CN116854477A - Silicon carbide ceramic with anisotropic resistivity, preparation method thereof and silicon carbide sheet product - Google Patents
Silicon carbide ceramic with anisotropic resistivity, preparation method thereof and silicon carbide sheet product Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 188
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 188
- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 61
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 62
- 238000000034 method Methods 0.000 claims description 37
- 239000011159 matrix material Substances 0.000 claims description 32
- 238000000151 deposition Methods 0.000 claims description 28
- 239000012495 reaction gas Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 230000008021 deposition Effects 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- 238000005137 deposition process Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000012159 carrier gas Substances 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 4
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 3
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 25
- 238000005245 sintering Methods 0.000 description 19
- 239000000843 powder Substances 0.000 description 8
- 239000002390 adhesive tape Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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Abstract
The application relates to the technical field of ceramic materials, and particularly discloses silicon carbide ceramic with anisotropic resistivity, a preparation method thereof and a silicon carbide sheet product. The silicon carbide ceramic comprises a high-purity silicon carbide insulating thin layer and a carbon-containing high-conductivity thin layer which are sequentially overlapped; the top layer and the bottom layer of the silicon carbide ceramic are both the high-purity silicon carbide insulating thin layers; in the high-purity silicon carbide insulating thin layer, the molar ratio of carbon to silicon is 0.8-2, and the thickness is 0.1-10mm; in the carbon-containing high-conductivity thin layer, the carbon-silicon molar ratio is 2-15, and the thickness is 0.05-3mm. The silicon carbide ceramic with high purity, high density and anisotropic resistivity can be prepared by the preparation method, and the anisotropic index of the resistivity of the silicon carbide ceramic is as high as 101.993.
Description
Technical Field
The application relates to the technical field of ceramic materials, in particular to silicon carbide ceramic with anisotropic resistivity, a preparation method thereof and a silicon carbide sheet product.
Background
Silicon carbide has the advantages of high hardness, high strength, high temperature resistance, corrosion resistance and the like due to the strong covalent bond property of Si-C bond, and has proper electrical characteristics. High quality silicon carbide parts are highly desirable in high value-added industries such as chip etching, aerospace, nuclear industry, and the like.
For the silicon carbide sheet functional product with high added value, the radial dimension is far greater than the thickness direction dimension, so that the radial resistance of the product is far greater than the thickness direction resistance of the product. When the workpiece is used for special purposes, the radial resistance of the workpiece is too large, so that the voltage at two ends of the workpiece is too strong, a large amount of static electricity is accumulated, and the actual use effect of the workpiece is affected. The whole resistivity of the workpiece is reduced by doping other elements, so that the thickness direction of the workpiece is broken down by current, and the use efficiency of the workpiece is lost. Therefore, the silicon carbide high-quality part with high resistivity in the thickness direction and low resistivity in the radial direction has wide application prospect.
In the related art, there are two methods of sintering and CVD for preparing high quality silicon carbide articles.
There are processes for preparing silicon carbide articles of anisotropic resistivity by sintering. The anisotropic conductivity is typically realized by directionally arranging graphene sheets doped in the silicon carbide, the axial (thickness direction) resistivity of the prepared silicon carbide product is controllable within the range of 96.9-0.97Ω & cm, the radial resistivity is controllable within the range of 59.23-0.7Ω & cm, and the mass fraction of the SiC matrix is 90.5-96.4wt%. However, due to the limitation of the process conditions, the sintering mode has the following disadvantages: firstly, siC powder needs to be sintered, and boron and carbon sintering aids need to be added in the sintering process, so that the purity of a silicon carbide product obtained after sintering is low, and is generally below 99%, and the use requirement of a high-grade clean room cannot be met; then, due to the limitation of the properties of the SiC material (weak sintering diffusion capability), the sintering temperature is required to be high (generally more than 1900 ℃), the sintering compactness is not high (generally less than 96%), the sintering condition is strict, and the prepared silicon carbide product has the condition of occurrence of gaps; moreover, although the axial resistivity and the radial resistivity of the silicon carbide workpiece prepared by the sintering method can be controlled within a certain range, the difference between the axial resistivity and the radial resistivity of the silicon carbide workpiece is not obvious, and the application effect cannot be well reflected; and the common sintering process is extremely easy to cause bending deformation, and silicon carbide workpieces with larger radial sizes are difficult to prepare.
The silicon carbide ceramic prepared by the traditional CVD process has the characteristics of high purity and high density, and the resistivity of the silicon carbide ceramic is highly isotropic. However, there is no report on the related technology for preparing high-purity and high-density anisotropic resistivity silicon carbide products by using a CVD mode at present.
By designing an adhesive route and adhering the conductive adhesive tape on the radial surface of the isotropic resistivity silicon carbide workpiece according to the route, the purpose of radially reducing the resistance can be achieved by means of the conductive adhesive tape adhered radially, and the performance requirement is met. However, the technical scheme is very easy to form a pollution source in a clean room, and the conductive adhesive tape needs to be frequently replaced in a high-temperature and corrosion environment, so that the continuous production is not facilitated, and the influence of frequently disassembling parts on the whole precision of the silicon carbide workpiece is large.
In view of the above, how to prepare high quality silicon carbide ceramic products with high purity, high density and high anisotropic resistivity is a problem to be solved.
Disclosure of Invention
The application provides silicon carbide ceramic with anisotropic resistivity, a preparation method thereof and a silicon carbide sheet product. The preparation method can prepare the silicon carbide ceramic with high purity, high density and anisotropic resistivity, and overcomes the defects of severe conditions and difficult preparation of large-size sheet parts when the silicon carbide ceramic with anisotropic resistivity is prepared by a sintering process in the related technology.
In a first aspect, the present application provides a silicon carbide ceramic with anisotropic resistivity, which adopts the following technical scheme:
a silicon carbide ceramic of anisotropic resistivity comprising a high purity silicon carbide insulating layer and a carbon-containing highly conductive layer stacked in sequence; the top layer and the bottom layer of the silicon carbide ceramic are both the high-purity silicon carbide insulating thin layers;
in the high-purity silicon carbide insulating thin layer, the molar ratio of carbon to silicon is 0.8-2, and the thickness is 0.1-10mm;
in the carbon-containing high-conductivity thin layer, the carbon-silicon molar ratio is 2-15, and the thickness is 0.05-3mm.
The silicon carbide ceramic with anisotropic resistivity provided by the application is formed by sequentially superposing a high-purity silicon carbide insulating thin layer and a carbon-containing high-conductivity thin layer, wherein the high-purity silicon carbide insulating thin layer is positioned on the top layer and the bottom layer of the silicon carbide ceramic, and is positioned between the conductive thin layers to serve as an intermediate layer. The silicon carbide ceramic surface provided by the application has higher purity (more than 99.967 percent), can meet the requirements of a higher-grade clean room, and has higher density (3.202 g/cm) 3 The above).
According to the application, the technological parameters in the CVD process are regularly changed, so that a carbon-containing high-conductivity thin layer is difficult to radially and regularly deposit in the deposition process, the functional requirement of anisotropic resistivity is met, and the high-quality preparation of the silicon carbide ceramic with high purity, high density and anisotropic resistivity is realized. Compared with the solution of designing a circuit and pasting a conductive adhesive tape in the related art, the silicon carbide ceramic prepared by the application endows the product with the radial conductive characteristic from the source, and the corresponding product can work in a high-grade clean room, so that pollution sources are greatly avoided, continuous operation can be realized in special environments such as high temperature, corrosion and the like, and the trouble of frequently detaching precise parts for replacing the conductive adhesive tape under actual working conditions is avoided.
Preferably, in the high-purity silicon carbide insulating thin layer, the molar ratio of carbon to silicon is 1.05-1.55, and the thickness is 0.5-1.5mm.
In a specific embodiment, the high purity silicon carbide insulating film may have a molar ratio of carbon to silicon of 0.8, 1.05, 1.25, 1.55, 2.
In some embodiments, the molar ratio of carbon to silicon in the high purity silicon carbide insulating film may be 0.8-1.05, 0.8-1.25, 0.8-1.55, 1.05-1.25, 1.05-1.55, 1.05-2, 1.25-1.55, 1.25-2, 1.55-2.
In a specific embodiment, the high purity silicon carbide insulating thin layer has a thickness of 0.1mm, 0.5mm, 1.25mm, 1.5mm, 2mm, 5mm, 10mm.
In some embodiments, the high purity silicon carbide insulating thin layer has a thickness of 0.1-0.5mm, 0.1-1.25mm, 0.1-2mm, 0.1-5mm, 0.1-10mm, 0.5-1.25mm, 0.5-2mm, 0.5-5mm, 0.5-10mm, 1.25-2mm, 1.25-5mm, 1.25-10mm, 2-5mm, 2-10mm, 5-10mm.
Preferably, in the carbon-containing high-conductivity thin layer, the molar ratio of carbon to silicon is 6-10, and the thickness is 0.3-2mm.
In a specific embodiment, the carbon-silicon molar ratio in the carbon-containing highly conductive thin layer may be 2, 6, 8, 10, 15.
In some embodiments, the carbon-silicon molar ratio in the carbon-containing highly conductive thin layer may be 2-6, 2-8, 2-10, 2-15, 6-8, 6-10, 6-15, 8-10, 8-15, 10-15.
In a specific embodiment, the thickness in the carbon-containing highly conductive thin layer is 0.05mm, 0.3mm, 0.6mm, 1mm, 2mm, 3mm.
In some embodiments, the thickness in the carbonaceous highly conductive thin layer is 0.05-0.3mm, 0.05-0.6mm, 0.05-1mm, 0.05-2mm, 0.3-0.6mm, 0.3-1mm, 0.3-2mm, 0.3-3mm, 0.6-1mm, 0.6-2mm, 0.6-3mm, 1-2mm, 1-3mm, 2-3mm.
Preferably, in the silicon carbide ceramic, the number of the high-purity silicon carbide insulating thin layers is n+1; the number of the carbon-containing high-conductivity thin layers is N; the N is 1-100.
In the preparation process of the silicon carbide ceramic, high-purity silicon carbide insulating thin layers and carbon-containing high-conductivity thin layers can be sequentially deposited in turn according to actual requirements, so that the purpose of anisotropy is achieved.
Preferably, the silicon carbide ceramic has a surface purity of 99.96-99.991% and a density of 3.2-3.21g/cm 3 The radial resistivity is 50-250 Ω & cm, and the axial resistivity is 900-6000 Ω & cm.
Preferably, the silicon carbide ceramic has a resistivity anisotropy index as high as 101.993.
In a second aspect, the present application provides a method for preparing the silicon carbide ceramic with anisotropic resistivity, which adopts the following technical scheme:
a preparation method of silicon carbide ceramic with anisotropic resistivity comprises the following steps:
sequentially depositing a high-purity silicon carbide insulating thin layer and a carbon-containing high-conductivity thin layer on a deposition matrix in turn by using high-purity silicon source gas and high-concentration carbon source gas through chemical vapor deposition, and removing the deposition matrix in an oxidation mode to prepare silicon carbide ceramic with anisotropic resistivity; the top layer and the bottom layer of the silicon carbide ceramic are both the high-purity silicon carbide insulating thin layers;
in the deposition process of the high-purity silicon carbide insulating thin layer, the molar ratio of a carbon-silicon gas source is 0.8-2; the reaction temperature is 1000-1350 ℃; the flow rate of the reaction gas is 200-1000sccm; the thickness is 0.1-10mm;
in the deposition process of the carbon-containing high-conductivity thin layer, the carbon-silicon gas source molar ratio is 2-15; the reaction temperature is 1000-1350 ℃; the flow rate of the reaction gas is 200-1000sccm; the thickness is 0.05-3mm.
In a specific embodiment, the reaction temperature may be 1000 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃.
In some specific embodiments, the reaction temperature may be 1000-1150 ℃, 1000-1200 ℃, 1000-1250 ℃, 1000-1300 ℃, 1150-1200 ℃, 1150-1250 ℃, 1150-1300 ℃, 1150-1350 ℃, 1200-1250 ℃, 1200-1300 ℃, 1200-1350 ℃, 1250-1300 ℃, 1250-1350 ℃.
In a specific embodiment, the reactant gas flow may be 200sccm, 300sccm, 500sccm, 700sccm, 1000sccm.
In some embodiments, the reactant gas flow rate may be 200-300sccm, 200-500sccm, 200-700sccm, 200-1000sccm, 300-500sccm, 300-700sccm, 300-1000sccm, 500-700sccm, 500-1000sccm, 700-1000sccm.
The application deposits the high-purity silicon carbide insulating thin layer by controlling the molar ratio of the carbon-silicon gas source, the reaction temperature and the reaction gas flow, and the thickness of the high-purity silicon carbide insulating thin layer is limited to be within the range. And further adjusting the molar ratio of the carbon-silicon gas source, the reaction temperature and the reaction gas flow rate to deposit the carbon-containing high-conductivity thin layer, wherein the thickness of the carbon-containing high-conductivity thin layer is limited to be within the range. In the process of depositing the carbon-containing high-conductivity thin layer, the carbon-silicon gas source molar ratio in the reaction gas is increased, the ratio of carbon elements is increased, and the crystal form of silicon carbide in the deposited thin layer is changed, so that the carbon-containing high-conductivity thin layer is obtained.
Compared with the silicon carbide ceramic with anisotropic resistivity prepared by a sintering method in the related art, the preparation method provided by the application has the advantages that the temperature is controlled within the range of 1000-1350 ℃, and the temperature of the sintering method in the related art is as high as 1900 ℃. Therefore, the preparation method of the application greatly reduces the process temperature and the preparation difficulty, and ensures the good formability of the silicon carbide ceramic.
In the deposition process, high-purity silicon carbide insulating thin layers and carbon-containing high-conductivity thin layers can be sequentially deposited in turn according to actual requirements, so that the purpose of anisotropy is achieved. The deposition times of the carbon-containing high-conductivity thin layer can be N, the high-purity silicon carbide insulating thin layer is N+1, the value range of N is 1-100, and the top layer and the bottom layer of the silicon carbide ceramic are both high-purity silicon carbide insulating thin layers.
Preferably, the temperature change rate is 1-2 ℃/min in the process of changing the deposition process of the high-purity silicon carbide insulating thin layer to the deposition process of the carbon-containing high-conductivity thin layer or in the process of changing the deposition process of the carbon-containing high-conductivity thin layer to the deposition process of the high-purity silicon carbide insulating thin layer, and the carbon-silicon gas source mole ratio, the reaction temperature and the reaction gas flow are uniformly adjusted to set parameters in the process of changing the temperature.
Preferably, the high purity silicon source gas is high purity SiH 4 SiH of high purity 3 Cl, high purity SiH 2 Cl 2 High purity SiHCl 3 High purity SiCl 4 High purity SiCH 3 Cl 3 One or more of the following.
Preferably, the high purity carbon source gas may be high purity CH 4 High purity C 2 H 6 High purity C 3 H 8 High purity C 4 H 10 One or more of them.
In the chemical vapor deposition process, H with high purity 2 The carrier gas is the carrier gas, and the flow rate of the carrier gas is 1-8slm; ar gas is used as diluent gas.
In the chemical vapor deposition process, the deposition matrix is a graphite matrix sheet.
Preferably, the oxidation removal of the graphite substrate sheet is accomplished using muffle furnace heating.
Preferably, the heating environment of the muffle furnace is an air atmosphere or a high-oxygen atmosphere.
Preferably, the temperature in the muffle furnace is 750-900 ℃.
In the application, the deposition matrix can be selected to be removed after the chemical vapor deposition process is finished in a mode of not damaging the quality of the deposited silicon carbide ceramic. In the embodiment of the application, the graphite matrix is selected as the deposition matrix, the graphite matrix can be completely removed by a heating oxidation mode after the chemical vapor deposition process is finished, and the heating temperature is only controlled to be 750-900 ℃ and is far less than the oxidation temperature 1350 ℃ of the silicon carbide ceramic in the process of removing the graphite matrix, so that the quality of the prepared silicon carbide ceramic is not damaged.
Preferably, the thickness of the deposition matrix does not exceed 3mm.
The thickness of the deposition matrix is limited to not more than 3mm, on one hand, the deposition matrix occupies less space in the CVD chamber, and more space can be reserved for depositing silicon carbide ceramics. On the other hand, the deposition matrix of this thickness can either act to stably deposit the silicon carbide ceramic or can be removed in a minimum amount of time after the deposition process results. Based on the above, the present application controls the thickness of the deposition substrate within the above-described range.
In a third aspect, the present application provides a silicon carbide wafer-like article. The silicon carbide sheet product is prepared from the silicon carbide ceramic with anisotropic resistivity.
In summary, the application has the following beneficial effects:
(1) According to the application, the technological parameters in the CVD process are regularly changed, so that the carbon-containing high-conductivity thin layer and the high-purity silicon carbide insulating thin layer are difficult to radially and regularly deposit in the deposition process, the functional requirement of anisotropic resistivity is met, and the high-quality preparation of the silicon carbide ceramic with high purity, high density and anisotropic resistivity is realized.
(2) Compared with the silicon carbide ceramic with anisotropic resistivity prepared by a sintering method in the related art, the preparation method provided by the application has the advantages that the temperature is controlled within the range of 1000-1350 ℃, and the temperature of the sintering method in the related art is as high as 1900 ℃. Therefore, the preparation method of the application greatly reduces the process temperature and the preparation difficulty, and ensures the good formability of the silicon carbide ceramic.
(3) The surface of the silicon carbide ceramic with anisotropic resistivity prepared by the application has higher purity (more than 99.962 percent), can meet the requirements of a clean room with higher grade, and has higher density (3.202 g/cm) 3 The above).
(4) The anisotropic resistivity silicon carbide sheet product provided by the application has the advantages that the highest ratio of the resistivity of a single product in the thickness direction/radial direction reaches 101.993, the anisotropic index of the resistivity is higher, and the anisotropic resistivity silicon carbide sheet product has obvious effect under actual working conditions.
(5) Compared with the solution of designing a circuit and pasting a conductive adhesive tape in the related art, the silicon carbide ceramic prepared by the application endows the product with the radial conductive characteristic from the source, and the corresponding product can work in a high-grade clean room, so that pollution sources are greatly avoided, continuous operation can be realized in special environments such as high temperature, corrosion and the like, and the trouble of frequently detaching precise parts for replacing the conductive adhesive tape under actual working conditions is avoided.
Drawings
FIG. 1 is a flow chart of a method for preparing silicon carbide ceramic provided by the application.
FIG. 2 is a schematic cross-sectional view of a silicon carbide ceramic of example 1 of the present application.
FIG. 3 is a sample view of the silicon carbide ceramic prepared in example 1 of the present application.
FIG. 4 is a sample graph of silicon carbide ceramic prepared in example 7 of the present application.
Detailed Description
The application provides silicon carbide ceramic and a preparation method thereof. The silicon carbide ceramic prepared by the preparation method has high purity and high density, and also has anisotropic resistivity, and can be used for producing various silicon carbide sheet products. The preparation method uses CVD equipment with the function of precisely controlling the gas flow.
Referring to fig. 1, the preparation method specifically includes the following steps:
(1) Preparation of the deposition matrix: a graphite substrate is placed within the CVD chamber as a deposition substrate. The thickness of the graphite matrix is not more than 3mm. The shape of the graphite matrix is closely related to the shape of the silicon carbide ceramic to be prepared, and a person skilled in the art can select a graphite matrix with a proper shape according to actual needs to prepare the silicon carbide ceramic with the required shape.
(2) Preparation of a high-purity silicon carbide insulating thin layer: selecting high-purity silicon source gas and high-purity carbon source gas, and controlling the parameters of carbon-silicon source gas mole ratio, reaction temperature, reaction gas flow and the like to obtain high-purity H 2 (99.999%) is a carrier gas, and a high-purity silicon carbide insulating thin layer is prepared by CVD on a graphite substrate with Ar gas as a diluent gas. The thickness of the high-purity silicon carbide insulating thin layer is 0.1-10mm.
In particular, the high purity silicon source gas may be high purity SiH 4 SiH of high purity 3 Cl, high purity SiH 2 Cl 2 High purity SiHCl 3 High purity SiCl 4 High purity SiCH 3 Cl 3 One or more of the following. In the art, high purity silicon source gas generally refers to a gas having a purity equal to or higher than 99.9999%.
Specifically, the high purity carbon source gas may be high purity CH 4 High purity C 2 H 6 High purity C 3 H 8 High purity C 4 H 10 One or more of them. In the art, high purity carbon source gas generally refers to a gas having a purity of 99.999% or higher.
Further, the molar ratio of the carbon-silicon gas source is 0.8-2. The reaction temperature is 1000-1350 ℃. The flow rate of the reaction gas is 200-1000sccm. The carrier gas flow is 1-8slm.
(3) Preparation of a carbonaceous high-conductivity thin layer: the carbon-containing high-conductivity thin layer is prepared on the high-purity silicon carbide insulating thin layer by CVD transverse deposition continuously by adjusting the molar ratio of the carbon-silicon gas source, changing the reaction temperature and changing the reaction gas flow. By adjusting the parameters in CVD, the ratio of carbon element in silicon carbide is increased in the deposition process, so that the crystal form of the silicon carbide is changed. The thickness of the carbon-containing high-conductivity thin layer is 0.05-3mm.
Specifically, the molar ratio of the carbon-silicon gas source is adjusted to 2-15. The reaction temperature is 1000-1350 ℃. The flow rate of the reaction gas is 200-1000sccm. The carrier gas flow is 1-8slm.
Preferably, the molar ratio of the carbon-silicon gas source, the reaction temperature and the reaction gas flow rate are gradually changed from the step (2) to the step (3).
Specifically, the reaction temperature is regulated to 1250 ℃ at a heating rate of 1-2 ℃/min, and the molar ratio of the carbon-silicon gas source is gradually regulated to 10 during the heating process, and the flow rate of the reaction gas is regulated to 500sccm.
(4) Repeated preparation of high-purity silicon carbide insulating thin layers: and (3) adjusting the parameters such as the molar ratio of the carbon-silicon gas source, the reaction temperature, the reaction gas flow and the like to be the same as those in the step (2), and continuously preparing the high-purity silicon carbide insulating thin layer on the carbon-containing high-conductivity thin layer by CVD. The thickness of the high-purity silicon carbide insulating thin layer is 0.1-10mm.
Specifically, the reaction temperature is regulated at a cooling speed of 1-2 ℃/min to be the same as that in the step (2), and the carbon-silicon gas source molar ratio and the reaction gas flow are gradually regulated to be the same as those in the step (2) in the cooling process.
Through the preparation of the steps, the silicon carbide product with the sandwich structure of the insulating-conducting-insulating thin layers is obtained.
(5) According to the actual working conditions, the step (3) and the step (4) can be repeated for a plurality of times to obtain sandwich conductive layers with different numbers, and the radial direction of the product can be provided with a plurality of conductive thin layers, so that the purpose of anisotropic conduction is achieved. The number of repetitions may be 1-100 times. In addition, for a single article, different schemes for depositing conductive thin layers on different layers can be implemented according to working conditions.
(6) And removing the graphite matrix and the silicon carbide workpiece deposited on the surface of the graphite matrix from the CVD chamber, and placing the graphite matrix and the silicon carbide workpiece in a muffle furnace for uniform heating until the graphite matrix is completely oxidized and removed, so as to obtain the silicon carbide ceramic with anisotropic resistivity, namely the silicon carbide sheet workpiece. Specifically, the muffle furnace is heated at 750-900 ℃.
In addition, the silicon carbide sheet product with anisotropic resistivity can be properly machined to meet specific use requirements.
Interpretation of the terms
CVD: chemical vapor deposition.
Sheet-like article: and the pointing area is large, and the thickness is thin.
Radial dimension: the top-down dimension, also referred to as the transverse direction, directed to the sheet-like article lie flat.
Thickness direction: pointing in the thickness direction of the sheet-like article is also referred to as the axial direction.
Resistivity: the intrinsic conductivity of the pointing material is independent of the structure.
Resistance: the electrical conductivity of the pointing article is related to the cross-sectional area and length of the article, in addition to the material of the article.
Resistivity anisotropy index: the difference in resistivity in different directions of the pointing material can be calculated by using the resistivity in the thickness direction/the resistivity in the radial direction.
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application.
The present application will be described in further detail with reference to examples, comparative examples, drawings and performance test results.
Examples
Example 1
This embodiment provides a silicon carbide ceramic of anisotropic resistivity.
The preparation method of the silicon carbide ceramic uses CVD equipment with a function of precisely controlling the gas flow, and specifically comprises the following steps:
(1) Preparation of the deposition matrix: a circular sheet of clean graphite substrate having a thickness of 2mm and a diameter of 15cm was placed at the deposition site in the CVD chamber.
(2) Preparation of a high-purity silicon carbide insulating thin layer: high purity SiH is selected 4 As the high-purity silicon source gas, high-purity CH is selected 4 As a high purity carbon source gas, H is of high purity 2 The gas flow is 5slm, ar gas with the flow rate of 7slm is used as diluent gas, the molar ratio of the carbon-silicon gas source is controlled to be 1.05, the reaction gas flow is 300sccm, the highest reaction temperature is 1150 ℃, and a high-purity silicon carbide insulating thin layer with the thickness of 1.25mm is prepared on a graphite substrate circular sheet by CVD.
(3) Preparation of a carbonaceous high-conductivity thin layer: and (3) adjusting the molar ratio of the carbon-silicon gas source, the reaction temperature and the reaction gas flow, adjusting the reaction temperature to 1250 ℃ at the heating rate of 1-2 ℃/min, gradually adjusting the molar ratio of the carbon-silicon gas source to 10 in the heating process, adjusting the reaction gas flow to 500sccm, and continuously preparing a layer of silicon carbide on the high-purity silicon carbide insulating thin layer through CVD transverse deposition, namely the carbon-containing high-conductivity thin layer with the thickness of 0.3mm.
(4) Repeated preparation of high-purity silicon carbide insulating thin layers: adjusting the molar ratio of the carbon-silicon gas source, the reaction temperature and the reaction gas flow, adjusting the reaction temperature to 1150 ℃ at a cooling speed of 1 ℃/min, and gradually adjusting the molar ratio of the carbon-silicon gas source to 1.05 in the cooling process; the reaction gas flow was 300sccm and a high purity silicon carbide insulating film was continuously prepared by CVD on a carbon-containing highly conductive film to a thickness of 1.25mm.
Referring to fig. 2, a silicon carbide article having a sandwich structure of insulating-conducting-insulating thin layers was obtained by the preparation of the above steps.
(5) And removing the graphite matrix and the silicon carbide workpiece deposited on the surface of the graphite matrix from the CVD chamber, and placing the graphite matrix and the silicon carbide workpiece in a muffle furnace for uniform heating at 800 ℃ until the graphite matrix is completely oxidized and removed, and referring to FIG. 3, obtaining the silicon carbide ceramic with anisotropic resistivity, namely the silicon carbide sheet workpiece.
Examples 2 to 10
Examples 2-10 provide an anisotropic resistivity silicon carbide ceramic, respectively.
The preparation method of the above example was the same as that of example 1, except that the parameters of each step were as shown in table 1.
The above embodiments differ in particular in that:
examples 1-3 differ in the silicon-to-carbon source molar ratio in the preparation of the high purity silicon carbide insulating thin layers of step (2) and step (4).
Examples 1, 4-6 differ in the silicon-carbon source molar ratio in the preparation of the carbon-containing highly conductive thin layer of step (3).
Examples 1, 7-8 differ in the type of carbon source gas and the flow rate of the reaction gas in the preparation of the carbonaceous highly conductive thin layer in step (2). FIG. 4 is a graph of a sample of the anisotropic resistivity silicon carbide ceramic of example 7 after machining.
Examples 1, 9-10 differ in the type of silicon source gas, the type of carbon source gas, and the flow rate of the reaction gas in the preparation of the carbonaceous highly conductive thin layer in step (2).
Table 1 parameters of the steps in examples 1-10
Comparative example
Comparative examples 1 to 4
Comparative examples 1-4 each provide a silicon carbide ceramic of anisotropic resistivity.
The preparation method of the above comparative example was the same as that of example 1, except that the parameters of each step were as shown in table 2.
The above comparative examples differ in particular in that:
comparative examples 1-2 differ in the silicon-to-carbon source molar ratio in the preparation of the high purity silicon carbide insulating thin layers of step (2) and step (4).
Comparative examples 3-4 differ in the silicon-carbon source molar ratio in the preparation of the carbonaceous highly conductive thin layer of step (3).
Comparative example 5
Comparative example 5 provides an anisotropically resistivity silicon carbide ceramic.
The preparation method of the above comparative example is different from that of example 1 in that only one deposition process is included, as shown in table 2.
Table 2 parameters of each step in comparative examples 1 to 5
Comparative example 6
Comparative example 6 provides an anisotropically resistivity silicon carbide ceramic. Which is manufactured by sintering in the related art.
The preparation method of the silicon carbide ceramic specifically comprises the following steps:
(1) Weighing 2g of graphene powder and 0.2g of PVP powder to 100g of ethanol, and dispersing to obtain graphene dispersion liquid; weighing 96.4g of SiC powder and B 4 C powder 0.6g and C powder 1.0g are poured into a ball milling tank, and the ball milling is carried out for 4 hours after the graphene dispersion liquid with good ultrasonic dispersion is poured.
(2) And (3) drying the obtained slurry in a 70 ℃ oven, and sieving the dried powder with a 100-mesh sieve. Loading the obtained powder into a graphite mold, SPS sintering under a vacuum atmosphere, heating to 1700 ℃ at a heating rate of 100 ℃/min under the pressure of 40MPa, heating to 2000 ℃ at a heating rate of 50-100 ℃/min, preserving heat for 7min, cooling, and taking out to obtain the silicon carbide material with anisotropic resistivity.
Performance test
The silicon carbide ceramics prepared in the above examples and comparative examples were subjected to the following examination.
The detection method comprises the following steps:
1. the silicon carbide ceramics prepared in the above examples and comparative examples were sampled in a block shape, silver paste thin layers were applied to both side surfaces in the thickness direction, and the thickness direction resistance thereof was measured using a high-precision multimeter, and the material thickness direction resistivity was calculated from the thickness and the sectional area.
2. And (3) taking a block sample of the silicon carbide ceramic prepared in the embodiment and the comparative example, coating silver paste thin layers on the two radial side surfaces, measuring the radial resistance of the silicon carbide ceramic, and calculating the radial resistivity of the silicon carbide ceramic according to the length and the sectional area of the silicon carbide ceramic.
3. The densities of the silicon carbide ceramics prepared in the above examples and comparative examples were measured by archimedes' method.
4. The purity of the silicon carbide ceramics prepared in the above examples and comparative examples was tested by Glow Discharge Mass Spectrometry (GDMS).
The test results are shown in Table 3.
TABLE 3 detection results for examples 1-10 and comparative examples 1-6
As shown by the detection result, the silicon carbide ceramic prepared by the preparation method provided by the application can meet the functional requirement of anisotropic resistivity, and the high-quality preparation of the silicon carbide ceramic with high purity, high density and anisotropic resistivity is realized.
As is clear from the results of comparative examples 1 to 6 and comparative examples 1 to 4, the molar ratio of the carbon-silicon gas source during the deposition of the high purity silicon carbide insulating thin layer and the carbon-containing high conductivity thin layer in the present application affects the production result. As is evident from the results of comparative examples 1-2, when the molar amount of the silicon carbide gas source during the deposition of the high purity silicon carbide insulating thin layer is less than 0.8 or more than 2, severe oxidation of the product occurs in step (5). As shown by the detection result of the comparative example 3, when the carbon-silicon gas source mole is less than 2 in the deposition process of the carbon-containing high-conductivity thin layer, the prepared silicon carbide ceramic cannot meet the functional requirement of anisotropic resistivity. As shown by the detection result of comparative example 4, when the mole of the carbon-silicon gas source in the deposition process of the carbon-containing high-conductivity thin layer is more than 15, the prepared silicon carbide ceramic can meet the functional requirement of anisotropic resistivity, but the strength of the carbon-containing high-conductivity thin layer is unstable, so that the prepared silicon carbide ceramic is extremely easy to fracture in the thickness direction, and the qualification rate of a finished product is low. Based on the above, the application controls the molar ratio of the carbon-silicon gas source in the deposition process of the high-purity silicon carbide insulating thin layer to be in the range of 0.8-2, and controls the molar ratio of the carbon-silicon gas source in the deposition process of the carbon-containing high-conductivity thin layer to be in the range of 2-15.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims (10)
1. The silicon carbide ceramic with anisotropic resistivity is characterized by comprising a high-purity silicon carbide insulating thin layer and a carbon-containing high-conductivity thin layer which are sequentially overlapped; the top layer and the bottom layer of the silicon carbide ceramic are both the high-purity silicon carbide insulating thin layers;
in the high-purity silicon carbide insulating thin layer, the molar ratio of carbon to silicon is 0.8-2, and the thickness is 0.1-10mm;
in the carbon-containing high-conductivity thin layer, the carbon-silicon molar ratio is 2-15, and the thickness is 0.05-3mm.
2. The anisotropic resistivity silicon carbide ceramic as claimed in claim 1, wherein the number of the high purity silicon carbide insulating thin layers in the silicon carbide ceramic is n+1; the number of the carbon-containing high-conductivity thin layers is N; the N is 1-100;
preferably, the silicon carbide ceramic has a surface purity of 99.96-99.991% and a density of 3.2-3.21g/cm 3 The radial resistivity is 50-250 Ω & cm, and the axial resistivity is 900-6000 Ω & cm;
preferably, the silicon carbide ceramic has a resistivity anisotropy index as high as 101.993.
3. A method for preparing a silicon carbide ceramic having anisotropic resistivity according to any of claims 1-2, said method comprising the steps of:
sequentially depositing a high-purity silicon carbide insulating thin layer and a carbon-containing high-conductivity thin layer on a deposition matrix in turn by using high-purity silicon source gas and high-concentration carbon source gas through chemical vapor deposition, and removing the deposition matrix in an oxidation mode to prepare silicon carbide ceramic with anisotropic resistivity; the top layer and the bottom layer of the silicon carbide ceramic are both the high-purity silicon carbide insulating thin layers;
in the deposition process of the high-purity silicon carbide insulating thin layer, the molar ratio of a carbon-silicon gas source is 0.8-2; the reaction temperature is 1000-1350 ℃; the flow rate of the reaction gas is 200-1000sccm; the thickness is 0.1-10mm;
in the deposition process of the carbon-containing high-conductivity thin layer, the carbon-silicon gas source molar ratio is 2-15; the reaction temperature is 1000-1350 ℃; the flow rate of the reaction gas is 200-1000sccm; the thickness is 0.05-3mm.
4. A method for producing anisotropic resistivity silicon carbide ceramic according to claim 3, wherein the rate of temperature change is 1-2 ℃/min during the process of changing the deposition process of the high purity silicon carbide insulating thin layer to the deposition process of the carbonaceous high conductivity thin layer or during the process of changing the deposition process of the carbonaceous high conductivity thin layer to the deposition process of the high purity silicon carbide insulating thin layer, and the carbon-silicon gas source molar ratio, the reaction temperature and the reaction gas flow rate are uniformly adjusted to the set parameters during the temperature change.
5. The method for producing anisotropic resistivity silicon carbide ceramic as claimed in claim 3, wherein the high purity silicon source gas is high purity SiH 4 SiH of high purity 3 Cl, high purity SiH 2 Cl 2 High purity SiHCl 3 High purity SiCl 4 High purity SiCH 3 Cl 3 One or more of the following.
6. The method for producing anisotropic resistivity silicon carbide ceramic according to claim 3, wherein the high purity carbon source gas is high purity CH 4 High purity C 2 H 6 High purity C 3 H 8 High purity C 4 H 10 One or more of them.
7. The method for preparing anisotropic resistivity silicon carbide ceramic as claimed in claim 3, wherein the high purity H is obtained in the chemical vapor deposition process 2 The carrier gas is the carrier gas, and the flow rate of the carrier gas is 1-8slm; ar gas is used as diluent gas.
8. A method of preparing anisotropic resistivity silicon carbide ceramic according to claim 3, wherein the deposition matrix is a graphite matrix sheet; preferably, the thickness of the deposition matrix does not exceed 3mm.
9. A method for producing anisotropic resistivity silicon carbide ceramic according to claim 3,
oxidation removal of the graphite substrate sheet is achieved by utilizing muffle furnace heating;
preferably, the heating environment of the muffle furnace is an air atmosphere or a high-oxygen atmosphere;
preferably, the temperature in the muffle furnace is 750-900 ℃.
10. A silicon carbide flake-like article, characterized in that it is produced from the anisotropic resistivity silicon carbide ceramic of any one of claims 1-2.
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