was investigated using EBSD and EDX, and was determined to be caused by a pronounced heterogeneity of the microstructure. While Hall-Petch strengthening and changes in the local chemistry had some effect on the measured hardness, the most likely cause of the large variation in local hardness was heterogeneity in the nanoscale oxide population. Microcantilevers were fabricated out of the irradiated layer cross-section in 14WT 1150 and 14YWT 1150. Larger microcantilevers, with &Tilde; 5 &mu;m beam depth, were placed with their beam centre at &Tilde; 0.026 dpa. Smaller microcantilevers, with &Tilde; 1.5 &mu;m beam depth, were placed with their beam centre at the Bragg peak, 0.2 dpa. Both the large and the small microcantilevers fabricated in 14WT 1150 (non-ODS) displayed significant irradiation hardening. In the ODS variant, 14YWT 1150, irradiation hardening appeared to be reduced. The work in this thesis successfully showed that it was possible to extract a close approximation of the macroscale yield stress from shallow irradiated layers, providing that the irradiation condition is carefully chosen in response to known size dependent behaviour. This thesis also investigated the size dependent behaviour of microcantilevers using a lengthscale dependent crystal plasticity UMAT, developed by Dunne et al. and implemented within ABAQUS 6.14-2 commercially available nite element software. The simulation of the GND density evolution with increasing plastic strain allowed their contribution to the microcantilever size effect, through mobile dislocation pinning, to be determined. This novel approach to modelling size effects in three dimensional finite element microcantilever models demonstrated that while it was possible to simulate a lengthscale-dependent response in finite element microcantilever models, the constitutive equation for the plastic velocity gradient needs to be more physically based in order the match the experimentally derived results; for example, a lengthscale-dependent term relating to the dislocation source density of the material. Although the apparent reduction of irradiation hardening in ODS in-house produced alloys showed great promise, these alloys also displayed a large amount of scatter in measured hardness and yield stress, attributed to the pronounced heterogeneity in the microstructure. Alloys with such signicant microstructural heterogeneity are not suitable for engineering or commercial use.

<p>Thorium dioxide (ThO₂) and metallic uranium (alpha-U) represent important alternative nuclear fuels. Investigating the behavior of defects introduced into these materials in an irradiation environment is critical for understanding microstructure evolution and property changes. The objective of this dissertation is to investigate the clustering of point defects in ThO₂ and alpha-U under irradiation, into voids and prismatic dislocation loops as a function of irradiation dose rate and temperature. To achieve this, we have developed a mean-field cluster dynamics (CD) model based on reaction rate theory to predict the evolution of self-interstitial atom (SIA) and vacancy loops in neutron-irradiated alpha-U. Detailed atomistic simulations have been carried out using molecular dynamics (MD) to study the configuration of such loops and compute their energetics, which are essential parameters of the CD model. Bond-boost hyper-MD simulations have been performed to compute the diffusivity of uranium SIA and vacancies, which govern the kinetics of the clustering phenomenon. Another CD model has been demonstrated for proton-irradiated ThO₂, considering the clustering of Th and O SIA and vacancies into SIA loops and voids, respectively, with varying sizes and stoichiometry. The compositions of all SIA loops and voids dictated by crystallography of ThO₂ in its fluorite structure have been presented in their respective cluster composition space (CCS). The CD model solves the density evolution of off-stoichiometric loops and voids, with irradiation, in their respective CCS. MD simulations have been performed to compute the energetics of different clusters in their CCS, as parameters of the CD model. Temperature-accelerated MD simulations have been performed to compute the diffusivity of Th and O point defects, that dictates the kinetics of defect clustering on irradiation. In alpha-U, the CD predictions show an accumulation of small sized vacancy loops and the growth of SIA loops with irradiation dose, which closely fits the reported size distribution of loops in neutron-irradiated alpha-U by Hudson and coworkers. The CD predicted density of defect clusters in proton-irradiated ThO₂, shows the evolution of near-stoichiometric SIA loops in their CCS. The size distribution of SIA loops at high irradiation doses closely corresponds to the transmission electron microscopy (TEM) observations reported in the literature. Also, the CD model did not predict the growth of voids and vacancy clusters, which is consistent with findings in literature. The model was further used to predict the density of sub-nanometric defect clusters and point defects, on low-dose irradiation, that significantly impairs the thermal conductivity of ThO₂. An extensive TEM and CD investigation has also been carried out to study the growth and coarsening of SIA loop and voids during post-irradiation isochronal annealing of ThO₂ at high temperatures.</p>

The effect of proton (H+) irradiation on uranium mononitride (UN) and UN compositefuel with 10 at.% ZrN (UN10at%ZrN) was examined. Protons of 2 MeV with fluences of1E17, 1E18, 1E19 and 1E20 ions/cm2 were accelerated towards the fabricated samples in orderto investigate the evolution of the micro-structure. Stopping and Range of Ions in Matter(SRIM) calculations were performed to determine the displacements per atom associatedwith the depth of the highest damage, for each fluence.X-Ray diffraction (XRD) was used in both samples to identify the chemical composition ofeach pellet, which revealed the low presence of oxygen. Based on scanning electron microscopy(SEM), deterioration of the samples surface was observed, as the proton fluence increased.The applied stress due to the irradiation, led to the cracking of the pellets at the highestfluences. Blisters and craters appear to surround the cracked region, which might originatefrom the significant levels of hydrogen implantation within the samples.From Electron backscatter diffraction (EBSD) analysis, the grain size of the UN10at%ZrNcomposite was found to be smaller than in UN, due to the nano-particle nature of the ZrNpowder. The latter technique was also used to observe the elevated irradiated regions, whichwere further investigated by atomic force microscopy (AFM). Nano-indentation detectedirradiation hardening for both samples in the irradiated regions. Focused ion beam (FIB)milling was applied to remove lamellas from the cracked regions in both UN and compositesamples in order to be analyzed by transmission electron microscopy (TEM). The latter mightreveals the formation of dislocation loops in the irradiated areas. / Effekten av protonbestrålning på urannitrid (UN) och UN-kompositbränsle med 10 at.% ZrN (UN10at%ZrN) undersöktes. Protoner på 2 MeV med total dos på 1E17, 1E18, 1E19 och 1E20 joner/cm2 accelererades mot de tillverkade proverna för att undersöka utvecklingen av mikrostrukturen under bestrålning. SRIM-beräkningar (Stopping and Range of Ions in Matter) utfördes för att bestämma profilen på skadan och jonimplanteringen i förhållande till djupet, för varje dosnivå.  Röntgendiffraktion (XRD) användes på båda proverna för att identifiera den kemiska sammansättningen av varje kuts, vilket visade att syrehalten var låg. Med hjälp av svepelektronmikroskopi (SEM) observerades en försämring av provernas yta när protonflödet ökade. Den resulterande mekaniska spänningen överskred provets brottstyrka på djupet, eftersom nitriderna inte är så duktila, vilket ledde till sprickbildning i proverna som utsattes för de högsta doserna. Blåsor och kratrar omger det spruckna området, vilket beror på betydande väteimplantering i provet.  Genom electron backscatter diffraction analys (EBSD) konstaterades att kornstorleken hos UN10at%ZrN-kompositen var mindre än hos UN, på grund av ZrN-pulvrets nanopartikelnatur. Den sistnämnda tekniken användes för att observera de högt bestrålade områdena, som undersöktes ytterligare med Atomic force microscopy (AFM). Genom nano-indientation upptäcktes bestrålningshärdning för båda proverna i de bestrålade områdena. Fräsning med en fokuserad jonstråle (FIB) användes för att avlägsna lameller från de spruckna områdena i både UN- och kompositprovet för att kunna analyseras med transmission electron microscopy (TEM). Det senare visade att det bildades dislokationer i de bestrålade områdena.