a b s t r a c tThis work is dedicated to the advanced in situ X-ray imaging and complementary ex situ investigations of the growth mechanisms when silicon solidifies on a monocrystalline seed oriented 〈110〉 in the solidification direction. It aims at deepening the fundamental understanding of the phenomena that occur throughout silicon crystal growth with a particular focus on mechanisms of formation of defects detrimental for photovoltaic applications. Namely, grain nucleation, grain boundary formation and evolution, grain competition, twining occurrence, dislocation generation and interaction with structural defects are explored and analysed. Nucleation of twin crystals preferentially occurs on {111} facets at the edge of the sample where solid e liquid e vapor triple point lines exist in interaction also with the crucible as well as, at grain boundary grooves at the solid e liquid interface (solid e solid e liquid triple lines), where two grains are in competition, either on the {111} facets of the groove or in the groove. Enhanced undercooling and/or stress accumulation levels are found to act as driving forces for grain nucleation. Additionally, it is demonstrated that twin formation has the property to relax stresses stored in the crystal during the growth process. However, grains formed initially in twin position can undergo severe distortion when they are in direct competition or when they are squeezed in e between grains. Moreover, we show by X-ray Bragg diffraction imaging that on the one hand, coherent S3 〈111〉 grain boundaries efficiently block the propagation of growth dislocations during the solidification process, while on the other hand, dislocations are emitted at the level of incoherent and/or asymmetric S27a 〈110〉 at the encounter with either S3 〈111〉 or S9 〈110〉 grain boundaries. Indeed, grain boundaries that deviate from the ideal coincidence orientation act as dislocation sources that spread inside the surrounding crystals.

This work is dedicated to the grain structure formation in silicon ingots with a particular focus on the crystal structure strain building and its implication in new grain nucleation process. The implied mechanisms are investigated by advanced in situ X-ray imaging techniques during silicon directional solidification. It is shown that the grain structure formation is mainly driven by Σ3 <111> twin nucleation. Grain competition phenomena occurring during the growth process lead to the creation of higher order twin boundaries, localised strained areas and associated crystal structure deformation. On the one hand, it is demonstrated that local strain building can be directly related to the characteristics of the twin boundaries created during silicon growth due to grain competition. On the other hand, space restriction due to competition during growth can be at the origin of local strain building as well. Finally, the accumulation of all these factors generating strain is responsible for spontaneous new grain nucleation. When occurring, both grain nucleation and subsequent grain structure reorganisation contribute to lower the strain in the growing ingot.It is demonstrated as well that the local distribution of the strained areas created during silicon growth is retrieved after cooling down, from melting temperature to room temperature, on top of an additional larger scale deformation of the sample due to the cooling down only.

To cite this version:Fabrice Guittonneau, Abdesselam Abdelouas, Bernd Grambow, Sandrine Huclier. The effect of high power ultrasound on an aqueous suspension of graphite. Ultrasonics Sonochemistry, Elsevier, 2010, 17, pp

In this research, Al-Fe-Cr quasicrystal (QC) reinforced Al-based metal matrix composites were in-situ manufactured by using selective laser melting (SLM) from the powder mixture. The parametrical optimization based on our previous work was performed with focus on laser scanning speed. From the optimized parameters, an almost dense (99.7%) free-crack sample was fabricated with an ultra-fine microstructure. A phase transition from decagonal QC Al 65 Cu 25 Fe 10 Cr 5 to icosahedral QC Al 91 Fe 4 Cr 5 could be observed as laser scanning speed decreases. Differential scanning calorimetry curves show that the QC phase is quiet stable until 500°C. And then, the effects of annealing temperature on the microstructural and mechanical properties were determined. The results indicate that the recrystallization and growth behavior of α-Al grains could be prevented by QC particle during annealing. Furthermore, the growth of QC particle, which tends to form a porous structure, leads an improvement of Young modulus and decline of ductility.

Si soft magnetic parts, using Ni coated high silicon steel powder, were manufactured by selective laser melting process. The type of defect changes from porosity to cracks and the relative density increases, from 50% to 99%, with the decreasing laser scanning speed. The microstructural analyses indicate that the low laser scanning speed fully melted the nickel coating and high-silicon steel core. The EBSD study showed that the separated island and lamellar mesostructures appeared on the top and side view respectively. Moreover, no apparent texture were observed. The magnetization saturation of SLM processed sample decreased, as the laser scanning speed was increased. Consequently, the magnetic properties of SLM processed Fe-Ni-Si alloy also showed anisotropic feature in building and scanning directions, which can be attributed to their different mesostructure.