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京都大学 / 0048 / 新制・課程博士 / 博士(エネルギー科学) / 甲第21889号 / エネ博第390号 / 新制||エネ||75(附属図書館) / 京都大学大学院エネルギー科学研究科エネルギー変換科学専攻 / (主査)教授 木村 晃彦, 教授 星出 敏彦, 教授 今谷 勝次 / 学位規則第4条第1項該当 / Doctor of Energy Science / Kyoto University / DGAM

Dans les applications nucléaires, les propriétés des matériaux peuvent subir des modifications importantes en raison de l'interaction destructive avec l'irradiation de particules au niveau des microstructures, qui affectent les propriétés globales. L'un des défis associés aux études de matériaux irradiés par des ions, c'est que la couche concernée, ou la profondeur de pénétration, est généralement très mince (0,1-100 um). Cette étude élargit la base des connaissances actuelles en matière de transport thermique dans les matériaux irradiés par des ions, en utilisant une approche expérimentale multiéchelles avec des méthodes basées sur des ondes thermiques. D'une manière pas encore explorée auparavant, quatre méthodes sont utilisées pour caractériser la couche irradiée par des protons dans ZrC : la microscopie thermique à balayage (SThM), la radiométrie photothermique (PTR) avec détection sur la face avant et balayage spatial, la thermographie infrarouge lock-In (IRT), et la PTR tomographique avec balayage en fréquence. Pour la première fois, le profil de conductivité thermique en profondeur d'un échantillon irradié est mesuré directement. Les profils obtenus par chacune des méthodes d'analyse spatiale sont comparés les uns aux autres et à la prévision numérique du profil endommagé. La nature complémentaire des différentes techniques valide le profil mesuré et la dégradation constatée de la conductivité thermique de l'échantillon de ZrC. / In nuclear applications, material properties can undergo significant alteration due to destructive interaction with irradiating particles at microstructural levels that affect bulk properties. One of the challenges associated with studies of ion-Irradiated materials is that the affected layer, or penetration depth, is typically very thin (~0.1-100 μm). This study expands the current knowledge base regarding thermal transport in ion-Irradiated materials through the use of a multiscaled experimental approach using thermal wave methods. In a manner not previously explored, four thermal wave methods are used to characterize the proton-Irradiated layer in ZrC including scanning thermal microscopy (SThM), spatial-Scanning front-Detection photothermal radiometry (PTR), lock-In IR thermography (lock-In IRT), and tomographic, frequency-Based PTR. For the first time, the in-Depth thermal conductivity profile of an irradiated sample is measured directly. The profiles obtained by each of the spatial scanning methods are compared to each other and the numerical prediction of the ion-Damage profile. The complementary nature of the various techniques validates the measured profile and the measured degradation of thermal conductivity in the ZrC sample.

Ziel des BMWi-Fördervorhabens 1501393 ist es, durch den Einsatz von Untersuchungsmethoden auf der nm-Skala einen Beitrag zur Aufklärung von Flusseffekten und von Late-Blooming-Effekten in bestrahlten RDB-Stählen zu leisten. Zur Untersuchung dieser Effekte wurde auf RDB-Stähle deutscher Reaktoren aus zwei bei der AREVA GmbH abgeschlossenen Vorhaben zurückgegriffen. Die Auswahl der Grundwerkstoffe und Schweißgüter erfolgte so, dass sich optimale Voraussetzungen für das Erreichen des Gesamtziels des Vorhabens ergeben. Die ausgewählten Untersuchungsmethoden umfassen mit der Neutronenkleinwinkelstreuung, der Atomsondentomographie und der Positronen-annihilationsspektroskopie solche Techniken, die die nm-skaligen bestrahlungsinduzierten Defekt-Fremdatom-Cluster bestmöglich und in komplementärer Weise zu detektieren und zu charakterisieren gestatten. Es wurde ein Flusseffekt auf die Größe der bestrahlungsinduzierten Fremdatomcluster, jedoch nicht auf den Volumenanteil und die mechanischen Eigenschaften gefunden. In einem Cu-armen RDB-Schweißgut wurde ein Late-Blooming-Effekt nachgewiesen, der sich in einem steilen Anstieg des Clustervolumenanteils und der Übergangstemperaturverschiebung nach einer Phase schwacher oder fehlender Zunahme niederschlägt. The BMWi project 1501393 aimed at contributing to the clarification of flux effects and late blooming effects in irradiated RPV steels by means of experimental techniques of sensitivity at the nm scale. The investigation of these effects was focussed on RPV steels, both base metal and weld of German reactors selected according to the objectives of the present project from two previous projects performed at AREVA GmbH. The complementary techniques of small-angle neutron scattering, atom probe tomography and positron annihilation spectroscopy were applied to detect and characterize the irradiation-induced nm-scale defect-solute clusters. A flux effect on the size of the irradiation-induced clusters but no flux effect on both cluster volume fraction and mechanical properties was found. For a low-Cu RPV weld, a late blooming effect was observed, which results in a steep slope of both cluster volume fraction and transition temperature shift after an initial stage of small or no change.

Ziel des BMWi-Fördervorhabens 1501393 ist es, durch den Einsatz von Untersuchungsmethoden auf der nm-Skala einen Beitrag zur Aufklärung von Flusseffekten und von Late-Blooming-Effekten in bestrahlten RDB-Stählen zu leisten. Zur Untersuchung dieser Effekte wurde auf RDB-Stähle deutscher Reaktoren aus zwei bei der AREVA GmbH abgeschlossenen Vorhaben zurückgegriffen. Die Auswahl der Grundwerkstoffe und Schweißgüter erfolgte so, dass sich optimale Voraussetzungen für das Erreichen des Gesamtziels des Vorhabens ergeben. Die ausgewählten Untersuchungsmethoden umfassen mit der Neutronenkleinwinkelstreuung, der Atomsondentomographie und der Positronen-annihilationsspektroskopie solche Techniken, die die nm-skaligen bestrahlungsinduzierten Defekt-Fremdatom-Cluster bestmöglich und in komplementärer Weise zu detektieren und zu charakterisieren gestatten. Es wurde ein Flusseffekt auf die Größe der bestrahlungsinduzierten Fremdatomcluster, jedoch nicht auf den Volumenanteil und die mechanischen Eigenschaften gefunden. In einem Cu-armen RDB-Schweißgut wurde ein Late-Blooming-Effekt nachgewiesen, der sich in einem steilen Anstieg des Clustervolumenanteils und der Übergangstemperaturverschiebung nach einer Phase schwacher oder fehlender Zunahme niederschlägt. The BMWi project 1501393 aimed at contributing to the clarification of flux effects and late blooming effects in irradiated RPV steels by means of experimental techniques of sensitivity at the nm scale. The investigation of these effects was focussed on RPV steels, both base metal and weld of German reactors selected according to the objectives of the present project from two previous projects performed at AREVA GmbH. The complementary techniques of small-angle neutron scattering, atom probe tomography and positron annihilation spectroscopy were applied to detect and characterize the irradiation-induced nm-scale defect-solute clusters. A flux effect on the size of the irradiation-induced clusters but no flux effect on both cluster volume fraction and mechanical properties was found. For a low-Cu RPV weld, a late blooming effect was observed, which results in a steep slope of both cluster volume fraction and transition temperature shift after an initial stage of small or no change.

O aumento do consumo de vegetais frescos e a globalização do mercado de hortaliças e frutas frescas provocaram um aumento na preocupação com as enfermidades transmitidas por alimentos (ETA) associadas a esses produtos. No Brasil, a produção de hortaliças orgãnicas vem crescendo, aproximadamente 40% ao ano. Considerando o exposto, foram analisadas 108 amostras de agrião orgãnico minimamente processado e irradiado coletadas, aleatoriamente, em produtores da região de São Roque, São Paulo, no período de novembro de 2005 a março de 2007, para avaliar a ecologia microbiana e a concentração de vitamina C ao longo da cadeia produtiva. As amostras de agrião orgãnico coletadas no campo e as de minimamente processado apresentaram populações superiores a 3,0 log UFC/g para aeróbios mesófilos, aeróbios psicrotróficos, Pseudomonas spp, coliformes termotolerantes e E. coli. Salmonella spp, E. coli 0157:H7 e L. monocytogenes não foram detectadas ao longo da cadeia produtiva. Comparando o processo mínimo com a combinação processo mínimo e irradiação constata-se que a combinação é mais eficiente uma vez que o processo mínimo seguido de exposição à dose de 1 kGy foi suficiente para reduzir de maneira significativa os diversos grupos de mícrorganismos no agrião. As concentrações de ácido ascórbico, ácido dehidroáscorbico e de vitamina C variaram em todas as etapas de processamento do agrião orgãnico minimamente processado e irradiado. Ao longo da vida-de-prateleira de agrião orgãnico minimamente processado e irradiado, a população de L. monocytogenes foi reduzida em, aproximadamente, 4,5, 5,5 e 5,9 ciclos log de acordo com as doses de 1 kGy, 2 kGye 3 kGy, respectivamente. Comportamento similar pode ser constatado para a população de Salmonella spp,. Os resultados da análise sensorial mostraram que o conhecimento ou não do processo de irradiação pelo consumidor não prejudica a aceitação e a intenção de compra do produto irradiado. Portanto o processo de irradiação visando a melhoria da qualidade de agrião orgânico é factível desde que sejam seguidas as Boas Práticas Agrícolas, Boas Práticas de Produção e Boas Práticas do Processo de Irradiação. / With the increase in the consumption of fresh vegetables and the globalization of the market for fresh fruits and vegetables, the concern with foodborne diseases associated with these products has also increased. In Brazil, the production of organic vegetables has increased approximately 40% per year in the last decade. Considering the above, 108 samples of irradiated, minimally processed, organic watercress from producers in the region of Sao Roque, Sao Paulo, were collected through November 2005 to March 2007, to assess the microbial ecology and vitamin C content. Samples of organic watercress collected at the farm level and at the industry level showed populations higher than 3,0 UFC/g for aerobic mesophilic, psychrotrophic, Pseudomonas spp, fecal coliforms and E. coli. Salmonella, E. coli O157:H7 and L. monocytogenes were not detected along the production chain. Comparing the minimal process and the combination of minimal process and irradiation, the combination was more efficient since even the lower dose (1 kGy) was sufficient to reduce the population of the various groups of microorganisms. The ascorbic acid, dehidroascorbic acid and vitamin C content varied at all stages of minimal processing as well as with the exposed doses of irradiation (1, 2 and 3 kGy). The population of L. monocytogenes decreased approximately 4.5, 5.5, and 5.9 log cycles, depending on the exposed doses, throughout the shelf life of irradiated minimally processed organic watercress. Similar behavior was showed by the Salmonella population. Sensory evaluation results showed that previous knowledge or none by consumers does not interfere with the acceptance and intention of purchase of irradiated minimally processed organic watercress. Thus the process of irradiation to improve the microbiological quality of minimally processed organic watercress is feasible provided that Good Agricultural Practice, Good Practice Production and Good Irradiation Practice are followed.

O aumento do consumo de vegetais frescos e a globalização do mercado de hortaliças e frutas frescas provocaram um aumento na preocupação com as enfermidades transmitidas por alimentos (ETA) associadas a esses produtos. No Brasil, a produção de hortaliças orgãnicas vem crescendo, aproximadamente 40% ao ano. Considerando o exposto, foram analisadas 108 amostras de agrião orgãnico minimamente processado e irradiado coletadas, aleatoriamente, em produtores da região de São Roque, São Paulo, no período de novembro de 2005 a março de 2007, para avaliar a ecologia microbiana e a concentração de vitamina C ao longo da cadeia produtiva. As amostras de agrião orgãnico coletadas no campo e as de minimamente processado apresentaram populações superiores a 3,0 log UFC/g para aeróbios mesófilos, aeróbios psicrotróficos, Pseudomonas spp, coliformes termotolerantes e E. coli. Salmonella spp, E. coli 0157:H7 e L. monocytogenes não foram detectadas ao longo da cadeia produtiva. Comparando o processo mínimo com a combinação processo mínimo e irradiação constata-se que a combinação é mais eficiente uma vez que o processo mínimo seguido de exposição à dose de 1 kGy foi suficiente para reduzir de maneira significativa os diversos grupos de mícrorganismos no agrião. As concentrações de ácido ascórbico, ácido dehidroáscorbico e de vitamina C variaram em todas as etapas de processamento do agrião orgãnico minimamente processado e irradiado. Ao longo da vida-de-prateleira de agrião orgãnico minimamente processado e irradiado, a população de L. monocytogenes foi reduzida em, aproximadamente, 4,5, 5,5 e 5,9 ciclos log de acordo com as doses de 1 kGy, 2 kGye 3 kGy, respectivamente. Comportamento similar pode ser constatado para a população de Salmonella spp,. Os resultados da análise sensorial mostraram que o conhecimento ou não do processo de irradiação pelo consumidor não prejudica a aceitação e a intenção de compra do produto irradiado. Portanto o processo de irradiação visando a melhoria da qualidade de agrião orgânico é factível desde que sejam seguidas as Boas Práticas Agrícolas, Boas Práticas de Produção e Boas Práticas do Processo de Irradiação. / With the increase in the consumption of fresh vegetables and the globalization of the market for fresh fruits and vegetables, the concern with foodborne diseases associated with these products has also increased. In Brazil, the production of organic vegetables has increased approximately 40% per year in the last decade. Considering the above, 108 samples of irradiated, minimally processed, organic watercress from producers in the region of Sao Roque, Sao Paulo, were collected through November 2005 to March 2007, to assess the microbial ecology and vitamin C content. Samples of organic watercress collected at the farm level and at the industry level showed populations higher than 3,0 UFC/g for aerobic mesophilic, psychrotrophic, Pseudomonas spp, fecal coliforms and E. coli. Salmonella, E. coli O157:H7 and L. monocytogenes were not detected along the production chain. Comparing the minimal process and the combination of minimal process and irradiation, the combination was more efficient since even the lower dose (1 kGy) was sufficient to reduce the population of the various groups of microorganisms. The ascorbic acid, dehidroascorbic acid and vitamin C content varied at all stages of minimal processing as well as with the exposed doses of irradiation (1, 2 and 3 kGy). The population of L. monocytogenes decreased approximately 4.5, 5.5, and 5.9 log cycles, depending on the exposed doses, throughout the shelf life of irradiated minimally processed organic watercress. Similar behavior was showed by the Salmonella population. Sensory evaluation results showed that previous knowledge or none by consumers does not interfere with the acceptance and intention of purchase of irradiated minimally processed organic watercress. Thus the process of irradiation to improve the microbiological quality of minimally processed organic watercress is feasible provided that Good Agricultural Practice, Good Practice Production and Good Irradiation Practice are followed.