CN111925229A - Method for preparing high-performance foamed ceramic by combining template method with chemical vapor infiltration method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 106
- 239000000126 substance Substances 0.000 title claims abstract description 41
- 230000008595 infiltration Effects 0.000 title claims abstract description 25
- 238000001764 infiltration Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000006260 foam Substances 0.000 claims description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 34
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000002518 antifoaming agent Substances 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- 239000011496 polyurethane foam Substances 0.000 claims description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
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- 229910052580 B4C Inorganic materials 0.000 claims description 6
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 6
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- 238000007254 oxidation reaction Methods 0.000 claims description 6
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- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 6
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- 229910026551 ZrC Inorganic materials 0.000 claims description 5
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 5
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 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 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- OFEAOSSMQHGXMM-UHFFFAOYSA-N 12007-10-2 Chemical compound [W].[W]=[B] OFEAOSSMQHGXMM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- LRTTZMZPZHBOPO-UHFFFAOYSA-N [B].[B].[Hf] Chemical compound [B].[B].[Hf] LRTTZMZPZHBOPO-UHFFFAOYSA-N 0.000 claims description 4
- XTDAIYZKROTZLD-UHFFFAOYSA-N boranylidynetantalum Chemical compound [Ta]#B XTDAIYZKROTZLD-UHFFFAOYSA-N 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- -1 hafnium nitride Chemical class 0.000 claims description 4
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
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- 238000000151 deposition Methods 0.000 description 15
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- 239000007789 gas Substances 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
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- 229920000049 Carbon (fiber) Polymers 0.000 description 3
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- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
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- 239000011148 porous material Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
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- 238000004108 freeze drying Methods 0.000 description 2
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- 239000004033 plastic Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
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- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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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
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Abstract
The invention relates to a method for preparing high-performance foamed ceramics by combining a template method with a chemical vapor infiltration method, which combines the template method with the chemical vapor infiltration method, does not need to add any sintering aid, prepares high-purity ceramic powder slurry, obtains a foamed ceramic framework by slurry coating, drying and template removal (optional) based on the template method, and then combines the chemical vapor infiltration method to densify the foamed ceramic framework to finally obtain the high-performance foamed ceramics. Compared with the traditional foamed ceramic preparation method, the preparation of various ultrahigh-temperature foamed ceramics can be realized without the limitation of preparation temperature. Compared with the traditional preparation method of the foamed ceramic, the method can realize the combined design and preparation of various components of the foamed ceramic based on different slurry and CVI precursor materials, so that the prepared foamed ceramic has designability and compatibility of various functions such as structure, bearing, electromagnetism and the like.
Description
Technical Field
The invention belongs to the technical field of foamed ceramic preparation, and relates to a method for preparing high-performance foamed ceramic by combining a template method with a chemical vapor infiltration method.
Background
The foamed ceramic not only has excellent physical and chemical properties of ceramic material such as high temperature resistance, corrosion resistance, thermal shock resistance and the like, but also has the properties of high porosity, high specific surface area, low density, low heat conduction and the like, and is widely applied to a plurality of fields such as filtration, catalysis, heat insulation, wave transmission, light structures and the like. Only China's foundry industry has a annual demand for the foamed ceramic filter of nearly 1 hundred million pieces, the output value can reach 6-7 hundred million yuan, the world foundry industry has an annual demand for the foamed ceramic filter of 10 hundred million pieces, and the economic benefit is considerable.
The traditional preparation method of the foamed ceramic mainly comprises a reaction sintering method, a pore-forming agent adding method, a direct foaming method, a molten salt method, a sol-gel method, a freeze drying method and the like. Wherein, the reaction sintering method needs to add a sintering aid to reduce the sintering temperature of the foamed ceramic, which will seriously limit the application of the foamed ceramic under the high temperature condition; the porosity of the product prepared by adding the pore-forming agent is difficult to improve, and the pore distribution is easy to cause non-uniformity; the direct foaming method has high requirements on raw materials, and the process conditions are not easy to control; the strength of the product prepared by the molten salt method is low, and the sintering furnace is easily corroded in the preparation process; the sol-gel method has low productivity and difficult control of process conditions; the freeze drying method has the advantage of flexible selection of raw materials, but the technological process is difficult to control.
Chinese patent application No. 201810885523.7, application publication No. CN109133933A, application publication No. 2019.1.4 discloses a high-strength silicon carbide foamed ceramic and a preparation method thereof by primary slurry-coating carbonization sintering. The method uses foamed plastic as a template, adopts a primary slurry coating carbonization sintering method, mixes high-carbon-residue resin, silicon powder, sintering aids and alcohol to prepare slurry with certain viscosity, and prepares the SiC foamed ceramic through slurry coating, carbonization and sintering. The method introduces a plurality of sintering aids, the purity of the components of the formed silicon carbide foam ceramic is not high, and the method of sintering resin carbon and silicon powder is adopted, so that the content of Si in the product is difficult to accurately control, and the mechanical properties, especially the high-temperature properties, of the silicon carbide foam ceramic are influenced.
Chinese patent "A preparation method of silicon carbide foamed ceramics" (application No. 201610257088.4, application publication No. CN105924207A, application publication No. 2016.9.7) discloses a preparation method of silicon carbide foamed ceramics. The method is a direct foaming method, short carbon fiber is added into polyurethane foam plastic raw materials to carry out foaming and crosslinking reaction to obtain a short carbon fiber/polyurethane foam blank, the short carbon fiber/polyurethane foam blank is thermally decomposed under the protection of inert gas to obtain a carbon foam blank, and the carbon foam blank and metal silicon are subjected to reaction sintering in a vacuum furnace to obtain silicon carbide foam ceramic. The method also has the problem that the Si content in the product is difficult to accurately control, and the performance of the foamed ceramic is influenced by residual Si.
In a paper published by Jiangxa et al, namely preparation of high-purity silicon carbide foamed ceramics (selected from No. 6-8 of No. 5 of Buddha mountain ceramics 2015), high-purity silicon carbide powder is used as a raw material, a small amount (0.6%) of boron carbide is added to be used as a sintering aid, the silicon carbide foamed ceramics are formed by adopting an organic foam slurry dipping process, and the silicon carbide foamed ceramics with the silicon carbide content of more than 98% are obtained by sintering at 1900 ℃ in an argon atmosphere. The method has the advantages of over-high sintering temperature, no contribution to large-scale industrial production, less than 1MPa of compressive strength, low strength and limited application.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing high-performance foamed ceramic by combining a template method with a chemical vapor infiltration method, and the foamed ceramic prepared by the method has high purity, excellent performance, uniform pore structure, compact muscles and bones and designable porosity; the process route is simple, and the large-scale production is easy to realize.
Technical scheme
A method for preparing high-performance foamed ceramic by combining a template method with a chemical vapor infiltration method is characterized by comprising the following steps:
step 1: adding high-purity ceramic powder, a binder, a defoaming agent, a plasticizer and a dispersing agent into an organic solvent, uniformly mixing, and putting into a ball milling tank for ball milling for 10-20 h to prepare slurry; the high-purity ceramic powder comprises, by mass, 15% -40% of high-purity ceramic powder, 50% -70% of organic solvent, 1% -4% of binder, 1% -4% of defoaming agent, 1% -4% of plasticizer and 1% -4% of dispersing agent; the organic solvents include, but are not limited to: one or more of ethanol, butanone, toluene and isopropanol;
step 2: soaking the template into the slurry prepared in the step (1) by adopting a template method for slurry hanging treatment, then taking out the template, and treating for 24-120 h in an air environment at the temperature of 20-60 ℃ for drying treatment to prepare a foam preform;
and step 3: placing the foam prefabricated body into a chemical gas phase furnace, carrying out chemical gas phase treatment, and placing the foam ceramic skeleton into the chemical gas phase furnace to densify the foam ceramic skeleton, so as to obtain the high-performance foam ceramic; the chemical vapor treatment is selected according to a deposition process and a ceramic powder material system required to be prepared;
and (3) repeating the operation of the step (2) and the operation of the step (3), changing the porosity of the foamed ceramic to be 50-95%, and obtaining the foamed ceramic with different properties.
Before the step 3, carrying out template removal treatment on the foam prefabricated body to obtain a foam ceramic framework; and 3, carrying out step 3 on the foamed ceramic framework.
When the template is removed, a pyrolysis-oxidation removal process is adopted for the polyurethane foam or resin foam template, namely, the foam preform is heated to 200-350 ℃ from the room temperature at the heating rate of 0.1-1 ℃/min under the air atmosphere, the temperature is kept for 1-4 h, then the temperature is continuously heated to 400-600 ℃ at the heating rate of 0.1-1 ℃/min, and the temperature is kept for 1-4 h.
The high-purity ceramic powder comprises but is not limited to one or more of ceramic powder or whisker in carbide, nitride, boride or oxide.
The grain size of the ceramic powder is selected to be 0.005-10 mu m, and the purity is more than 90%.
The diameter of the ceramic whisker is 1-5 mu m, the length-diameter ratio is 5-15, and the purity is more than 90%.
Such carbides include, but are not limited to: silicon carbide, boron carbide, zirconium carbide, titanium carbide, hafnium carbide, or tantalum carbide.
The nitrides include, but are not limited to: silicon nitride, boron nitride, aluminum nitride, titanium nitride, hafnium nitride, or tantalum nitride.
The borides include, but are not limited to: zirconium boride, hafnium boride, tantalum boride, titanium boride or tungsten boride.
The oxides include, but are not limited to: alumina, zirconia, titania, or silica.
Advantageous effects
The invention provides a method for preparing high-performance foamed ceramics by combining a template method with a chemical vapor infiltration method, which combines the template method with the chemical vapor infiltration method, does not need to add any sintering aid, prepares high-purity ceramic powder slurry, obtains a foamed ceramic framework by slurry coating, drying and template removal (optional) based on the template method, and then combines the chemical vapor infiltration method to densify the foamed ceramic framework to finally obtain the high-performance foamed ceramics.
Compared with the traditional foamed ceramic preparation method, the method can realize the preparation of various ultrahigh-temperature foamed ceramics, such as zirconium boride, tantalum carbide and the like, and the ultrahigh-temperature foamed ceramics cannot be prepared by a sintering method, but can be easily obtained by the method without the limitation of the preparation temperature.
Compared with the traditional preparation method of the foamed ceramic, the method can realize the combined design and preparation of various components of the foamed ceramic based on different slurry and CVI precursor materials, so that the prepared foamed ceramic has designability and compatibility of various functions such as structure, bearing, electromagnetism and the like.
Drawings
FIG. 1 is a photograph of the macro-morphology of the high performance silicon carbide ceramic foam prepared in example 1
FIG. 2 is a microstructure of the high performance silicon carbide ceramic foam prepared in example 1
FIG. 3 is an XRD pattern of the high performance silicon carbide ceramic foam prepared in example 1
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the invention discloses a method for preparing foamed ceramic by combining a template method with a chemical vapor infiltration method, which comprises the following steps:
step 1: adding high-purity ceramic powder, a binder, a defoaming agent, a plasticizer and a dispersing agent into an organic solvent, fully and uniformly mixing, and preparing to obtain slurry.
Step 2: and (3) soaking a template with a certain size into the slurry prepared in the step (1) by adopting a template method for full slurry coating treatment, then taking out the template, removing redundant slurry, and then drying to prepare the foam prefabricated body.
And step 3: according to the material and the use requirement of the template, template removal treatment can be carried out on the foam prefabricated body to obtain a foam ceramic framework; alternatively, the retained template may be selected.
And 4, step 4: and (3) putting the foamed ceramic skeleton into a chemical vapor furnace, and performing chemical vapor treatment to densify the foamed ceramic skeleton, so as to obtain the high-performance foamed ceramic.
And 5: the operation of the step 2 and the step 4 is repeated, the porosity of the foamed ceramic can be changed, and the foamed ceramic with different properties can be obtained.
The porosity of the prepared foamed ceramic is 50-95%.
In the step 1, the slurry is prepared from high-purity ceramic powder, an organic solvent, a binder, a defoaming agent, a plasticizer and a dispersing agent according to a certain proportion: the high-purity ceramic powder comprises, by mass, 15% -40% of high-purity ceramic powder, 50% -70% of organic solvent, 1% -4% of binder, 1% -4% of defoaming agent, 1% -4% of plasticizer and 1% -4% of dispersing agent.
In the step 1, the high-purity ceramic powder may be powder or whisker, and the material includes, but is not limited to, one or more of carbide (such as silicon carbide, boron carbide, zirconium carbide, titanium carbide, hafnium carbide, tantalum carbide, etc.), nitride (such as silicon nitride, boron nitride, aluminum nitride, titanium nitride, hafnium nitride, tantalum nitride, etc.), boride (such as zirconium boride, hafnium boride, tantalum boride, titanium boride, tungsten boride, etc.), oxide (such as aluminum oxide, zirconium oxide, titanium oxide, silicon oxide, etc.), and any other ceramic powder or whisker. The grain size of the ceramic powder is selected to be 0.005-10 mu m, and the purity is more than 90%; the diameter of the ceramic whisker is 1-5 mu m, the length-diameter ratio is 5-15, and the purity is more than 90%.
In the step 1, the organic solvent is formed by mixing one or more of ethanol, butanone, toluene and isopropanol according to a certain proportion.
In the step 1, the step of fully mixing is to mix the high-purity ceramic powder, the binder, the defoaming agent, the plasticizer and the dispersing agent by using an organic solvent, and then put the mixture into a ball milling tank for ball milling for 10 to 20 hours.
In the step 2, the template is an organic template or an inorganic template, the organic template includes but is not limited to polyurethane foam, resin foam, and the like, and the inorganic template includes but is not limited to carbon foam, diatomite, zeolite, and the like.
In the step 2, the drying is carried out for 24-120 h in an air environment at the temperature of 20-60 ℃.
In the step 3, the template removal treatment is an optional step, different removal processes can be selected according to the material of the template, and the template can be selected not to be removed if the template has no influence on the final performance. For example, for a polyurethane foam or resin foam template, a pyrolysis-oxidation removal process can be adopted, namely, a foam preform is heated to 200-350 ℃ from room temperature at a heating rate of 0.1-1 ℃/min in an air atmosphere, the temperature is kept for 1-4 hours, then the temperature is continuously heated to 400-600 ℃ at a heating rate of 0.1-1 ℃/min, and the temperature is kept for 1-4 hours.
In the step 4, the chemical vapor treatment of the foamed ceramic skeleton is to place the foamed ceramic skeleton into a chemical vapor furnace for ceramic densification, and the specific deposition process is realized by adjusting corresponding reaction parameters according to a material system to be prepared. Chemical vapor deposition ceramics include, but are not limited to, carbide ceramics (e.g., silicon carbide, boron carbide, zirconium carbide, titanium carbide, hafnium carbide, tantalum carbide, etc.), nitride ceramics (e.g., silicon carbide, boron carbide, zirconium carbide, titanium carbide, hafnium carbide, tantalum carbide, etc.), and the likeSilicon nitride, boron nitride, aluminum nitride, titanium nitride, hafnium nitride, tantalum nitride, etc.), boride ceramics (e.g., zirconium boride, hafnium boride, tantalum boride, titanium boride, tungsten boride, etc.), oxide ceramics (e.g., alumina, zirconia, titania, silica, etc.), and the like. For example, the chemical vapor phase preparation of silicon carbide ceramics uses trichloromethylsilane (MTS) as precursor, hydrogen as carrier gas and diluent gas, argon as protective gas, MTS: H2The ratio of Ar to Ar is 1: 5-15: 10-20, the deposition temperature is 900-1200 ℃, the total air pressure of the deposition furnace is 0.5-5 kPa, and the deposition time is 20-200 h. For example, chemical vapor preparation of silicon nitride ceramics from silicon tetrachloride (SiCl)4) And ammonia (NH)3) Hydrogen as carrier gas and diluent gas, argon as protective gas, SiCl4∶NH3∶H2The ratio of Ar to Ar is 2-3: 4-5: 5-15: 10-20, the deposition temperature is 750-1000 ℃, the total air pressure of the deposition furnace is 0.5-5 kPa, and the deposition time is 20-200 h.
Example 1
The method for preparing the high-performance silicon carbide foamed ceramic by combining the template method with the chemical vapor infiltration process comprises the following steps:
(1) high-purity silicon carbide powder (the particle diameter d50 is 0.05 mu m, the purity is 99 percent), ethanol, a binder, a defoaming agent, a plasticizer and a dispersing agent are mixed according to the mass ratio of 30 percent: 60 wt%: 3 wt%: 2 wt%: 3 wt%: 2 wt% of the mixture is put into a ball milling tank for ball milling for 12 hours;
(2) cutting polyurethane foam into a square shape to be used as a template, soaking and hanging slurry, removing redundant slurry by adopting an extrusion method, and placing in an air environment at 30 ℃ for 72 hours to fully dry the slurry to obtain a foam preform;
(3) placing the foamed prefabricated body after the slurry coating and drying in a tubular furnace, carrying out pyrolysis-oxidation treatment in the air atmosphere, wherein the heating rate is 0.5 ℃/min, heating to 300 ℃ from room temperature, preserving heat for 2 hours, then continuously heating to 450 ℃ at 0.5 ℃/min, and preserving heat for 2 hours to obtain a foamed ceramic framework consisting of silicon carbide powder;
(4) placing the foamed ceramic skeleton in a chemical gas-phase furnace for silicon carbide ceramic densificationTrichloromethylsilane (MTS) is used as a precursor, hydrogen is used as a carrier gas and a diluent gas, argon is used as a protective gas, and MTS: H2The ratio of Ar to Ar is 1:12:10, the deposition temperature is 1000 ℃, the total air pressure of a deposition furnace is 0.6kPa, and the deposition time is 50 h. Finally obtaining the high-performance silicon carbide foam ceramic.
The silicon carbide ceramic foam obtained in this example had a porosity of 95% and a density of 0.22g/cm3。
Example 2
The method for preparing the high-performance silicon carbide foamed ceramic by combining the template method with the chemical vapor infiltration process comprises the following steps:
(1) silicon carbide crystal whisker (diameter is 1 mu m, length-diameter ratio is 10-15, purity is 99%) and ethanol, butanone, binder, defoaming agent, plasticizer and dispersant, wherein the mass ratio is 30 wt%: 30 wt%: 30 wt%: 3 wt%: 2 wt%: 3 wt%: 2 wt% of the mixture is put into a ball milling tank for ball milling for 18 hours;
(2) cutting polyurethane foam into a square shape to be used as a template, soaking and hanging slurry, removing redundant slurry by adopting an extrusion method, placing the template in a drying box at 50 ℃ for 48 hours, and fully drying the template to obtain a foam prefabricated body;
(3) placing the foamed prefabricated body after the slurry coating and drying in a tubular furnace, carrying out pyrolysis-oxidation treatment in the air atmosphere, wherein the heating rate is 0.5 ℃/min, heating to 300 ℃ from room temperature, preserving heat for 2 hours, then continuously heating to 450 ℃ at 0.5 ℃/min, and preserving heat for 2 hours to obtain a foamed ceramic framework consisting of silicon carbide whiskers;
(4) placing a foamed ceramic skeleton in a chemical vapor deposition furnace for silicon carbide densification, wherein trichloromethylsilane (MTS) is used as a precursor, hydrogen is used as a carrier gas and a diluent gas, argon is used as a protective gas, and the ratio of MTS to H is2The ratio of Ar to Ar is 1:12:10, the deposition temperature is 1100 ℃, the total pressure of the deposition furnace is 5kPa, and the deposition time is 50 h.
(5) And (5) repeating the steps (2), (3) and (4) to obtain the high-performance silicon carbide foam ceramic.
The silicon carbide ceramic foam prepared in this example had a porosity of 88% and a density of 0.28g/cm3。
Example 3
The method for preparing the high-performance silicon nitride foamed ceramic by combining the template method with the chemical vapor infiltration process comprises the following steps of:
(1) silicon nitride crystal whisker (diameter is 1 mu m, length-diameter ratio is 5-10, purity is 95%) and ethanol, butanone, toluene, binder, defoaming agent, plasticizer and dispersant, wherein the mass ratio is 40 wt%: 15 wt%: 15 wt%: 15 wt%: 4 wt%: 3 wt%: 4 wt%: 4 wt% of the mixture is put into a ball milling tank for ball milling for 12 hours;
(2) cutting polyurethane foam into a square shape to be used as a template, soaking and hanging slurry, removing redundant slurry by adopting an extrusion method, and placing in an air environment at 30 ℃ for 72 hours to fully dry the slurry to obtain a foam preform;
(3) placing the foamed prefabricated body after the slurry coating and drying in a tubular furnace, carrying out pyrolysis-oxidation treatment in the air atmosphere, wherein the heating rate is 0.1 ℃/min, heating to 300 ℃ from room temperature, preserving heat for 2 hours, then continuously heating to 500 ℃ at 0.1 ℃/min, preserving heat for 1.5 hours, and obtaining a foamed ceramic framework consisting of silicon nitride whiskers;
(4) the foamed ceramic skeleton is set inside a chemical vapor deposition furnace for densification of silicon nitride with silicon tetrachloride (SiCl)4) And ammonia (NH)3) Hydrogen as carrier gas and diluent gas, argon as protective gas, SiCl4∶NH3∶H2The ratio of Ar to Ar is 3: 4.5: 12:10, the deposition temperature is 800 ℃, the total air pressure of the deposition furnace is 2kPa, and the deposition time is 60 hours. Finally obtaining the high-performance silicon nitride foamed ceramic.
The silicon nitride ceramic foam obtained in this example had a porosity of 92% and a density of 0.24g/cm3。
The macro-morphology picture, the micro-morphology and the XRD result of the high-performance silicon carbide foam ceramic prepared by the invention are respectively shown in figure 1, figure 2 and figure 3. As can be seen from the figure, the prepared foamed ceramic has the advantages of uniform integral structure, compact pore ribs, high purity of 99 percent and high strength, and has great application potential in the aspects of filtration, catalysis, biomedicine, aerospace and the like.
Claims (10)
1. A method for preparing high-performance foamed ceramic by combining a template method with a chemical vapor infiltration method is characterized by comprising the following steps:
step 1: adding high-purity ceramic powder, a binder, a defoaming agent, a plasticizer and a dispersing agent into an organic solvent, uniformly mixing, and putting into a ball milling tank for ball milling for 10-20 h to prepare slurry; the high-purity ceramic powder comprises, by mass, 15% -40% of high-purity ceramic powder, 50% -70% of organic solvent, 1% -4% of binder, 1% -4% of defoaming agent, 1% -4% of plasticizer and 1% -4% of dispersing agent; the organic solvents include, but are not limited to: one or more of ethanol, butanone, toluene and isopropanol;
step 2: soaking the template into the slurry prepared in the step (1) by adopting a template method for slurry hanging treatment, then taking out the template, and treating for 24-120 h in an air environment at the temperature of 20-60 ℃ for drying treatment to prepare a foam preform;
and step 3: placing the foam prefabricated body into a chemical gas phase furnace, carrying out chemical gas phase treatment, and placing the foam ceramic skeleton into the chemical gas phase furnace to densify the foam ceramic skeleton, so as to obtain the high-performance foam ceramic; the chemical vapor treatment is selected according to a deposition process and a ceramic powder material system required to be prepared;
and (3) repeating the operation of the step (2) and the operation of the step (3), changing the porosity of the foamed ceramic to be 50-95%, and obtaining the foamed ceramic with different properties.
2. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: before the step 3, carrying out template removal treatment on the foam prefabricated body to obtain a foam ceramic framework; and 3, carrying out step 3 on the foamed ceramic framework.
3. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 2, which is characterized in that: when the template is removed, a pyrolysis-oxidation removal process is adopted for the polyurethane foam or resin foam template, namely, the foam preform is heated to 200-350 ℃ from the room temperature at the heating rate of 0.1-1 ℃/min under the air atmosphere, the temperature is kept for 1-4 h, then the temperature is continuously heated to 400-600 ℃ at the heating rate of 0.1-1 ℃/min, and the temperature is kept for 1-4 h.
4. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the high-purity ceramic powder comprises but is not limited to one or more of ceramic powder or whisker in carbide, nitride, boride or oxide.
5. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the grain size of the ceramic powder is selected to be 0.005-10 mu m, and the purity is more than 90%.
6. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the diameter of the ceramic whisker is 1-5 mu m, the length-diameter ratio is 5-15, and the purity is more than 90%.
7. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: such carbides include, but are not limited to: silicon carbide, boron carbide, zirconium carbide, titanium carbide, hafnium carbide, or tantalum carbide.
8. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the nitrides include, but are not limited to: silicon nitride, boron nitride, aluminum nitride, titanium nitride, hafnium nitride, or tantalum nitride.
9. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the borides include, but are not limited to: zirconium boride, hafnium boride, tantalum boride, titanium boride or tungsten boride.
10. The method for preparing high-performance foamed ceramics by combining the template method with the chemical vapor infiltration method according to claim 1, which is characterized in that: the oxides include, but are not limited to: alumina, zirconia, titania, or silica.
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