CN117819977B - Silicon carbide composite ceramic material and preparation method and application thereof - Google Patents
Silicon carbide composite ceramic material and preparation method and application thereof Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 100
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 75
- 238000002156 mixing Methods 0.000 claims abstract description 48
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 37
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000835 fiber Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 29
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 18
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 18
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 16
- -1 yttrium oxide modified silicon carbide Chemical class 0.000 claims abstract description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 55
- 238000010438 heat treatment Methods 0.000 claims description 39
- 238000001354 calcination Methods 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000010304 firing Methods 0.000 abstract description 6
- 238000009987 spinning Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 238000007590 electrostatic spraying Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 230000002572 peristaltic effect Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 235000015895 biscuits Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 241000531116 Blitum bonus-henricus Species 0.000 description 1
- 235000008645 Chenopodium bonus henricus Nutrition 0.000 description 1
- 101100371219 Pseudomonas putida (strain DOT-T1E) ttgE gene Proteins 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical class [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a silicon carbide composite ceramic material and a preparation method and application thereof, wherein silicon carbide particles and yttrium chloride solution are mixed and treated and calcined to obtain nano yttrium oxide modified silicon carbide, then the nano yttrium oxide modified silicon carbide is mixed with barium nitrate solution, ammonium oxalate solution is added for precipitation reaction, and the mixture is calcined again to obtain pretreated silicon carbide particles; then ball-milling and mixing the pretreated silicon carbide particles with basic magnesium carbonate, boric acid, cobalt nitrate and zirconia fibers to obtain a mixture; and finally, pressing the mixture into a blank, and sintering to obtain the finished product. The preparation method is simple, the firing temperature is low, the toughness of the obtained composite ceramic material is good, the composite ceramic material can be used for manufacturing aerospace structural parts and the like, and the application prospect is good.
Description
Technical Field
The invention belongs to the technical field of ceramic material preparation, and particularly relates to a silicon carbide composite ceramic material, and a preparation method and application thereof.
Background
The silicon carbide ceramic material has wide application in the industrial fields of petroleum, chemical industry, microelectronics, machinery, automobiles, aerospace, papermaking, laser, steel, nuclear energy, processing and the like, and has the advantages of low density, high strength, high temperature resistance, good thermal stability, small thermal expansion coefficient, oxidation resistance, corrosion resistance, radiation resistance and the like.
Silicon carbide is a covalent bond compound, however, and the diffusion rate of carbon and silicon atoms during sintering is very low, making it difficult to sinter by sintering means commonly used for ionomer materials. At present, silicon carbide ceramic materials are usually sintered by methods such as pressureless sintering, hot isostatic pressing sintering, reactive sintering and the like, wherein the hot isostatic pressing sintering can only prepare silicon carbide ceramic materials with simple shapes, the hot isostatic pressing sintering can obtain silicon carbide ceramic materials with complex shapes, but the biscuit is required to be encapsulated, so that the industrial production is difficult to realize. Although pressureless sintering and reactive sintering can prepare silicon carbide ceramic materials with complex shapes, the high-temperature performance of the obtained ceramic materials is poor. Pure silicon carbide powder can be densified by hot pressing, but requires sintering temperature exceeding 2000 ℃, and has high energy consumption and high cost.
In addition, the toughness of the pure silicon carbide ceramic material is poor, the conventional deformation processing can not be performed, the mechanical processing is quite difficult, and the diversified processing of ceramic products is affected.
Thus, lowering firing temperature and improving toughness are short plates of technology that limit the development of current silicon carbide ceramic materials.
Patent CN102030534B discloses a preparation method of silicon carbide ceramic, which comprises the following specific steps: firstly, forming a main material by a mixture of silicon carbide, lanthanum oxide and silicon dioxide, and performing ball milling and mixing on the main material, a dispersing agent, a binder and deionized water to prepare water-based silicon carbide slurry; spray granulating the water-based silicon carbide slurry to obtain silicon carbide powder particles; dry-pressing the silicon carbide powder particles for one-step molding to obtain a high-density silicon carbide blank; and (3) putting the silicon carbide green body into a vacuum high-temperature sintering furnace for sintering at 1750-1800 ℃ for 0.5-2 hours to obtain the silicon carbide ceramic. The firing temperature of the preparation method is reduced, but the firing temperature is still higher, and the bending strength of the obtained silicon carbide ceramic is lower.
The patent CN104030686B discloses a high-toughness silicon carbide ceramic and a preparation method thereof, firstly, silicon carbide, a toughening agent titanium carbide, sintering auxiliary carbon and boron carbide are uniformly mixed, then, uniformly mixed powder is put into a ball mill, water-soluble resin and distilled water are added for ball milling, the well-ball-milled powder is dried by a steam drying box, the powder is added into a steel mould after being dried, a biscuit is obtained by compression molding, the sintering is carried out in a vacuum furnace, the sintering temperature is 2100-2200 ℃, the heat preservation time is 1-3 hours, and the sintered biscuit is subjected to surface grinding processing to obtain a final product. The preparation method of the patent technology still needs very high sintering temperature, high energy consumption and high production cost.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a silicon carbide composite ceramic material, a preparation method and application thereof, reduce the firing temperature and improve the toughness of products.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
1. The preparation method of the silicon carbide composite ceramic material comprises the following specific steps:
(1) Firstly mixing silicon carbide particles with yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, then mixing the nano yttrium oxide modified silicon carbide with barium nitrate solution, adding ammonium oxalate solution, carrying out precipitation reaction, and calcining again to obtain pretreated silicon carbide particles;
(2) Then ball-milling and mixing the pretreated silicon carbide particles with basic magnesium carbonate, boric acid, cobalt nitrate and zirconia fibers to obtain a mixture;
(3) And finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material.
Preferably, in the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 100-200 nm and beta-silicon carbide with the particle size of 30-50 nm according to the mass ratio of 10:1, and mixing.
Preferably, in the step (1), the mass ratio of the silicon carbide particles to the yttrium chloride solution is 4-5: 1, yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol 10-12 times of the yttrium chloride; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: and (3) uniformly stirring and mixing the silicon carbide particles and the yttrium chloride solution, standing for 15-20 minutes, and recovering ethanol under reduced pressure to obtain premixed powder.
Preferably, in the step (1), the process conditions of calcination are: calcining at 750-850 deg.c for 1.5-2.5 hr.
Preferably, in the step (1), adding an ammonium oxalate solution under the stirring condition of 300-500 r/min, standing for 5-7 min, centrifuging for 8-10 min at 5000-7000 r/min, and taking out precipitates to obtain the pretreated silicon carbide particles; the mass ratio of the nanometer yttrium oxide modified silicon carbide to the barium nitrate solution to the ammonium oxalate solution is 4-5: 8-10: 2 to 3, the mass concentration of the barium nitrate solution is 0.02 to 0.04 percent, and the mass concentration of the ammonium oxalate solution is 3 to 4 percent.
Preferably, in the step (1), the process conditions of the re-calcination are as follows: calcining at 600-650 deg.c for 50-60 min.
Preferably, in the step (2), the mass ratio of the pretreated silicon carbide particles to the basic magnesium carbonate, cobalt nitrate and zirconia fibers is 4: 2-3: 0.3 to 0.4: 1-2, the basic magnesium carbonate and boric acid in equimolar quantity.
Preferably, in the step (2), the zirconia fiber is obtained by the following preparation method: firstly stirring zirconium oxychloride and dispersing in deionized water with the weight being 2 times that of the zirconium oxychloride, then adding glacial acetic acid, stirring and heating to 50-60 ℃, adding basic zirconium carbonate while stirring, adding yttrium nitrate, stirring and mixing uniformly, removing excessive water by reduced pressure distillation, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 3-5 mu m; wherein, the mol ratio of zirconium oxychloride, glacial acetic acid, zirconium basic carbonate and yttrium nitrate is 0.6-0.7: 0.3:1: and 0.15, dividing the basic zirconium carbonate into three parts, and feeding in batches.
More preferably, the mixture is concentrated to a viscosity of 2 to 3 mPas to obtain a concentrated solution; the specific method of electrostatic spraying comprises the following steps: injecting the concentrated solution into a spinning cylinder at a constant speed through a peristaltic pump, wherein the diameter of a spinning hole is 0.8mm, the electrostatic pressure is 4000-5000 kW, the feeding rate is 0.2-0.3 mL/min, the temperature of hot air is 70-80 ℃, and the humidity is less than or equal to 50%.
Further preferably, the process conditions of the heat treatment are: heating to 600-700 ℃ at 2-3 ℃/min, preserving heat for 70-80 minutes, heating to 1300-1350 ℃ at 15-17 ℃/min, preserving heat for 60-70 minutes, and naturally cooling to room temperature.
Preferably, in the step (2), the ball milling process conditions are as follows: ball milling is carried out for 6 to 7 hours at the speed of 300 to 400 r/min.
Preferably, in the step (3), the mixture is pressed into a blank by cold isostatic pressing, and the specific process conditions are as follows: the pressure is 200-220 MPa, and the time is 10-12 minutes.
Preferably, in the step (3), the sintering process conditions are as follows: heating to 1000-1100 ℃ at 10-15 ℃/min, preserving heat for 40-50 min, heating to 1500-1550 ℃ at 5-7 ℃/min, preserving heat for 150-200 min, and cooling to room temperature (25 ℃) along with a furnace.
2. A silicon carbide composite ceramic material is obtained by the preparation method.
3. The silicon carbide composite ceramic material is applied to manufacturing of aerospace structural members.
Compared with the prior art, the invention has the following beneficial effects:
Firstly mixing silicon carbide particles with yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, then mixing the nano yttrium oxide modified silicon carbide with barium nitrate solution, adding ammonium oxalate solution, carrying out precipitation reaction, and calcining again to obtain pretreated silicon carbide particles; then ball-milling and mixing the pretreated silicon carbide particles with basic magnesium carbonate, boric acid, cobalt nitrate and zirconia fibers to obtain a mixture; and finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material. The preparation method is simple, the firing temperature is low, the toughness of the obtained composite ceramic material is good, the composite ceramic material can be used for manufacturing aerospace structural parts and the like, and the application prospect is good.
The silicon carbide particles adopt the combination of alpha-silicon carbide and beta-silicon carbide with different particle sizes, and in the sintering process, the beta-silicon carbide promotes the combination of microscopic particles, reduces the sintering difficulty, is beneficial to the reduction of the sintering temperature and improves the toughness of the product.
The silicon carbide particles are not directly fed, but are subjected to surface treatment by sequentially utilizing yttrium chloride solution and barium nitrate solution, the surface of the silicon carbide particles is modified with nano yttrium oxide, and further the surface of the silicon carbide particles is precipitated with modified barium oxide, so that the surface modification synergistic effect of the two steps plays a role in sintering assistance, reduces sintering temperature and improves the toughness of products.
Basic magnesium carbonate, boric acid and cobalt nitrate are added into the mixture, and under the catalysis of the cobalt nitrate, the basic magnesium carbonate reacts with the boric acid to generate magnesium borate whisker among silicon carbide particles, so that the uniformity of the product is good, the magnesium borate whisker plays a role in toughening, and the toughness of the product is further improved.
Zirconia fiber is also added into the mixture, and the zirconia fiber can cooperate with the surface modification component of the silicon carbide particles to play a role in sintering assistance, reduce the sintering temperature and cooperate with the magnesium borate whisker to further improve the toughness of the product.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
All goods in the invention are purchased through market channels unless specified otherwise.
Example 1
The preparation method of the silicon carbide composite ceramic material comprises the following specific steps:
(1) Firstly, mixing 4kg of silicon carbide particles with 1kg of yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, then mixing 4kg of nano yttrium oxide modified silicon carbide with 8kg of barium nitrate solution with the mass concentration of 0.02%, adding 2kg of ammonium oxalate solution with the mass concentration of 3%, carrying out precipitation reaction, and calcining again to obtain pretreated silicon carbide particles;
(2) Then 4kg of pretreated silicon carbide particles are taken and mixed with 2kg of basic magnesium carbonate, boric acid (the same molar quantity as the basic magnesium carbonate), 0.3kg of cobalt nitrate and 1kg of zirconia fiber in a ball milling way, so as to obtain a mixture;
(3) And finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material.
In the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 100nm and beta-silicon carbide with the particle size of 30nm according to the mass ratio of 10:1, and mixing.
The yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol 10 times of the yttrium chloride; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: and (3) uniformly stirring and mixing the silicon carbide particles and the yttrium chloride solution, standing for 15 minutes, and recovering ethanol under reduced pressure to obtain premixed powder.
The calcining process conditions are as follows: calcining at 750 ℃ for 1.5 hours.
Adding ammonium oxalate solution under the stirring condition of 300r/min, standing for 5min, centrifuging for 8 min at 5000r/min, and taking out precipitate to obtain the pretreated silicon carbide particles.
The process conditions for the re-calcination are as follows: calcination was carried out at 600℃for 50 minutes.
In the step (2), the zirconia fiber is obtained by the following preparation method: stirring and dispersing 12mol of zirconium oxychloride in deionized water with the weight being 2 times that of the zirconium oxychloride, then adding 6mol of glacial acetic acid, stirring and heating to 50 ℃, adding 20mol of basic zirconium carbonate while stirring, adding 3mol of yttrium nitrate when the reaction solution becomes transparent, stirring and uniformly mixing, distilling under reduced pressure to remove excessive moisture, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 3 mu m; wherein, basic zirconium carbonate is divided into three parts and fed in batches.
Concentrating to viscosity of 2mPa.s to obtain concentrated solution; the specific method of electrostatic spraying comprises the following steps: injecting the concentrated solution into a spinning cylinder at constant speed through a peristaltic pump, wherein the diameter of a spinning hole is 0.8mm, the electrostatic pressure is 4000kW, the feeding rate is 0.2mL/min, the temperature of hot air is 70 ℃, and the humidity is less than or equal to 50%.
The heat treatment process conditions are as follows: heating to 600 ℃ at 2 ℃/min, preserving heat for 70 minutes, heating to 1300 ℃ at 15 ℃/min, preserving heat for 60 minutes, and naturally cooling to room temperature.
The ball milling process conditions are as follows: ball milling is carried out for 6 hours at 300 r/min.
In the step (3), the mixture is pressed into a blank by adopting cold isostatic pressing, and the specific process conditions are as follows: the pressure is 200MPa and the time is 10 minutes.
The sintering process conditions are as follows: heating to 1000 ℃ at 10 ℃/min, preserving heat for 40 minutes, heating to 1500 ℃ at 5 ℃/min, preserving heat for 150 minutes, and cooling to room temperature (25 ℃) along with a furnace.
Example 2
The preparation method of the silicon carbide composite ceramic material comprises the following specific steps:
(1) Firstly, mixing 5kg of silicon carbide particles with 1kg of yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, then mixing 5kg of nano yttrium oxide modified silicon carbide with 10kg of barium nitrate solution with the mass concentration of 0.04%, adding 3kg of ammonium oxalate solution with the mass concentration of 4%, carrying out precipitation reaction, and calcining again to obtain pretreated silicon carbide particles;
(2) Then 4kg of pretreated silicon carbide particles are taken and mixed with 3kg of basic magnesium carbonate, boric acid (the same molar quantity as the basic magnesium carbonate), 0.4kg of cobalt nitrate and 2kg of zirconia fiber in a ball milling way, so as to obtain a mixture;
(3) And finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material.
In the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 200nm and beta-silicon carbide with the particle size of 50nm according to the mass ratio of 10:1, and mixing.
The yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol which is 12 times of the yttrium chloride in weight; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: and (3) uniformly stirring and mixing the silicon carbide particles and the yttrium chloride solution, standing for 20 minutes, and recovering ethanol under reduced pressure to obtain premixed powder.
The calcining process conditions are as follows: calcining at 850 ℃ for 2.5 hours.
Adding ammonium oxalate solution under the stirring condition of 500r/min, standing for 7 min, centrifuging for 10 min at 7000r/min, and taking out precipitate to obtain the pretreated silicon carbide particles.
The process conditions for the re-calcination are as follows: calcination was carried out at 650℃for 60 minutes.
In the step (2), the zirconia fiber is obtained by the following preparation method: stirring and dispersing 14mol of zirconium oxychloride in deionized water with the weight being 2 times that of the zirconium oxychloride, adding 6mol of glacial acetic acid, stirring and heating to 60 ℃, adding 20mol of basic zirconium carbonate while stirring, adding 3mol of yttrium nitrate when the reaction solution becomes transparent, stirring and uniformly mixing, distilling under reduced pressure to remove excessive moisture, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 5 mu m; wherein, basic zirconium carbonate is divided into three parts and fed in batches.
Concentrating to viscosity of 3mPa.s to obtain concentrated solution; the specific method of electrostatic spraying comprises the following steps: injecting the concentrated solution into a spinning cylinder at constant speed through a peristaltic pump, wherein the diameter of a spinning hole is 0.8mm, the electrostatic pressure is 5000kW, the feeding rate is 0.3mL/min, the temperature of hot air is 80 ℃, and the humidity is less than or equal to 50%.
The heat treatment process conditions are as follows: heating to 700 ℃ at 3 ℃/min, preserving heat for 80 minutes, heating to 1350 ℃ at 17 ℃/min, preserving heat for 70 minutes, and naturally cooling to room temperature.
The ball milling process conditions are as follows: ball milling is carried out for 7 hours at 400 r/min.
In the step (3), the mixture is pressed into a blank by adopting cold isostatic pressing, and the specific process conditions are as follows: the pressure is 220MPa and the time is 12 minutes.
The sintering process conditions are as follows: heating to 1100 ℃ at 15 ℃/min, preserving heat for 50 minutes, heating to 1550 ℃ at 7 ℃/min, preserving heat for 200 minutes, and cooling to room temperature (25 ℃) along with a furnace.
Example 3
The preparation method of the silicon carbide composite ceramic material comprises the following specific steps:
(1) Firstly, mixing 4.5kg of silicon carbide particles with 1kg of yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, then mixing 4.5kg of nano yttrium oxide modified silicon carbide with 9kg of barium nitrate solution with the mass concentration of 0.03%, adding 2.5kg of ammonium oxalate solution with the mass concentration of 3.5%, precipitating, reacting, and calcining again to obtain pretreated silicon carbide particles;
(2) Then 4kg of pretreated silicon carbide particles are taken and mixed with 2.5kg of basic magnesium carbonate, boric acid (the same molar quantity as basic magnesium carbonate), 0.35kg of cobalt nitrate and 1.5kg of zirconia fiber in a ball milling way, so as to obtain a mixture;
(3) And finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material.
In the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 200nm and beta-silicon carbide with the particle size of 40nm according to the mass ratio of 10:1, and mixing.
The yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol which is 11 times of the yttrium chloride in weight; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: and (3) uniformly stirring and mixing the silicon carbide particles and the yttrium chloride solution, standing for 18 minutes, and recovering ethanol under reduced pressure to obtain premixed powder.
The calcining process conditions are as follows: calcining at 800 ℃ for 2 hours.
Adding ammonium oxalate solution under the stirring condition of 400r/min, standing for 6 min, centrifuging for 9 min at 6000r/min, and taking out precipitate to obtain the pretreated silicon carbide particles.
The process conditions for the re-calcination are as follows: calcination was carried out at 630℃for 55 minutes.
In the step (2), the zirconia fiber is obtained by the following preparation method: firstly, stirring and dispersing 13mol of zirconium oxychloride in deionized water with the weight being 2 times that of the zirconium oxychloride, then adding 6mol of glacial acetic acid, stirring and heating to 55 ℃, adding 20mol of basic zirconium carbonate while stirring, adding 3mol of yttrium nitrate when the reaction solution becomes transparent, stirring and uniformly mixing, distilling under reduced pressure to remove excessive moisture, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 4 mu m; wherein, basic zirconium carbonate is divided into three parts and fed in batches.
Concentrating to viscosity of 3mPa.s to obtain concentrated solution; the specific method of electrostatic spraying comprises the following steps: the concentrated solution is injected into a spinning cylinder at a constant speed through a peristaltic pump, the diameter of a spinning hole is 0.8mm, the electrostatic pressure is 4500kW, the feeding rate is 0.3mL/min, the temperature of hot air is 75 ℃, and the humidity is less than or equal to 50%.
The heat treatment process conditions are as follows: heating to 650 ℃ at 2.5 ℃/min, preserving heat for 75 minutes, heating to 1350 ℃ at 16 ℃/min, preserving heat for 65 minutes, and naturally cooling to room temperature.
The ball milling process conditions are as follows: ball milling is carried out for 6.5 hours at 400 r/min.
In the step (3), the mixture is pressed into a blank by adopting cold isostatic pressing, and the specific process conditions are as follows: the pressure is 210MPa and the time is 11 minutes.
The sintering process conditions are as follows: heating to 1050 ℃ at 12 ℃/min, preserving heat for 45 minutes, heating to 1550 ℃ at 6 ℃/min, preserving heat for 180 minutes, and cooling to room temperature (25 ℃) along with a furnace.
Comparative example
The preparation method of the silicon carbide composite ceramic material comprises the following specific steps:
(1) Firstly, mixing 4kg of silicon carbide particles with 1kg of yttrium chloride solution, and calcining to obtain pretreated silicon carbide particles;
(2) Then 4kg of pretreated silicon carbide particles are taken and mixed with 2kg of basic magnesium carbonate, boric acid (the same molar quantity as the basic magnesium carbonate), 0.3kg of cobalt nitrate and 1kg of zirconia fiber in a ball milling way, so as to obtain a mixture;
(3) And finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material.
In the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 100nm and beta-silicon carbide with the particle size of 30nm according to the mass ratio of 10:1, and mixing.
The yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol 10 times of the yttrium chloride; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: and (3) uniformly stirring and mixing the silicon carbide particles and the yttrium chloride solution, standing for 15 minutes, and recovering ethanol under reduced pressure to obtain premixed powder.
The calcining process conditions are as follows: calcining at 750 ℃ for 1.5 hours.
In the step (2), the zirconia fiber is obtained by the following preparation method: stirring and dispersing 12mol of zirconium oxychloride in deionized water with the weight being 2 times that of the zirconium oxychloride, then adding 6mol of glacial acetic acid, stirring and heating to 50 ℃, adding 20mol of basic zirconium carbonate while stirring, adding 3mol of yttrium nitrate when the reaction solution becomes transparent, stirring and uniformly mixing, distilling under reduced pressure to remove excessive moisture, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 3 mu m; wherein, basic zirconium carbonate is divided into three parts and fed in batches.
Concentrating to viscosity of 2mPa.s to obtain concentrated solution; the specific method of electrostatic spraying comprises the following steps: injecting the concentrated solution into a spinning cylinder at constant speed through a peristaltic pump, wherein the diameter of a spinning hole is 0.8mm, the electrostatic pressure is 4000kW, the feeding rate is 0.2mL/min, the temperature of hot air is 70 ℃, and the humidity is less than or equal to 50%.
The heat treatment process conditions are as follows: heating to 600 ℃ at 2 ℃/min, preserving heat for 70 minutes, heating to 1300 ℃ at 15 ℃/min, preserving heat for 60 minutes, and naturally cooling to room temperature.
The ball milling process conditions are as follows: ball milling is carried out for 6 hours at 300 r/min.
In the step (3), the mixture is pressed into a blank by adopting cold isostatic pressing, and the specific process conditions are as follows: the pressure is 200MPa and the time is 10 minutes.
The sintering process conditions are as follows: heating to 1500 ℃ at 10 ℃/min, preserving heat for 40 minutes, heating to 1900 ℃ at 5 ℃/min, preserving heat for 150 minutes, and cooling to room temperature (25 ℃) along with a furnace.
Test examples
The composite ceramic materials obtained in examples 1 to 3 and comparative example are respectively subjected to performance investigation, and the bending strength is tested by adopting a three-point bending method with specific reference to GB/T6569-2006, fine ceramic bending strength test method; the fracture toughness is tested by adopting a three-point bending method with reference to GB/T23806-2009 method Single-sided Pre-crack Beam (SEPB) method, a fine ceramic fracture toughness test method.
The test results are shown in Table 1.
TABLE 1 Performance test results of composite ceramic materials
As is clear from Table 1, the composite ceramic materials obtained in examples 1 to 3 were high in flexural strength and fracture toughness and had good toughness. The comparative example omits the surface modification of barium oxide when the silicon carbide particles are pretreated, the sintering temperature is higher, the bending strength and the fracture toughness are obviously reduced, and the two-step surface modification of the silicon carbide particles is cooperated to assist the sintering, so that the product performance is improved.
The technical idea of the present invention is described by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must be implemented depending on the above embodiments. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of individual raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (6)
1. The preparation method of the silicon carbide composite ceramic material is characterized by comprising the following specific steps:
(1) Firstly mixing silicon carbide particles with yttrium chloride solution, calcining to obtain nano yttrium oxide modified silicon carbide, and then
Mixing nano yttrium oxide modified silicon carbide with barium nitrate solution, adding ammonium oxalate solution, carrying out precipitation reaction, and calcining again to obtain pretreated silicon carbide particles;
(2) Then ball-milling and mixing the pretreated silicon carbide particles with basic magnesium carbonate, boric acid, cobalt nitrate and zirconia fibers to obtain a mixture;
(3) Finally, pressing the mixture into a blank, and sintering to obtain the composite ceramic material;
In the step (1), the silicon carbide particles are prepared by mixing alpha-silicon carbide with the particle size of 100-200 nm and beta-silicon carbide with the particle size of 30-50 nm according to the mass ratio of 10:1, mixing;
in the step (1), the mass ratio of the silicon carbide particles to the yttrium chloride solution is 4-5: 1, yttrium chloride solution is obtained by dissolving yttrium chloride in absolute ethyl alcohol 10-12 times of the yttrium chloride; the specific method for mixing the silicon carbide particles with the yttrium chloride solution comprises the following steps: uniformly stirring and mixing silicon carbide particles and yttrium chloride solution, standing for 15-20 minutes, and recovering ethanol under reduced pressure to obtain premixed powder;
In the step (1), the calcining process conditions are as follows: calcining at 750-850 ℃ for 1.5-2.5 hours;
In the step (1), the mass ratio of the nanometer yttrium oxide modified silicon carbide, the barium nitrate solution and the ammonium oxalate solution is 4-5: 8-10: 2 to 3, the mass concentration of the barium nitrate solution is 0.02 to 0.04 percent, and the mass concentration of the ammonium oxalate solution is 3 to 4 percent;
in the step (1), the process conditions of the re-calcination are as follows: calcining at 600-650 ℃ for 50-60 minutes;
in the step (2), the mass ratio of the pretreated silicon carbide particles to the basic magnesium carbonate, the cobalt nitrate and the zirconia fiber is 4: 2-3: 0.3 to 0.4: 1 to 2; equimolar amount of basic magnesium carbonate and boric acid;
In the step (3), the sintering process conditions are as follows: heating to 1000-1100 ℃ at 10-15 ℃/min, preserving heat for 40-50 min, heating to 1500-1550 ℃ at 5-7 ℃/min, preserving heat for 150-200 min, and cooling to room temperature along with a furnace.
2. The preparation method of claim 1, wherein in the step (1), an ammonium oxalate solution is added under the stirring condition of 300-500 r/min, the mixture is kept stand for 5-7 minutes, and the mixture is centrifuged for 8-10 minutes at 5000-7000 r/min, and the precipitate is taken out, so that the pretreated silicon carbide particles are obtained.
3. The method of claim 1, wherein the zirconia fiber is obtained by the following method of preparation: firstly stirring zirconium oxychloride and dispersing in deionized water with the weight being 2 times that of the zirconium oxychloride, then adding glacial acetic acid, stirring and heating to 50-60 ℃, adding basic zirconium carbonate while stirring, adding yttrium nitrate, stirring and mixing uniformly, removing excessive water by reduced pressure distillation, concentrating, carrying out electrostatic blowing to obtain gel fiber, and carrying out heat treatment to obtain the zirconium oxide fiber with the diameter of 3-5 mu m; wherein, the mol ratio of zirconium oxychloride, glacial acetic acid, zirconium basic carbonate and yttrium nitrate is 0.6-0.7: 0.3: 1: 0.15, uniformly dividing the basic zirconium carbonate into three parts, and feeding in batches; the ball milling process conditions are as follows: ball milling is carried out for 6 to 7 hours at the speed of 300 to 400 r/min.
4. The method according to claim 1, wherein in the step (3), the mixture is pressed into a blank by cold isostatic pressing, and the specific process conditions are as follows: the pressure is 200-220 MPa, and the time is 10-12 minutes.
5. A silicon carbide composite ceramic material obtained by the production method according to any one of claims 1 to 4.
6. The use of a silicon carbide composite ceramic material according to claim 5 in the manufacture of aerospace structural members.
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