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We investigated the effect of the solution flow on crystalline morphology in the off-axis 4H-SiC solution growth. In particular, we focused on the relation between the Si solution flow and step flow directions. In step parallel flow in which the solution drifted transversely to the step flow direction of the off-axis substrate, it was possible to attain a better surface morphology than in the flow in which the solution drifted toward the other direction. Furthermore, it was found that the surface morphology was found to be improved as the solution flow velocity increased. These improvements in the morphological stability are presumed to be caused by aligning the solute concentration fluctuation along the steps.

We performed top-seeded solution growth of 4H-SiC for obtaining longer length crystal. Si-Cr and Si-Ti melts were used as solvents. Meniscus formation technique was applied to the present study. Special attention was paid to improve the process stability during long-term growth. One of major technological problems in the solution growth is that the precipitation of polycrystalline SiC which hiders the stable single crystal growth. Another problem is the fluctuation of supersaturation at the growth interface during the growth. Through the optimization of growth process conditions, we have successfully grown 4H-SiC single crystals up to 14 mm long with three-inch-diameter, and evaluated their crystalline quality.

In this study, we have investigated the rate-limiting process of 4H-SiC solution growth using Si-Cr based melt, and have tried high-speed growth. It is revealed that the rate-limiting process of SiC growth under our experimental condition is interface kinetics, which can be controlled by such factors as temperature and supersaturation of carbon. By enhancing the interface kinetics, SiC crystal has been grown at a high rate of 2 mm/h. The FWHM values of X-ray rocking curves and threading dislocation density of the grown crystals are almost the same as those of seed crystal. Possibility of high-speed and high-quality growth of 4H-SiC has been indicated.

4H-SiC single crystal with 3-inch diameter was grown by top seeded solution growth (TSSG) technique. We used a new convection control member called “Immersion Guide (IG)” which causes the high and homogenous fluid flow in the solution. As a result, we achieved relatively high growth rate and morphological stability

Crystallinity of 4H-SiC bulk crystal obtained by solution growth technique was characterized mainly by KOH etching of the off-ground and serially ground specimen. Marked reduction of basal plane dislocation, threading edge and screw dislocations during the growth of on-axis crystal was confirmed. Cross-sectional TEM observation revealed the rapid reduction behavior of threading dislocations microscopically. AFM observation of as-grown morphology showed that screw dislocation dipoles is related to the reduction of threading screw dislocations and single domain formation, which is essential for establishing the high crystallinity.

We have grown high-quality long cylindrical (12 mm thick) 4H-SiC bulk crystals by the meniscus formation technique, which was first applied for the solution growth of bulk SiC. It enabled long-term growth by suppressing parasitic reactions such as polycrystal precipitation around the seed crystal. In addition, we could control the growth angle from −22° to 61° by adjusting the meniscus height. The thickness of the grown cylindrical crystals was 12 mm, which is the largest reported until now, and corresponded to a growth rate of 0.6 mm/h. Smooth morphology growth was maintained on the (000-1) C-face. In cross-sectional transmission optical microscopy images, few solvent inclusions and voids were observed. XRD measurements revealed that the FWHM values of the grown crystals were almost the same as those of the seed crystal.

We attempted the traveling solvent method (TSM) growth of SiC on 6H-SiC(0001) substrates using Si and Si-M (M=Ti, Cr and Dy) solvents at growth temperatures of 1500-1800°C. It was confirmed that 4H-SiC polytype was extremely stabilized in the highly carbon dissolved liquid phase. 4H-SiC growth on 6H-SiC, i.e. hetropolytype epitaxial growth, was observed only from Si-Dy solvent. The Dy content above 60at% was necessary to obtain 100% 4H-SiC polytype.

We performed solution growth of SiC single crystals from Si-Ti-C ternary solution using the accelerated crucible rotation technique (ACRT). It was confirmed that the growth rate exceeding 200 μm/hr was achievable by several ACRT conditions. This high growth rate might be due to the enhancement of the carbon transport from the graphite crucible to the growth interface using the ACRT. Moreover, the incorporation of inclusions of the Si-Ti solvent in the grown crystal was significantly suppressed by using the ACRT. It was thought that the intensive convection near the growth interface resulted in not only the marked increase of SiC growth rate but also the superior homogeneity in the surface morphology. It was concluded that faster stable growth can be accomplished in the SiC solution growth using the ACRT.