This study aimed to grow single crystals with low dislocation density using a heat exchange method using room temperature water, and investigated the effect of the structure of the heat exchanger under the crucible on the defects and dislocation density of the single crystals and the shape of the solid-liquid interface of the crystals, and obtained the following conclusions. The dislocation density of sapphire single crystal grown at 2,200℃ for 30 min and a growth rate of 0.2℃/min was 0.92x103pcs/㎠. Mo guard was used to stabilize the solid-liquid interface grown from seeds, and sapphire single crystals with a diameter of 130㎜ and a height of 75㎜ were grown.
Solid state grain growth (SSCG) is a method of growing large single crystals from seed single crystals by abnormal grain growth in a small-grained matrix. During grain growth, pores are often trapped in the matrix and remain in single crystals. Aerosol deposition (AD) is a method of manufacturing films with almost full density from nano grains by causing high energy collision between substrates and ceramic powders. AD and SSCG are used to grow single crystals with few pores. BaTiO3 films are coated on (100) SrTiO3 seeds by AD. To generate grain growth, BaTiO3 films are heated to 1,300 oC and held for 10 h, and entire films are grown as single crystals. The condition of grain growth driving force is ΔGmax < ΔGc ≤ ΔGseed. On the other hand, the condition of grain growth driving force in BaTiO3 AD films heat-treated at 1,100 and 1,200 oC is ΔGc < ΔGmax, and single crystals are not grown.
Single crystals, which have complexed composition, are fabricated by solid state grain growth. However, it is hard to achieve stable properties in a single crystal due to trapped pores. Aerosol deposition (AD) is suitable for fabrication of single crystals with stable properties because this process can make a high density coating layer. Because of their unique features (nano sized grains, stress inner site), it is hard to fabricate single crystals, and so studies of grain growth behavior of AD film are essential. In this study, a BaTiO3 coating layer with ~ 9 μm thickness is fabricated using an aerosol deposition method on (100) and (110) cut SrTiO3 single crystal substrates, which are adopted as seeds for grain growth. Each specimen is heat-treated at various conditions (900, 1,100, and 1,300℃ for 5 h). BaTiO3 layer shows different growth behavior and X-ray diffraction depending on cutting direction of SrTiO3 seed. Rectangular pillars at SrTiO3 (100) and laminating thin plates at SrTiO3 (110), respectively, are observed.
Grain-growth behavior in the 95Na1/2Bi1/2TiO3-5BaTiO3 (mole fraction, NBT-5BT) system has been investigated with the addition of Na2CO3. When Na2CO3 is added to NBT-5BT, the growth rate is higher than desired and grains are already impinging each other during the initial stage of sintering. The grain size decreases as the sintering temperature increases. With the addition of Na2CO3, a liquid phase infiltrates the interfaces between grains during sintering. The interface structure can be changed to be more faceted and the interface migration rate can increase due to fast material transport through the liquid phase. As the sintering temperature increases, the impingement of abnormal grains increases because the number of abnormal grains increases. Therefore, the average grain size of abnormal grains can be decreased as the temperature increases. The phenomenon can provide evidence that grain coarsening in NBT-5BT with addition of Na2CO3 is governed by the growth of facet planes, which would occur via mixed control.
The γ/γ´ two-phases, commonly known as a eutectic structure, are observed in the γ interdendritic region of a Nibase superalloy. However, the growth behavior of the γ/γ´ two-phases, whether it is of eutectic or peritectic nature, has not been decidedly established. Directional solidifications were, thus, performed with the planar interface at a low growth rate of 0.5 μm/s in order to promote macro segregation. Directional solidification started with the γ planar interface and the γ´ phase nucleated on the γ planar interface at the solidification fraction of 0.75. The γ/γ´ two-phases showed the γ´ rod structure as major phase and the γ minor phase between γ´ rods, and the volume fraction of the γ phase changed continuously with an increasing solidification fraction. The two-phase γ/γ´ is seen as the coupled peritectic.
A stoichiometric mixture of evaporating materials for ZnAl2Se4 single-crystal thin films was prepared in a horizontalelectric furnace. These ZnAl2Se4 polycrystals had a defect chalcopyrite structure, and its lattice constants were a0=5.5563Åand c0=10.8897Å.To obtain a single-crystal thin film, mixed ZnAl2Se4 crystal was deposited on the thoroughly etched semi-insulating GaAs(100) substrate by a hot wall epitaxy (HWE) system. The source and the substrate temperatures were 620oCand 400oC, respectively. The crystalline structure of the single-crystal thin film was investigated by using a double crystal X-ray rocking curve and X-ray diffraction ω-2θ scans. The carrier density and mobility of the ZnAl2Se4 single-crystal thin filmwere 8.23×1016cm−3 and 287m2/vs at 293K, respectively. To identify the band gap energy, the optical absorption spectra ofthe ZnAl2Se4 single-crystal thin film was investigated in the temperature region of 10-293K. The temperature dependence ofthe direct optical energy gap is well presented by Varshni's relation: Eg(T)=Eg(0)−(αT2/T+β). The constants of Varshni'sequation had the values of Eg(0)=3.5269eV, α=2.03×10−3eV/K and β=501.9K for the ZnAl2Se4 single-crystal thin film.The crystal field and the spin-orbit splitting energies for the valence band of the ZnAl2Se4 were estimated to be 109.5meVand 124.6meV, respectively, by means of the photocurrent spectra and the Hopfield quasicubic model. These results indicatethat splitting of the ∆so definitely exists in the Γ5 states of the valence band of the ZnAl2Se4/GaAs epilayer. The threephotocurrent peaks observed at 10K are ascribed to the A1-, B1-exciton for n=1 and C21-exciton peaks for n=21.
Two-dimensional (2D) nano patterns including a two-dimensional Bravais lattice were fabricated by laser interference lithography using a two step exposure process. After the first exposure, the substrate itself was rotated by a certain angle, 90˚ for a square or rectangular lattice, 75˚ for an oblique lattice, and 60˚ for a hexagonal lattice, and the 90˚ and laser incident angle changed for rectangular and the 45˚ and laser incident angle changed for a centered rectangular; we then carried out a second exposure process to form 2D bravais lattices. The band structure of five different 2D nano patterns was simulated by a beam propagation program. The presence of the band-gap effect was shown in an oblique and hexagonal structure. The oblique latticed ZnO nano-photonic crystal array had a pseudo-bandgap at a frequency of 0.337-0.375, 0.575-0.596 and 0.858-0.870. The hexagonal latticed ZnO nano-crystallite array had a pseudo-bandgap at a frequency of 0.335-0.384 and 0.585-0.645. The ZnO nano structure with an oblique and hexagonal structure was grown through the patterned opening window area by a hydrothermal method. The morphology of 2D nano patterns and ZnO nano structures were investigated by atomic force microscopy and scanning electron microscopy. The diameter of the opening window was approximately 250 nm. The height and width of ZnO nano-photonic crystals were 380 nm and 250 nm, respectively.
Single crystal ZnIn2S4 layers were grown on thoroughly etched semi-insulating GaAs(100) substrateat 450oC with hot wall epitaxy (HWE) system by evaporating ZnIn2S4 source at 610oC. The crystalline structureof the single crystal thin films was investigated by the photoluminescence (PL) and double crystal X-ray rockingcurve (DCRC). The temperature dependence of the energy band gap of the ZnIn2S4 obtained from theabsorption spectra was well described by the Varshni’s relation, Eg(T)=2.9514eV-(7.24×10−4eV/K)T2/(T+489K). After the as-grown ZnIn2S4 single crystal thin films were annealed in Zn-, S-, and In-atmospheres, theorigin of point defects of ZnIn2S4 single crystal thin films has been investigated by the photoluminescence (PL)at 10K. The native defects of VZn, VS, Znint, and Sint obtained by PL measurements were classified as a donorsor acceptors type. And we concluded that the heat-treatment in the S-atmosphere converted ZnIn2S4 singlecrystal thin films to an optical p-type. Also, we confirmed that In in ZnIn2S4/GaAs did not form the nativedefects because In in ZnIn2S4 single crystal thin films existed in the form of stable bonds.
결정성장 도중 전류에 의해 고/액 계면에서 발생하는 Peltier 열을 이용하면 온도구배의 증가와 이에 따른 성장속도의 증가 및 결정성의 향상에 기여할 것이라 예상되어, 고/액 계면에서 복합적으로 발생하는 Peltier 효과를 조사하였다. 전류 밀도, 극성 및 온도구배의 변화에 따른 고상과 액상 및 그 계면에서의 온도변화로부터 이론적 추론에 의해 Peltier 열, Thomson 열 및 Joule 열만의 영향으로 분류할 수 있었고, 고상/액상 계에 대한 Peltier 계수 및 Thomson 계수도 구할 수 있었다.
P-type Si(111)기판 위에 3C-SiC박막 성장시 TMS(tetramethylsilane)유량, 반응온도, 반응압력, 가스공급방법등 다양한 성장변수에 따른 박막의 결정성변화를 연구하였다. 증착된 막은 모두 (111)방향성만을 나타내었고, free Si, C의 존재는 관찰할 수 없었다. TMS 유량 0.5 sccm에서, 1100-1200˚C의 반응온도에서 , 반응압력 12-50Torr 조건에서 비록 dislocation과 twin등이 발결되었으나 단결정 3C-SiC 박막을 성장시킬 수 있었으며, 박막의 결정성은 기판에 흡착된 Si-종과 C-종이migration할 수 있는 시간과 에너지에 크게 영향 받음을 확인할 수 있었다. 또한 SiC/Si계면에서 carbonization공정에서 관찰되는 것으로 알려진 void를 관찰할 수 있었으며, 이러한 void의 발생은 기체공급방법을 달리함으로서 제거할 수 있음을 확인할 수 있었다.
결정 성장 조절체를 이용하여 수용액 중에서 직접 α산화철을 제조하였으며, 염기도에 따른 생성물의 입자 특성과 반응기구, α산화철의 생성 과정과 침상형 입자의 생성 반응 기구를 고찰하였다. pH 9.0이하에서는 hexagonalgudxo, pH 10.75-11.75범위에서는 ellipsoidal 또는 rectangular 형태의 α-Fe2O3입자로 각각 생성되었으며, pH12.50이상에서는 acicular 형태의 α-FeOOH입자가 생성되었다. pH 10.75-11.75범위에서 제조된 생성물의 염기도는 결정 성장 조절제의 해리에 의해 생성된 수산기 이온(OH-) 때문에 반응물의 염기도에 대비해 약간 증가하는 현상을 나타내었다. 결정 성장 조절제로 사용한 구연상은 제이철 수산화물에 구연산 음이온(R-COO-) 형태로 흡착되어 생성물인 α산화철의 입자 형태를 침상 형태로 유도하였다.
K6P4 O13 flux로부터 30×40×70㎣ 크기의 inclusion이 없는 KTP 단결성을 성장시켰다 성장된 KTP 결정의 SHG 출력 특성 측정 결과 위상정합각은 θ=90˚, φ=23.3˚이었고, φ방향의 angular acceptance는 약 2˚이었다. KTP 결정내 굴절율 변화에 따른 위상정합각 편차는 최대 0.17˚까지 변하였다. 또한 Nd : YAG와 brewster plate를 채용한 내부공진형의 diode pumped SHG module에 KTP 결정을 삽입하여 20mW의 녹색 laser를 얻었다.
아라고나이트는 탄산칼슘(CaCO3)의 동질이상 중 하나이며, 해양 생태계를 포함한 다양한 환경에서 생물학적 및 이화학적 침전 과정을 통해 형성된다. 이러한 아라고나이트의 형성 및 성장뿐만 아니라 아라고나이트 내 스트론튬(Sr)과 같은 미량원소의 치환 특성은 화학종의 농도와 온도와 같은 핵심 인자들에 의해 많은 영향을 받는다. 본 연구에서는 해양 생태계와 유사한 용액 온도와 아라고나이트에 대한 이 용액의 다양한 포화도 조건에서 아라고나이트 내 Sr 병합 특성이 규명되었다. 반응 용액의 주입속도(0.085-17 mL/min), 반응 용액의 이온 농도([Ca]=[CO3] 0.01-1M), 혼합 용액의 온도(5-40 oC)의 다양한 실험 조건에서 컨스턴트-에디션 (constant-addition) 방법을 통해 순수한 아라고나이트가 합성되었다. 또한, 모든 Sr 병합 실험 조건(0.02-0.5 M, 15-40 oC)에서도 순수한 아라고나이트가 형성되었다. 합성된 아라고나이트의 결정도와 결정크기는 포화도 및 온도가 증가함에 따라 상대적으로 더 크게 증가하며 아라고나이트 결정이 더 많이 성장하였음을 지시하였다. 그러나 BET-비표면적을 이용하여 계산된 결정성장속도는 결정 형상 변화에 크게 영향을 받는 것으로 나타나 해석에 주의가 요구된다. 아라고나이트 내 Sr의 분배계수(KSr)는 반응이온의 농도가 0.02에서 0.5 M로 증가할 때 2.37에서 1.57로, 온도가 15에서 40˚C로 증가할 때 1.90에서 1.54로 감소하였으며, 모든 조건에서 KSr 값이 1보다 높게 관찰되었다. 이러한 결과는 KSr가 결정성장속도와 역의 상관관계로서 아라고나이트 내 Sr 병합이 호정성 관계임을 나타낸다.
본 연구에서는 보수 모르타르와 직접 혼합 가능한 결정성장형 자기치유 고상캡슐을 제조하였으며, 자기치유 고상캡슐이 혼합된 보수 모르타르의 품질 및 균열 치유 성능 특성을 평가하였다. 자기치유 고상캡슐을 혼합한 보수 모르타르의 테이블 플로우 및 공기량 평가 결과 혼합율에 관계없이 테이블 플로우 및 공기량은 큰 영향이 없는 것으로 나타났다. 압축강도는 캡슐 혼합율이 증가할수록 강도가 감소하는 경향이 나타났다. 정수위 투수시험에 따른 균열 치유 특성 평가 결과 초기 투수량이 감소하는 결과가 나타났으며, 시간 경과에 따라 반응 생성물 발생하여 균열이 치유되는 것을 확인 할 수 있었다.