Method for growing crystal by reducing atmosphere Kyropoulos method

A technology of crystal growth and Kyropoulos method, applied in single crystal growth, crystal growth, chemical instruments and methods, etc., can solve problems such as difficulty in obtaining high-quality lithium aluminate crystals, volatilization, temperature field and temperature gradient distribution asymmetry , to achieve the effect of low energy loss, low material loss and good versatility

Inactive Publication Date: 2009-11-18
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Invention 200710073268.8 (application number) is based on the patent ZL200310112171.5 and relates to "a lithium aluminate crystal growth method". In addition to the defects of the patent ZL200310112171.5, the invention has an observation window on the side wall of the heat preservation cover. The observation window will lead to asymmetry of the temperature field and temperature gradient distribution, causing strong gas convection between the inner cavity of the insulation cover above the melt and the outside of the cover. A large number of experimental results have proved that the above observation window is the cause of lithium aluminate crystal growth. The fundamental reason for the volatilization of serious components, so it is difficult to obtain high-quality lithium aluminate crystals using this kind of heat preservation cover

Method used

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  • Method for growing crystal by reducing atmosphere Kyropoulos method

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Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: Adopt the Kyropoulos method of the present invention to grow lithium aluminate crystal

[0022] According to molar ratio Al 2 o 3 : Li 2 CO 3 =1: 1 Take by weighing the dried raw materials with a purity of 99.999%, mix them uniformly, press them into cakes under a pressure of 40MPa, and pre-sinter them at 1100°C for 10 hours; put the sintered block into the tungsten-molybdenum alloy crucible 7, and into the pull furnace, such as figure 1 As shown in the figure: 1-The upper cover of the insulation cover, 2-Hard graphite felt (or zirconia) insulation cover, 3-Seed crystal, 4-Crystal, 5-Quartz barrel, 6-Induction coil, 7-Tungsten-molybdenum alloy Crucible, 8-graphite felt, 9-human eye, 10-observation window on the upper side of the furnace wall, 11-seed crystal rod, 12-observation window on the upper cover of the heat preservation cover, 13-tungsten-molybdenum alloy afterheater, 14-furnace wall, 15-melt, 16-tray. Fill graphite felt 8 around the tungsten...

Embodiment 2

[0024] Embodiment 2: Adopt the Kyropoulos method of the present invention to grow lithium gallate crystal

[0025] According to molar ratio Ga 2 o 3 : Li 2 CO 3 =1: 1 Take by weighing the dried raw materials with a purity of 99.999%, mix them uniformly, press them into cakes under a pressure of 40MPa, and pre-sinter them at 1100°C for 10 hours; put the sintered block into the tungsten-molybdenum alloy crucible 7, and into the pull furnace, such as figure 1 As shown in the figure: 1-The upper cover of the insulation cover, 2-The hard graphite felt insulation cover, 3-Seed crystal, 4-Crystal, 5-Quartz barrel, 6-Induction coil, 7-Molybdenum crucible, 8-Graphite felt, 9-human eye, 10-observation window on the upper side of the furnace wall, 11-seed crystal rod, 12-observation window on the upper cover of the heat preservation cover, 13-tungsten-molybdenum alloy afterheater, 14-furnace wall, 15-melt, 16- tray. Fill graphite felt 8 around the molybdenum crucible 7, put a tungs...

Embodiment 3

[0026] Embodiment 3: GGG crystals grown by the Kyropoulos method of the present invention

[0027] Pack the GGG block into the tungsten crucible 7 and put it into the pulling furnace, such as figure 1 As shown in the figure: 1-Insulation cover upper cover, 2-Zirconium oxide insulation cover, 3-Seed crystal, 4-Crystal, 5-Quartz barrel, 6-Induction coil, 7-Tungsten crucible, 8-Graphite felt, 9 -human eye, 10-observation window on the upper side of the furnace wall, 11-seed crystal rod, 12-observation window on the upper cover of the heat preservation cover, 13-tungsten afterheater, 14-furnace wall, 15-melt, 16-tray. Graphite felt 8 is filled around the tungsten crucible 7, a tungsten afterheater 13 is placed above the crucible, a zirconia heat preservation cover 2 is put on the outside of the tungsten afterheater 13, and the heat preservation cover upper cover 1 is covered. Then close the furnace and evacuate (better than 0.1Pa), and then fill it with high-purity N 2 After the...

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Abstract

The invention relates to a method for growing crystal by reducing atmosphere Kyropoulos method; the method is characterized in that on the basis of growing crystal by induction heating pulling method, a tungsten, or molybdenum, or tungsten molybdenum alloy crucible is used; graphite felt which is arranged outside the crucible is used as a heat insulator; the reducing atmosphere is formed at high temperature; a hard graphite felt heat cover or a zirconia brick heat cover combined with a tungsten molybdenum after heater are placed above the crucible to preserve heat for fused mass in the crucible and the crystal grows; an observation window is arranged at the upper cover of the heat cover and the upper side of a furnace wall to ensure uniformity and symmetry of temperature field and temperature gradient distribution; the observation window arranged at the upper cover of the heat cover and the upper side of the furnace wall are used to observe the fused mass and the conventional pulling method is used to carry out parallel shouldering on inoculating crystal; then power is reduced at a certain speed, meanwhile, the crystal can be slightly pulled or not pulled, that is the Kyropoulos method; after crystallization is over, power is continued to be reduced to lower the temperature of the crystal. With the method of the invention adopted, large-size and high-quality crystal can be grown at low cost.

Description

technical field [0001] The invention relates to a crystal growth method, in particular to a method for growing crystals by a reducing atmosphere kerosene method, which can obtain large-sized and high-quality crystals. Background technique [0002] Growing large-size, high-quality crystals at a lower cost is the relentless goal pursued by scientists and technicians engaged in crystal growth. There are many methods of crystal growth, but the most commonly used and most important is to grow crystals from the melt, which mainly includes the pulling method, the temperature gradient method and the Kyropoulos method. [0003] Among them, the pulling method is the most commonly used method for growing high-quality single crystals from the melt. This method can grow important gemstones such as sapphire, ruby, yttrium aluminum garnet, gadolinium gallium garnet and spinel. crystals. However, the growth of compound crystals by the pulling method usually requires expensive platinum, ir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B15/00
Inventor 周圣明林辉
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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