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A method of preparing silicon carbide single crystal by using long crystal component

A technology of silicon carbide single crystal and silicon carbide powder, which is applied in the direction of chemical instruments and methods, single crystal growth, single crystal growth, etc., can solve the problem of slow atmosphere transmission, difficulty in further increasing the diameter of seed crystal expansion, and failure to improve Ingot quality and other issues, to improve the diameter size and crystal quality, reduce the generation of carbon inclusions, and ensure the effect of crystal growth rate

Active Publication Date: 2022-02-11
SICC CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A method of preparing silicon carbide single crystal by using long crystal component
  • A method of preparing silicon carbide single crystal by using long crystal component
  • A method of preparing silicon carbide single crystal by using long crystal component

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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 application provides a crystal growth assembly for preparing a single crystal by PVT method, comprising: a crucible and a heating device positioned above the crucible; the heating device is provided with a plurality of concentrically arranged annular heating temperature zones, so that the In the heating and / or crystal growth stage, the axial temperature gradient in the crucible is adjusted by controlling the overall heating temperature of a plurality of concentrically arranged annular heating temperature zones, and by controlling the temperature of each annular heating temperature zone in a plurality of concentrically arranged annular heating temperature zones The heating temperature regulates the radial temperature gradient in the crucible. The device for preparing silicon carbide single crystal provided by this application can control the axial temperature gradient and radial temperature gradient of the temperature field in the crucible to increase the growth rate of the crystal, ensure the stability of the crystal growth environment, and maintain a larger crystal edge diameter ladder, improve edge quality, and obtain larger silicon carbide single crystals at the same time.

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 for preparing single crystals by 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 interface rise. The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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