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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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Crystal Growth of rutiles doped with Impurity Ions by Floating Zone Method (부유대용융법에 의한 불순이온 주입된 $TiO_2$단결정 성장 연구)

  • 이성영;유영문;김병호
    • Proceedings of the Korea Crystallographic Association Conference
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    • 1999.04a
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    • pp.1-1
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    • 1999
  • 부유대용융법에 의하여 불순이온의 종류와 각 이온의 주입 농도를 달리하는 Rutile 단결정을 성장하였다. 성장된 결정으로부터 제조한 박편시료를 이용하여 결정결함과 광투과도에 미치는 각 불순이온의 영향을 조사하였다. 결정성장용 주원료로 99.99%의 TiO2를 사용하고, 불순이온 주입을 위한 원료로서 99.99%의 Al2O3, H3BO3, Ga2O3, Sc2O3, V2O5, Fe2O3, ZrO2, Er2O3, Cr2O3를 각각 사용하였다. 불순이온의 종류에 따르는 영향을 조사하기 위하여 TiO2 99.8 atomic%-불순이온 0.2atomic%의 조성이 되도록 각 이온별로 원료를 정밀하게 평량하고 균일 혼합하였다. 불순 이온의 첨가량에 따르는 영향을 조사하기 위하여 Al2O3는 각각 pure, 0.2, 0.4, 0.6 atomic%를, Cr2O3는 pure, 0.003, 0.05, 0.2 atomic%를 각각 치환하여 원료를 조합하였다. 균일 혼합된 원료를 직경 8mm의 고무 튜브에 넣고 CIP(Cold Isostatic Press0에서 2000kg/$\textrm{cm}^2$의 압력으로 성형한 후 150$0^{\circ}C$에서 1시간 소결함으로서 결정성장용 다결정 원료를 합성하였다. 합성된 다결정을 double ellipsoidal mirror 내에 설치하고,halogen lamp로 가열하여 원료의 한쪽 끝을 용융한 다음, 20rpm의 회전속도, 3-5mm/hr의 성장속도로 하는 유속 1$\ell$/min의 O2 분위기속에서 부유대용융법에 의하여 결정을 성장하였다. 성장된 결정을 성장축에 수직한 방향으로 각각 절단, 연삭, 연마한 박편을 이용하여 편광하에서 low-angle grain boundaries 및 기타의 결정결함을 관찰하였으며, 0.3$\mu\textrm{m}$~0.8$\mu\textrm{m}$ 범위 및 0.6$\mu\textrm{m}$~3.4$\mu\textrm{m}$ 범위에서의 투과 및 흡수 스펙트럼을 측정하였다. 결정 성장 결과 B3+, Er3+, Cr3+ 이온은 Ti4+ 이온과 이온의 크기 차이가 심하여 결정의 정상적인 성장을 방해하는 물성을 나타냈고, V5+, Cr3+ 이온은 흑색의 결정, Fe3+ 이온은 적갈색의 결정으로 성장되었다. Al3+, Zr4+, Al3+의 순서로 투과도가 높아지는 것이 관찰되었다. 불순이온의 농도에 따른 영향으로서 Al3+ 이온의 경우 주입농도가 높아질수록 low angle boundary와 oxygen deficiency가 감소하였고, 투과율은 조금 감소하거나 큰 차이가 없는 것으로 나타났다. 반면에 Cr3+ 이온을 주입한 경우 0.003 atomic%에서 최적의 물성을 보였으며, 주입농도가 높아질수록 결정성장이 어려워지고 광의 투과도가 급격히 저하되었다.

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Synthesis and Defect-Structure Analysis of $ThO_2-Tm_2O_3$ Solid Solutions ($ThO_2-Tm_2O_3$ 고용체의 합성 및 결함구조해석)

  • Don Kim;Chang Kwon Kang;Keu Hong Kim;Jae Shi Choi
    • Journal of the Korean Chemical Society
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    • v.31 no.6
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    • pp.491-497
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    • 1987
  • $ThO_2-Tm_2O_3$ (TDT) solid solutions containing 1,3,5,8,10, and 15 mol% $Tm_2O_3$ were synthesized from spectroscopically pure $ThO_2$ and $Tm_2O_3$ polycrystalline powders. The TDT solid solutions were indentified to the fluorite structure by the X-ray powder technique. The values of the lattice parameter were decreased with increasing amount of $Tm_2O_3$ incorporated. But, there was no linearity for the samples containing 8, 10, and 15 mol% $Tm_2O_3$. It was concluded that these samples became incomplete solid solutions. From the intensity analyses of X-ray diffraction patterns, the residual factor was found below 0.13 even for the 15 mol% TDT system. lt was confirmed from the DTA and TGA analyses that any phase transitions did not occur under the experimental condition executed. Comparing the pycnometric density with the lattice parameter obtained from XRD, it was suggested that the predominant defect model be an oxygen vacancy.

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Improvement of Structure and Electrochemical Properties of LiNi0.5Mn1.5O4 for High Voltage Class Cathode Material by Cr Substitution (Cr 치환을 이용한 고전압용 양극 활물질 LiNi0.5Mn1.5O4의 구조와 전기화학적 성능의 개선)

  • Eom, Won-Sob;Kim, Yool-Koo;Cho, Won-Il;Jang, Ho
    • Journal of the Korean Electrochemical Society
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    • v.8 no.2
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    • pp.82-87
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    • 2005
  • The cathode material, $LiNi_{0.5}Mn_{1.5}O_4$, for high voltage applications of Li-ion batteries exhibits impurity phases due to oxygen deficiency during the high temperature heat treatment. The impurity phase reduces the electrochemical properties of the electrode since the deficiency spinel structure disturbs the lithium ion intercalation and deintercalation. In this study, Cr-substituted $LiNi_{0.5-x}Mn_{1.5}Cr_xO_4(0{\leq}x{\leq}0.05)$ powders are synthesized by a sol-gel method in order to reduce the amount of the impurity phases in the $LiNi_{0.5-x}Mn_{1.5}Cr_xO_4$. Thermal analysis of the cathode material shows that the $LiNi_{0.5}Mn_{1.5}O_4$ without Cr substitution looses $2\%$ of its weight due to oxygen deficiency but the amount of weight loss is diminished when Cr is substituted. XRD analysis also supports the reduction of the impurity phases in the cathode after chromium substitution, suggesting that the improvement of the electrochemical properties such as the capacity retention and electrochemical stability are attributed to the low content of impurity phases in the Cr-substituted $LiNi_{0.5-x}Mn_{1.5}Cr_xO_4.$

Effects on the Magnetic Property Changes due to the defect in the Nuclear Reactor Vessel Material Irradiated by Fast Neutron (고속 중성자 조사에 의한 원자로 용기재료내의 결함생성이 자기적 특성변화에 미치는 영향)

  • Jeong, Myeong-Mo;Kim, Gil-Su;Jang, Gi-Sang;Yu, Geun-Bae;Park, Deok-Geun;Kim, Gil-Mu;Yun, In-Seop;Hong, Chi-Yu
    • Korean Journal of Materials Research
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    • v.9 no.12
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    • pp.1240-1244
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    • 1999
  • In order to assess the effects on the magnetic properties due to the defect in the material irradiated by fast neutron ranging $10^0-10^{18}n/cm^2$, the magnetic properties such as maximum magnetic induction, coercivity, remanence, Barkhausen Noise Amplitude(BNA), Barkhausen Noise Energy(BNE) and hardness were measured. It is shown that the magnetic properties and hardness do not change by the fast neutron irradiation under $10^{17}n/cm^2$. Therefore, in this experiment, it is understood that the magnetic properties decrease by the increase of hardness. This measurement method can be used to evaluate the neutron irradiation embrittlement nondestructively since the magnetic properties and hardness do change by the neutron irradiation over $10^{17}n/cm^2$ consistently.

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The Relative Effectiveness of Various Radiation Sources on the Resistivity Change in n-Type Silicon

  • Jung, Wun
    • Nuclear Engineering and Technology
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    • v.1 no.2
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    • pp.91-101
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    • 1969
  • Resistivity changes of n-type float-zone silicon crystals with 6.4$\times$10$^{14}$ to 1.25$\times$10$^{17}$ phosphorus atoms/㎤ due to irradiation by (1) 1 MeV electrons, (2) two types of research reactors, and (3) $Co^{60}$ ${\gamma}$-ray sources were investigated. The results were analyzed on the basis of a simple exponential formula derived by Buehler. While the formula gave a fair fit in the low fluence range in most cases, the deviation was quite appreciable in the case of 1 MeV electron irradiation, and a linear change gave better fit in some cases. The large change in the carrier removal rate in electron-irradiated samples in the high fluence range was analyzed in detail in terms of the Fermi level cross-over of the defect levels. Based on the damage constants evaluated from the initial portion of data where the formula was applicable, the relative effectiveness of various radiation sources in causing the resistivity change in n-type silicon was compared. The TRIGA Mark II reactor neutrons, for example, were found to be about 40 times more effective than 1 MeV electrons. The dependence of the damage constant on the initial carrier concentration was also examined. The physical basis of the exponential law and the effect of the Fermi level cross-over of the defect levels on the resistivity change in the high fluence ranges are discussed.

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Classification of cold regions and analysis of the freeze-thaw repetition cycle based on heat transfer quantity by freezing test (실내동결시험을 통한 열류량 분석에 따른 동결-융해 조건 분석 및 한랭지역의 분류)

  • An, Jai-Wook;Seo, Jeong-Eun;Jung, Min-Hyung;Seong, Joo-Hyun
    • Journal of Korean Tunnelling and Underground Space Association
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    • v.20 no.6
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    • pp.957-972
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    • 2018
  • Tunnels constructed in cold regions can cause serious defects such as cracks and leaks due to external temperature changes in the portals and vents. In order to prevent the freezing damage of the tunnel, appropriate measures should be applied to the section where the freeze damage is concerned. However, the specific criteria and contents for judging whether or not the anti-freeze measures are applied are not presented. In this study, the laboratory freezing tests on the temperature changes of the concrete specimens under freezing conditions were carried out. And the freeze-thaw repetition cycle (F), which can judge the possibility of freezing damage, were presented based on the heat transfer quantity (W) by experimental results of case studies. Also, we propose a classification of cold regions considering the climatic characteristics of Korea for using it to efficient design and maintenance.

Studies on the Electrochemical Dissolution for the Treatment of 10 g-Scale Zircaloy-4 Cladding Hull Wastes in LiCl-KCl Molten Salts (LiCl-KCl 용융염 내에서 10 g 규모의 Zircaloy-4 폐 피복관 처리를 위한 전기화학적 용해 연구)

  • Lee, You Lee;Lee, Chang Hwa;Jeon, Min Ku;Kang, Kweon Ho
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.10 no.4
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    • pp.273-280
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    • 2012
  • The electrochemical behaviors of 10 g-scale fresh and oxidized Zircaloy-4 cladding hulls were examined in $500^{\circ}C$ LiCl-KCl molten salts to confirm the feasibility of the electrorefining process for the treatment of hull wastes. In the results of measuring the potential-current response using a stainless steel basket filled with oxidized Zircaloy-4 hull specimens, the oxidation peak of Zr appears to be at -0.7 to -0.8 V vs. Ag/AgCl, which is similar to that of fresh Zircaloy-4 hulls, while the oxidation current is found to be much smaller than that of fresh Zircaloy-4 hulls. These results are congruent with the outcome of current-time curves at -0.78 V and of measuring the change in the average weight and thickness after the electrochemical dissolution process. Although the oxide layer on the surface affects the uniformity and rate of dissolution by decreasing the conductivity of Zircaloy-4 hulls, electrochemical dissolution is considered to occur owing to the defect of the surface and phase properties of the Zr oxide layer.

Cu Electroplating on the Si Wafer and Reliability Assessment of Low Alpha Solder Bump for 3-D Packaging (3차원 실장용 실리콘 웨이퍼 Cu 전해도금 및 로우알파솔더 범프의 신뢰성 평가)

  • Jung, Do Hyun;Lee, Joon Hyung;Jung, Jae Pil
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2012.11a
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    • pp.123-123
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    • 2012
  • 최근 연구되고 있는 TSV(Through Silicon Via) 기술은 Si 웨이퍼 상에 직접 전기적 연결 통로인 관통홀을 형성하는 방법으로 칩간 연결거리를 최소화 할 수 있으며, 부피의 감소, 연결부 단축에 따른 빠른 신호 전달을 가능하게 한다. 이러한 TSV 기술은 최근의 초경량화와 고집적화로 대표되는 전자제품의 요구를 만족시킬 수 있는 차세대 실장법으로 기대를 모으고 있다. 한편, 납땜 재료의 주 원료인 주석은 주로 반도체 소자의 제조, 반도체 칩과 기판의 접합 및 플립 칩 (Flip Chip) 제조시의 범프 형성 등 반도체용 배선재료에 널리 사용되고 있다. 최근에는 납의 유해성 때문에 대부분의 전자제품은 무연솔더를 이용하여 제조되고 있지만, 주석을 이용한 반도체 소자가 고밀도화, 고 용량화 및 미세피치(Fine Pitch)화 되고 있기 때문에, 반도체 칩의 근방에 배치된 주석으로부터 많은 알파 방사선이 방출되어 메모리 셀의 정보를 유실시키는 소프트 에러 (Soft Error)가 발생되는 위험이 많아지고 있다. 이로 인해, 반도체 소자 및 납땜 재료의 주 원료인 주석의 고순도화가 요구되고 있으며, 특히 알파 방사선의 방출이 낮은 로우알파솔더 (Low Alpha Solder)가 요구되고 있다. 이에 따라 본 연구는 4인치 실리콘 웨이퍼상에 직경 $60{\mu}m$, 깊이 $120{\mu}m$의 비아홀을 형성하고, 비아 홀 내에 기능 박막증착 및 전해도금을 이용하여 전도성 물질인 Cu를 충전한 후 직경 $80{\mu}m$의 로우알파 Sn-1.0Ag-0.5Cu 솔더를 접합 한 후, 접합부 신뢰성 평가를 수행을 위해 고속 전단시험을 실시하였다. 비아 홀 내 미세구조와 범프의 형상 및 전단시험 후 파괴모드의 분석은 FE-SEM (Field Emission Scanning Electron Microscope)을 이용하여 관찰하였다. 연구 결과 비아의 입구 막힘이나 보이드(Void)와 같은 결함 없이 Cu를 충전하였으며, 고속전단의 경우는 전단 속도가 증가할수록 취성파괴가 증가하는 경향을 보였다. 본 연구를 통하여 전해도금을 이용한 비아 홀 내 Cu의 고속 충전 및 로우알파 솔더 볼의 범프 형성이 가능하였으며, 이로 인한 전자제품의 소프트에러의 감소가 기대된다.

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Comparison of push-out bond strength of post according to cement application methods (시멘트 도포 방법에 따른 포스트의 push-out 접착 강도 비교)

  • Kim, Seo-Ryeong;Yum, Ji-Wan;Park, Jeong-Kil;Hur, Bock;Kim, Hyeon-Cheol
    • Restorative Dentistry and Endodontics
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    • v.35 no.6
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    • pp.479-485
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    • 2010
  • Objectives: The aim of this study was to compare the push-out bond strengths of resin cement/fiber post systems to post space dentin using different application methods of resin cement. Materials and Methods: Thirty extracted human premolars were selected and randomly divided into 3 groups according to the technique used to place the cement into root canal: using lentulo-spiral instrument (group Lentulo), applying the cement onto the post surface (group Direct), and injecting the material using a specific elongation tip (group Elongation tip). After shaping and filling of the root canal, post space was drilled using Rely-X post drill. Rely-X fiber post was seated using Rely-X Unicem and resin cement was light polymerized. The root specimens were embedded in an acrylic resin and the specimens were sectioned perpendicularly to the long axis using a low-speed saw. Three slices per each root containing cross-sections of coronal, middle and apical part of the bonded fiber posts were obtained by sectioning. The push-out bond strength was measured using Universal Testing Machine. Specimens after bond failure were examined using operating microscope to evaluate the failure modes. Results: Push-out bond strengths were statistically influenced by the root regions. Group using the elongation tip showed significantly higher bond strength than other ways. Most failures occurred at the cement/dentin interface or in a mixed mode. Conclusions: The use of an elongation tip seems to reduce the number of imperfections within the selfadhesive cement interface compared to the techniques such as direct applying with the post and lentulospiral technique.