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Carbon-ceramic composite material crucible containing Si3N4 and BN composite coating and preparation method of carbon-ceramic composite material crucible

A carbon-ceramic composite material and composite coating technology, which is applied in chemical instruments and methods, polycrystalline material growth, self-melting liquid pulling method, etc., can solve the problems of poor wettability, reduce the frequency of replacement, etc., and achieve dense coating , enhance life, good strength effect

Active Publication Date: 2021-08-03
HUNAN SHIXIN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the technical problems existing in the use of quartz crucibles and carbon-carbon crucibles in the existing single crystal silicon production process, the object of the present invention is to provide a Si-containing 3 N 4 A carbon-ceramic composite material crucible with BN composite coating and a preparation method thereof, using the carbon-ceramic crucible as a substrate, depositing Si on its pores and surfaces (inner and outer surfaces) 3 N 4 coating, and then deposited a BN coating, the present invention only needs to use a single crucible to produce single crystal silicon, through carbon ceramic crucible substrate, Si 3 N 4 The synergistic effect of the coating and the BN coating greatly improves the high temperature stability and silicon corrosion resistance of the crucible. At the same time, the surface of the crucible has poor wettability to silicon, which avoids the silicon crystal sticking to the pot after the production of single crystal silicon. It is difficult to clean, which not only prolongs the service life of the crucible, but also reduces the frequency of crucible replacement and improves the production efficiency of monocrystalline silicon

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Acupuncture preform: the density of acupuncture preparation is 0.58±0.02g / cm 3 carbon fiber crucible preform;

[0033] (2) Heat treatment of the prefabricated body: the carbon fiber crucible prefabricated body is heat-treated at a high temperature at 2000°C under an argon protective atmosphere, and the density change is 0.56±0.02g / cm 3 ;

[0034] (3) Densification of the preform: the density is 0.56±0.02g / cm 3 The prefabricated carbon fiber crucible is densified to 1.45g / cm by passing 1:1 propylene and nitrogen at 980±5°C and furnace pressure 1±0.2KPa 3 Get a charcoal crucible;

[0035] (4) Charcoal heat treatment: heat-treat the charcoal crucible at 2300°C for 3 hours to obtain the charcoal crucible matrix;

[0036] (5) High-temperature siliconizing: place the carbon-charcoal crucible base on the silicon powder, and then siliconize at 1900°C and furnace pressure lower than 1000pa to obtain the carbon-ceramic crucible base;

[0037] (6) Si 3 N 4 Coating Depos...

Embodiment 2

[0045] (1) Acupuncture preform: the density of acupuncture preparation is 0.58±0.02g / cm 3 carbon fiber crucible preform;

[0046] (2) Heat treatment of the prefabricated body: the carbon fiber crucible prefabricated body is heat-treated at a high temperature at 2000°C under an argon protective atmosphere, and the density change is 0.56±0.02g / cm 3 ;

[0047] (3) Densification of the preform: the density is 0.56±0.02g / cm 3 The prefabricated carbon fiber crucible is densified to 1.44g / cm by passing 1:1 propylene and nitrogen at 980±5°C and furnace pressure 1KPa 3 Get a charcoal crucible;

[0048] (4) Charcoal heat treatment: heat-treat the charcoal crucible at 2300°C for 3 hours to obtain the charcoal crucible matrix;

[0049] (5) High-temperature siliconizing: place the carbon-charcoal crucible base on the silicon powder, and then siliconize at 1900°C and furnace pressure lower than 1000pa to obtain the carbon-ceramic crucible base;

[0050] (6) Si 3 N 4 Coating Depositio...

Embodiment 3

[0059] (1) Acupuncture preform: the density of acupuncture preparation is 0.58±0.02g / cm 3 carbon fiber crucible preform;

[0060] (2) Heat treatment of the prefabricated body: the carbon fiber crucible prefabricated body is heat-treated at a high temperature at 2000°C under an argon protective atmosphere, and the density change is 0.56±0.02g / cm 3 ;

[0061] (3) Densification of the preform: the density is 0.56±0.02g / cm 3 The prefabricated carbon fiber crucible is densified to 1.46g / cm by passing 1:1 propylene and nitrogen at 980±5°C and furnace pressure 1KPa 3 Get a charcoal crucible;

[0062] (4) Charcoal heat treatment: heat-treat the charcoal crucible at 2300°C for 3 hours to obtain the charcoal crucible matrix;

[0063] (5) High-temperature siliconizing: place the carbon-charcoal crucible base on the silicon powder, and then siliconize at 1900°C and furnace pressure lower than 1000pa to obtain the carbon-ceramic crucible base;

[0064] (6) Si 3 N 4 Coating Depositio...

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Abstract

The invention discloses a carbon-ceramic composite material crucible containing a Si3N4 and BN composite coating and a preparation method of the carbon-ceramic composite material crucible. The carbon-ceramic composite material crucible is prepared by sequentially depositing an Si3N4 coating and a BN coating on a carbon-ceramic crucible substrate. According to the invention, a carbon-ceramic crucible is used as a substrate, the Si3N4 coating is deposited on the pores and the surfaces (the inner surface and the outer surface) of the carbon-ceramic crucible, and then the BN coating is deposited. According to the invention, monocrystalline silicon is produced only by adopting a single crucible, and the high-temperature stability and the silicon corrosion resistance of the crucible are greatly improved through the synergistic effect of the carbon-ceramic crucible substrate, the Si3N4 coating and the BN coating; and meanwhile, the wettability of the surface of the crucible to silicon is poor, so that the problem that silicon crystal is adhered to the crucible and is difficult to clean after monocrystalline silicon production is avoided, the service life of the crucible is prolonged, the replacement frequency of the crucible is reduced, and the production efficiency of monocrystalline silicon is improved.

Description

technical field [0001] The invention belongs to the technical field of thermal field tooling / components for single crystal silicon drawing furnaces, and in particular relates to a Si-containing 3 N 4 A carbon-ceramic composite crucible with BN composite coating and a preparation method thereof. Background technique [0002] At present, the most widely used method in the production of monocrystalline silicon is the Czochralski method: that is, the monocrystalline silicon rod is drawn in a monocrystalline silicon furnace, and the quartz crucible containing polycrystalline silicon is placed in a carbon-carbon composite material crucible. However, when this method is used for production, the temperature in the monocrystalline silicon furnace is as high as 1500°C, and the quartz crucible containing polycrystalline silicon will soften at this temperature, and it often needs to be replaced after 400-500 hours of use. It is often firmly stuck to the carbon-carbon composite materia...

Claims

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Application Information

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IPC IPC(8): C04B41/89C04B35/573C04B35/622C30B29/06C30B15/10
CPCC04B41/89C04B41/52C04B35/573C04B35/622C30B29/06C30B15/10C04B2235/77C04B2235/96C04B2235/5248C04B2235/614C04B2235/428C04B41/5066C04B41/4531C04B41/5064
Inventor 陈振宇朱苏华周娩红
Owner HUNAN SHIXIN NEW MATERIALS CO LTD
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