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THÈSE Ahmed Nouri Numerical and Experimental Study of Silicon

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THÈSE Ahmed Nouri Numerical and Experimental Study of Silicon THÈSE Pour obtenir le grade de DOCTEUR DE L’UNIVERSITE DE GRENOBLE ALPES Préparée dans le cadre d’une cotutelle internationale entre l’Université Grenoble Alpes et l’Université de Laghouat Spécialité : Matériaux, mécanique, génie civil, électrochimie Présentée par Ahmed Nouri Thèse dirigée par Kader Zaidat et Iben Khaldoun Lefkaier et codirigée par Yves Delannoy, Guy Chichignoud et Bachir Helifa préparée au sein des laboratoires : SIMaP-EPM et LPM dans Les écoles Doctorale : IMEP-2 et SM Numerical and Experimental study of silicon crystallisation by Kyropoulos process for photovoltaic applications Thèse soutenue publiquement le 07 Mars 2017. devant le jury composé de : M. Kheirreddine, Lebbou Directeur de recherche à l’Université de Lyon 1, (Président) M. Matias Velázquez Chargé de recherche à l’institut ICMCB, CNRS, Bordeaux, (Rapporteur) M. Aissa Belgacem-Bouzida Professeur à l’Universite de Batna, (Rapporteur) M. Bachir Bentria Professeur, Université de Laghouat, (Examinateur) M. Kader Zaidat Professeur à l’Université Grenoble Alpes, (Directeur de Thèse) M. Iben Khaldoun Lefkaier Professeur à l’Université de Laghouat, (Directeur de Thèse) M. Yves Delannoy Professeur à l’Université Grenoble Alpes, (Co-Directeur de Thèse) M. Guy Chichignoud Chargé de recherche, CNRS, Grenoble, (Co-Directeur de Thèse) M. Bachir Helifa Maitre de conférences, Université de Laghouat, (Co-Directeur de Thèse) To those who believe in a better world for the future generations . To my family. Abstract Kyropoulos technique is a top seeding crystal growth process with the potential to produce large diameter ingots of high crystalline quality. The crystal grows inside the melt at low thermal gradient without contact with the crucible. Despite its advantages, the technique has not been fully investigated for the production of silicon. 3D numerical modeling of the full furnace was performed to understand the effect of heat transfer and fluid dynamics on solidification. An experimental Kyropoulos setup with a square crucible and three heating elements (top, bottom and side heaters) was developed in parallel to grow silicon ingots for photovoltaic applications. The obtained numerical results explained why no growth was possible in the starting configuration. Radiation heating was more concentrated on the center and heat loss from the sides was high. The addition of a radiation shield tube in the central zone and the increase of side heating created a cold area around the seeding zone. Growth from the seed was possible in these conditions and crystal enlargement was achieved by decrease of power in the upper heater. To enhance the growth conditions, a third configuration was created by adding a cold heat sink in the top to provide local central cooling of the melt and better heat extraction from the seed. The crystal growth in Kyropoulos process for silicon was found to be sensitive to symmetry loss. Numerical investigation showed that a strong coupled effect between radiations heat exchange in the top and melt flow is the leading cause for dissymmetric growth. The sudden increase of emissivity of silicon during solidification coupled with the slowdown of melt flow near the crystal increased the growth rate of any appearing dissymmetry towards one preferential direction. Control of the top radiation cooling, by keeping the top heater temperature close to melting point, and addition of crystal rotation to homogenize the melt allowed a consistent symmetric crystal growth. The investigation showed that it is possible to control the shape of the final ingot to have a square horizontal section using two main approaches: by fluid dynamics control or by structural growth kinetics control. Numerical simulation showed that it is possible to have a square horizontal cross section of the ingot using the balance between heat diffusion and advection in the melt. Two different cases could be obtained according to the values of Peclet number. For the case of higher Peclet number, the square horizontal cross section was made by the flow coming from the four corners i of the crucible, while in the case of lower Peclet number , the crystal square horizontal cross section was inherited directly from the walls of the crucible. For the latter case, the square shape of the ingot section could not be fully completed in the corners due to the localized effect of higher Peclet number in the corners. Structural growth kinetics control was also used to obtain a square ingot cross section. The developed experimental prototype succeeded to stabilize monocrystalline faceted growth in the <111> direction giving silicon crystals with a perfectly square horizontal cross section. Résumé Le procédé Kyropoulos et un procédé de croissance cristalline par trempe de germe permettant potentiellement de produire des lingots de grand diamètre et de haute qualité cristalline. La croissance progresse dans un bain à faible gradient thermique et sans contact avec le creuset. Malgré ses avantages, le procédé Kyropoulos n’a pas été exploité pour la production du silicium. Le présent travail a pour but d’étudier l’utilisation du procédé Kyropoulos pour produire des cristaux de silicium de haute qualité avec une section horizontale carrée. Un model numérique 3D du processus, avec calcule de la thermique, de la mécanique des fluides et de la solidification, a été créé pour comprendre l’effet des transferts thermiques et de la mécanique des fluides sur la solidification. Un dispositif expérimental doté d’un creuset carré et de trois zones de chauffe (haut, bas et coté) a été développé en parallèle pour faire croitre des cristaux de silicium pour des applications photovoltaïques. L’analyse numérique a permis de comprendre l’effet de la répartition du chauffage par rayonnement au-dessus de la charge de silicium et de quantifier les pertes thermiques à travers les côtés dans le dispositif expérimental. Ces bilant ont permis de développer différente configurations fonctionnelles du four. L’ajout d’un écran contre le rayonnement autour de la zone de trempe et l’augmentation du chauffage des cotés ont permis de créer une zone froide autour du germe et d’orienter les boucles de convection pour devenir descendantes au centre. La croissance à partir du germe était possible par diminution de la puissance dans l’élément chauffant du haut. Afin d’améliorer encore les conditions de croissance, une troisième configuration du procédé a été développée par l’ajout d’un échangeur thermique froid autour du ii germe pour augmenter le refroidissement de la zone centrale et améliorer l’extraction de chaleur à partir du germe. L’étude a montré que le procédé Kyropoulos pour le silicium est sensible à la croissance dissymétrique. La cause principale pour cette dissymétrie de croissance étant un effet conjugué entre l’augmentation de refroidissement par rayonnement, lié au changement d’émissivité du silicium durant la solidification, et le ralentissement des boucles de convection dans le bain du côté du cristal. Le contrôle du rayonnement, en gardant la température de l’élément chauffant du haut proche de la température de fusion du silicium, et l’homogénéisation du bain par ajout de la rotation du cristal ont permis d’avoir une croissance symétrique du cristal à partir du germe. Le présent travail propose deux méthodes de contrôle possibles pour obtenir une section horizontale carrée du lingot de silicium: un control basé sur la mécanique des fluides et un control basé sur la cinétique de croissance structurale. Les résultats numériques montrent qu’il est possible d’obtenir un lingot de section horizontale carrée en utilisant les transferts thermiques par diffusion et par advection dans le bain. Deux cas peuvent être distingués suivant le nombre de péclet: dans le cas à nombre de péclet élevé la forme carrée de la section horizontale du lingot est issue de l’écoulement venant des quatre coins du creuset, tandis que dans le cas à faible nombre de Péclet, la forme carrée de la section horizontale du lingot est issue directement des faces du creuset. Pour ce dernier cas, la forme de la section horizontale du lingot n’était pas complètement carrée aux coins à cause d’un fort écoulement localisé dans les coins. Pour le cas de contrôle de forme par la cinétique de croissance structurale, le prototype expérimental développé a permis de stabilisé la croissance facettée des facettes <111> dans le silicium donnants des mono cristaux de section horizontale de forme carré. iii Acknowledgement I would like to express my sincere thanks to my phD director dr Kader Zaidat for his guidance, patience, and continuous feedback. His effort to provide opportunities for discovery and acquirement of new scientific insight made this thesis an ongoing adventure. I would like to thank my phD director Khaled Lefkaier for his guidance and encouragements. His remarks and advises were a great support to reshape my choices in order to accomplish this work. I would like to thank my co-director Yves Delannoy for his most appreciated guidance and support. I am grateful that he made himself available to help and guide me through this work. His incisive insight have been an important asset during this work. I would like to thank my co-director Guy Chichignoud for his constant support and guidance. His investment in my thesis was a foundation that helped to shape this work. I would like to thank my co-director Bachir Helifa for his valorous availability and guidance. His will to support me unconditionally gave me confidence to move forward and beyond. I would like to thank the members of the jury who honored me by accepting to review and comment my work I am grateful to Professor Thierry Duffar for receiving me for discussions. His valuable explanations and comment are most appreciated. I am also thankful to Professor Yves Fautrelle for accepting to discuss my work. ii I am grateful to Professor Koichi Kakimoto for receiving me in his laboratory.
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