• Title/Summary/Keyword: Crucible

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Melting of Al2O3 powder using the skull melting method (Skull melting법에 의한 Al2O3 파우더 용융)

  • Choi, Hyun-Min;Kim, Young-Chool;Seok, Jeong-Won
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.29 no.1
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    • pp.24-31
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    • 2019
  • The current study demonstrates an efficient procedure to create ingots from $Al_2O_3$ powder using the skull melting method to use these ingots as a starting material in conventional methods for growing synthetic single-crystal sapphire. Dimension of the cold crucible was 24 cm in inner diameter and 30 cm in inner height, 15 kg of $Al_2O_3$ powder was completely melted within 1 h at an oscillation frequency of 2.75 MHz, maintained in the molten state for 3 h, and finally air-cooled. The areal density and components of the cooled ingot by parts were analyzed through scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS). The areal density and $Al_2O_3$ content of the ingot were related to the temperature distribution inside the cold crucible during high-frequency induction heating, and the area with high temperature was high tends to be high in areal density and purity.

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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Corium melt researches at VESTA test facility

  • Kim, Hwan Yeol;An, Sang Mo;Jung, Jaehoon;Ha, Kwang Soon;Song, Jin Ho
    • Nuclear Engineering and Technology
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    • v.49 no.7
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    • pp.1547-1554
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    • 2017
  • VESTA (Verification of Ex-vessel corium STAbilization) and VESTA-S (-small) test facilities were constructed at the Korea Atomic Energy Research Institute in 2010 to perform various corium melt experiments. Since then, several tests have been performed for the verification of an ex-vessel core catcher design for the EU-APR1400. Ablation tests of an impinging $ZrO_2$ melt jet on a sacrificial material were performed to investigate the ablation characteristics. $ZrO_2$ melt in an amount of 65-70 kg was discharged onto a sacrificial material through a well-designed nozzle, after which the ablation depths were measured. Interaction tests between the metallic melt and sacrificial material were performed to investigate the interaction kinetics of the sacrificial material. Two types of melt were used: one is a metallic corium melt with Fe 46%, U 31%, Zr 16%, and Cr 7% (maximum possible content of U and Zr for C-40), and the other is a stainless steel (SUS304) melt. Metallic melt in an amount of 1.5-2.0 kg was delivered onto the sacrificial material, and the ablation depths were measured. Penetration tube failure tests were performed for an APR1400 equipped with 61 in-core instrumentation penetration nozzles and extended tubes at the reactor lower vessel. $ZrO_2$ melt was generated in a melting crucible and delivered down into an interaction crucible where the test specimen is installed. To evaluate the tube ejection mechanism, temperature distributions of the reactor bottom head and in-core instrumentation penetration were measured by a series of thermocouples embedded along the specimen. In addition, lower vessel failure tests for the Fukushima Daiichi nuclear power plant are being performed. As a first step, the configuration of the molten core in the plant was investigated by a melting and solidification experiment. Approximately 5 kg of a mixture, whose composition in terms of weight is $UO_2$ 60%, Zr 10%, $ZrO_2$ 15%, SUS304 14%, and $B_4C$ 1%, was melted in a cold crucible using an induction heating technique.

The current status in the silicon crystal growth technology for solar cells (태양전지용 규소 결정 성장 기술 개발의 현황)

  • Lee, A-Young;Lee, Dong-Gue;Kim, Young-Kwan
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.2
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    • pp.47-53
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    • 2014
  • Three kinds of crystalline silicon have been used for the solar cell grade. First of all, single crystalline silicon is the main subject to enhance the production yield. Most of the efforts are focused on the control of the melt-crystal interface shape affected by the crystal-crucible rotation rate. The main subject in the multi-crystalline silicon ingot is the contamination control. Faster Ar gas flow above the melt surface will lower the carbon contamination in the crystal. And also, twin boundary electrically inactive is found to be more effective than grain boundary for the improvement of the MCLT. In the case of mono-like silicon material, propagation of the multi-crystalline silicon growing from the inner side crucible is the problem lowering the portion of the single crystalline part at the center of the ingot. Crystal growing apparatus giving higher cooling rate at the bottom and lower cooling rate at the side crucible was suggested as the optimum solution obtaining higher quality of the mono-like silicon ingot. Proper application of the seeds at the bottom of the crucible would be one of the solutions.

Scientific Analysis and Conservation Treatment of the Kettle Excavated from Hwangnam-dong, Gyeongju (경주(慶州) 황남동(皇南洞) 출토(出土) 철부(鐵釜)의 보존처리(保存處理) 및 과학적분석(科學的分析))

  • Moon, Sunyoung;Jeon, Ikhwan;Yu, Heisun
    • Conservation Science in Museum
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    • v.4
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    • pp.23-32
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    • 2003
  • As the kettle excavated from a site in Hwangnam-dong, Gyeongju was presumed to have been used as a melting crucible in a glass production workplace, we decided to prove its usage by scientific analysis. First, we performed conservation treatment to find the original status of the kettle, and then SEM-EDS and XRD analysis of the five corrosions created on the surface of the kettle. The fragment of the spout, which played a crucial role for the kettle to be considered as a melting crucible, was discovered during the conservation treatment. So the mouth rim of the kettle was restored to perfection. When we observed the microstructure of the metal sample, it was proved to be cast iron gradually cooled without heat treatment. In the corrosion products, the main components were Fe and O and other components such as P, Si, Ca, and S were found. The main compounds were quartz, vivianite, goetheite, akaganite, lepidocrocite, hematite, etc. Although these components were used as raw materials for making glass, these were found not in the melting status but mere raw materials. This can be an evidence to show these site where the kettle was excavated had been a glass production workplace. However, it is not sure that the kettle was used as a melting crucible. Moreover, if we consider the organic mold and sand clay accumulated in the well site when the kettle was excavated at first, we can see this as a formative factor of the corrosions of the kettle. Therefore, we concluded that the kettle is a typical cast iron and was not used as a melting crucible of glass.

A study on the calcination process of synthetic silica powder for quartz glass crucibles (석영유리 도가니용 합성 실리카 분말의 하소공정에 관한 연구)

  • Yang, Jae-Kyo;Jin, Yun-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.4
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    • pp.128-135
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    • 2022
  • The inside of a quartz glass crucible for semiconductor processing, called a transparent layer, is manufactured using synthetic silica powder. Bubbles existing in the transparent layer of the crucible cause a problem of reducing the quality of the crucible as well as the yield of the silicon ingot. Therefore, the main goal of the synthetic silica powder, which is the raw material of the transparent layer, is to minimize the bubble generation factor. For this purpose, in the case of synthetic silica powder, it is necessary to minimize silanol groups, carbon and pores. In this study, synthetic silica gel was prepared using the sol-gel method, and changes in carbon content and specific surface area were investigated according to calcination temperature and dwelled time in a two-stage calcination process. The first-stage calcination process was performed between 500℃ and 600℃ and the second-stage calcination process was performed between 1000℃ and 1100℃. The dwelled time was carried out from 10 minutes to a maximum of 12 hours. The carbon content of the powder calcined at 1000℃ for 1 hour was 0.0031 wt.%, and the specific surface area of the powder calcined at 1100℃ for 12 hours was 16.6 m2/g.

Study on the feasibility of metallic saggar for synthesizing NCM cathode active materials-I (NCM 계 양극활물질 합성용 금속질 내화갑 가능성 연구-I)

  • Yong Il Park;Ji Hun Jung;Sung Hyun Woo;Jung Heon Lee;Hyeong-Jun Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.3
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    • pp.103-107
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    • 2024
  • In this study, nickel, a pure metal material, was proposed as a saggar for synthesizing NCM [Li(NixCoyMnz)O2] cathode active material. Nickel is known as a metal that is resistant to oxidation and has a high melting point. Nickel is one of the main components of NCM cathode material and was expected to be free from problems with contamination from saggar during cathode material synthesis. We sought to confirm the possibility of nickel as a saggar for synthesizing NCM cathode active materials. When a Ni metal crucible and Ni0.8Co0.1Mn0.1(OH)2 (NCM 811) precursor material were reacted at 900℃ for a long time, the change in the reaction layer on the surface of the crucible over time was analyzed. The nickel crucible reaction layer formed during heat treatment at 900℃ was nickel oxide, and is thought to have been created by simultaneous oxygen diffusion from the cathode precursor oxide and reaction with oxygen in the atmosphere. The change in thickness of the oxide layer appears to slow down after 480 hours, which suggests that the rate of oxygen diffusion from the precursor is reduced. It remained combined without falling out of the crucible until 480 hours. However, it was confirmed that the oxide layer falls off after 720 hours, so it is thought that it can be used as saggar for NCM synthesis only for a certain period of time.