CN113307644A - Method for nitriding modified reaction sintering silicon carbide ceramic surface - Google Patents
Method for nitriding modified reaction sintering silicon carbide ceramic surface Download PDFInfo
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- CN113307644A CN113307644A CN202110669667.0A CN202110669667A CN113307644A CN 113307644 A CN113307644 A CN 113307644A CN 202110669667 A CN202110669667 A CN 202110669667A CN 113307644 A CN113307644 A CN 113307644A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 131
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000005245 sintering Methods 0.000 title claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 47
- 238000005121 nitriding Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title description 4
- 238000002156 mixing Methods 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 16
- 239000006229 carbon black Substances 0.000 claims abstract description 16
- 239000004917 carbon fiber Substances 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 8
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 8
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 238000004381 surface treatment Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- 235000015895 biscuits Nutrition 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000000855 fermentation Methods 0.000 claims description 5
- 230000004151 fermentation Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 239000002985 plastic film Substances 0.000 claims description 5
- 229920006255 plastic film Polymers 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 15
- 239000010703 silicon Substances 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 10
- 229910017464 nitrogen compound Inorganic materials 0.000 abstract 1
- 150000002830 nitrogen compounds Chemical class 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
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Abstract
The invention relates to a surface nitriding modified reaction sintering silicon carbide ceramic and a preparation method thereof, wherein the reaction sintering silicon carbide ceramic comprises silicon carbide, carbon black, carbon fibers, a binder, a dispersant and deionized water; the binder is prepared by mixing carboxymethyl cellulose and PAF-II type powdery binder in any ratio; the dispersing agent is prepared by mixing polyethylene glycol and polyvinylpyrrolidone in any ratio. The preparation method comprises the steps of mixing, material standing, sintering and surface treatment. The invention introduces flowing nitrogen under certain pressure, so that the nitrogen reacts with free silicon to generate silicon and nitrogen compounds, thereby prolonging the service life and improving the corrosion resistance of the reaction sintered silicon carbide.
Description
Technical Field
The invention relates to a method for sintering a silicon carbide ceramic surface by a nitridation modification reaction, belonging to the technical field of silicon carbide modification.
Background
Silicon carbide has excellent properties such as high hardness, high-temperature strength, good oxidation resistance, good thermal stability, low coefficient of thermal expansion, high thermal conductivity, and good corrosion resistance, and thus can be used as a seal ring, a grinding medium, a grinding disc, an anti-spring plate, a nozzle, a magnetic pump piece, a roller rod in a kiln, and the like. The preparation of the silicon carbide ceramic comprises pressureless sintering, hot-pressing sintering, hot isostatic pressing sintering, spark plasma sintering, reaction sintering and the like, wherein the reaction sintering is used for preparing the silicon carbide ceramic, the sintering temperature is low, the size of a product is reduced, the compactness is high, the economic benefit is good, and the industrial cost is lower, but the reaction sintering needs to use molten silicon to infiltrate a silicon carbide ceramic biscuit containing carbon, so that the prepared ceramic product contains free silicon. Since the melting point of silicon is 1400 ℃, the presence of free silicon in the reaction-sintered silicon carbide shortens the service life of the reaction-sintered silicon carbide at high temperature and the corrosion resistance thereof is greatly reduced.
Patent document CN110304933A discloses PyC-SiCWThe pyrolytic carbon coating on the surface reacts with liquid silicon in P during the reaction sintering processyC-SiCWGenerating a SiC coating on the surface in situ, wherein the SiC coating is prepared by mixing SiCWIs isolated from the high-temperature liquid silicon, thereby avoiding the liquid silicon from being coupled with SiC at high temperatureWAnd (3) erosion damage. The SiC coating is formed on the surface of the ceramic to improve the erosion resistance of the ceramic; the invention aims to reduce the content of free silicon and improve the corrosion resistance of reaction sintered silicon carbide, namely reaction sinteringThe free silicon in the bonded silicon carbide ceramic reacts with nitrogen to form silicon nitride. There is currently little literature on the treatment of reaction-sintered silicon carbide surfaces, particularly where nitrogen is used to treat the surface of reaction-sintered silicon carbide ceramics.
Disclosure of Invention
The invention provides a reaction sintering silicon carbide ceramic with surface nitridation modification and a preparation method thereof, which are low in cost and easy to realize, aiming at the problem that reaction sintering silicon carbide is used as a kiln roller and has poor lithium battery corrosion resistance at high temperature. The technical scheme of the invention is as follows:
the surface nitriding modified reaction sintering silicon carbide ceramic comprises the following raw materials in parts by weight:
5-40 parts of silicon carbide, 2-7 parts of carbon black, 3-8 parts of carbon fiber, 2-6 parts of binder, 0.1-0.4 part of dispersant and 10-40 parts of deionized water;
the binder is prepared by mixing carboxymethyl cellulose and PAF-II type powdery binder in any ratio; the dispersing agent is prepared by mixing polyethylene glycol and polyvinylpyrrolidone in any ratio.
Preferably, the silicon carbide is selected from the group consisting of silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, and silicon carbide of F1200.
Preferably, the weight ratio of the silicon carbide of F90, the silicon carbide of F120, the silicon carbide of F180 and the silicon carbide of F1200 is 1:2:1: 2; mixing the carboxymethyl cellulose and the PAF-II type powdery binder in a weight ratio of 1: 1; mixing the polyethylene glycol and the polyvinylpyrrolidone in a weight ratio of 2: 1; the particle diameters of the carbon black and the carbon fiber are respectively 0.5-1 μm and 7-8 μm.
The preparation method of the surface nitriding modified reaction sintering silicon carbide ceramic comprises the following steps:
(1) mixing material
Taking deionized water, fully dissolving a dispersing agent and a binder, weighing silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, silicon carbide of F1200, carbon black and carbon fiber, mixing materials for 8-20 hours by using a roller mixer at normal temperature, and uniformly mixing the components to obtain a mixture A;
(2) material for fermentation
Placing the mixture A prepared in the step (1) into a plastic film, standing for 10-24 hours at normal temperature, and placing the mixture A into an extruder to extrude a needed ceramic blank;
(3) sintering
Placing the ceramic biscuit prepared in the step (2) in a vacuum reaction sintering furnace, and sintering at the temperature of 1500-1850 ℃ for 5-12h to prepare silicon carbide ceramic;
(4) surface treatment
Placing the reaction sintering silicon carbide in a high-temperature furnace, heating and introducing flowing high-purity nitrogen gas simultaneously to generate reaction sintering silicon carbide ceramic with surface nitriding modification; the nitrogen reacts with free silicon on the surface of the reaction sintering silicon carbide at high temperature to generate a compound of nitrogen and silicon, so that the lithium-ion corrosion resistance of the reaction sintering silicon carbide is improved.
Further, in the step (4), the reaction sintered silicon carbide is placed in a high-temperature furnace with the flow rate of 15-25m3Flowing high-purity nitrogen is introduced into the high-temperature furnace, the heating temperature is 1250-.
Compared with the prior art, the invention has the following advantages:
according to the invention, the reaction-sintered silicon carbide ceramic is prepared by taking a composite binder, a composite dispersant, a composite carbon source, silicon carbide with different particle sizes and deionized water as raw materials, and carrying out material mixing, material standing, sintering and surface treatment. The prepared reaction sintering ceramic is put into a high-temperature furnace, flowing nitrogen is introduced under certain pressure, and the nitrogen and free silicon react to generate a compound of nitrogen and silicon at certain heat treatment temperature and time, so that the service life and the corrosion resistance of the reaction sintering silicon carbide are improved.
Drawings
FIG. 1 is an XPS plot of reactive sintered silicon carbide nitrided at 1350 ℃;
FIG. 2 is a corrosion picture of a battery material, wherein 2A is a corrosion picture of an untreated silicon carbide sintered lithium battery material; and 2B is a corrosion picture of the silicon carbide sintered lithium battery material subjected to nitriding treatment.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1: surface nitriding modified reaction sintering silicon carbide ceramic and preparation method thereof
The surface nitriding modified reaction sintering silicon carbide ceramic comprises the following raw materials in parts by weight:
30 parts of silicon carbide, 5 parts of carbon black, 5 parts of carbon fiber, 4 parts of binder, 0.3 part of dispersant and 20 parts of deionized water;
the silicon carbide is selected from a mixture of silicon carbide of F90, silicon carbide of F120, silicon carbide of F180 and silicon carbide of F1200, and the weight ratio of the silicon carbide to the silicon carbide is 1:2:1: 2; the adhesive is prepared by mixing carboxymethyl cellulose and PAF-II type powdery adhesive in a weight ratio of 1: 1; the dispersing agent is formed by mixing polyethylene glycol and polyvinylpyrrolidone in a weight ratio of 2: 1; the particle diameters of the carbon black and the carbon fiber are 0.7 μm and 7 μm, respectively.
The preparation method of the surface nitriding modified reaction sintering silicon carbide ceramic comprises the following steps:
(1) mixing material
Taking deionized water, fully dissolving a dispersing agent and a binder, weighing silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, silicon carbide of F1200, carbon black and carbon fiber, mixing materials for 10 hours by using a roller mixer at normal temperature, and uniformly mixing the components to obtain a mixture A;
(2) material for fermentation
Placing the mixture A prepared in the step (1) into a plastic film for standing for 18 hours at normal temperature, and placing the standing mixture A into an extruder to extrude a needed ceramic blank;
(3) sintering
Placing the ceramic biscuit prepared in the step (2) in a vacuum reaction sintering furnace, and sintering for 10 hours at 1600 ℃ to prepare silicon carbide ceramic;
(4) surface treatment
Placing the reaction sintered silicon carbide into a high-temperature furnace at a flow rate of 15m3And/h, introducing flowing high-purity nitrogen into the high-temperature furnace, heating the high-temperature furnace to 1250 ℃, and keeping the temperature for 8h to obtain the surface nitriding modified reaction-sintered silicon carbide ceramic.
The surface nitridation modified reaction sintered silicon carbide ceramic obtained in the example was tested to have a flexural strength of 317MPa and a fracture toughness of 3MPa m1/2。
Example 2: surface nitriding modified reaction sintering silicon carbide ceramic and preparation method thereof
The surface nitriding modified reaction sintering silicon carbide ceramic comprises the following raw materials in parts by weight:
15 parts of silicon carbide, 4 parts of carbon black, 6 parts of carbon fiber, 4 parts of binder, 0.2 part of dispersant and 15 parts of deionized water;
the silicon carbide is selected from a mixture of silicon carbide of F90, silicon carbide of F120, silicon carbide of F180 and silicon carbide of F1200, and the weight ratio of the silicon carbide to the silicon carbide is 1:2:1: 2; the adhesive is prepared by mixing carboxymethyl cellulose and PAF-II type powdery adhesive in a weight ratio of 2: 1; the dispersing agent is formed by mixing polyethylene glycol and polyvinylpyrrolidone in a weight ratio of 2: 1; the particle diameters of the carbon black and the carbon fiber are 0.6 μm and 8 μm, respectively.
The preparation method of the surface nitriding modified reaction sintering silicon carbide ceramic comprises the following steps:
(1) mixing material
Taking deionized water, fully dissolving a dispersing agent and a binder, weighing silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, silicon carbide of F1200, carbon black and carbon fiber, mixing materials for 15 hours by using a roller mixer at normal temperature, and uniformly mixing the components to obtain a mixture A;
(2) material for fermentation
Placing the mixture A prepared in the step (1) into a plastic film for standing for 15 hours at normal temperature, and placing the standing mixture A into an extruder to extrude a needed ceramic blank;
(3) sintering
Placing the ceramic biscuit prepared in the step (2) in a vacuum reaction sintering furnace, and sintering for 7 hours at 1750 ℃ to prepare silicon carbide ceramic;
(4) surface treatment
Placing the reaction sintered silicon carbide into a high-temperature furnace at a flow rate of 20m3And/h, introducing high-purity flowing nitrogen into the high-temperature furnace, heating at 1300 ℃, and keeping the temperature for 6h to obtain the surface nitriding modified reaction-sintered silicon carbide ceramic.
The test shows that the bending strength of the reaction sintering silicon carbide ceramic with the surface modified by nitridation obtained in the embodiment is 379MPa, and the fracture toughness is 3.24 MPa.m1/2。
Example 3: surface nitriding modified reaction sintering silicon carbide ceramic and preparation method thereof
The surface nitriding modified reaction sintering silicon carbide ceramic comprises the following raw materials in parts by weight:
35 parts of silicon carbide, 7 parts of carbon black, 7 parts of carbon fiber, 5 parts of binder, 0.4 part of dispersant and 40 parts of deionized water;
the adhesive is prepared by mixing carboxymethyl cellulose and PAF-II type powdery adhesive in a weight ratio of 1: 1; the dispersing agent is prepared by mixing polyethylene glycol and polyvinylpyrrolidone in a weight ratio of 1: 1; the silicon carbide is F90 silicon carbide, F120 silicon carbide, F180 silicon carbide and F1200 silicon carbide which are mixed in a weight ratio of 1:1:1: 1; the particle diameters of the carbon black and the carbon fiber are 0.5 μm and 7 μm, respectively.
The preparation method of the surface nitriding modified reaction sintering silicon carbide ceramic comprises the following steps:
(1) mixing material
Taking deionized water, fully dissolving a dispersing agent and a binder, weighing silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, silicon carbide of F1200, carbon black and carbon fiber, mixing for 18 hours by using a roller mixer at normal temperature, and uniformly mixing the components to obtain a mixture A;
(2) material for fermentation
Placing the mixture A prepared in the step (1) into a plastic film for standing for 20 hours at normal temperature, and placing the standing mixture A into an extruder to extrude a needed ceramic blank;
(3) sintering
Placing the ceramic biscuit prepared in the step (2) in a vacuum reaction sintering furnace, and sintering at 1800 ℃ for 5-12h to prepare silicon carbide ceramic;
(4) surface treatment
The reaction-sintered silicon carbide was placed in a high-temperature furnace at a flow rate of 23m3Flowing high-purity nitrogen is introduced into the high-temperature furnace, the heating temperature is 1350 ℃, the heat preservation time is 4h, the bending strength of the modified reaction sintering silicon carbide ceramic is 425MPa, and the fracture toughness is 3.76 MPa.m1/2。
Claims (8)
1. The surface nitriding modified reaction sintering silicon carbide ceramic is characterized by comprising the following raw materials in parts by weight:
5-40 parts of silicon carbide, 2-7 parts of carbon black, 3-8 parts of carbon fiber, 2-6 parts of binder, 0.1-0.4 part of dispersant and 10-40 parts of deionized water;
the binder is prepared by mixing carboxymethyl cellulose and PAF-II type powdery binder in any ratio; the dispersing agent is prepared by mixing polyethylene glycol and polyvinylpyrrolidone in any ratio.
2. The reaction sintered silicon carbide ceramic of claim 1, wherein the silicon carbide is selected from the group consisting of a mixture of silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, and silicon carbide of F1200.
3. The reaction-sintered silicon carbide ceramic of claim 2, wherein the weight ratio of the silicon carbide of F90, the silicon carbide of F120, the silicon carbide of F180, and the silicon carbide of F1200 is 1:2:1: 2.
4. The reaction sintered silicon carbide ceramic of claim 1, wherein the carboxymethyl cellulose and the PAF-ii type powdered binder are mixed in a weight ratio of 1: 1.
5. The reaction sintered silicon carbide ceramic of claim 1, wherein the polyethylene glycol and polyvinylpyrrolidone are mixed in a weight ratio of 2: 1.
6. The reaction-sintered silicon carbide ceramic according to claim 1, wherein the carbon black and the carbon fiber have particle diameters of 0.5 to 1 μm and 7 to 8 μm, respectively.
7. The method for producing reaction-sintered silicon carbide ceramic according to any one of claims 1 to 6, comprising the steps of:
(1) mixing material
Taking deionized water, fully dissolving a dispersing agent and a binder, weighing silicon carbide of F90, silicon carbide of F120, silicon carbide of F180, silicon carbide of F1200, carbon black and carbon fiber, mixing materials for 8-20 hours by using a roller mixer at normal temperature, and uniformly mixing the components to obtain a mixture A;
(2) material for fermentation
Placing the mixture A prepared in the step (1) into a plastic film, standing for 10-24 hours at normal temperature, and placing the mixture A into an extruder to extrude a needed ceramic blank;
(3) sintering
Placing the ceramic biscuit prepared in the step (2) in a vacuum reaction sintering furnace, and sintering at the temperature of 1500-1850 ℃ for 5-12h to prepare silicon carbide ceramic;
(4) surface treatment
And placing the reaction sintering silicon carbide into a high-temperature furnace, heating and introducing flowing high-purity nitrogen gas simultaneously, thereby generating the reaction sintering silicon carbide ceramic with the surface subjected to nitridation modification.
8. The production method according to claim 7, wherein in the step (4), the reaction-sintered silicon carbide is placed in a high-temperature furnace at a flow rate of 15 to 25m3Flowing high-purity nitrogen is introduced into the high-temperature furnace, the heating temperature is 1250-.
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