Nobuhiro Okada

High-Speed Growth of 4H-SiC Single Crystal Using Si-Cr Based Melt

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.

Solution growth of SiC crystal with high growth rate using accelerated crucible rotation technique

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.

Top-Seeded Solution Growth of 4H-SiC Bulk Crystal Using Si-Cr Based Melt

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.

Crystallinity Evaluation of 4H-SiC Single Crystal Grown by Solution Growth Technique Using Si-Ti-C Solution

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.

Solution Growth of Single Crystalline 6H-SiC from Si-Ti-C Ternary Solution

Solution growth of 6H-SiC single crystal from Si-Ti-C ternary solution using the accelerated crucible rotation technique (ACRT) was performed. The SiC growth rate exceeding 200 μm/hr was achieved in several ACRT conditions. Such a high growth rate can be ascribed to the enhancement of the carbon transport from the graphite crucible to the growth interface due to the use of the ACRT. The incorporation of inclusions of Si-Ti solvent in the grown SiC crystal was also significantly suppressed by using the ACRT. The intensive convection near the growth interface induced by the ACRT 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 could be accomplished in the SiC solution growth using the ACRT. The obtained SiC self-standing crystal exhibited homogeneous green colour without cracks and inclusions. We investigated the crystalline quality of the grown SiC crystal by means of X-ray diffraction. The, ω-scan rocking curves of (0006) reflection measured by X-ray diffraction provided the FWHM of 15-20 arc-second showing the excellent crystallinity of the solution grown 6H-SiC single crystal.

Top-seeded solution growth of 3 inch diameter 4H-SiC bulk crystal using metal solvents

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.

Growth of Large Diameter 4H-SiC by TSSG Technique

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

Development of finite element analysis method for three-dimensional hot bending and direct quench (3DQ) process

The automotive industry has been focusing on developing lighter vehicles to improve fuel economy and crash safety. In order to meet these requirements, Three Dimensional Hot Bending and Direct Quench (3DQ) Technology has been developed, which enables a manufacturer to form hollow tubular automotive parts with a tensile strength of 1,470 MPa or over. 3DQ is a type of consecutive forming that allows bending and quenching at the same time, with a tube feeding device, an induction heater, a cooling device, and a bending device. In this research, a coupled thermomechanical-metallurgical finite element analysis (FEA) method has been developed to investigate the deformation behavior and to predict the forming capability of 3DQ. In the developed FEA procedure, the temperature distribution was calculated with electro magnetic and heat transfer analysis, and the flow stress was defined by transformation models and linear mixture rule. An experimental formula was used to track the ferrite-austenite transformation, a...

Crystal Growth of 4H-SiC on 6H-SiC by Traveling Solvent Method

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.

Effect of Solution Drift on Crystalline Morphology in the Solution Growth of Off-Axis 4H-SiC Crystals

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.