• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 优先权
    • 专利摘要:
    New methods have been proposed for the production of high quality GaAs, GaP and InP single crystals. First, in order to prevent lattice defects caused by the difference in vapor pressure of the elements, a Mo container and a lid are prepared in the production of single crystal, and PBN (Pyrolytic Boron Nitride) and a sample which do not react with Ga or In are put in, and elements having high vapor pressure are blown away. The Mo lid was sealed with an electron beam welder to minimize this. At this time, the ideal gas relation pV = nRT was used to consider the amount of Ga, In and As or P in space. Second, an electric furnace using heat radiation from a tungsten mesh heater in a high vacuum of ˜10 -6 Torr was used to minimize the transition of single crystals or grain boundaries resulting from convection under high pressure. Finally, the vessel support rod was rotated at 5 to 10 rpm to minimize the weakening of crystalline due to the horizontal thermal gradient.
    公开号:KR19990007600A
    申请号:KR1019980042456
    申请日:1998-10-12
    公开日:1999-01-25
    发明作者:권용성
    申请人:윤영덕；
    IPC主号:
    专利说明:

    GS, GS, INP of high quality single crystal manufacturing apparatus and method
    The present invention relates to a method for producing high quality single crystals of GaAs, GaP and InP, which are materials having high vapor pressure, and are a major problem in the production of high quality single crystals. This happens (for GaAs or GaP (InP) a defect of As or P occurs). It is an object of the present invention to prevent this from happening and to produce high quality single crystals of (GaAs, GaP and InP).
    Conventionally, when preparing single crystals of GaP, GaAs, and InP, which have high vapor pressure, Czochralski method using liquid encapsulation (LEC) method and Bridgman method under high pressure are used. Liquid encapsulation method has to apply high pressure uniformly from the outside, and it is difficult to control the pressure according to the material with different vapor pressure, and the device is very complicated and the price is very expensive. In addition, since the Bridgeman method requires high pressure, the device is complicated and very expensive, and since it is not in a vacuum state, convection of gas used for high pressure occurs, causing fluctuations in temperature, thereby causing problems with high-quality single crystal growth. In both cases, the material with high vapor pressure no matter how high pressure is applied, until the equilibrium is reached, the elements escape due to evaporation, causing defects in the single crystal. However, of the above two methods, high-quality single crystal growth is realized only by the Bridgeman method, which is relatively easy to control pressure.
    The technical problem required to solve the problems in the above conventional method is as follows.
    1. Resolving lattice defects caused by differences in vapor pressure of members
    2. Resolving deterioration of crystalline due to fluctuation of temperature due to convection under high pressure
    3. Resolving deterioration of crystalline due to horizontal thermal gradient in electric furnace
    1 is a cross-sectional view of a molybdenum container and lid.
    2 is a cross-sectional view of a molybdenum container and a lid containing a material to be manufactured and welded with an electron beam welder.
    3 is a cross-sectional view of a high vacuum electric furnace using a tungsten mesh heater as a GaAs, GaP, InP single crystal manufacturing apparatus.
    ※ Explanation of codes for main parts of drawing
    1. Molybdenum Container 2. Molybdenum Lid
    3. Welding part 4. PBN
    5. Sample 6. BN Powder
    7. Tungsten Mesh Heater 8. Tungsten Radiation Film
    9. Thermocouple 10. Molybdenum Container
    11. Electrode 12. Vessel Support
    13. Water Inlet 14 Water Outlet
    15. High vacuum
    To solve the problems described above, follow these steps.
    1. Solution of Grid Defects Due to Vapor Pressure Difference of Members
    Produce Mo using a shelf as shown in Figure 1. The container (1) and lid (2) are then washed several times with acetone to remove organics such as oil. It is heated for 4 hours in a vacuum electric furnace (Fig. 3) at a temperature higher than the melting point of the material to be prepared. This prevents the introduction of impurities in the manufacture of the material to be produced by removing the impurities contained in the container.
    Then, since Ga or In reacts with Mo at a high temperature, an unreacted PBN (4) is placed in a container, and BN powder (6) is filled in the container and PBN. This is put into a vacuum electric furnace again (FIG. 3) and heated at 1800 ° C. for 4 hours.
    Then, put the material to be prepared in the PBN, cover the lid (2) and put in the electron beam welding machine weld the lid and the container part (3) to be completely sealed.
    At this time, care should be made to the lid (2) so that there is no space in the container (1). If there is a space, there is a high vapor pressure element (ie, As or P) in the space and a high quality single crystal cannot be obtained. But you can't completely eliminate space. Because the welding of Mo should be raised to three times the melting point of the material to be produced (about 3000 ℃ for Mo). At this time, Mo has a thermal conductivity, and when the lid 2 is in contact with the material, elements having a high vapor pressure of the material to be manufactured are blown away, so that high-quality single crystal growth is impossible. To avoid this problem, leave a gap of 1 cm between the material and the lid. Then, since space is formed in the portion, there is a high vapor pressure element (ie, As or P) in the space. Therefore, this elemental amount should be considered. As or P does not have any interaction between atoms at high temperature, so it can be regarded as an ideal gas. The ideal gas relation pV = nRT is used to produce GaAs, GaP or InP from Ga, In and As or P in consideration of the amount of space in the space.
    2. Solution to deterioration of crystalline due to fluctuations in temperature due to convection under high pressure
    In this way, the sealed product is put in an electric furnace (Fig. 3) to produce a single crystal. Due to the temperature disturbance during the production of single crystals, transitions or grain boundaries in the single crystals are reduced. The disturbance of temperature is due to the convention. If only radiant heat is present, there is little disturbance of temperature. Convection is present in electric furnaces used under conventional high pressures. In the present invention, an electric furnace using thermal radiation energy was used by flowing a current through the tungsten mesh heater 10 in a high vacuum 15 of ˜10 −6 Torr to minimize tropical flow. The temperature control of this furnace is based on the feedback method of current. In doing so, the disturbance of the temperature at 1500 ° C. was ± 0.5 degrees or less.
    3. Resolving deterioration of crystalline due to horizontal thermal gradient in electric furnace
    Even without this vertical temperature disturbance, there may be a horizontal temperature gradient. This results from the vessel coming off from the center of the heater. In order to minimize this, the container supporting rods 12 can be rotated. If the rotation is too fast, it will cause the solid solution to be manufactured to oscillate, resulting in reverse transition or grain boundary, and if it is too late, it will not be effective because it will not eliminate the horizontal temperature gradient. The optimum condition is 5-10 rpm.
    The high-quality single crystals are grown by the Bridgeman method using the three technical methods described above.
    The single crystals obtained under these conditions had much lower lattice defects and better crystal quality than the high quality single crystals obtained by using the Vertical Bridgman method and the Liquid Encapsulation Enhancement Method (LEC) under high pressure. If this single crystal growth technology is applied to full-scale mass production of compound semiconductor wafers, it will not only activate device manufacturing for high-grade devices (ICs) and laser diodes in the optical communication field, but also import imports and export increase effects. It will have a big impact.
    权利要求:
    Claims (2)
    [1" claim-type="Currently amended] To produce high-quality single crystals of GaAs, GaP and InP, lattice defects of crystals are created due to the difference in vapor pressure of the elements. In order to prevent this, a manufacturing method is grown by using a closed system in which a member is placed in a Mo container (2) and a lid (1) is made and completely welded with an electron beam welder.
    [2" claim-type="Currently amended] In order to manufacture single crystals of GaAs, GaP, and InP, conventionally, high pressure is used to suppress generation of lattice defects of crystal due to the difference in vapor pressure of constituent elements. At this time, convection is formed due to high pressure. This convection is a factor that lowers the temperature stability of the electric furnace. Because of this, there is a limit of high quality crystal production. A device that raises the temperature using only radiant heat by using a tungsten mesh heater (7) by making the electric furnace inside a vacuum state due to the anxiety of temperature stability caused by convection.
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    同族专利:
    公开号 | 公开日
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    法律状态:
    1998-10-12|Application filed by 윤영덕
    1998-10-12|Priority to KR1019980042456A
    1999-01-25|Publication of KR19990007600A
    优先权:
    申请号 | 申请日 | 专利标题
    KR1019980042456A|KR19990007600A|1998-10-12|1998-10-12|GS, GS, INP of high quality single crystal manufacturing apparatus and method|
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