• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.4
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• pp.152-158
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• 2018

PVT (Physical Vapor Transport) method has advantages in producing high quality, large scale wafers where many researches are being carried out to commercialize nitride semiconductors. However, complex process variables cause various defects when it had non-equilibrium growth conditions. Annealing process after crystal growth has been widely used to enhance the crystallinity. It is important to set appropriate temperature, pressure, and annealing time to improve crystallinity effectively. In this study, the effect of the annealing conditions on the crystalline structure variation of the AlN single crystal grown by PVT method was investigated with synchrotron whitebeam X-ray topography, electron backscattered diffraction (EBSD), and Rietveld refinement. X-ray topography analysis showed secondary phases, sub-grains, impurities including carbon inclusion in the single crystal before annealing. EBSD analyses identified that sub-grains with slightly tilted basal plane appeared and the overall number of grains increased after the annealing process. Rietveld refinement showed that the stress caused by the temperature gradient during the annealing process between top and bottom in the hot zone not only causes distortion of grains but also changes the lattice constant.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.113-114
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• 2009

Silicon carbide is one of the most attractive and promising wide band-gap semiconductor material with excellent physical properties and huge potential for electronic applications. Up to now, the most successful method for growth of large SiC crystals with high quality is the physical vapor transport (PVT) method [1, 2]. Since further reduction of defect densities in larger crystal are needed for the true implementation of SiC devices, many researchers are focusing to improve the quality of SiC single crystal through the process modifications for SiC bulk growth or new material implementations [3, 4]. It is well known that for getting high quality SiC crystal, source materials with high purity must be used in PVT method. Among various source materials in PVT method, a SiC powder is considered to take an important role because it would influence on crystal quality of SiC crystal as well as optimum temperature of single crystal growth, the growth rate and doping characteristics. In reality, the effect of powder on SiC crystal could definitely exhibit the complicated correlation. Therefore, the present research was focused to investigate the quality difference of SiC crystal grown by conventional PVT method with using various SiC powders. As shown in Fig. 1, we used three SiC powders with different particles size. The 6H-SiC crystals were grown by conventional PVT process and the SiC seeds and the high purity SiC source materials are placed on opposite side in a sealed graphite crucible which is surrounded by graphite insulation[5, 6]. The bulk SiC crystal was grown at $2300^{\circ}C$ of the growth temperature and 50mbar of an argon pressure. The axial thermal gradient across the SiC crystal during the growth is estimated in the range of $15\sim20^{\circ}C/cm$. The chemical etch in molten KOH maintained at $450^{\circ}C$ for 10 min was used for defect observation with a polarizing microscope in Nomarski mode. Electrical properties of bulk SiC materials were measured by Hall effect using van der Pauw geometry and a UV/VIS spectrophotometer. Fig. 2 shows optical photographs of SiC crystal ingot grown by PVT method and Table 1 shows electrical properties of SiC crystals. The electrical properties as well as crystal quality of SiC crystals were systematically investigated.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.6
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• pp.215-219
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• 2016

Vanadium-doped SiC crystals have been grown by using a porous graphite inner crucible filled with vanadium carbide (VC) and by using a porous graphite plate and SiC + VC powders, respectively. Semi-insulating SiC crystals were grown onto the 6H-SiC seed crystals by PVT (Physical Vapor Transport) method. The grown crystals were indicated to be 6H-SiC polytype by XRD. As result of SIMS analysis, vanadium-rich precipitates were observed when the vanadium concentration was relatively higher than the maximum solubility of vanadium ($3-5{\times}10^{17}cm^{-3}$) in vanadium-doped SiC crystals, which resulted in degradation of crystal quality.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.24 no.10
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• pp.799-802
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• 2011

In this study, SiC single-crystal ingots were prepared on two seed crystals with different doping level by using the physical vapor transport (PVT) technique; then, SiC crystal wafers sliced from the grown SiC ingot were systematically investigated to find the effect of seed doping level on the doping concentration and crystal quality of the SiC. To exclude extra effects induced by adjustment of the process parameters, we simultaneously grew the SiC crystals on two seed crystals with different level, which were fabricated from previous two SiC crystal ingots.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.11a
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• pp.207-207
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• 2006

We investigated the effects of hydrogen addition to the growth process of SiC single crystal using sublimation physical vapor transport(PVT) techniques. Hydrogen was periodically added to an inert gas for the growth ambient during the SiC bulk growth Grown 2"-SiC single crystals were proven to be the polytype of 6H-SiC and carrier concentration levels of about $10^{17}/cm^3$ was determined from Hall measurements. As compared to the characteristics of SiC crystal grown without using hydrogen addition, the SiC crystal without definitely exhibited lower carrier concentration and lower microplpe density as well as reduced growth rate.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.14 no.2
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• pp.50-57
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• 2004

Mercurous Bromide ($Hg_2Br_2$) crystals hold promise for many acousto-optic and opto-electronic applications. This material is prepared in closed ampoules by the physical vapor transport (PVT) growth method. We investigate the effects of solutal convection on the crystal growth rate in a horizontal configuration for diffusive-convection conditions and purely diffusion conditions achievable in a low gravity environment. Our results show that the growth rate is decreased by a factor of one-fourth with a ten reduction of gravitational acceleration near y = 2.0 cm. For 0.1 $g_O$ the growth rate pattern exhibits relatively flat which is intimately related to diffusion-dominated processes. The growth rate nonuniformity is regardless of aspect ratio across the interfacial positions from 0 to 1.5. Also, the effect of a factor of the ten reduction in the gravitational acceleration is same to both Ar = 5 and 2. The enlargement in the molecular weight of B from 50 to 500 by a factor 4 causes a decrease in the maximum growth rate by the same factor, indicative of the effect of solutal gradients.

• Korean Journal of Materials Research
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• v.28 no.12
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• pp.732-737
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• 2018

We develop a purification process of $Hg_2Br_2$ raw powders using a physical vapor transport(PVT) process, which is essential for the fabrication of a high performance acousto-optic tunable filter(AOTF) module. Specifically, we characterize and compare three $Hg_2Br_2$ powders: $Hg_2Br_2$ raw powder, $Hg_2Br_2$ powder purified under pumping conditions, and $Hg_2Br_2$ powder purified under vacuum sealing. Before and after purification, we characterize the powder samples through X-ray diffraction and X-ray photoelectron spectroscopy. The corresponding results indicate that physical properties of the $Hg_2Br_2$ compound are not damaged even after the purification process. The impurities and concentration in the purified $Hg_2Br_2$ powder are evaluated by inductively coupled plasma-mass spectroscopy. Notably, compared to the sample purified under pumping conditions, the purification process under vacuum sealing results in a higher purity $Hg_2Br_2$ (99.999 %). In addition, when the second vacuum sealing purification process is performed, the remaining impurities are almost removed, giving rise to $Hg_2Br_2$ with ultra-high purity. This high purification process might be possible due to independent control of impurities and $Hg_2Br_2$ materials under the optimized vacuum sealing. Preparation of such a highly purified $Hg_2Br_2$ materials will pave a promising way toward a high-quality $Hg_2Br_2$ single crystal and then high performance AOTF modules.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.25 no.4
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• pp.127-134
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• 2015

Aluminum nitride (AlN) single crystals have attracted much attention for a next-generation semiconductor application because of wide bandgap (6.2 eV), high thermal conductivity ($285W/m{\cdot}K$), high electrical resistivity (${\geq}10^{14}{\Omega}{\cdot}cm$), and high mechanical strength. The bulk AlN single crystals or thin film templates have been mainly grown by PVT (sublimation) method, flux method, solution growth method, and hydride vapor phase epitaxy (HVPE) method. Since AlN suffers difficulty in commercialization due to the defects that occur during single crystal growth, crystalline quality improvement via defects analyses is necessary. Etch pit density (EPD) analysis showed that the growth misorientations and the defects in the AlN surface exist. Transmission electron microscopy (TEM) and electron back-scattered diffraction (EBSD) analyses were employed to investigate the overall crystalline quality and various kinds of defects. TEM studies show that the morphology of the AlN is clearly influenced by stacking fault, dislocation, second phase, etc. In addition EBSD analysis also showed that the zinc blende polymorph of AlN exists as a growth defects resulting in dislocation initiator.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.26 no.12
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• pp.863-866
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• 2013

SiC crystal ingots were grown on 6H-SiC dual-seed crystals with different surface roughness and different seed orientation by a PVT (Physical Vapor Transport) method. 4H and 15R-SiC were grown on seed crystal with high root-mean-square (rms) value. The polytype of grown crystal on the seed crystal with lower rms value was confirmed to be 6H-SiC. On the other hand, all SiC crystals grown on seed crystals with different seed orientation were proven to be 6H-SiC. The surface roughness of seed crystals had no effect on the crystal structure of the grown crystals. However, the crystal quality of 6H-SiC single crystals grown on the on-axis seed were revealed to be slightly better than that of 6H-SiC crystal grown on the off-axis seed.

• Journal of the Korean Ceramic Society
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• v.48 no.4
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• pp.312-315
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• 2011

The effect of slurry composition and wafer flatness on a material removal rate (MRR) and resulting surface roughness which are evaluation parameters to determine the CMP characteristics of the on-axis 6H-SiC substrate were systematically investigated. 2-inch SiC wafers were fabricated from the ingot grown by a conventional physical vapor transport (PVT) method were used for this study. The SiC substrate after the CMP process using slurry added oxidizers into slurry consisted of KOH-based colloidal silica and nano-size diamond particle exhibited the significant MRR value and a fine surface without any surface damages. SiC wafers with high bow value after the CMP process exhibited large variation in surface roughness value compared to wafer with low bow value. The CMPprocessed SiC wafer having a low bow value of 1im was observed to result in the Root-mean-square height (RMS) value of 2.747 A and the mean height (Ra) value of 2.147 A.