CN112279648A - Pressureless sintering high-toughness silicon carbide and preparation method thereof - Google Patents
Pressureless sintering high-toughness silicon carbide and preparation method thereof Download PDFInfo
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- CN112279648A CN112279648A CN202011131754.2A CN202011131754A CN112279648A CN 112279648 A CN112279648 A CN 112279648A CN 202011131754 A CN202011131754 A CN 202011131754A CN 112279648 A CN112279648 A CN 112279648A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 92
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000001272 pressureless sintering Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 38
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000005011 phenolic resin Substances 0.000 claims abstract description 35
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 26
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- 230000001050 lubricating effect Effects 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 19
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/565—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 based on silicon carbide
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/668—Pressureless sintering
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Abstract
The invention discloses pressureless sintering high-toughness silicon carbide, which comprises the following raw materials in parts by weight: 96-98 parts of silicon carbide, 0.8-1.2 parts of boron carbide, 1-3 parts of graphene, 0.6-0.8 part of dispersant, 4-6 parts of binder, 5-7 parts of phenolic resin, 0.8-1.2 parts of lubricating liquid and 90-110 parts of deionized water. The invention has the beneficial effects that: in the preparation process of the pressureless sintering high-toughness silicon carbide, the graphene is added into the silicon carbide, so that the fracture toughness of a sealing ring of the prepared silicon carbide material is about 20 percent higher than that of the common pressureless sintering silicon carbide; the preparation method of pressureless sintering high-toughness silicon carbide is simple and easy to operate.
Description
Technical Field
The invention relates to the technical field of materials, in particular to pressureless sintering high-toughness silicon carbide and a preparation method thereof.
Background
With the increasingly strict requirements on materials in the fields of development of science and technology, sealing, armor industry and the like, the development of a novel high-performance material is urgently needed. The silicon carbide ceramic has excellent high-temperature strength, wear resistance and corrosion resistance, and good electric conductivity and thermal conductivity, so that the silicon carbide ceramic is widely applied to various industries such as aerospace, machinery, automobiles and the like, and is also an important material in the military field.
The sealing material commonly adopted at present is made of single silicon carbide, but the prepared silicon carbide has larger brittleness and lower fracture toughness, the breaking strength of the silicon carbide ceramic sintered under normal pressure is generally about 400MPa, the silicon carbide ceramic is very easy to jump during the processing, the wear resistance is not high, the service life is short, and the requirements of the fields of sealing, armor industry and the like on the high-toughness and high-strength silicon carbide ceramic are difficult to meet.
Disclosure of Invention
The invention aims to provide a preparation method of silicon carbide with high toughness.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides pressureless sintering high-toughness silicon carbide, which comprises the following raw materials in parts by weight: 96-98 parts of silicon carbide, 0.8-1.2 parts of boron carbide, 1-3 parts of graphene, 0.6-0.8 part of dispersant, 4-6 parts of binder, 5-7 parts of phenolic resin, 0.8-1.2 parts of lubricating liquid and 90-110 parts of deionized water.
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight as a preferred embodiment: 96-97 parts of silicon carbide, 0.9-1.1 parts of boron carbide, 1.5-2.5 parts of graphene, 0.6-0.7 part of dispersant, 4.5-5.5 parts of binder, 5.5-6.5 parts of phenolic resin, 0.9-1.1 parts of lubricating liquid and 98-102 parts of deionized water.
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight as a preferred embodiment: 97 parts of silicon carbide, 1.0 part of boron carbide, 2 parts of graphene, 0.7 part of dispersing agent, 5 parts of binder, 6 parts of phenolic resin, 1.0 part of lubricating liquid and 100 parts of deionized water.
The pressureless sintered high-toughness silicon carbide is characterized in that the dispersant is produktkkv 5088 as a preferred embodiment.
The pressureless sintering high-toughness silicon carbide is prepared by adopting a preferable embodiment that the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf35
The pressureless sintered high-toughness silicon carbide is preferably prepared by using a phenolic resin 8022 as the phenolic resin.
The phenolic resin 8022 is prepared from the following raw materials in parts by weight: 70-74 parts of phenolic resin, 3.5-4.5 parts of phenol, 0.1-0.9 part of formaldehyde and 20-25 parts of water.
The pressureless sintered high-toughness silicon carbide is preferably prepared by using glycerol as the lubricating fluid.
The second aspect of the invention provides a preparation method of pressureless sintering high-toughness silicon carbide, which comprises the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill for grinding, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, and uniformly mixing and stirring to obtain a mixed material;
(2) and sequentially sieving, granulating, pressing and sintering the mixed material to obtain the pressureless sintering high-toughness silicon carbide.
In the pressureless sintering preparation method of high-toughness silicon carbide, as a preferred embodiment, in the step (1), the grinding time is 1.5-2.5 h; the mixing and stirring time is 5-7 h.
In the above method for preparing pressureless sintering high-toughness silicon carbide, as a preferred embodiment, in the step (2), the mesh number of the screen used for the screening treatment is 300-400 meshes.
Compared with the prior art, the invention has the beneficial effects that:
in the preparation process of the pressureless sintering high-toughness silicon carbide, the graphene is added into the silicon carbide, so that the fracture toughness of a sealing ring of the prepared silicon carbide material is about 20 percent higher than that of the common pressureless sintering silicon carbide;
the preparation method of pressureless sintering high-toughness silicon carbide is simple and easy to operate.
Detailed Description
In order to better understand the essence of the present invention, the following detailed description is made with reference to the examples, which are not intended to limit the present invention, but are merely illustrative, and modifications, substitutions or improvements can be made without departing from the spirit and principle of the present invention.
In the present example, 1 part by weight means 1 kg.
Example 1
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight: 96 parts of silicon carbide, 0.8 part of boron carbide, 1 part of graphene, 0.6 part of dispersing agent, 4 parts of binder, 5 parts of phenolic resin, 0.8 part of lubricating liquid and 90 parts of deionized water;
the dispersant is produktkkv 5088;
the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf 35;
the phenolic resin is phenolic resin 8022;
the lubricating liquid is glycerol;
the preparation method of the pressureless sintering high-toughness silicon carbide in the embodiment 1 comprises the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill, grinding for 1.5h, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, mixing and stirring for 5h, and uniformly stirring to obtain a mixed material;
(2) and sieving the mixed material by a screen with the mesh number of 300, granulating, pressing and sintering the mixed material in sequence to obtain the pressureless sintering high-toughness silicon carbide.
Example 2
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight: 96 parts of silicon carbide, 0.9 part of boron carbide, 1.5 parts of graphene, 0.6 part of dispersing agent, 4.5 parts of binder, 5.5 parts of phenolic resin, 0.9 part of lubricating liquid and 98 parts of deionized water;
the dispersant is produktkkv 5088;
the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf 35;
the phenolic resin is phenolic resin 8022;
the lubricating liquid is glycerol.
The preparation method of pressureless sintering high-toughness silicon carbide described in embodiment 2 comprises the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill, grinding for 1.8h, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, mixing and stirring for 5.5h, and uniformly stirring to obtain a mixed material;
(2) and sieving the mixed material by a screen with the mesh number of 320 meshes, granulating, pressing and sintering the mixed material in sequence to obtain the pressureless sintering high-toughness silicon carbide.
Example 3
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight: 97 parts of silicon carbide, 1.0 part of boron carbide, 2 parts of graphene, 0.7 part of dispersing agent, 5 parts of binder, 6 parts of phenolic resin, 1.0 part of lubricating liquid and 100 parts of deionized water;
the dispersant is produktkkv 5088;
the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf 35;
the phenolic resin is phenolic resin 8022;
the lubricating liquid is glycerol;
the pressureless sintering method for preparing high toughness silicon carbide as described in example 3 includes the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill, grinding for 2h, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, mixing and stirring for 6h, and uniformly stirring to obtain a mixed material;
(2) and sieving the mixed material by a sieve with 350 meshes, granulating, pressing and sintering the mixed material in sequence to obtain the pressureless sintering high-toughness silicon carbide.
Example 4
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight: 97 parts of silicon carbide, 1.1 parts of boron carbide, 2.5 parts of graphene, 0.7 part of dispersing agent, 5.5 parts of binder, 6.5 parts of phenolic resin, 1.1 parts of lubricating liquid and 102 parts of deionized water;
the dispersant is produktkkv 5088;
the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf 35;
the phenolic resin is phenolic resin 8022;
the lubricating liquid is glycerol.
The preparation method of pressureless sintering high-toughness silicon carbide described in embodiment 4 includes the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill, grinding for 2.2h, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, mixing and stirring for 6.5h, and uniformly stirring to obtain a mixed material;
(2) and sieving the mixed material by a screen with the mesh number of 380, granulating, pressing and sintering the mixed material in sequence to obtain the pressureless sintering high-toughness silicon carbide.
Example 5
The pressureless sintering high-toughness silicon carbide comprises the following raw materials in parts by weight: 98 parts of silicon carbide, 1.2 parts of boron carbide, 3 parts of graphene, 0.8 part of dispersing agent, 6 parts of binder, 7 parts of phenolic resin, 1.2 parts of lubricating liquid and 110 parts of deionized water;
the dispersant is produktkkv 5088;
the binder is a mixture of a binder zusoplast 9002 and a binder optipix paf 35;
the phenolic resin is phenolic resin 8022;
the lubricating liquid is glycerol;
the preparation method of the pressureless sintering high-toughness silicon carbide, disclosed by the embodiment 5, comprises the following steps of:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill, grinding for 2.5h, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, mixing and stirring for 7h, and uniformly stirring to obtain a mixed material;
(2) and sieving the mixed material by a sieve with 400 meshes, granulating, pressing and sintering the mixed material in sequence to obtain the pressureless sintering high-toughness silicon carbide.
Comparative example 1
The pressureless sintered high toughness silicon carbide of comparative example 1 differs from the pressureless sintered high toughness silicon carbide of example 3 in that: the pressureless sintered high toughness silicon carbide described in comparative example 1 contains 0.6 parts by weight of graphene.
Comparative example 2
The pressureless sintered high toughness silicon carbide of comparative example 2 differs from the pressureless sintered high toughness silicon carbide of example 3 in that: the pressureless sintered high-toughness silicon carbide as described in comparative example 2 contains 3.8 parts by weight of graphene.
The invention relates to a performance research of pressureless sintering high-toughness silicon carbide
The fracture toughness of pressureless sintered high-toughness silicon carbide according to examples 1 to 5 and comparative examples 1 to 2 of the present invention was measured by a grooving method, and the results are shown in table 1:
TABLE 1 fracture toughness of pressureless sintered high toughness SiC
As can be seen from Table 1, the fracture toughness of the pressureless sintered high-toughness silicon carbide of the present invention is significantly higher than that of the pressureless sintered high-toughness silicon carbide of comparative examples 1 and 2 by more than 20%.
The pressureless sintering high-toughness silicon carbide of the comparative example 1 has low density and poor toughness of a finished product because the content of graphene is lower than that of the pressureless sintering high-toughness silicon carbide graphene; while the content of graphene in the pressureless sintered high-toughness silicon carbide described in comparative example 2 is too high, the final product has over-sintered crystal grains growing to reduce the performance of the product.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The pressureless sintering high-toughness silicon carbide is characterized by comprising the following raw materials in parts by weight: 96-98 parts of silicon carbide, 0.8-1.2 parts of boron carbide, 1-3 parts of graphene, 0.6-0.8 part of dispersant, 4-6 parts of binder, 5-7 parts of phenolic resin, 0.8-1.2 parts of lubricating liquid and 90-110 parts of deionized water.
2. The pressureless sintered high-toughness silicon carbide according to claim 1, comprising the following raw materials in parts by weight: 96-97 parts of silicon carbide, 0.9-1.1 parts of boron carbide, 1.5-2.5 parts of graphene, 0.6-0.7 part of dispersant, 4.5-5.5 parts of binder, 5.5-6.5 parts of phenolic resin, 0.9-1.1 parts of lubricating liquid and 98-102 parts of deionized water.
3. The pressureless sintered high-toughness silicon carbide according to claim 1, comprising the following raw materials in parts by weight: 97 parts of silicon carbide, 1.0 part of boron carbide, 2 parts of graphene, 0.7 part of dispersing agent, 5 parts of binder, 6 parts of phenolic resin, 1.0 part of lubricating liquid and 100 parts of deionized water.
4. The pressureless sintered high toughness silicon carbide of claim 1 wherein the dispersant is produktkkv 5088.
5. The pressureless sintered high toughness silicon carbide of claim 1, wherein the binder is a mixture of zusoplast 9002 and optipix paf 35.
6. The pressureless sintered high toughness silicon carbide of claim 1, wherein the phenolic resin is phenolic resin 8022.
7. The pressureless sintered high toughness silicon carbide of claim 1, wherein the lubricating fluid is glycerol.
8. A method for pressureless sintering of high toughness silicon carbide according to any of claims 1 to 7, characterized by the following steps:
(1) adding silicon carbide, boron carbide, a dispersing agent and deionized water into a ball mill for grinding, adding a binder, phenolic resin, a lubricating liquid and graphene into the ball mill after grinding is finished, and uniformly mixing and stirring to obtain a mixed material;
(2) and sequentially sieving, granulating, pressing and sintering the mixed material to obtain the pressureless sintering high-toughness silicon carbide.
9. The method for preparing pressureless sintered high-toughness silicon carbide according to claim 8, wherein in the step (1), the grinding time is 1.5-2.5 h; the mixing and stirring time is 5-7 h.
10. The method for preparing pressureless sintered high-toughness silicon carbide as claimed in claim 8, wherein in the step (2), the mesh number of the screen used for the screening treatment is 300-400 meshes.
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CN116003135A (en) * | 2022-12-26 | 2023-04-25 | 何思义 | Preparation method of reaction sintering silicon carbide ceramic granulating powder |
CN116789454A (en) * | 2023-07-04 | 2023-09-22 | 北京亦盛精密半导体有限公司 | Silicon carbide ceramic and preparation method thereof |
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