• Title/Summary/Keyword: Czochralski Single Crystal Growth

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Single Crystal Growth of $(TeO_2)$ by CZ Technique (용액인상법에 의한 파라텔루라이트 $(TeO_2)$ 단결정 육성)

  • Sohn, Wook;Jang, Young-Nam;Bae, In-Kook;Chae, Soo-Chun;Moon, H-Soo
    • Korean Journal of Crystallography
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    • v.6 no.2
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    • pp.141-157
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    • 1995
  • Single crystals of TeO2 with large diameter were grown by Czochralski technique with auto-diameter control system. The ratio of crystal to crucible was 60-70%. The effect of critical pulling and rotation rate on the crystal quality was studied. Optimum growth parameters for high quality crystal pulling rate was less than 1.2 mm/hr. The solid-liquid interface was convex at the rotation rate of 10-23 rpm and concave at the rotation rate of more than 25 rpm, depending on the size of crystal and crucible. The platinum concentration in the melts is one of the main factors of the constitutional supercooling and thus the bubble entrapment in the growing crystal. Growth axis was confirmed to {110} direction during the whole growth procedure. Infrared spectrometric study and dislocation density measurment by chemical etching method on the grown crystal were performed. Finally, the reasons of cooperation of striations, inclusions, and optical inhomogeneities were discussed.

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Crystal Growth of LiNbO3 for SAW Devices (SAW Device 응용을 위한 LiNbO3 단결정 성장)

  • 최종건;오근호
    • Journal of the Korean Ceramic Society
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    • v.25 no.1
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    • pp.78-82
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    • 1988
  • Good quality LiNbO3 single crystals which can be applied to SAW devices, were grown by Czochralski method. It was observed that the gas-bubbles were concentrated in ring shape at the outer part of grown crystals, and this anomaly was illustrated by modeling the mechanism of gas-bubble entrapment according to the melt flow pattern in the crucible. And this mechanism was also encertained by observation of solid-liquid interface shape of grown crystals. The optimal condition for good quality crystals was known that the solid-liquid interface shape was slightly concave.

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Growth Properties of Tungsten-Bronze Sr1-xBaxNb2O6 Single Crystals (텅스텐 브론즈 Sr1-xBaxNb2O6 단결정의 성장 특성)

  • Joo, Gi-Tae;Kang, Bonghoon
    • Korean Journal of Materials Research
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    • v.22 no.12
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    • pp.711-716
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    • 2012
  • Tungsten bronze structure $Sr_{1-x}Ba_xNb_2O_6$ (SBN) single crystals were grown primarily using the Czochralski method, in which several difficulties were encountered: striation formation and diameter control. Striation formation occurred mainly because of crystal rotation in an asymmetric thermal field and unsteady melt convection driven by thermal buoyancy forces. To optimize the growth conditions, bulk SBN crystals were grown in a furnace with resistance heating elements. The zone of $O_2$ atmosphere for crystal growth is 9.0 cm and the difference of temperature between the melt and the top is $70^{\circ}C$. According to the growth conditions of the rotation rate, grown SBN became either polycrystalline or composed of single crystals. In the case of as-grown $Sr_{1-x}Ba_xNb_2O_6$ (x = 0.4; 60SBN) single crystals, the color of the crystals was transparent yellowish and the growth axis was the c-axis. The facets of the crystals were of various shapes. The length and diameter of the single crystals was 50~70 mm and 5~10 mm, respectively. Tungsten bronze SBN growth is affected by the temperature profile and the atmosphere of the growing zone. The thermal expansion coefficients on heating and on cooling of the grown SBN single crystals were not matched. These coefficients were thought to influence the phase transition phenomena of SBN.

The $PbWO_{4}:Nb$ single crystal growth and its optical properties ($PbWO_{4}:Nb$ 단결정의 성장과 그 광학적 특성)

  • 장경동;김도형;양희선;이상걸;박효열;이진호;이동욱;이상윤
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.2
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    • pp.141-148
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    • 1999
  • High quality pure and Nb-doped $PbWO_{4}$ Single Crystal were grown from a 50 %~50 % mixture of Lead oxide (PbO) and Tungsten oxide $(WO_{3})$ by Czochralski method in Iridium crucible. The stoichiometric deviation correspond to the selective loss of the crystal constituents is found to be responsible for the yellowish coloration of $PbWO_{4}$. Through the X-ray powder diffraction experiment, we have investigated the lattice constant variations of each $PbWO_{4}$ crystals. We also present information on their photoluminescence (PL), optical absoption properties and Raman spectra. The temperature dependence of PL intensity and FWHM (Full Width Half Maximum) were measured in the temperature range 10 K~300 K. One observes a slight temperature dependence in the low temperature region and PL intensity decreases over 200 K by thermal quenching. The activation energy, Huang-Rhys coupling constant and inhomogenious brodenning acquired from their temperature dependence.

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The intrinsic instabilities of fluid flow occured in the melt of Czochralski crystal growth system

  • Yi, Kyung-Woo;Koichi Kakimoto;Minoru Eguchi;Taketoshi Hibiya
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06a
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    • pp.179-200
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    • 1996
  • The intrinsic instabilities of fluid flow occurred in the melt of the Czochralski crystal growth system Czochralski method, asymmetric flow patterns and temperature profiles in the melt have been studied by many researchers. The idea that the non-symmetric structure of the growing equipment is responsible for the asymmetric profiles is usually accepted at the first time. However further researches revealed that some intrinsic instabilities not related to the non-symmetric equipment structure in the melt could also appear. Ristorcelli had pointed out that there are many possible causes of instabilities in the melt. The instabilities appears because of the coupling effects of fluid flow and temperature profiles in the melt. Among the instabilities, the B nard type instabilities with no or low crucible rotation rates are analyzed by the visualizing experiments using X-ray radiography and the 3-D numerical simulation in this study. The velocity profiles in the Silicon melt at different crucible rotation rates were measured using X-ray radiography method using tungsten tracers in the melt. The results showed that there exits two types of fluid flow mode. One is axisymmetric flow, the other is asymmetric flow. In the axisymmetric flow, the trajectory of the tracers show torus pattern. However, more exact measurement of the axisymmetrc case shows that this flow field has small non-axisymmetric components of the velocity. When fluid flow is asymmetric, the tracers show random motion from the fixed view point. On the other hand, when the observer rotates to the same velocity of the crucible, the trajectory of the tracer show a rotating motion, the center of the motion is not same the center of the melt. The temperature of a point in the melt were measured using thermocouples with different rotating rates. Measured temperatures oscillated. Such kind of oscillations are also measured by the other researchers. The behavior of temperature oscillations were quite different between at low rotations and at high rotations. Above experimental results means that the fluid flow and temperature profiles in the melt is not symmetric, and then the mode of the asymmetric is changed when rotation rates are changed. To compare with these experimental results, the fluid flow and temperature profiles at no rotation and 8 rpm of crucible rotation rates on the same size of crucible is calculated using a 3-dimensional numerical simulation. A finite different method is adopted for this simulation. 50×30×30 grids are used. The numerical simulation also showed that the velocity and flow profiles are changed when rotation rates change. Futhermore, the flow patterns and temperature profiles of both cases are not axisymmetric even though axisymmetric boundary conditions are used. Several cells appear at no rotation. The cells are formed by the unstable vertical temperature profiles (upper region is colder than lower part) beneath the free surface of the melt. When the temperature profile is combined with density difference (Rayleigh-B nard instability) or surface tension difference (Marangoni-B nard instability) on temperature, cell structures are naturally formed. Both sources of instabilities are coupled to the cell structures in the melt of the Czochralski process. With high rotation rates, the shape of the fluid field is changed to another type of asymmetric profile. Because of the velocity profile, isothermal lines on the plane vertical to the centerline change to elliptic. When the velocity profiles are plotted at the rotating view point, two vortices appear at the both sides of centerline. These vortices seem to be the main reason of the tracer behavior shown in the asymmetric velocity experiment. This profile is quite similar to the profiles created by the baroclinic instability on the rotating annulus. The temperature profiles obtained from the numerical calculations and Fourier transforms of it are quite similar to the results of the experiment. bove esults intend that at least two types of intrinsic instabilities can occur in the melt of Czochralski growing systems. Because the instabilities cause temperature fluctuations in the melt and near the crystal-melt interface, some defects may be generated by them. When the crucible size becomes large, the intensity of the instabilities should increase. Therefore, to produce large single crystals with good quality, the behavior of the intrinsic instabilities in the melt as well as the effects of the instabilities on the defects in the ingot should be studied. As one of the cause of the defects in the large diameter Silicon single crystal grown by the

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Preparation and characterization of nearly stoichiometric $LiNbO_3$ crystals by VTE method (VTE법에 의한 nearly stoichiometric $LiNbO_3$의 성장 및 특성)

  • 김상수;유동선
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.1
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    • pp.6-17
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    • 1997
  • Lithium niobate single crystals with various [Li]/[Nb] ratios were grown by the Czochralski method from melts having compositions varing between 48.6 ~ 58.0 mol % $Li_2O$. A vapor transport equilibration technique has been used to improve the homogeneity and adjust the [Li]/[Nb] ratio in small $LiNbO_3$ single crystals grown by the Czochralski method. When equilibrated with a Li-rich powder (65 mol%$Li_2O$), containing a mixture of $LiNbO_3$ and $Li_3NbO_4$, crystals of nearly stoichiometric composition can be obtained. This was established by studying the composition dependence of the following properties; lineshape, intensity and linewidth for the electron paramagnetic resonance (EPR) of $Fe^{3+}$ energy of the fundamental absorption edge and $OH^-$ absorption spectra.

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Congruent Melt Composition of $LiTaO_3$ Single Crystal ($LiTaO_3$ 단결정의 완전용융조성)

  • 정대식;박병학;김유성;노용래
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.3 no.2
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    • pp.99-106
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    • 1993
  • A relationship $(T_c = -17.869C^2+1840.2C-46623)$ between Curie Temperature$(T_c)$ and (C), $Li_2O$ mole percent(%) was established from the measurement results of Curie temperature $(T_c)$) analysed by DTA(Differential Thermal Analysis) in the range from 48.50 to 49.00 $Li_2O$ mole %. Congruent melt composition of $LiTaO_3$ single crystal was to be 48.65 $Li_2O$ mole % and its Curie temperature was also determined to be $610{\pm}1^{\circ}C$ from the results of Curie temperature difference, ${\Delta}T (T_{c(Top)}-T{_c(Tail)})$ of Czochralski grown $LiTaO_3$ crystals and the distribution coefficient(k). The k was calculated from $LiO_2$ mole ratio of initial melt to final melt and initial crystal to final crystal in the range from 48.60 to 48.70 $Li_2O$ mole %.

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A promising new piezoelectric material -Langasite and its related compounds-

  • Kawanaka, Hiroyuki;Takeda, Hiroaki;Shimamura, Kiyoshi;Onozato, Norio;Fukuda, Tsuguo
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1997.06a
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    • pp.145-145
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    • 1997
  • Recent progress of electric technology requires new piezoelectric crystals having superior properties such as zero temperature coefficients and large electromechanical coupling factors. We have developed a series of new leading chandidates, La$_3$Ga5SiO14(langasite, LGS), La3Nb0.5Ga5.5O14(LNG), La3Ta0.5O14(LTG), to satisfy those requirements. High quality LGS, LNG and LTG single crystals, with dimensions of 2 inches in diameter, were successfully grown by the Czochralski method at a pulling rate of 1mm/h. Since no variation of chemical composition was observed when whole melt in a crucible was crystallized, congruency of these compositions was confirmed. Physical constants such as elastic constants, dielectric constants and piezoelectric constants were measured. Filters and oscillators made of grown LGS, LNG and LTG single crystals showed superior properties such as three times wider passband than that of quartz, low insertion loss and easy processing, Langasite family crystals were shown to be superior materials to other known materials such as quartz, LiTaO$_3$, $\alpha$-AlPO$_4$ and Li$_2$B$_4$O7.

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Crystal Growth of Yb:YCa4O(BO3)3 and Investigation of Spectroscopic and Thermal Properties (Yb:YCa4O(BO3)3 단결정 성장과 분광 및 열적 특성 연구)

  • Kim, Choong-Ryeul;Lee, Hyeon-Jun;Yu, Young-Moon
    • Journal of the Korean Ceramic Society
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    • v.39 no.8
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    • pp.795-800
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    • 2002
  • Yb:$YCa_4O(BO_3)_3$ (Yb:YCOB) single crystal, in which the concentration of $Yb^{3+}$ ion 20 at%, was grown by the Czocharalski method using an iridium crucible under N2 atmosphere. The optimum growth parameters to get a high quality of single crystals were found to be 1.5∼2 mm/h of pulling rate and 10∼20 rpm of rotation rate. According to the results of spectroscopic properties, absorption edge of Yb:YCOB was 236 nm. Two strong absorption line due to $Yb^{3+}$ ions were observed at 900 and 975 nm. Thermal expansion coefficients of Yb:YCOB crystal along a, b and c crystallographic axes from 320 to 650 K were 12.1${\times}10^{-6}$/K, 5.9${\times}10^{-6}$/K, 12.9${\times}10^{-6}$/K, respectively. Specific heat was 0.162 $cal/g{\cdot}K$ at 330 K.

KCl Crystal Growth and High Energy X Ray Expose of Properties (KCl 단결정의 성장 및 고 에너지 X선 조사 특성)

  • Park, Cheol-Woo
    • The Journal of Korean Society for Radiation Therapy
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    • v.20 no.1
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    • pp.31-36
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    • 2008
  • Purpose: X ray irradiates material for dose distribution confirmation through material color variation to evaluate about possibility. Materials and Methods: That is rare earth material to pure KCl and KCl impurity Eu adding 0.5mol% by Czochralski method each single crystal grow and observed color variation of KCl X ray irradiation use of linear accelerator. Results: High energy X ray irradiation KCl:Eu show the blue fluorescence with purple color that pure KCl single crystal can confirm by show was not observed, but was colored violet. Conclusion: Colors variation of KCl founds stable color center from radiation and this color variation will be used usefully to X ray measurement material and phantom.

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