• Title/Summary/Keyword: Czochralski Single Crystal Growth

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A TECHNIQUE TO OPTICALLY DETERMINE THE STOICHIOMETRY OF $C_2$ GROWN LITHIUM NIOBATE CRYSTALS (Czochralski법으로 성장시킨 $LiNbO_3$단결정의 화학양론(Stoichiometry)을 결정하기 위한 광학적 방법)

  • Kim, You-Song
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.1 no.2
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    • pp.1-14
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    • 1991
  • In growing single crystals, which exhibit incongruent melting behavor, it is extremely difficult to maintain the stoichiometry of its chemical compositions for given crystals. For instance, $LiNbO_3$ is a typical one which exhibits such incongruent melt, especially with a large solid solution region that makes it difficult to maintain the chemical compositions. Such a variation can then cause a serious problem for the practical applications in designing a precision electro /optic device. Of the known methods of determining its composition and quality, an optical technique of measuring refractive index of the crystals has been implemented. This technique is also capable of determining optical uniformity of the grown crystals and the chemical compositions. The technique used for such characterizations is herein described and some of results are discussed.

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Crystal Growth of Yb:YAG and Fabrication of Microchip Laser Device (Yb:YAG 단결정 성장과 마이크로칩 레이저 소자 제조)

  • 이성영;김충렬;김도진;정석종;유영문
    • Journal of the Korean Ceramic Society
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    • v.38 no.8
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    • pp.771-776
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    • 2001
  • 용액인상법으로 질소분위기 하에서 Yb$^{3+}$ 이온이 각각 5, 15, 25 at% 치환된 Yb:Y$_3$Al$_{5}$ O$_{12}$ (Yb:YAG) 단결정을 이리듐 도가니를 사용하여 성장시켰다. 양질의 단결정을 성장시키기 위한 인상속도와 회전속도는 각각 2mm/h와 10rpm이었다. 흡수 및 형광스펙트럼 측정결과, Yb$^{3+}$ 이온의 농도가 높아짐에 따라 흡수계수가 선형적으로 증가하였고, 1051nm 파장을 중심으로 1020~1050nm 영역에서 선폭이 확대된 강한 형광스펙트럼을 나타내었다. 한편, 성장된 단결정을 이용하여 마이크로칩 레이저용 소자를 정밀하게 제조하였다.

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Research for High Quality Ingot Production in Large Diameter Continuous Czochralski Method (대구경 연속성장 초크랄스키법에서 고품질 잉곳 생산을 위한 연구)

  • Lee, Yu Ri;Jung, Jae Hak
    • Current Photovoltaic Research
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    • v.4 no.3
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    • pp.124-129
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    • 2016
  • Recently industry has voiced a need for optimally designing the production process of low-cost, high-quality ingots by improving productivity and reducing production costs with the Czochralski process. Crystalline defect control is important for the production of high-quality ingots. Also oxygen is one of the most important impurities that influence crystalline defects in single crystals. Oxygen is dissolved into the silicon melt from the silica crucible and incorporated into the crystalline a far larger amount than other additives or impurities. Then it is eluted during the cooling process, there by causing various defect. Excessive quantities of oxygen degrade the quality of silicone. However an appropriate amount of oxygen can be beneficial. because it eliminates metallic impurities within the silicone. Therefore, when growing crystals, an attempt should be made not to eliminate oxygen, but to uniformly maintain its concentration. Thus, the control of oxygen concentration is essential for crystalline growth. At present, the control of oxygen concentration is actively being studied based on the interdependence of various factors such as crystal rotation, crucible rotation, argon flow, pressure, magnet position and magnetic strength. However for methods using a magnetic field, the initial investment and operating costs of the equipment affect the wafer pricing. Hence in this study simulations were performed with the purpose of producing low-cost, high-quality ingots through the development of a process to optimize oxygen concentration without the use of magnets and through the following. a process appropriate to the defect-free range was determined by regulating the pulling rate of the crystals.

The Crystal Growth of $Bi_{12}GeO_{20}$ Single Crystal by the CZ Technique with New Weighing Sensor (II) (새로운 무게센서에 의한 $Bi_{12}GeO_{20}$ 단결정 육성연구(II))

  • 장영남;배인국
    • Korean Journal of Crystallography
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    • v.9 no.1
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    • pp.30-38
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    • 1998
  • A new frequency weighing sensor was applied to grow Bi12GeO20 crystals in the auto-di-ameter control system of Czochralski method. The rotation rate was varied in the range of 23 to 21 rpm to preserve flat interface in a given heat configuration. To prevent the constitutional super-cooling from the evaporation loss, 105% stoichiometric amount of Bi2O3 was employed, equivalent to 6.18 molar ratio of Bi2O3 to GeO2. Transparent and light brown Bi12GeO20 single crystal in uniform diameter was grown. The dislocation density was determined to be 103/cm2 corresponding to the optical quality in commercial applications. The grown crystal measured diameter 25 mm and length 70 mm and the preferred growth direction was confirmed to be <110>.

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Analysis of surface defect in RE : YAG (RE = Nd3+, Er3+, Yb3+) single crystal using chemical polishing and etching (화학적 polishing 및 etching을 통한 RE : YAG (RE = Nd3+, Er3+, Yb3+) 단결정의 표면 결함 분석)

  • Shim, Jang Bo;Kang, Jin Ki;Lee, Young Kuk
    • 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.

A Numerical study of the fluctuation behavior of the oxygen concentration and the temperature in the silicon melt of Czochralski crystal growth system

  • Yi, Kyung-Woo;Kim, Min-Cheol
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1997.06a
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    • pp.197-201
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    • 1997
  • The momentum, heat and mass trasfer phenomena in the silicon melt of the Czochralki crystal growth system are calculated using a three dimensional numerical simulation thechnique. Even though axisymmetrical boundary conditions are imposed to all calculations in a 3cm diameter crucible, several types of non-axisymmetric profiles of velocities, temperature and oxygen concentration appeared in the melt. Because of the non-axisymmetric profiles of velocities, temperature and oxygen concentration appeared in the melt. Because of the non-axisymmetric profiles and rotations of fluid induced by the crucible rotation, temperatures and oxygen concentrations in the silicon melt fluctuate. The rotating velocity of the profile is calculated from the phase shift of the data of temperature or oxygen at two different points which have same radius from center but 90 degree angular difference. From this calculation, it is found that the rotating veolocity of the oxygen and temperature is different from the crucible rotation rates. Therefore the frequencies of the oscillating temperature and oxygen concentrations are not same to the frequencies of the crucible rotations. Futhermore, the components of the frequencies of the temperature and oxygen concentration at the same point are not same. The fluctuation behaviors of the temperature or oxygen themselves are also different when the points are different. The calculation show that the temperature and the oxygen concentration near the interface also fluctuate. The results suggest that the striation pattern found in the grown silicon single crystals may ben generated by the oxygen concentration and the temperature oscillations of the melt occurred near the interface.

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Growth and defect structures of undoped and heavily MgO-doped LiNbO3 single crystals (Undoped and heavily MgO-doped $LiNbO_3$ 결정의 성장 및 결함구조)

  • 김상수
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.5
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    • pp.447-453
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    • 1999
  • Congruent $LiNbO_3$ crystals with doped Mg and codoped with Mn or Fe were grown by the Czochralski method. It is known that the physical properties of $LiNbO_3$ depend strongly on the addition of Mg and transition metals. This is established by studying the following properties; XRD patterns, the phase transition temperature, energy of the fundamental absorption edge, the shape of the absorption band of the $OH^-$ vibration and lines of the ESR of $Fe^{3+},\; Mn^{2+}$. The position of the UV absorption edge and the shape and peak point of the absorption band of the $OH^-$ vibrational band changed monotonously up to a critical concentration of $Mg^{2+}$ ions. The mechanism of the incorporation of Mg ions changes at this concentration. The transition temperature was estimated by measuring the dielectric temperature behavior up to $1230^{\circ}C$ in a frequency range of 100Hz to 10MHz. EPR of $Mn^{2+}\;and\; Fe^{3+}$ ions were employed to investigated the Mg doping effects in the $LiNbO_3$ crystal. The increase of linewidths and the asymmetry of signals were observed in all crystals. New signals of $Fe^{3+}$ arising from the new centers were observed I the heavily Mg-doped crystals.

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Growth of $LiTaO_3$ and Fe doped-LiTaO3 single crystal as holographic storage material (홀로그래피 소자재료 $LiTaO_3$단결정 성장)

  • 김병국;윤종규
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.2
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    • pp.193-204
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    • 1998
  • The single crystal of the $LiTaO_3$has large electro-optic effects, so it is applied to optical switch, acousto-optic deflector, and optical memory device as hologram using photorefractive effect. In this study, optic-grade undoped $LiTaO_3$and Fe:LiTaO$LiTaO_3$single crystals were grown by the Czochralski method and optical transmission and absorption spectrums were measured in the wavelength of UV-VIS range. The curie temperature was determined with DSC and by measuring capacitance for the grown undoped crystal and ceramic powder samples of various Li/Ta ratio. In case of having a 48.6 mol% $Li_2O$ as a starting Li/Ta ratio, the results of concentration variations were below 0.01 mol% $Li_2O$ all over the crystal, so it was confirmed that $LiTaO_3$single crystals were grown under congruent melting composition having optical homogeneity. The curie temperature of the Fe:$LiTaO_3$crystal was increased with increased with increased doped Fe concentrations;by the ratio of $7.5^{\circ}C$ increase per Fe 0.1 wt%. Also, the optical transmittance was about 78 %, which was sufficient for optical device.

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The Growth of $MgO:LiNbO_3$ Single Crystal by Czochralski Method and its Density Measurement (Czochralski법에 의한 $MgO:LiNbO_3$단결정 성장과 밀도 측정)

  • Kim, Il-Won;Park, Bong-Chan;Kim, Gap-Jin
    • Korean Journal of Crystallography
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    • v.4 no.2
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    • pp.74-85
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    • 1993
  • Single crystals of LiNbO3 have found extensive application in electro-optic and nonlinear optic devices. However, laser-induced refartive index inhomogeneities, which have been labeled opical damage impose limits on device optical damage in LiNbO3 is imporved if more than 4.5 rml% MgO is added to the melt The laser damage thrueshold increased as much as 100 times better then that of undoped crystals. The MgO doped cystal has thus been urterlsiv81y studied since then. In the study, Mgo:LiNbOs(MLA) single crystals dopsd with 0, 2.5, 5.0, 7.5, 10.0 mol% MgO have been grown by the czocrualski technique. The metls were prepared in the platinum crluible and 15∼20mm diameter crystals were grown with a length of 20∼30mm in a resitance heater. The growth rate was 2.5mm/hr, the rotation speed 15rpn. Before sawing MLN single crystals were annealed for 24 hours under atmosphere at a temperature of 1080℃. After sawing, we have found an annual ring cross section of MNA crystals only in the direction of perpendicilar to the c-axis. Nonuniform dispusion of MgO was pointed out that the cuties of the state of oxide were strongly affected by oxygen partial pressure in.

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Crystal Growth of $Cr:Al_2O_3$ and $Ti:Al_2O_3$ by Czochralski Technique (용액인상법에 의한 $Cr:Al_2O_3$$Ti:Al_2O_3$ 단결정 육성)

  • Yu, Yeong-Mun;Lee, Yeong-Guk;Park, Ro-Hak
    • Korean Journal of Crystallography
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    • v.6 no.1
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    • pp.1-13
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    • 1995
  • Cr:A12O3 and Ti:A12O3 single crystals were grown by Czochralski method, and the effects of crystal growth parameters such as pulling rate, rotation rate, dopant and growth atmosphere on crystal quality were investigated. And spectroscopic properties including lasing efficiency were also measured. Single crystals, sized of 20mm in diameter and 100-135mm in length, were successfully grown from the seed of <001> direction. With the doping level of 0.5w/o Cr2O3, pulling rate 2.0mm/hr, rotation rate of 30rpm and inert atmosphere by nitrogen gas, high quality crystals of Cr:A12O3 were grown. While in case of Ti:A12O3 crystals, high quality crystals were grown under the conditions of the doping level of 0.25w/o TiO2, pulling rate of 1.5mm/hr, rotation rate of 30rpm and reducing atmosphere by hydrogen - nitrogen mixed gas. It was confirmed that Cr3+ ion which maintains its ionoc valence during growth easily de-bubbled than Ti4+ ion which changes its valence, Fe3+ ion also has do-bubbling effect to Ti:A12O3 crystal and the reducing atmosphere by 90% N2 - 10% H2 mixed gas gave effective result on the changing of Ti4+ to Ti3+ and de-bubbling. As a result of spectroscopic measurements of Cr:A12O3 crystal, 4A2 →4F2 and 4F1 absorption transitions and E →4A2(R1) and 2A →4A2(R2) fluorenscence transitions were confirmed. And it was measured that wavelengths of laser R1 and R2 transitions were 696±5nm and 692±5nm respectively, line width of these transitions were 12A, and life-time of fluorenscence was 152μsec. In case of Ti:A12O3 crystals, it was confirmed that absortion transition of 4T2→4E and fluorescence transition of 4E→4T2 with wide range of 650-1050nm was occured. And 147μsec of life-time of fluorescence, 125.4 of figure of merit and 9% of laser efficience were also measured.

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