CN116240520A - Silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and preparation method and application thereof - Google Patents

Silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and preparation method and application thereof Download PDF

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CN116240520A
CN116240520A CN202211672868.7A CN202211672868A CN116240520A CN 116240520 A CN116240520 A CN 116240520A CN 202211672868 A CN202211672868 A CN 202211672868A CN 116240520 A CN116240520 A CN 116240520A
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boron nitride
pyrolytic
silicon carbide
pyrolytic graphite
layer
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陈宏�
董家海
斯超波
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Changshu Tongle Electronic Materials Co ltd
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Changshu Tongle Electronic Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C23C16/325—Silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/342—Boron nitride
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]

Abstract

The invention discloses a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and a preparation method and application thereof, wherein a pyrolytic graphite heating layer is deposited on the surface of a pyrolytic boron nitride substrate by adopting a CVD (chemical vapor deposition) process; secondly, continuously depositing a pyrolytic boron nitride insulating layer on the pyrolytic boron nitride substrate deposited with the pyrolytic graphite heating layer by adopting a CVD process, and fully covering the pyrolytic graphite heating layer and the pyrolytic boron nitride substrate; and finally, depositing a compact silicon carbide protective layer on the surface of the pyrolytic boron nitride insulating layer. The pyrolytic graphite heating layer is wrapped at the middle position by the pyrolytic boron nitride insulating layer, and the pyrolytic boron nitride insulating layer is further completely wrapped by the silicon carbide protective layer. The silicon carbide-boron nitride-pyrolytic graphite composite heating sheet prepared by utilizing the high conductivity of the pyrolytic graphite heating layer and the high-temperature resistance, oxidation resistance and high radiation characteristics of the silicon carbide protective layer can realize the electric heating requirement of 800-1600 ℃, and has the advantages of light weight, high purity, high stability and long service life.

Description

Silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and preparation method and application thereof
Technical Field
The invention relates to the technical field of electric heating materials, in particular to a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet, a preparation method and application thereof.
Background
The graphite material has excellent electric conductivity, heat conductivity, high temperature resistance and good chemical stability, is commonly used as a heating element material in a high-temperature electric heating furnace used in a non-oxidizing atmosphere, and is difficult to heat by using a graphite heating element in electric heating equipment required by the semiconductor industry. The CVD process is a method for preparing high-purity materials, and the prepared pyrolytic graphite layer has the impurity content less than 5ppm and can meet the requirement of semiconductor equipment on the purity of a heating element part. Meanwhile, graphite volatilizes to consume self-heating element materials, so that the service life of the self-heating element materials is shortened, and the resistivity of the self-heating element materials is changed. On the other hand, since some semiconductor devices are required to be thin and lightweight for the heat generating body part, and have high and uniform heat generating efficiency. The traditional static pressure graphite is formed by stacking graphite particles, so that the static pressure graphite cannot be processed too thin, the thickness is slightly thin, the strength is obviously reduced, and the heating efficiency is also sharply reduced. Therefore, the structural performance of the heating element needs to be optimally designed to obtain the high-temperature heating element with high purity, corrosion resistance, oxidation resistance, light weight, thinness and high efficiency.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and a preparation method thereof, which are used for obtaining a silicon carbide-boron nitride-pyrolytic graphite composite heating body for high-temperature electric heating and have the advantages of high purity, corrosion resistance, oxidation resistance, thinness and high efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of silicon carbide-boron nitride-pyrolytic graphite composite heating sheet, adopt CVD process (chemical vapor deposition) to deposit pyrolytic graphite heating layer on pyrolytic boron nitride substrate surface at first; secondly, continuously depositing a pyrolytic boron nitride insulating layer on the pyrolytic boron nitride substrate deposited with the pyrolytic graphite heating layer by adopting a CVD process, and fully covering the pyrolytic graphite heating layer and the pyrolytic boron nitride substrate; and finally, depositing a compact silicon carbide protective layer on the surface of the pyrolytic boron nitride insulating layer. The pyrolytic graphite heating layer is wrapped at the middle position by the pyrolytic boron nitride insulating layer, and the pyrolytic boron nitride insulating layer is further completely wrapped by the silicon carbide protective layer.
Preferably, the thickness of the pyrolytic graphite heating layer is 10-500 μm, and the thickness of the pyrolytic boron nitride substrate is 0.1-2mm.
The pyrolytic graphite heat generating layer may have a thickness in any number in the range of 10 to 500. Mu.m, such as any one of 10 μm,20 μm,50 μm,80 μm,100 μm,150 μm,200 μm,250 μm,300 μm,350 μm,400 μm,450 μm,500 μm, etc.
The pyrolytic boron nitride substrate may have a thickness in any number in the range of 0.1-2mm, such as any of a thickness of 0.1mm,0.2mm,0.5mm,1mm,1.2mm,1.4mm,1.6mm,1.8mm,2mm, etc.
In any of the above schemes, it is preferable that a CVD process is used to continuously deposit pyrolytic boron nitride insulating layers on the pyrolytic boron nitride substrate deposited with the pyrolytic graphite heating layer, the upper and lower surfaces of the pyrolytic graphite heating layer are covered completely, and the thickness of the pyrolytic boron nitride insulating layers on the upper and lower surfaces of the pyrolytic graphite heating layer is different.
In any of the above embodiments, it is preferable that the thickness of the pyrolytic boron nitride insulating layer on one side is 0.1 to 2mm, and the thickness of the pyrolytic boron nitride insulating layer on the other side is 0.2 to 4mm.
In any of the above schemes, it is preferable that the thickness of the pyrolytic boron nitride insulating layer positioned above the pyrolytic graphite heating layer is 0.1-2mm, and the thickness of the pyrolytic boron nitride insulating layer positioned below the pyrolytic graphite heating layer is 0.2-4mm.
In any of the above schemes, it is preferable to deposit a dense silicon carbide protective layer on the surface of the pyrolytic boron nitride insulating layer, and the thickness of the silicon carbide protective layer is 10-200 μm. The silicon carbide protective layer completely encapsulates the pyrolytic boron nitride insulating layer and may be any number of thicknesses ranging from 10 to 200 μm, such as 10 μm,20 μm,50 μm,70 μm,80 μm,100 μm,120 μm,140 μm,160 μm,180 μm,200 μm.
In any of the above schemes, preferably, the preparation method specifically comprises the following steps:
step (1), thinning a pyrolytic boron nitride block body into a sheet shape to obtain a pyrolytic boron nitride substrate;
embedding a pyrolytic boron nitride substrate in a graphite mold, only leaking out the upper surface of the pyrolytic boron nitride substrate, embedding and wrapping the rest part of the pyrolytic boron nitride substrate by the graphite mold, putting the pyrolytic boron nitride substrate in a high-temperature atmosphere reaction furnace, and introducing a mixed gas containing a carbon source and argon gas for chemical vapor deposition of pyrolytic graphite to obtain a pyrolytic graphite heating layer;
step (3), taking out the sample processed in the step (2), carrying out laser etching processing on the pyrolytic graphite heating layer deposited on the surface of the sample, and removing the pyrolytic graphite heating layer in the redundant area, wherein the pyrolytic graphite heating layer in the area which is not subjected to laser etching processing forms a conductive circuit;
step (4), placing the sample treated in the step (3) in a high-temperature atmosphere reaction furnace, and introducing NH 3 、BCl 3 And N 2 Vapor deposition of pyrolytic boron nitride layer, and fully coating the sample to obtain a pyrolytic boron nitride insulating layer;
stopping ventilation and performing high-temperature vacuum pretreatment;
step (6), introducing CH 3 SiCl 3 、H 2 And (3) depositing a silicon carbide protective layer on the mixed gas of Ar, wherein the silicon carbide protective layer fully coats the sample treated in the step (5);
and (7) taking out the sample treated in the step (6), and processing graphite electrode ports at two ends of the sample.
In any of the above embodiments, it is preferable that the pyrolytic boron nitride block in the step (1) is thinned to 0.1 to 2mm, processed into a sheet shape, and has a surface roughness Ra of 0.1 to 2. Mu.m.
In any of the above schemes, it is preferable that in the step (2), the total flow of the mixed gas containing the carbon source and the argon is 10-100L/min, the molar ratio of the carbon source to the argon is 1:0.5-20, the temperature of chemical vapor deposition is 1800-2400 ℃, and the deposition time is 2-50 h.
In the step (2), the total flow rate of the mixed gas of the carbon source and the argon is any number of 10-100L/min, such as 10L/min,20L/min, 30L/min, 50L/min,80L/min and 100L/min. The molar ratio of carbon source to argon may be any number from 1:0.5 to 20, such as 1:0.5, or 1:1, or 1:3, or 1:5, or 1:8, or 1:10, or 1:12, or 1:15, or 1:18, or 1:20. The chemical vapor deposition temperature may be any number of 1800 ℃ to 2400 ℃, such as 1800 ℃,1900 ℃,2000 ℃,2100 ℃,2200 ℃,2300 ℃,2400 ℃; the deposition time may be any number from 2 to 50 h, such as 2 h,5 h,10 h,15 h,20 h,30 h,40 h,50 h.
In any one of the above embodiments, preferably, in the step (2), the carbon source is CH 4 、C 2 H 4 、C 2 H 6 、C 3 H 6 、C 3 H 8 At least one of them.
The carbon source may be CH 4 Or C 2 H 4 Or C 2 H 6 Or C 3 H 6 Or C 3 H 8 May also be CH 4 、C 2 H 4 、C 2 H 6 、C 3 H 6 、C 3 Equal proportion of H8, or CH 4 、C 2 H 4 、C 2 H 6 、C 3 H 6 、C 3 Equal proportions of two or more of H8.
In any of the above embodiments, in the step (4), NH 3 、BCl 3 And N 2 The total flow of the mixed gas is 10-100L/min, wherein NH 3 And BCl 3 The molar ratio of (2) is 1:0.2-2, NH 3 And N 2 The molar ratio of (2) is 1:1, the vapor deposition temperature is 1500-2000 ℃, and the deposition time is 1-50 h.
NH 3 、BCl 3 And N 2 The total flow of the mixed gas of (2) can be any of 10-100L/minThe number is, for example, 10L/min,20L/min,50L/min,80L/min,100L/min.
NH 3 And BCl 3 The molar ratio of (2) is 1:0.2-2, such as NH 3 And BCl 3 The molar ratio of (2) may be 1:0.2,1:0.5, 1:1, 1:1.5, 1:2.
In any of the above schemes, it is preferable that in the step (5), after stopping ventilation, the temperature is raised to 2400-2800 ℃ for high-temperature vacuum pretreatment, and the temperature is kept at 1-100 h.
In step (5), the high temperature vacuum pretreatment may be performed at any number of 2400-2800 ℃, such as 2400 ℃,2500 ℃,2600 ℃,2700 ℃ and 2800 ℃.
In any of the above schemes, preferably, in the step (6), the temperature is reduced to 1000-1500 ℃, and CH is introduced 3 SiCl 3 、H 2 And Ar, continuing depositing a silicon carbide protective layer for 2-50 h, wherein the deposition time is CH 3 SiCl 3 、H 2 The total flow rate of the mixed gas with Ar is 10-200L/min, CH 3 SiCl 3 And H 2 The molar ratio of (2) is 1:1-20, H 2 And Ar molar ratio is 1:0.2-2.
In step (6), CH 3 SiCl 3 、H 2 The total flow rate of the mixed gas with Ar may be any number of 10 to 200L/min, for example, 10L/min,20L/min,50L/min,80L/min,100L/min,120L/min,140L/min,160L/min,180L/min,200L/min.
In any of the above embodiments, it is preferable that in the step (7), the surface of the silicon carbide protective layer is further treated to control the surface roughness Ra to 1 to 5 μm.
The invention also discloses a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet, which is obtained by adopting the preparation method of any one of the above.
Preferably, the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet consists of a pyrolytic boron nitride substrate, a pyrolytic graphite heating layer, a pyrolytic boron nitride insulating layer and a silicon carbide protective layer, wherein the total thickness is 1-7mm, and the pyrolytic graphite heating layer, the pyrolytic boron nitride insulating layer and the silicon carbide protective layer are sequentially arranged from inside to outside.
The invention also discloses application of the prepared silicon carbide-boron nitride-pyrolytic graphite composite heating sheet in the field of electric heating.
The invention has the following beneficial effects:
the invention discloses a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet, a preparation method and application thereof, wherein the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet prepared by utilizing the high conductivity of a pyrolytic graphite heating layer and the high insulativity, high heat conductivity and high temperature resistance, oxidation resistance and high radiation characteristics of a silicon carbide protective layer can realize the electric heating requirement of 800-1600 ℃, and has the advantages of light weight, high purity, high stability and long service life. Because the pyrolytic graphite heating layer is prepared by adopting a CVD process, the pyrolytic graphite heating layer and the pyrolytic boron nitride substrate (matrix) can be tightly combined, and the thickness is controllable, and the thermal insulation layer can be realized from submicron level to millimeter level, so that the conductivity and the heating efficiency can be adjusted. By utilizing the high-temperature corrosion resistance of pyrolytic boron nitride and silicon carbide, the pyrolytic graphite heating layer can be effectively prevented from being corroded and oxidized. The oxidation resistance temperature of the boron nitride is only 800 ℃, so that the oxidation resistance temperature of the material can be increased to 1600 ℃ by the outermost silicon carbide protective layer.
Drawings
FIG. 1 is a schematic view of a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet prepared in example 1 of the present invention;
FIG. 2 is a diagram of a conductive circuit formed by laser etching after depositing a pyrolytic graphite layer on the surface of boron nitride during the preparation of a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to example 1 of the present invention;
FIG. 3 is a side view of a finished product of the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet prepared in example 1 of the present invention;
reference numerals:
1. a pyrolytic graphite heating layer; 2. pyrolyzing the boron nitride insulating layer; 3. a silicon carbide protective layer; 4. pyrolytic nitrogen
And (3) a boron carbide substrate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. The starting materials in the examples below are commercially available.
Example 1
The preparation method of the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet comprises the following steps:
(1) According to the design size requirement, the diameter of the high-purity pyrolytic boron nitride block with the size requirement is 100-700mm, the high-purity pyrolytic boron nitride block with the purity of 99.999% is thinned to 0.1-2mm, and the pyrolytic boron nitride block is subjected to surface treatment, so that the pyrolytic boron nitride block is processed into a sheet shape with the specified size, and the surface roughness Ra is 0.1-2 mu m, and the pyrolytic boron nitride substrate 4 is obtained.
(2) Embedding the pyrolytic boron nitride substrate treated in the step (1) into a graphite mold (the graphite mold is high-purity static pressure graphite, the impurity content is less than 99.9995%) so as to avoid depositing pyrolytic graphite layers on the back and the side surfaces of the pyrolytic boron nitride substrate, then putting the pyrolytic boron nitride substrate into a high-temperature atmosphere reaction furnace for chemical vapor deposition, thereby obtaining a pyrolytic graphite heating layer 1 on the surface of the pyrolytic boron nitride substrate 4, mixing mixed gas containing carbon source and argon according to a certain proportion, then introducing the mixed gas into the high-temperature atmosphere reaction furnace, controlling the total flow of the mixed gas to be 10-100L/min, controlling the temperature of the chemical vapor deposition to be 1800-2400 ℃, the deposition time to be 2-50 h, and the molar ratio of the carbon source to the argon to be 1:0.5-20, wherein the carbon source is CH 4 、C 2 H 4 、C 2 H 6 、C 3 H 6 、C 3 H 8 One of them.
(3) And (3) carrying out laser etching processing on the pyrolytic graphite heating layer 1 deposited on the surface of the sample processed in the step (2) according to the design of the circuit to form a conductive circuit, and removing the redundant pyrolytic graphite heating layer 1 at the same time as shown in fig. 2.
(4) Placing the sample treated in the step (3) in a high-temperature atmosphere reaction furnace to deposit pyrolytic boron nitride, obtaining a pyrolytic boron nitride insulating layer 2 which can fully cover the pyrolytic graphite heating layer 1 by 360 degrees, and carrying out NH (NH) treatment 3 、BCl 3 And N 2 Mixing according to a certain proportion, introducing into a high-temperature reaction furnace for vapor deposition, wherein the total flow of gas is controlled to be 10-100L/min, and NH is contained 3 And BCl 3 The molar ratio of (2) is 1:0.2-2, NH 3 And N 2 The molar ratio of (2) is 1:1, the vapor deposition temperature is 1500-2000 ℃, and the deposition time is 1-50 h.
(5) Stopping ventilation after vapor deposition, continuously heating to 2400-2800 ℃ for high-temperature vacuum pretreatment (vacuum degree is less than 100 Pa), and preserving heat for 1-100 h, so that the pyrolytic graphite heating layer 1 can be further graphitized, the conductivity of the pyrolytic graphite heating layer is improved, and residual stress can be removed from the pyrolytic boron nitride insulating layer 2, so that the combination of the pyrolytic graphite heating layer is firmer.
(6) Subsequently, the temperature is reduced to 1000-1500 ℃ to continue depositing the SiC coating to obtain the SiC protective layer 3, in particular, CH 3 SiCl 3 、H 2 Mixing Ar with the mixture according to a certain proportion, and then introducing the mixture into a high-temperature reaction furnace, wherein the total flow of gas is controlled to be 10-200L/min and CH 3 SiCl 3 And H 2 The molar ratio of (2) is 1:1-20, H 2 And argon gas mole ratio of 1:0.2-2, and the deposition time is 2-50 h.
(7) And (3) taking out the sample processed in the step (6) after cooling to normal temperature, processing graphite electrode ports at two ends of the sample according to the design, carrying out surface treatment on the silicon carbide protective layer 3, and controlling the surface roughness Ra of the silicon carbide protective layer to be 1-5 mu m to obtain the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet, wherein the structure is shown in figure 1, and the physical diagrams are shown in figures 2 and 3.
Example 2
A method for preparing a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet is similar to example 1, except that NH is added in step (4) 3 、BCl 3 And N 2 Mixing according to a certain proportion, introducing into a high-temperature reaction furnace for vapor deposition, wherein the total flow of gas is controlled to be 10-100L/min, and NH is contained 3 And BCl 3 The molar ratio of (2) is 1:3, NH 3 And N 2 The molar ratio of (2) is 1:2, the vapor deposition temperature is 1400 ℃, the deposition time is 1-50 h, and the prepared silicon carbide-boron nitride-pyrolytic graphite composite heating sheet has weaker bonding of the pyrolytic boron nitride insulating layer 2 and is easy to fall off.
Example 3
Silicon carbide (SiC) roomThe preparation method of the boron nitride-pyrolytic graphite composite heating sheet is similar to example 1, except that in step (6), the SiC coating is continuously deposited by reducing the temperature to 800 ℃ to obtain the silicon carbide protective layer 3, and CH is formed at the moment 3 SiCl 3 、H 2 Ar is mixed according to a certain proportion and then is introduced into a high-temperature reaction furnace, the total flow of gas is controlled to be 10-200L/min, the molar ratio of CH3SiCl3 to H2 is 0.5:1-20, and the molar ratio of H2 to argon is 1:3, the deposition time is 2-50 h. The silicon carbide protective layer 3 in the prepared silicon carbide-boron nitride-pyrolytic graphite composite heating sheet has more thin defects, and can only meet the electric heating requirement of 600-1000 ℃.
The present invention is not limited to the above-mentioned embodiments, and any person skilled in the art, based on the technical solution of the present invention and the inventive concept thereof, can be replaced or changed within the scope of the present invention.

Claims (9)

1. The preparation method of the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet is characterized by comprising the following steps of: firstly, depositing a pyrolytic graphite heating layer (1) on the surface of a pyrolytic boron nitride substrate (4) by adopting a CVD process; then, continuously depositing a pyrolytic boron nitride insulating layer (2) on the pyrolytic boron nitride substrate (4) deposited with the pyrolytic graphite heating layer (1) by adopting a CVD process, and fully covering the pyrolytic graphite heating layer (1) and the pyrolytic boron nitride substrate (4); finally, depositing a silicon carbide protective layer (3) on the surface of the pyrolytic boron nitride insulating layer (2), wherein the method comprises the following steps:
step (1), thinning the pyrolytic boron nitride block body into a flake shape to obtain a pyrolytic boron nitride substrate (4);
embedding a pyrolytic boron nitride substrate (4) in a graphite mold, only leaking out the upper surface of the pyrolytic boron nitride substrate (4), embedding and wrapping the rest part by the graphite mold, putting the graphite mold into a high-temperature atmosphere reaction furnace, and introducing a mixed gas containing a carbon source and argon gas for chemical vapor deposition of pyrolytic graphite to obtain a pyrolytic graphite heating layer (1);
step (3), taking out the sample treated in the step (2), carrying out laser etching processing on the pyrolytic graphite heating layer (1) deposited on the surface of the sample, and removing the pyrolytic graphite heating layer (1) in the redundant area, wherein the pyrolytic graphite heating layer (1) in the area which is not subjected to laser etching processing forms a conductive circuit;
step (4), placing the sample treated in the step (3) in a high-temperature atmosphere reaction furnace, and introducing NH 3 、BCl 3 And N 2 Vapor deposition of a pyrolytic boron nitride layer, and full cladding of the sample to obtain a pyrolytic boron nitride insulating layer (2), wherein NH 3 Gas and BCl 3 The molar ratio of the gas is 1:0.2-2, NH 3 And N 2 The molar ratio of (2) is 1:1, and the vapor deposition temperature is 1500-2000 ℃;
stopping ventilation and performing high-temperature vacuum pretreatment;
step (6), introducing CH 3 SiCl 3 、H 2 And Ar, wherein CH 3 SiCl 3 And H 2 The molar ratio of (2) is 1:1-20, H 2 And Ar molar ratio is 1:0.2-2, depositing a silicon carbide protective layer (3), and fully coating the sample treated in the step (5) by the silicon carbide protective layer (3);
and (7) taking out the sample treated in the step (6), and processing graphite electrode ports at two ends of the sample.
2. The method for preparing the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 1, wherein the method comprises the following steps: in the step (2), the total flow of the mixed gas containing the carbon source and the argon is 10-100L/min, the molar ratio of the carbon source to the argon is 1:0.5-20, the chemical vapor deposition temperature is 1800-2400 ℃, and the deposition time is 2-50 h.
3. The method for preparing the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 1, wherein the method comprises the following steps: in the step (2), the carbon source is CH 4 、C 2 H 4 、C 2 H 6 、C 3 H 6 、C 3 H 8 Is to of (a)One less.
4. The method for preparing the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 1, wherein the method comprises the following steps: in step (4), NH 3 、BCl 3 And N 2 The total flow of the mixed gas is 10-100L/min, and the deposition time is 1-50 h.
5. The method for preparing the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 1, wherein the method comprises the following steps: in the step (5), after stopping ventilation, heating to 2400-2800 ℃ for high-temperature vacuum pretreatment, and preserving heat for 1-100 h.
6. The method for preparing the silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 1, wherein the method comprises the following steps: in the step (6), the temperature is reduced to 1000-1500 ℃ and CH is introduced 3 SiCl 3 、H 2 And Ar, continuing to deposit a silicon carbide protective layer (3) for 2-50 h, wherein CH 3 SiCl 3 、H 2 And Ar is 10-200L/min.
7. A silicon carbide-boron nitride-pyrolytic graphite composite heating sheet obtained by the production method according to any one of claims 1 to 6.
8. The silicon carbide-boron nitride-pyrolytic graphite composite heating sheet according to claim 7, wherein: the thermal decomposition boron nitride insulating layer comprises a thermal decomposition boron nitride substrate (4), a thermal decomposition graphite heating layer (1), a thermal decomposition boron nitride insulating layer (2) and a silicon carbide protective layer (3), wherein the total thickness is 1-7mm, and the thermal decomposition graphite heating layer (1), the thermal decomposition boron nitride insulating layer (2) and the silicon carbide protective layer (3) are sequentially arranged from inside to outside.
9. Use of a silicon carbide-boron nitride-pyrolytic graphite composite heating sheet obtained by the production method according to any one of claims 1 to 6 in the field of electric heating.
CN202211672868.7A 2022-12-26 2022-12-26 Silicon carbide-boron nitride-pyrolytic graphite composite heating sheet and preparation method and application thereof Pending CN116240520A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116803951A (en) * 2023-07-19 2023-09-26 北京亦盛精密半导体有限公司 High-purity high-resistivity silicon carbide workpiece and forming process thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116803951A (en) * 2023-07-19 2023-09-26 北京亦盛精密半导体有限公司 High-purity high-resistivity silicon carbide workpiece and forming process thereof
CN116803951B (en) * 2023-07-19 2024-03-05 北京亦盛精密半导体有限公司 High-purity high-resistivity silicon carbide workpiece and forming process thereof

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