• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.327-327
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• 2012

사파이어는 우수한 광학적, 물리적, 화학적 특성을 가지고 있는 물질 중의 하나이며, 청색 발광특성을 나타내는 GaN와 격자상수, 열팽창 계수가 가장 유사할 뿐만 아니라 가격도 상대적으로 저렴하기 때문에 GaN 성장을 위한 기판으로 사용될 수 있다. 실제로 사파이어는 프로젝터와 전자파 장치, 군사용 장비 등 다양한 분야에 응용되고 있으며, 발광 다이오드(LED)를 위한 기판으로 활용됨으로써 그 수요가 급격히 증가하고 있다. 그러나 사파이어 결정의 성장 중에 생길 수 있는 전위(dislocation)와 적층결함(stacking fault) 등의 결정 결함들은 결정 내에 존재하여 역학적, 전기적 성질에 큰 영향을 미칠 수 있다. 특히 사파이어가 청색 발광소자의 기판으로 사용되는 경우, 사파이어 기판 내부의 결정 결함은 증착되는 박막 특성에 영향을 미치게 된다. 따라서 사파이어의 보다 나은 응용을 위해서는 결정 결함에 대한 평가기술과 결함의 형성 메커니즘 등에 대한 이해가 필요하다. 특히, 결함의 정량적 평가 기술의 개발은 사파이어의 상용화에 중요한 핵심요소 중 하나이다. 결정을 산이나 염기 등을 이용하여 화학적 식각을 하게 되면 분자나 원자 간의 결합이 약한 부분이나 높은 에너지 상태에 있는 부분부터 반응을 하게 되는데, 이러한 반응을 통해 결정의 표면에 형성되는 것을 에치 피트(etch pit)라고 한다. 일반적으로 결정 내에 존재하는 전위는 높은 에너지 상태이므로, 이러한 에치 피트는 전위와 관련되어 있다. 따라서 사파이어 결정과 같은 결정질 물질은 표면의 식각을 통하여 관찰되는 에치 피트 등의 형상이나 반응성 등을 평가하여 결정 특성을 연구할 수 있다. 본 연구는 화학적 식각법으로 사파이어 결정의 특성을 평가하기 위하여 진행하였다. 사파이어 결정의 식각을 위하여 다양한 산-염기 용액들이 사용되었다. 식각 용액의 종류에 따른 사파이어 결정의 식각거동을 연구하고, 표면에 나타나는 형상을 연구하여 사파이어 결정의 구조적 특성을 파악하였다. 특히, 에치 피트 형성거동의 시간 및 온도 의존성에 관한 연구를 진행하였다.

• Korean Journal of Crystallography
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• v.7 no.1
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• pp.73-80
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• 1996

The single crystal growth has been carried out with the newly designed 1-T HB(single temperature zone horizontal Bridgman) system for GaAs crystals of 2 inch diameter doped with Si, Zn or undoped. With this method, incidence probability of single crystallinity was shown to be 0.73. Lattice defects evaluated from EPD(etch pit density) measurement were in the range of 5,000-20,000/cm2, dependent upon the doping condition. For the undoped GaAs crystals, carrier concentrations from the Hall measurement were ∼1×1016/cm3 at the seed part, which were less than half the concentrations of double of triple temperature zone(2-T, 3-T) HB grown crystals. By the 1-T HB method, therefore, GaAs crystals can be grown successfully with better yield and higher purity.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.35 no.5
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• pp.504-508
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• 2022

Single crystal gallium oxide (Ga₂O₃) has been an emerging material for power semiconductor applications. However, the defect distribution of Ga₂O₃ substrates needs to be carefully characterized to improve crystal quality during crystal growth. We analyzed the type and the distribution of defects on commercial (-201) Ga₂O₃ substrates to get a basic standard prior to growing Ga₂O₃ crystals. Etch pit technique was employed to expose the type of defects on the Ga₂O₃ substrates. Synchrotron white beam X-ray topography was also utilized to observe the defect distribution by a nondestructive manner. We expect that the observation of defect distribution with three-dimensional geometry will also be useful for other crystal planes of Ga₂O₃ single crystals.

• Korean Journal of Metals and Materials
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• v.46 no.3
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• pp.169-173
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• 2008

Characteristics of etching and induced surface morphology variation by wet-etching of n-type GaN were investigated using phosphoric acidic solutions. Generally, the etch-rate was increased as the temperature of the etch solutions was increased, and the highest etch rate of about $300{\AA}/min$ was achieved at the temperature of $180^{\circ}C$. The morphology variation of the etched surface was observed by optical microscopy and atomic force microscopy. Initially, high density of hexagonal holes or pits were formed on the etched surface at the time of 40 min with the bimodal size of $20{\mu}m$ or $5{\mu}m$, respectively. However, as the etching time was increased further, the lateral size of the hexagonal holes or pits was increased, and finally, joined and merged together at the time of 100 min. This means that the etching of n-type GaN by phosphoric acidic solutions proceeded through the lateral widening and the merging of initial holes and pits.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.5
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• pp.196-201
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• 2014

We investigated defects and surface polarity in AlN and GaN by using wet chemical etching. Therefore, the effectiveness and reliability of estimating the single crystals by defect selective etching in NaOH/KOH eutectic alloy have been successfully demonstrated. High-quality AlN and GaN single crystals were etched in molten NaOH/KOH eutectic alloy. The etching characteristics and surface morphologies were carried out by scanning electron microscope (SEM) and atomic force microscope (AFM). The etch rates of AlN and GaN surface were calculated by etching depth as a function of etching time. As a result, two-types of etch pits with different sizes were revealed on AlN and GaN surface, respectively. Etching produced hexagonal pits on the metal-face (Al, Ga) (0001) plane, while hexagonal hillocks formed on the N-face. On etching rate calibration, it was found that N-face had approximately 109 and 15 times higher etch rate than the metal-face of AlN and GaN, respectively. The size of etch pits increased with an increase of the etching time and they tend to merge together with a neighbouring etch pits. Also, the chemical mechanism of each etching process was discussed. It was found that hydroxide ion ($OH^-$) and the dangling bond of nitrogen play an important role in the selective etching of the metal-face and N-face.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.4
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• pp.131-134
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• 2016

The conditions for chemical polishing and etching technique were investigated to reveal surface defects in RE : YAG ($RE=Nd^{3+},\;Er^{3+},\;Yb^{3+}$) single crystals grown by Czochralski method. The optimal condition for chemical polishing was in 85 % $H_3PO_4$ solution at $330^{\circ}C$ for 30 minutes with a specimen fixed in the vertical direction. In addition, the optimal condition for chemical etching was in 85 % $H_3PO_4$ solution at $260^{\circ}C$ for 1 hour, and $70{\sim}80{\mu}m$ sized triangular etch pits were observed on (111) face. As a result of defect density analysis, $1.9{\times}10^3/cm^2$ for Nd(1 %) : YAG, $4.3{\times}10^2/cm^2$ for Er(7.3 %) : YAG, and $5.1{\times}10^2/cm^2$ for Yb(15 %) : YAG were measured.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.4
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• pp.135-139
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• 2014

The hydride vapor phase epitaxy (HVPE) grown GaN samples to precisely measure the surface characteristics was applied to a molten KOH/NaOH wet chemical etching. The etching rate by molten KOH/NaOH wet chemical etching method was slower than that by conventional etching methods, such as phosphoric and sulfuric acid etching, which may be due to the formation of insoluble coating layer. Therefore, the molten KOH/NaOH wet chemical etching is a better efficient method for the evaluation of etch pits density. The grown GaN single crystals were characterized by using X-ray diffraction (XRD) and X-ray rocking curve (XRC). The etching characteristics and surface morphologies were studied by scanning electron microscopy (SEM). From etching results, the optimum etching condition that the etch pits were well independently separated in space and clearly showed their shape, was $410^{\circ}C$ and 25 min. The etch pits density obtained by molten KOH/NaOH wet chemical etching under optimum etching condition was around $2.45{\times}10^6cm^{-2}$, which is commercially an available materials.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.13 no.4
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• pp.168-171
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• 2003

$YMnO_{3}$ single crystals have been grown by a floating zone technique and the optimal growth conditions were investigated. Their crystallinity and microstructure were characterized by the chemical etch pit patterns, their distribution and the compositional difference depending on the G value. In particular, the microstructural feature was interpreted in terms of compositional deviation along radial direction on (1010) growth plane.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.5
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• pp.202-206
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• 2010

Single crystals of $ZnWO_4$ were grown successfully in the [100], [010] and [001] directions using the Czochralski method. The growth parameters and the formation of slip plane in $ZnWO_4$ crystals were studied. $ZnWO_4$ crystals had a cleavage plane of (010). The dislocation density on the (010) plane at the center of the crystal was lower than that of the edge region. It was inferred that the high density at the edge of the crystals was caused by the thermal gradient during crystal growth. The etch pit arrangement revealed the (100) slip plane to be most active during crystal growth.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.6
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• pp.237-241
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• 2014

We investigated the optimal etching conditions and properties of the surface change due to molten KOH/NaOH chemical wet etching using an AlN wafer which has been put to practical use in the present study. Results were observed using a scanning electron microscope after 5 minutes etching at $350^{\circ}C$, was found to have a surface form of the respective other Al-face, the N-face. In particular, etch-pit in the form of a hexagon, which is observed in the Al-face appeared, It was calculated at $2{\times}10^6/cm^2{\sim}10^{10}/cm^2$ dislocation density. In the case of N-face, lattice defects in the form of the hexagonal pyramids is formed. It was discovered that in order to observe the orientation of the wafer, which corresponds to the C-axis direction of the resulting hexagonal AlN which was analyzed using XRD (0002) and is a state of being oriented in the (0004) plane. The Radius of curvature of AlN wafer was 1.6~17 m measured by DC-XRD rocking curve position.