Crystal growth assembly for preparing single crystals through PVT method and method for preparing single crystal

A technology for growing crystals and components, which is applied in the field of single crystal preparation devices, and can solve problems such as difficult growth of crystal ingots, reduction of atmosphere supersaturation, micropipes, etc., and achieve large axial temperature gradients and radial temperature gradients, and promote Thickness increase, effect of increasing growth rate

Active Publication Date: 2021-03-12
SICC CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, with the growth of the crystal, the gas-phase transmission distance of the raw material is gradually shortened, and the temperature difference between the crystal growth interface and the raw material interface is gradually reduced. The growth interface is placed in a high-temperature region, which makes the temperature of the growth interface rise. The temperature gradient in the z-axis direction, that is, the axial temperature gradient gradually decreases, and the decrease of the axial temperature gradient will, on the one hand, lead to slower atmosphere transmission, making it difficult for the ingot to grow thicker; Meteorological composition Si in the interface region m C m As the concentration increases, the probability of interaction will also increase, and in severe cases, polymorphism will occur due to the decrease in the supersaturation of the atmosphere.
[0004] At the same time, during the SiC crystal growth process, with the growth of the crystal edge size, the radial temperature gradient gradually decreases, which leads to the acceleration of the growth rate of the edge region of the crystal. On the one hand, it is easy to produce micropipes, Polytype, edge polycrystalline and other defects, on the other hand, it is difficult to further increase the diameter of the seed crystal
[0005] Therefore, when using the PVT method to prepare silicon carbide single crystals, especially in the crystal growth stage, the instability of the axial temperature gradient and radial temperature gradient limits the improvement of the quality and size of silicon carbide single crystals
Patent CN211497869U provides a crystal annealing treatment device, by setting heaters above, below and around the crucible, so as to eliminate the stress inside the crystal and reduce the probability of crystal cracking, but this device is for the post-treatment of the crystal that has grown , cannot increase the crystal size, nor can it play a role in improving the quality of the boule

Method used

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  • Crystal growth assembly for preparing single crystals through PVT method and method for preparing single crystal
  • Crystal growth assembly for preparing single crystals through PVT method and method for preparing single crystal
  • Crystal growth assembly for preparing single crystals through PVT method and method for preparing single crystal

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Experimental program
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Effect test

Embodiment 1

[0070] This embodiment provides a method for preparing a high-quality silicon carbide single crystal, the method comprising the following steps:

[0071] Step 1: Mix silicon carbide powder with a particle size of 1000 μm (that is, the second silicon carbide powder, the same below) and carbon powder with a particle size of 1000 μm in a mass ratio of 5:1 to obtain a mixed powder, and then mix the The mixed powder is loaded into the bottom of the crucible and paved, and then a layer of pure silicon carbide powder with a particle size of 300 microns (i.e. the first silicon carbide powder, the same below) is placed on the top of the mixed powder, wherein the mixed powder The mass is 3kg, the mass of pure silicon carbide powder is 1kg, that is, the total mass of crystal growth raw materials is 4kg;

[0072] Step 2: Fix the silicon carbide seed crystal on the inner side of the upper cover of the crucible, adjust the position of the upper cover of the crucible to the lowest position, ...

Embodiment 2

[0080] This embodiment provides a method for preparing a high-quality silicon carbide single crystal, the method comprising the following steps:

[0081] Step 1: Mix silicon carbide powder with a particle size of 800 μm and carbon powder with a particle size of 600 μm evenly in a mass ratio of 5:2 to obtain a mixed powder, then put the mixed powder into the bottom of the crucible and spread it flat, then Place a layer of pure silicon carbide powder with a particle size of 200 microns above the mixed powder, wherein the quality of the mixed powder is 3.5kg, the quality of the pure silicon carbide powder is 1kg, that is, the total mass of the crystal growth raw material is 4.5kg ;

[0082] Step 2: Fix the silicon carbide seed crystal on the inner side of the upper cover of the crucible, adjust the position of the upper cover of the crucible to the lowest position, merge it with the crucible, and assemble the crystal growth furnace completely;

[0083] Step 3: Turn on the air pu...

Embodiment 3

[0090] This embodiment provides a method for preparing a high-quality silicon carbide single crystal, the method comprising the following steps:

[0091] Step 1: Mix silicon carbide powder with a particle size of 800 μm and carbon powder with a particle size of 800 μm in a mass ratio of 6:1 to obtain a mixed powder, then put the mixed powder into the bottom of the crucible and spread it flat, then Place a layer of pure silicon carbide powder with a particle size of 400 microns above the mixed powder, wherein the quality of the mixed powder is 3.5kg, the quality of the pure silicon carbide powder is 1kg, that is, the total mass of the crystal growth raw material is 4.5kg ;

[0092] Step 2: Fix the silicon carbide seed crystal on the inner side of the upper cover of the crucible, adjust the position of the upper cover of the crucible to the lowest position, merge it with the crucible, and assemble the crystal growth furnace completely;

[0093] Step 3: Turn on the exhaust pump,...

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Abstract

The invention provides a crystal growth assembly for preparing single crystals through a PVT method. The crystal growth assembly comprises a crucible and a heating device located above the crucible. The heating device is provided with a plurality of concentrically arranged annular heating temperature zones, so that the axial temperature gradient in the crucible is adjusted by controlling the overall heating temperature of the plurality of concentrically arranged annular heating temperature zones in the heating and / or crystal growth stage of single crystal preparation; and the radial temperature gradient in the crucible is adjusted by controlling the heating temperature of each annular heating temperature zone in the plurality of concentrically arranged annular heating temperature zones. According to the device for preparing the silicon carbide single crystal, the axial temperature gradient and the radial temperature gradient of the temperature field in the crucible can be controlled, so that the growth rate of the crystal is increased, the stable growth environment of the crystal is ensured, a relatively large crystal edge diameter gradient is maintained, the edge quality is improved, and meanwhile, the silicon carbide single crystal with a relatively large size is obtained.

Description

technical field [0001] The application belongs to the technical field of single crystal preparation devices, and in particular relates to a crystal growth component and a method for preparing a single crystal by using a PVT method. Background technique [0002] When using the PVT method to prepare silicon carbide single crystals, the silicon carbide seed crystal is fixed on the inner top of the crucible cover and does not move. The crucible is filled with silicon carbide crystal growth raw materials, and the decomposed gas phase of the crystal growth raw materials after sublimation condenses into crystals at the seed crystal. . [0003] However, with the growth of the crystal, the gas-phase transmission distance of the raw material is gradually shortened, and the temperature difference between the crystal growth interface and the raw material interface is gradually reduced. The growth interface is placed in a high-temperature region, which makes the temperature of the growth...

Claims

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Application Information

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IPC IPC(8): C30B29/36C30B23/00
CPCC30B29/36C30B23/00C30B23/002
Inventor 王宗玉高超宁秀秀李霞潘亚妮高宇晗方帅赵树春杨晓俐张九阳
Owner SICC CO LTD
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