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Furnace monocrystal isothermal annealing method and tool

An isothermal annealing, single crystal technology, applied in the direction of single crystal growth, chemical instruments and methods, crystal growth, etc., can solve the problems of single crystal cracks, increase costs, etc., to simplify the process, reduce the risk of cracks, and reduce single crystal heat. effect of stress

Inactive Publication Date: 2012-07-25
BEIJING HUAJINCHUANGWEI ELECTRONICS CO LTD
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0002] When growing a single crystal by the physical vapor transport method, a certain temperature gradient is required as the driving force for crystallization. However, if the above temperature gradient is maintained during cooling and annealing after the growth is complete, thermal stress will easily be generated inside the single crystal, and in severe cases, it will lead to a single crystal. crystal cracks
In addition, even if the obtained single crystal is free from macroscopic stress cracking, additional annealing will increase the cost

Method used

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  • Furnace monocrystal isothermal annealing method and tool
  • Furnace monocrystal isothermal annealing method and tool

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Effect test

Embodiment 1

[0015] Before growing the silicon carbide single crystal by the physical vapor transport method, the insulation plug 6 is separated from the heat dissipation channel 5 by about 400mm in advance, so that there is a temperature gradient during the growth of the single crystal. After the growth is over, lower the above-mentioned insulation plug 6 by about 400 mm through the pull rod 7 on the upper end of the insulation plug 6, tightly cover the heat dissipation channel on the upper part of the seed crystal, and reduce the heating power by 70% at the same time, so as to prevent the grown single crystal from being damaged due to excessive temperature. After being sublimated and then kept warm for 1 hour, the whole single crystal can reach the annealing start temperature uniformly. Finally, the method of isothermal annealing with the furnace is adopted, and the temperature is lowered to room temperature within 24 hours to obtain a silicon carbide single crystal without thermal stress....

Embodiment 2

[0017] Before using the physical vapor transport method to grow the aluminum nitride single crystal, the insulation plug 6 is separated from the heat dissipation channel 5 by about 10mm in advance, so that there is a temperature gradient during the growth of the single crystal. After the growth is over, raise the crucible 2 by about 10mm through the tie rod 8 at the bottom of the insulation tube 1, tightly cover the heat dissipation channel on the upper part of the seed crystal, and reduce the heating power by 10% at the same time, so as to prevent the grown single crystal from being sublimated due to excessive temperature , and then keep it warm for 48 hours, so that the whole single crystal can evenly reach the annealing starting temperature, and finally use the method of isothermal annealing with the furnace to drop to room temperature within 24 hours, and obtain an aluminum nitride single crystal with small thermal stress. However, if the aluminum nitride single crystal gro...

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Abstract

The invention belongs to the technical field of monocrystal preparation, and relates to a furnace monocrystal isothermal annealing method and tool, in particular to an annealing method and tool after the growth of monocrystal with a physical vapor transportation method is finished. The method comprises the steps of: covering an insulating plug on a radiating channel at the top of a crucible after the growth of monocrystal with the physical vapor transportation method is finished, reducing the heating power by about 10-70%, and then insulating for 1 hour to 48 hours; and finally adopting isothermal furnace annealing method to cool to room temperature, thus obtaining monocrystal with small thermal stress. The furnace monocrystal isothermal annealing tool comprises the crucible, wherein the radiating channel is arranged at the top of the crucible, the insulating plug is arranged above the radiating channel, and the insulating plug or the crucible can move up and down. Compared with the prior art of gradient cooling with temperature and additional annealing, the method and tool provided by the invention not only can greatly decrease the thermal stress of the monocrystal and lower the crack risk of monocrystal, but also can simplify the process and lower the cost as the monocrystal can be directly machined after the growth is finished and the furnace annealing is completed.

Description

technical field [0001] The invention belongs to the technical field of single crystal preparation, and in particular relates to an annealing method and tooling after single crystal growth by physical vapor transport method. Background technique [0002] When growing a single crystal by the physical vapor transport method, a certain temperature gradient is required as the driving force for crystallization. However, if the above temperature gradient is maintained during cooling and annealing after the growth is complete, thermal stress will easily be generated inside the single crystal, and in severe cases, it will lead to a single crystal. Crystal cracks. In addition, even if the obtained single crystal is free from macroscopic stress cracking, additional annealing will increase the cost. Contents of the invention [0003] The purpose of the present invention is to avoid the thermal stress inside the single crystal and affect the quality of the single crystal caused by the...

Claims

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Application Information

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IPC IPC(8): C30B23/00C30B33/02
Inventor 倪代秦吴星赵岩何丽娟王雷杨巍马晓亮李晋
Owner BEIJING HUAJINCHUANGWEI ELECTRONICS CO LTD
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