• Title/Summary/Keyword: Floating zone melting

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$LiTaO_3$ single crystal growth by the halogen floating zone method I. Growth characteristics of LT single crystals (Halogen floating zone 법에 의한 $LiTaO_3$ 단결정 성장$I.LiTaO_3$단결정 성장특성)

  • 류정호;임창성;오근호
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.4
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    • pp.528-535
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    • 1997
  • $LiTaO_3$ single crystals of congruently melting composition were grown by the halogen lamp type floating zone system. Calcination and sintering parameters for the growth were established. Optimum crystal growth conditions were investigated by a controlling of growth rates, rotation speeds and atmospheres. Based on the melting aspect and the shape of molten zone, stable conditions could not be found in air or Na atmosphere. However the growth stability in Ar atmosphere was more regular than that in air or $N_2$. The grown crystals were characterized using Laue back reflection, Curie temperature, refractive index and transmittance. Curie temperature fluctuation in the section of the grown crystal part of top, body and tail was $1^{\circ}C$.

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Purification and Single Crystal Growth of Molybdenum by Electron Beam Floating Zone Melting (Electron Beam Floating Zone Melting에 의한 몰리브덴의 정련 및 단결정 성장에 관한 연구)

  • 최용삼;지응준
    • Korean Journal of Crystallography
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    • v.3 no.2
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    • pp.85-97
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    • 1992
  • EBFZM( Electron Beam Floating Zone Melting) 법을 이용하여 몰리브덴에서의 금속계 불순물과 침입형 불순물의 정련기구 및 단결정 성장기구를 연구하 였다. Fe, Cr, Co등의 금속계 불순물은 몰리브덴과의 평형증기압의 차이에 따른 불순물의 선택적 증발에 의하여 우수한 정련효과를 나타내며, 몰리브덴보다 응점이 높은 Ta, W는 잘 제거되지 않았다. 한편 대역 정제에 의한 정련효과는 미약함을 확인하였다. EBF ZM은 C,0,N등의 침입형 불순물의 정련에도 효과적 이었다. 본 연구의 모든 조건에서 몰리브덴은 단결정으로 성장하였으며 2차 재결정 epitaxy에 의한 단결 정 성장기구가 제시되었다. 몰리브덴 단결정 내의 전 위밀도는 strain-anneal법에 의한 단결정의 경우보다 높았으며,본 실험의 열처리 조건에서는 변화하지 않았다. The purification and single crystal growth mechanisms of molybdenum were analysed in EBFZM ( electron beam floating zone melting). Metallic impurities of Fe, Cr, Co were purified efficiently but Ta and W were not removed well in this study. It was due to a preferential evaporation of the elements caused by the difference in equillibrium vapor pressure between the elements and molybdenum. The pu- rification effect by zone refining was not significant. The EBFZM also refined the interstitial impurities of C, 0 and N, effectively. The single crystals of molybdenum were grown regardless of the experimental conditions and the secondary recrystallization epitaxy was surge sled as a growth mechanism. The dislocation density in single crystal was higher than that by strain-anneal method, and was not reduced by heat treatments.

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Study on the Purification and Single Crystal Growth of Niobium Metal by Electron Beam Floating Zone Melting (Electron Beam Floating Zone Melting에 의한 니오븀의 정련 및 단결정 성장에 관한 연구)

  • 최용삼;확준섭
    • Korean Journal of Crystallography
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    • v.3 no.2
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    • pp.72-84
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    • 1992
  • The investigation has been carried out for purification, single crystal growth mechanism and convective phenomena in EBFZM of Nb metal. It is found that the EBFZM refined effectively oxygen and nitrogen, the interstitial impurities in Nb, but carbon was increased slightly by backstream of diffusion pump oil. The mechanism of single crystal growth associated with the second recrystallieation in Nb was suggested from the relationship between texture of starting materials and the crystal growth in EBFZM. It was observed from the investigation of convection phenomena in molten zone that the Marangoni convection was dominant in molten zone, which caused the striation in Nb and increased the purification effect of oxygen and nitrogen.

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Spinel$(MgAl_2O_4)$ single crystal growth by floating zone method (Floating zone 법에 의한 Spinel$(MgAl_2O_4)$단결정 성장)

  • Seung Min Kang;Byong Sik Jeon;Keun Ho Orr
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.3
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    • pp.325-335
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    • 1994
  • The spinel $MgO.Al_20_3$ single crystals were grown by FZ (floating zone) method. Its melting point is about, $2135^{\circ}C$ and is important to the process of the growth from the melt. There have been some reports of the growth by Czochralski and Verneuil method. However, this study is the first trial to the spinel crystal with the application of FZ method. In this study, $MgAl_2O_4$ spinel crystals were grown by using FZ method which uses the ellipsoidal mirror furnace having infrared halogen lamps as a heat source. With dopants of transition metal ions, it was possible to melt the feed rod which does not absorb the infrared rays due to the transparent properties to infrared ray of spinel itself and the red, green and blue colored spinel single crystals could be grown more easily. As a conclusion, the purpose of this study is to find the spinel single crystal growth mechanism with respect to th growth interfaces and molten zone stability and to characterize the state of growth resulting from the concavity to the melt of interfaces.

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Effects of microstructures of the sintered rod on the single crystal grown by the floating zone method (Floating zone법에 의한 결정성장시 소결봉의 미세구조에 의한 영향)

  • 신재혁;오근호
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.5 no.3
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    • pp.250-260
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    • 1995
  • In general, a sintered rod is used as a feed in the growth of crystals by the floating zone(FZ) method. The sintering condition of the feed rod affected the stability of molten zone because it influenced the interface shape between the feed and the melt during the crystal growth. In this study, rutile and ruby crystals were chosen as samples to analyze the effect of the microstructures of the feed rods. In sintering of the feed rod for the growth of rutile and ruby single crystals, the difference of grain size between the inner and the outer region of the feed rod increased with the sintering temperature and dwelling time. As a result, it altered melting behavior of the feed. The uniform grain size of the sintered rod was necessary for the optimum growing condition of crystals. The effect of pores in the feed rod was not a dominant factor to grow crystals by the FZ method, which was confirmed by growing crystals with nonsinterd rods as feeds.

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Phase Orientation of TiC-$TiB_2$-SiC Ternary Eutectic Composite Prepared by an FZ Method

  • Tu, Rong;Li, Wenjun;Goto, Takashi
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09b
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    • pp.859-860
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    • 2006
  • TiC-$TiB_2$-SiC system was a ternary eutectic, whose eutectic composition was 34TiC-$22TiB_2$-44SiC (mol%). TiC-$TiB_2$-SiC ternary eutectic composite were synthesized by a floating zone method using TiC, $TiB_2$ and SiC powders as starting materials. The TiC-$TiB_2$-SiC eutectic composite showed a lamellar texture. TiC(022), $TiB_2(010)$ and SiC(111) of the eutectic composite were perpendicular to the growth direction. TiC-$TiB_2$-SiC ternary eutectic composite had specific relationship among the crystal planes: TiC[011]//$TiB_2[010]$//SiC[112], TiC(200)//$TiB_2$(001)//SiC(402) and $TiC(1\bar{1}1)$//$TiB_2(101)$//SiC(220).

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The Synthesis of Vanadium-Doped Forsterite by the $H_2O_2$-Assisted Sol-Gel Method, and the Growth of Single Crystals of Vanadium-Doped Forsterite by the Floating Zone Method

  • 박동곤;Mikio Higuchi;Rudiger Dieckmann;James M. Burlitch
    • Bulletin of the Korean Chemical Society
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    • v.19 no.9
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    • pp.927-933
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    • 1998
  • Polycrystalline powder of vanadium-doped forsterite (Vδ $Mg_2SiO_4$) was synthesized by the $H_2O_2$-assisted sol-gel method. The vanadium dopant, which was added as VO$(OMe)_3$ in methanol, went through several redox reactions as the sol-gel reaction proceeded. Upon adding VO$(OMe)_3$ to a mixture of $Mg(OMe)_2$ and Si$(OEt)_4$ in methanol, V(V) reduced to V(IV). As hydrolysis reaction proceeded, the V(IV) oxidized all back to V(V). Apparently, some of the V(V) reduced to V(IV) during subsequent gelation by condensation reaction. The V(IV) remained even after heat treatment of the gel in highly oxidizing atmosphere. The crystallization of the xerogel around 880 ℃ readily produced single phase forsterite without any minor phase. Using the polycrystalline powder as feeding stock, single crystals of vanadium-doped forsterite were grown by the floating zone method in oxidizing or reducing atmosphere. The doping was limited in low level because of the high partitioning of the vanadium in liquid phase during melting. The greenish single crystal absorbed visible light of 700∼1100 nm. But, no emission was obtained in near infrared range.

Optical process of polysilicaon on insulator and its electrical characteristics (절연체위의 다결정실리콘 재결정화 공정최적화와 그 전기적 특성 연구)

  • 윤석범;오환술
    • Electrical & Electronic Materials
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    • v.7 no.4
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    • pp.331-340
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    • 1994
  • Polysilicon on insulator has been recrystallized by zone melting recrystallization method with graphite strip heaters. Experiments are performed with non-seed SOI structures. When the capping layer thickness of Si$\_$3/N$\_$4//SiO$\_$2/ is 2.0.mu.m, grain boundaries are about 120.mu.m spacing and protrusions reduced. After the seed SOI films are annealed at 1100.deg. C in NH$\_$3/ ambient for 3 hours, the recrystallized silicon surface has convex shape. After ZMR process, the tensile stress is 2.49*10$\^$9/dyn/cm$\^$2/ and 3.74*10$\^$9/dyn/cm$\^$2/ in the seed edge and seed center regions. The phenomenon of convex shape and tensile stress difference are completely eliminated by using the PSG/SiO$\_$2/ capping layer. The characterization of SOI films are showed that the SOI films are improved in wetting properties. N channel SOI MOSFET has been fabricated to investigate the electrical characteristics of the recrystallized SOI films. In the 0.7.mu.m thickness SOI MOSFET, kink effects due to the floating substrate occur and the electron mobility was calculated from the measured g$\_$m/ characteristics, which is about 589cm$\^$2//V.s. The recrystallized SOI films are shown to be a good single crystal silicon.

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The Study on the Crystal Growing of Mn-Zn Ferrite Single Crystals by Floating Zone Method (Floating Zone법에 의한 Mn-Zn Ferrite 단결정성장에 관한 연구)

  • 정재우;오근호
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.2 no.1
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    • pp.10-19
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    • 1992
  • Mn - Zn Ferrite has physical properties of the high initial permeability, saturation magnetic flux density, and low loss factor as a representative magnetic material of soft ferrites, in addition the mechanical property is excellent as a single crystal. Therefore it is important electronic components and used for VTR Head. Mn - Zn Ferrite single crystals with the diameter 8mm were grown in atmosphere mixed with $O_2$ and Ar gas by the Floating Zone(FZ) method that impurities can not be incorporated to the crystals because of not-using the crucible to put in the melt, and the sharp temperature gradient results from making a focus at one point utilizing the infrared ray emitted from the halogen lamp as a heat source. During the crystal growing, the highest temperature of melting area was maintained to be $1650^{\circ}C$, growth rate and rotation rate were 10 mm/hr, 20 rpm respectively. The phases and the growth directions of crystals were determined from the analysis of X RD patterns, Laue, TEM diffraction patterns and etch pit shapes were observed by the optical microscope through the chemical etching. The corelation of optimum conditions for acquiring the better crystals was found out with the growth rate, the length and diameter of melt at the interface according to the diameter of feed rod, and the patterns of growing interface also studied.

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