• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.2
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• pp.55-60
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• 2022

In this study, a heat treatment experiment was conducted to select a new melt composition that can easily control the unintentionally doped nitrogen (N-UID) without degrading the SiC single crystal quality during TSSG process. The experiment was carried out for about 2 hours at a temperature of 1900℃ under Ar atmosphere. The used melt composition is based on either Si-Ti 10 at% or Si-Cr 30 at%, and also Co or Sc transition metals, which are effective for carbon solubility, were added at 3 at%, respectively. After the experiment, the crucible was cross-sectionally cut, and evaluated the Si-C reaction layer on the crucible-melt interface. As a result, with Sc addition, Si-C reaction layers uniformly occurred with a Si-infiltrated layer (~550 ㎛) and a SiC interlayer (~23 ㎛). This result represented that the addition of Sc is an effective transition metal with high carbon solubility and can feed carbon sources into the melt homogeneously. In addition, Sc is well known to have low reactivity energy with nitrogen compared to other transition metals. Therefore, we expect that both growth rate and Nitrogen UID can be controlled by Si-Sc based melt in the TSSG process.

• Korean Journal of Crystallography
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• v.4 no.1
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• pp.42-48
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• 1993

KTP(KTiOPO4) single crystals were grown by the TSSG(top seeded solution growth) method using the Ksp401s flux. A heat-pipe based growing furnace was used, and the temperature stability and the homogenity of the growing solution in the platinum crucible were within the level of It 0.5℃ and ±0.9℃, respectively. The effects of some operating variables such as operating temperature range, initial cooling rate, forced stirring, reuse of the flux were investigated. As the initial cooling rate was decreased to the degree of 0.1℃/hr and some proper stirring effect by the crystal rotation was introduced to the present experimental condition, bigger and better crystals without inclusion grew. A single crystal with the maximum sixte of 44 ×39 ×17mm3 was obtained and showed the SHG conversion efficiency of 21.39) even without the anti-refilection coating.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.5 no.1
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• pp.19-24
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• 1995

Large size potassium lithium niobate (KLN) crystals with dimensions of $8{\times}6{\times}2 mm^3$ were grown by the top - seeded solution growth (TSSG) method. The extraordinary refractive index $n_e$at the second harmonic frequency for KLN crystal depends on the composition and decreases in this crystal due to the large Li content. KLN crystal was characterized by observation in UV - VIS spectrometry. It is transparent from the ultraviolet to infrared spectral regions that the transmission limit and cut- off wavelength are about 350 and 380 nm.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1999.06a
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• pp.227-250
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• 1999

The reproducibility of successive growth of Bi12TiO20(BTO) single crystals using a top-seeded solution growth (TSSG) pulling method was evaluated by measuring the lattice constants and their standard deviations. A substantial phase diagram in the region close to the stoichiometric BTO was established experimentally for this purpose, and the existence of a retrograde solid solution close to a BTO was clarified. It was emphasize that a starting solution, with a 10.0~10.1 mol% TiO2 concentration, results in large single crystals with a highly homogeneous lattice constant of within $\pm$1x10-4$\AA$, when the solidified fraction of the grown crystal is less than about 45%. A wavelength dispersion of refractive index was measured for the first time, an it was verified that the refractive index of BTO is larger than that of BSO(Bi12TiO20), allowing the voltage sensitivity of EOS higher than the case with BSO as a probe head.

• Korean Journal of Crystallography
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• v.3 no.2
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• pp.120-128
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• 1992

Single crysals of BaTiO3 were grown by TSSG technique at various cooling rates. Morpolo girts, defects and domain structures of the grown crystals were investigated. At the cooling rates below 0.5℃/hr, equant single crystals were obtained and the 11111 faces were dominantly developed. If the cooling rate was much faster or if the vortical temperature gradient in the so lotion was very large, the solution became unstable and the needle formed BasTil04 o crystals were precipitated. Two sets of parallel lamella domains are arranged perpendicular to each other and the irregularly shaped boundaries are fixed between them. These sets of domains show remarkable orientation contrast in x-ray topography. Heating the crystal above 127℃, the phase transition from tetragonal to cubic occurs. The phase transition front (PTF) moves in the direction of temperature gradient. Domains in the tetragonal phase are successively rearranged and regular strain patterns appear in the cubic phase. The habit plane of PTF in BaTi03 is found to deviate from a l1101 lattice plane by app roximately 9°.

• Korean Journal of Crystallography
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• v.3 no.1
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• pp.37-43
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• 1992

KTiOP04 is a nonlinear optical crystal which is most widely used for frequency doubling of the radiation of Nd : YAG laser. In the experiment, sin ale crystals of KTiOP04 were grown by TSSG technique using 3K2W04·P2O5 flux. Low temperature gradient furnace suitable for KTP single crystal growth was used. Seed crystal was placed at the surface of the solution for the purpose of better observation of the growing crystals and the possibility of diameter control. Solution included 66.7mol% KTiOP04 for all experiments and its saturation temperature was 1020℃. The conditions of single crystal growth were as follows: cooling rate 0.2℃/h, crystal rotation rate 50rpm, c -axis seed. Using these conditions, single crystals up to 23 ×25×25mm3 have been groan from about 100cc solution. We have also observed a change in the crystal growth habit which resulted in the formation of large (201) faces and small (100) faces. And some crystals have (101) faces.

• Journal of the Korean Ceramic Society
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• v.56 no.6
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• pp.589-595
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• 2019

The top-seeded solution growth (TSSG) method is an effective approach for the growth of high-quality SiC single crystals. In this method, the temperature gradient in the melt is the key factor determining the crystal growth rate and crystal quality. In this study, the effects of the aperture at the top of the hot-zone on the growth of the SiC single crystal obtained using the TSSG method were evaluated using multiphysics simulations. The temperature distribution and C concentration profile in the Si melt were taken into consideration. The simulation results showed that the adjustment of the aperture at the top of the hot-zone and the temperature gradient in the melt could be finely controlled. The surface morphology, crystal quality, and polytype stability of the grown SiC crystals were investigated using optical microscopy, high-resolution X-ray diffraction, and micro-Raman spectroscopy, respectively. The simulation and experimental results suggested that a small temperature gradient at the crystal-melt interface is suitable for growing high-quality SiC single crystals via the TSSG method.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1999.06a
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• pp.167-185
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• 1999

In the present paper, KLN crystals have been grown along <001>, <100> and <110> directions by the top seeded solution growth (TSSG) method from Li-richer melts with different compositions. The morphologies of KLN crystals grown along different directions have been studied, and the well-developed facets have been unambiguously indexed using X-ray goniometer and stereographic projection analysis. The growth mechanism and defects such as cracks and inclusions were discussed on the basis of observations of facets on the crystal-melt interfaces. The crystal compositions were determined by chemical analysis method. The structure and lattice constants of KLN crystals were determined and calculated on the basis of XRD data by using TREOR90 and PIRUM programs. The Curie temperature and optical absorption were determined by dielectric constant peak and spectrum measurements, respectively. The blue SHG characteristics of a KLN sample were also investigated using a pulsed dye laser. PACS: 42.70.M;81.10;81.10A;42.65.K.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.9 no.4
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• pp.424-431
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• 1999

The reproducibility of successive growth of $Bi_{12}TiO_{20}$ (BTO) single crystlas using a top-seeded solution growth (TSSG) pulling method was evalutated by measuring the lattice constants and their standard deviations. A substantial phase diagram in the region close to the stoichiometric BTO was established expermentally for this purpose, and the existence of a retrograde solid solution close to a BTO was clarified. It was emphasized that a starting solution, with a 10.0~10.1 mol% $TiO_{2}$ concentration, results in large single crystals with a highly homogeneous lattice constant of within ${\pm}1{\times}10^{-4}\AA$, when the solidified fraction of the grown crystal is less than about 45 %. A wavelength dispersion of refractive index was measrued for the first time, and it was verified that the refractive index of BTO is larger than that of BSO($Bi_{12}TiO_{20}$), allowing the voltage sensitivity of EOS higher than the case with BSO as a probe head.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.32 no.6
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• pp.516-521
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• 2019

The top seeded solution growth (TSSG) method is an alternative technique to grow high-quality SiC crystals that has been actively studied for the last two decades. However, the TSSG method has different issues that need to be resolved when compared to the commercial SiC crystal growing method, i.e., physical vapor transport (PVT). A particular issue of the TSSG method of results from the presence of liquid droplets on the grown crystal that can remain even after crystal growth; this induces residual stress on the crystal surface. Hence, the residual droplet causes several unwanted effects on the crystal such as the initiation of micro-cracks, micro-pipes, and polytype inclusions. Therefore, this study investigated the formation of the residual droplet through multiphysics simulations and lead to the development of a liquid droplet removal method. As a result, we found that although residual liquid droplets significantly apply residual stress on the grown crystal, these could be vaporized by adopting thermal annealing processes after the relevant crystal growing steps.