CN116239368B - Preparation method of ceramic-metal composite material and ceramic-metal composite material - Google Patents
Preparation method of ceramic-metal composite material and ceramic-metal composite material Download PDFInfo
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- CN116239368B CN116239368B CN202310220159.3A CN202310220159A CN116239368B CN 116239368 B CN116239368 B CN 116239368B CN 202310220159 A CN202310220159 A CN 202310220159A CN 116239368 B CN116239368 B CN 116239368B
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- ceramic
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- microspheres
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- 239000002905 metal composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 239000000919 ceramic Substances 0.000 claims abstract description 163
- 239000004005 microsphere Substances 0.000 claims abstract description 104
- 239000002131 composite material Substances 0.000 claims abstract description 96
- 229910052751 metal Inorganic materials 0.000 claims abstract description 94
- 239000002184 metal Substances 0.000 claims abstract description 94
- 239000002243 precursor Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 41
- 150000003839 salts Chemical class 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000007731 hot pressing Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 239000011230 binding agent Substances 0.000 claims abstract description 29
- 239000000839 emulsion Substances 0.000 claims abstract description 28
- 239000004094 surface-active agent Substances 0.000 claims abstract description 24
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 230000004048 modification Effects 0.000 claims abstract description 7
- 238000012986 modification Methods 0.000 claims abstract description 7
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 50
- 239000000243 solution Substances 0.000 claims description 43
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 34
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 32
- 239000002244 precipitate Substances 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 229920000053 polysorbate 80 Polymers 0.000 claims description 15
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 11
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 11
- 229920001661 Chitosan Polymers 0.000 claims description 11
- 108010010803 Gelatin Proteins 0.000 claims description 11
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 11
- 239000001099 ammonium carbonate Substances 0.000 claims description 11
- 229920000159 gelatin Polymers 0.000 claims description 11
- 239000008273 gelatin Substances 0.000 claims description 11
- 235000019322 gelatine Nutrition 0.000 claims description 11
- 235000011852 gelatine desserts Nutrition 0.000 claims description 11
- DKMROQRQHGEIOW-UHFFFAOYSA-N Diethyl succinate Chemical compound CCOC(=O)CCC(=O)OCC DKMROQRQHGEIOW-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 9
- RPTHSTHUXCCDTE-UHFFFAOYSA-N ethanolate;nickel(2+) Chemical compound CCO[Ni]OCC RPTHSTHUXCCDTE-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000000661 sodium alginate Substances 0.000 claims description 9
- 235000010413 sodium alginate Nutrition 0.000 claims description 9
- 229940005550 sodium alginate Drugs 0.000 claims description 9
- 229920000936 Agarose Polymers 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- 229920002749 Bacterial cellulose Polymers 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000005016 bacterial cellulose Substances 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- JHLCADGWXYCDQA-UHFFFAOYSA-N calcium;ethanolate Chemical compound [Ca+2].CC[O-].CC[O-] JHLCADGWXYCDQA-UHFFFAOYSA-N 0.000 claims description 2
- 150000001868 cobalt Chemical class 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000009423 ventilation Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 39
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 32
- 229910052759 nickel Inorganic materials 0.000 description 31
- 239000000377 silicon dioxide Substances 0.000 description 22
- 239000007864 aqueous solution Substances 0.000 description 14
- 229910000480 nickel oxide Inorganic materials 0.000 description 14
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 14
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 14
- -1 then Substances 0.000 description 13
- 239000011157 advanced composite material Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 229910010293 ceramic material Inorganic materials 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 238000007493 shaping process Methods 0.000 description 7
- 238000000352 supercritical drying Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- VXPFEVUAMVPPQU-UHFFFAOYSA-N dioxosilane nickel Chemical compound [Ni].O=[Si]=O VXPFEVUAMVPPQU-UHFFFAOYSA-N 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 210000001161 mammalian embryo Anatomy 0.000 description 5
- 238000004945 emulsification Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000004971 Cross linker Substances 0.000 description 3
- LFYMLMKKOJHYFY-UHFFFAOYSA-N [O-2].[Al+3].[Ni+2] Chemical compound [O-2].[Al+3].[Ni+2] LFYMLMKKOJHYFY-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- VIOXBIMGPUGGBQ-UHFFFAOYSA-L aluminum nickel(2+) oxygen(2-) carbonate Chemical compound C([O-])([O-])=O.[O-2].[Al+3].[Ni+2] VIOXBIMGPUGGBQ-UHFFFAOYSA-L 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- SPAGIJMPHSUYSE-UHFFFAOYSA-N Magnesium peroxide Chemical compound [Mg+2].[O-][O-] SPAGIJMPHSUYSE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 238000009824 pressure lamination Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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Abstract
The invention provides a preparation method of a ceramic-metal composite material and the ceramic-metal composite material, wherein the method comprises the following steps: adding the ceramic powder, the binder A and the sintering aid into water for ball milling uniformly to obtain ceramic slurry; uniformly stirring the ceramic slurry and the binder B, adding a surfactant and an organic solvent, and stirring and emulsifying to obtain ceramic emulsion; adding the ceramic emulsion into a cross-linking agent solution, and then separating to obtain ceramic microspheres; adding ceramic microspheres into a solution of metal salt for surface modification treatment, and obtaining ceramic-metal precursor composite microspheres after precipitation reaction; carrying out hot pressing treatment on the ceramic-metal precursor composite microspheres to obtain ceramic-metal precursor composite material blanks; and reducing the ceramic-metal precursor composite material blank, and then sintering to obtain the ceramic-metal composite material.
Description
Technical Field
The invention relates to the technical field of ceramic-metal composite materials, in particular to a preparation method of a ceramic-metal composite material and the ceramic-metal composite material.
Background
The high-performance alumina-based ceramic has potential application prospects in severe environments such as corrosion and high temperature due to excellent mechanical properties, corrosion resistance and oxidation stability, but the low cracking resistance greatly limits the application of the high-performance alumina-based ceramic. From the design point of view of the composite material, the introduction of a ductile phase (usually metal) into the ceramic material can combine the performance advantages of ceramic and metal, and due to the ductility of the metal, when the metal is damaged, the metal layer can induce cracks to deflect and can shear deformation, and the damage mode can improve the toughness of the composite material while the advantages of high strength and high hardness of the ceramic material are maintained to the greatest extent. Residual compressive stresses caused by the mismatch in thermal expansion of some ceramics and metals also contribute to increased strength and toughness.
Several effective methods have been developed. One such method is to induce the ordered growth of ice crystals, and exclude the ceramic slurry from between the ice crystal layers, thereby obtaining a highly ordered layered ceramic scaffold. Composite materials having a nacre-like structure can be produced by fragmenting a frame infiltrated with a second phase. Another method is to obtain a tough ceramic material with a fine structure by densification of the ceramic microchip after ordered assembly with the aid of an external field, such as magnetic force, vacuum, gravity, etc. The layer-by-layer self-assembly strategy is also often applied to the preparation of nacre-like films, which are stacked to give a bulk material with a regular multi-layer structure, however, using non-deformable sheet-like film elements, defects are inevitably generated in the bulk material due to disordered stacking of the sheets during assembly. Moreover, these solutions currently do not allow, due to their own limitations, the rapid preparation of ceramic-metal composites with fine microstructures in large quantities.
Disclosure of Invention
Accordingly, it is a primary object of the present invention to provide a method for preparing a ceramic-metal composite material and a ceramic-metal composite material, so as to at least partially solve at least one of the above-mentioned problems.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
as a first aspect of the present invention, there is provided a method for preparing a ceramic-metal composite material, comprising: adding the ceramic powder, the binder A and the sintering aid into water for ball milling uniformly to obtain ceramic slurry; uniformly stirring the ceramic slurry and the binder B, adding a surfactant and an organic solvent, and stirring and emulsifying to obtain ceramic emulsion; adding the ceramic emulsion into a cross-linking agent solution, and then separating to obtain ceramic microspheres; adding ceramic microspheres into a solution of metal salt for surface modification treatment, and obtaining ceramic-metal precursor composite microspheres after precipitation reaction; carrying out hot pressing treatment on the ceramic-metal precursor composite microspheres to obtain ceramic-metal precursor composite material blanks; and reducing the ceramic-metal precursor composite material blank, and then sintering to obtain the ceramic-metal composite material.
As a second aspect of the present invention, there is provided a ceramic-metal composite material prepared by the above-described preparation method.
Based on the technical scheme, the preparation method of the ceramic-metal composite material and the ceramic-metal composite material provided by the invention at least comprise one or a part of the following beneficial effects:
the invention provides a preparation method of a ceramic-metal composite material, wherein, firstly, the prefabricated ceramic slurry, a surfactant, a binder B solution, an organic solvent and the like are mixed, emulsified, separated and dried according to a certain proportion, after ceramic microspheres are obtained, metal precursors are modified on the surfaces of the ceramic microspheres, and then, the ceramic-metal composite material can be obtained through tabletting, reduction and hot-press sintering. The method can be used for rapidly preparing large-size ceramic-metal composite materials with characteristics of pearl-like layered structures in a large scale, is suitable for compounding various metals and various ceramics, and the obtained composite materials have toughness far higher than that of common ceramic materials and are easy to mold. In addition, as the ceramic-metal composite material is formed by molding ceramic-metal precursor composite microsphere elements through pressure, the deformation process of the spherical elements can spontaneously fill gaps in the material, so that the defects of a plurality of layered composite materials obtained by using non-deformable sheet elements, which are caused by unordered overlapping in the stacking process of the non-deformable elements, are avoided, and the performance of the material is greatly improved.
The ceramic-metal composite material provided by the invention has a pearl-like layered structure and a finer pearl-like brick-mud structure, has mechanical properties far higher than those of common ceramic materials, has high strength and toughness, and is easy to shape.
Drawings
FIG. 1 is a flow chart of a method of preparing a ceramic-metal composite according to an embodiment of the invention;
FIG. 2 is a graph of temperature and pressure versus time during sintering of an alumina-nickel advanced composite ceramic according to an embodiment of the invention;
FIG. 3 is a scanning electron microscope image of alumina ceramic microspheres according to an embodiment of the present invention;
FIG. 4 is a sample view of an alumina-nickel advanced composite ceramic according to an embodiment of the present invention;
FIG. 5 is a scanning electron microscope image of a broken section of an alumina-nickel advanced composite ceramic according to an embodiment of the present invention;
FIG. 6 is a scanning electron microscope image of alumina grains of an alumina-nickel advanced composite ceramic according to an embodiment of the present invention;
FIG. 7 is a stress-strain curve of an alumina-nickel advanced composite ceramic according to an embodiment of the invention.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
In the process of realizing the invention, how to prepare ceramic-metal composite materials with fine microstructures in large batch and rapidly is a technical difficulty of realizing the ceramic-metal composite materials with high strength and high toughness. The invention provides a preparation method of a ceramic-metal composite material, wherein, firstly, the prefabricated ceramic slurry, a surfactant, a binder B, an organic solvent and the like are mixed, emulsified, separated and dried according to a certain proportion to obtain ceramic microspheres, then, metal precursors are modified on the surfaces of the ceramic microspheres, and then, the ceramic-metal composite material can be obtained through tabletting, reduction, hot-press sintering. The method can be used for rapidly preparing large-size ceramic-metal composite materials with characteristics of pearl-like layered structures in a large scale, is suitable for compounding various metals and various ceramics, has pearl-like layered structures and finer pearl-like brick-mud structures, has mechanical properties far higher than those of common ceramic materials, has high strength and toughness, and is easy to shape.
It should be noted that, in the present invention, some terms are defined as follows:
a ductile metal salt having a melting point of 1400 ℃ or higher: is a salt composed of a metal element having a ductile melting point of 1400 ℃ or higher and an acid ion. Specifically, according to an embodiment of the present invention, a method of preparing a ceramic-metal composite material is provided. Fig. 1 is a flowchart of a method for preparing a ceramic-metal composite according to an embodiment of the present invention, which specifically includes the following operations S110 to S160.
In operation S110: adding the ceramic powder, the adhesive A and the sintering aid into water, and ball milling uniformly to obtain ceramic slurry.
According to an embodiment of the present invention, the ceramic powder includes a compound containing a metal element and a non-metal element bonded by an ionic bond or a covalent bond; the binder A comprises at least one of polyvinyl alcohol, polyethylene glycol, chitosan, carboxymethyl cellulose sodium salt, hydroxypropyl cellulose, sodium polyacrylate, sodium alginate, bacterial cellulose and gelatin; the sintering aid comprises at least one of magnesium oxide, yttrium oxide, copper oxide, titanium oxide, calcium oxide and silicon oxide; the mass ratio of the ceramic powder, the binder, the sintering aid and the water is 15-30: 1 to 3:0 to 2: preferably, the mass ratio of the ceramic powder, the binder, the sintering aid and the water is 15-30: 1 to 3:0.2 to 2:80 to 100, and the ball milling time is 12 to 24 hours, for example, 12 hours, 16 hours, 20 hours, and 24 hours.
Wherein the compound containing a metal element and a non-metal element, which are bonded by ionic bond or covalent bond, includes at least one of alumina, zirconia, silica, silicon carbide, and boron nitride.
According to the embodiment of the invention, the mass ratio of the binder is not more than 10% of the ceramic powder, and the mass ratio of the sintering aid is not more than 10% of the ceramic powder.
In operation S120, after the ceramic slurry and the binder B are uniformly stirred, a surfactant and an organic solvent are added, and stirred and emulsified to obtain a ceramic emulsion.
According to an embodiment of the present invention, after uniformly stirring the ceramic slurry with the binder B, adding the surfactant and the organic solvent, stirring and emulsifying includes operations S121 and S122.
In operation S121, the ceramic slurry and the binder B are uniformly stirred to obtain a mixed solution.
In operation S122, after adding the surfactant and the organic solvent to the mixed solution, heating and maintaining the temperature for a while, and then maintaining the temperature and stirring the mixture for emulsification.
Wherein, the volume ratio of the ceramic slurry, the binder B, the surfactant and the organic solvent is 5-10: 5-10: 2 to 5:50 to 60. The heating and heat preserving temperature ranges from 50 ℃ to 90 ℃, for example, 50 ℃,60 ℃,70 ℃,80 ℃ and 90 ℃; the heating and heat-preserving time ranges from 10 minutes to 20 minutes, for example, 10 minutes, 15 minutes and 20 minutes; the incubation and stirring time may be 10 minutes to 60 minutes, for example, 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, and 60 minutes.
According to embodiments of the present invention, the manner of stirring may be, but is not limited to, any one of magnetic stirring and mechanical stirring.
According to the embodiment of the invention, the ceramic slurry, the binder B, the surfactant and the organic solvent are added in a volume ratio which is too high or too low, so that the prepared ceramic emulsion is not beneficial to forming deformable ceramic microspheres subsequently, and the deformable ceramic-metal precursor composite microspheres are obtained by further processing, therefore, the volume ratio of the ceramic slurry, the binder B, the surfactant and the organic solvent is 5-10: 5-10: 2 to 5:50 to 60.
According to the embodiment of the invention, the temperature range of heating and heat preservation at 50-90 ℃ is more easily achieved and well controlled than other too high or too low temperature ranges while being beneficial to the emulsification process; the heating and heat-preserving time of 10 minutes to 20 minutes before the heat-preserving stirring operation is beneficial to the uniform heating of the ceramic slurry, and the emulsification process of the ceramic slurry is easier to promote than other heating and heat-preserving ranges which are too high or too low.
According to an embodiment of the present invention, the polysaccharide includes at least one of agarose, gelatin, cellulose, and chitosan; the surfactant comprises at least one of span-40, span-80, tween-40, tween-80, cetyltrimethylammonium bromide and sodium dodecyl sulfate; the organic solvent comprises at least one of n-hexane, cyclohexane and diethyl succinate.
In operation S130, after the ceramic emulsion is added to the crosslinker solution, a separation process is performed to obtain ceramic microspheres.
According to an embodiment of the present invention, after adding the ceramic emulsion to the crosslinker solution, a separation process is performed to obtain ceramic microspheres including operations S131 and S133.
In operation S131, after the ceramic emulsion is dropped to the crosslinker solution, spherical precipitates are separated and washed.
In operation S132, the washed spherical precipitate is freeze-dried to obtain ceramic microspheres having an uneven particle size distribution ratio.
In operation S132, the ceramic microspheres with non-uniform particle size distribution ratio are classified and sieved to obtain ceramic microspheres with uniform particle size distribution ratio, so that the finally obtained ceramic-metal composite material has a uniform pearl-like layered structure.
Wherein the cross-linking agent comprises at least one of nickel ethoxide and calcium ethoxide, and the concentration of the cross-linking agent solution ranges from 0.008g/mL to 0.01g/mL, for example, 0.008g/mL,0.009g/mL and 0.01g/mL.
According to the embodiment of the invention, the particle size of the ceramic microspheres can be controlled by the stirring speed, the surfactant type and the using amount in the emulsification process for preparing the ceramic emulsion, and the ceramic microspheres with higher particle size distribution ratio can be obtained by further sieving after crosslinking. Therefore, the controllability of the particle size of the ceramic microspheres is beneficial to controlling the structure of the ceramic-metal composite material, so that the mechanical property of the ceramic-metal composite material is regulated and controlled, and the preparation process is simple and controllable and can be used for industrialized mass preparation.
In operation S140, the ceramic microspheres are added to a solution of a metal salt to perform surface modification treatment, and a precipitation reaction is performed to obtain ceramic-metal precursor composite microspheres.
According to the embodiment of the invention, ceramic microspheres are added into a solution of metal salt for surface modification treatment, and after precipitation reaction, ceramic-metal precursor composite microspheres are obtained, which specifically comprises operations S141-S143.
In operation S141, ceramic microspheres are dispersed into a solution of a metal salt to obtain a ceramic microsphere metal salt dispersion.
In operation S142, an ammonium bicarbonate solution is slowly added dropwise to the ceramic microsphere metal salt dispersion to obtain a ceramic microsphere metal salt precipitate.
In operation S143, a binder is added to the ceramic microsphere metal salt precipitate, and after stirring uniformly, a drying treatment is performed to obtain ceramic-metal precursor composite microspheres.
Wherein the metal salt includes at least one metal salt having a ductile melting point of 1400 ℃ or more, and the concentration of the metal salt in the solution ranges from 0.1mol/L to 0.15mol/L, and may be, for example, 0.1mol/L,0.12mol/L,0.14mol/L,0.15mol/L; the concentration of the ammonium bicarbonate solution is in the range of 0.1mol/L to 0.15mol/L, for example, 0.1mol/L,0.12mol/L,0.14mol/L and 0.15mol/L.
Wherein the metal salt comprises at least one of ferric salt, nickel salt and cobalt salt.
According to the embodiment of the invention, the ceramic-metal precursor composite microsphere is powder. In operation S150, the ceramic-metal precursor composite microsphere is subjected to hot pressing treatment to obtain a ceramic-metal precursor composite green body.
According to an embodiment of the invention, the ceramic-metal precursor composite green body is a sheet-like element.
According to the embodiment of the invention, in the hot pressing process of the ceramic-metal precursor composite microsphere, the pressure range of the hot pressing process is 2-10 kN.
According to the embodiment of the invention, the ceramic-metal precursor composite microsphere is a spherical element, and the spherical element is changed into a sheet element through hot pressing treatment (the pressure range is 2-10 kN), so that the formation of a pearl-like layered structure is further facilitated.
According to the embodiment of the invention, the ceramic-metal precursor composite blank still has the performance of variable shape.
In operation S160, the ceramic-metal precursor composite green body is reduced and then sintered to obtain the ceramic-metal composite.
According to an embodiment of the present invention, after the ceramic-metal precursor composite ligand is reduced, sintering treatment is performed to obtain a ceramic-metal composite, which specifically includes operations S161 to S163.
In operation S161, air is introduced into the ceramic-metal precursor composite green body at a certain temperature to remove the organic matters.
In operation S162: and (3) introducing hydrogen and argon into the ceramic-metal precursor composite material blank body from which the organic matters are removed, so as to reduce the surface of the ceramic-metal precursor composite material blank body to obtain a metal simple substance.
Operation S163: and sintering the ceramic-metal precursor composite material blank after the reduction treatment under the protection of inert gas to obtain the ceramic-metal composite material.
Wherein the temperature range at a certain temperature is 500-900 ℃, and the time range of air ventilation is 1-4 hours, for example, 1 hour, 2 hours, 3 hours and 4 hours; the time for introducing the hydrogen and argon gas is 1 to 4 hours, for example, 1 hour, 2 hours, 3 hours, and 4 hours; the sintering treatment temperature range is 1300-1500 ℃ and the pressure range is 2-10 kN;
the temperature holding time for the sintering treatment is 5 minutes to 30 minutes, and may be, for example, 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes, or 30 minutes.
According to the embodiment of the invention, hydrogen and argon are introduced into the ceramic-metal precursor composite material blank body from which the organic matters are removed, so that metal salt on the surface of the blank body is reduced to obtain a metal simple substance.
According to the embodiment of the invention, the ceramic-metal composite material is formed by pressure molding of the blank of the deformable ceramic-metal precursor composite material, and the blank is further expanded and deformed in the process of pressure lamination, so that gaps generated in the lamination process can be spontaneously filled, a plurality of defects generated by unordered overlapping in the stacking process of the undeformed sheet-shaped elements, which are caused by the ceramic-metal composite material obtained by using the undeformed sheet-shaped elements, are avoided, and the performance of the material is greatly improved.
According to the embodiment of the invention, the sintering treatment temperature of 1300-1500 ℃ is kept for 5-30 minutes, and the sintering treatment pressure range of 2-10 kN is set, so that the sintering of the compound serving as ceramic powder in the ceramic-metal precursor composite material blank is facilitated, and meanwhile, the temperature keeping time and the sintering treatment pressure range are easier to realize the superposition of a plurality of ceramic-metal precursor composite material blanks than other sintering treatment temperatures which are too high and too low, so that the ceramic-metal composite material is formed.
According to an embodiment of the present invention, the above preparation method further includes that the binder B is obtained by:
uniformly stirring the adhesive B and water under the water bath condition to obtain the adhesive B;
wherein the temperature range of the water bath condition is 50-95 ℃, and the stirring time range of the water bath condition is 1-3 hours, for example, 1 hour, 2 hours and 3 hours; the concentration range of the adhesive B is 0.01 g/mL-0.05 g/mL.
According to an embodiment of the present invention, the water in the operation S110 and the preparation of the binder B may include any one of tap water, deionized water, and ultrapure water.
According to the embodiment of the invention, the ceramic-metal composite material is prepared through the operation steps S110-S160, the method is simple to operate, the flow is simple and controllable, the reaction is safe and reliable, the cost is low, the preparation can be performed in large quantity, and the microstructure and the mechanical property of the obtained ceramic-metal composite material can be regulated and controlled through simple material proportion change. In addition, the ceramic-metal composite material prepared by the method has wider application prospect than the traditional ceramic material.
According to the embodiment of the invention, due to deformability of the ceramic microspheres for preparing the ceramic-metal composite material, the ceramic-metal composite material can be further subjected to pressure molding according to actual use requirements, and can be shaped into any one of a sheet, a bowl, a saddle, a wafer and a square.
According to an embodiment of the present invention, there is also provided a ceramic-metal composite material prepared by the above method.
According to the embodiment of the invention, the ceramic-metal composite material has a layered structure similar to nacre and a finer nacre brick-mud structure, wherein the nacre brick-mud structure is formed by inserting metal layers (a mud structure in the nacre brick-mud structure) between flattened ceramic microspheres and wrapping the flattened ceramic microspheres (a brick structure in the nacre brick-mud structure). The metal layer is a flexible layer similar to a nacre lamellar structure.
According to the embodiment of the invention, the toughness of the ceramic-metal composite material is far higher than that of the traditional ceramic material, and the ceramic-metal composite material is easy to mold and shows high-strength toughness at normal temperature and high temperature.
The following describes the technical scheme of the invention in detail by listing a plurality of specific embodiments. It should be noted that the following specific embodiments are only examples and are not intended to limit the present invention.
Example 1: preparation of alumina-nickel composite ceramic by agar-Tween 80 system
(1) According to the formula of 19.5% of alumina nano powder, 0.5% of silicon dioxide, 2% of sodium alginate and 78% of deionized water, preparing alumina ceramic slurry, and ball milling for 24 hours.
(2) The obtained alumina ceramic slurry was heated to 50 ℃ in a water bath, mixed with a hot agarose solution, tween-80 (surfactant), diethyl succinate (organic solvent), and magnetically stirred and emulsified to obtain a water-in-oil alumina ceramic emulsion, and the specific addition amounts are shown in table 1.
Table 1: alumina ceramic slurry, agarose solution, addition amount of tween-80 and diethyl succinate
(3) And (3) dripping the alumina ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing the water-phase microspheres, separating the microspheres, washing and drying to obtain the alumina ceramic microspheres.
(4) Dispersing the alumina ceramic microspheres prepared in the step (3) in 150mL of 0.15mol/L nickel chloride aqueous solution, slowly dripping 0.15mol/L ammonium bicarbonate aqueous solution until bubbles are not generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, and filtering to obtain alumina ceramic microsphere metal salt precipitate. Adding 1-3 mL of chitosan with mass concentration of 2% into the precipitate, uniformly stirring, freeze-drying or supercritical drying after using absolute ethyl alcohol for exchange, and hot-pressing and tabletting after drying (the pressure used for hot pressing is 2-10 kN) to obtain an alumina-nickel carbonate composite material embryo body.
(5) Placing the alumina-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, treating for 2 hours at 700 ℃ by using the muffle furnace to remove organic matters of the alumina-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydride for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced aluminum oxide-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace (the time-varying curve of the temperature and the pressure in the sintering process is shown as figure 2) so as to obtain the flaky aluminum oxide-nickel composite ceramic by shaping.
Firstly, carrying out morphology characterization on the alumina ceramic microspheres obtained in the step (2):
FIG. 3 is a scanning electron microscope image of alumina ceramic microspheres according to an embodiment of the invention.
As shown in FIG. 3, the alumina ceramic microspheres are spherical, and the length of the sphere diameter ranges from 100 μm to 200 μm.
And further carrying out morphology characterization on the aluminum oxide-nickel composite ceramic.
FIG. 4 is a sample of the alumina-nickel composite ceramic according to the embodiment of the present invention.
As shown in fig. 4, the alumina-nickel composite ceramic is in the form of a sheet having a diameter size of the order of cm and a diameter size of 3 cm. In addition, the diameter size of the alumina-nickel composite ceramic can be adjusted according to practical use conditions, and is not limited to the centimeter level.
FIG. 5 is a scanning electron microscope image of a broken section of an alumina-nickel composite ceramic according to an embodiment of the present invention.
As shown in fig. 5, the fracture cross section of the alumina-nickel composite ceramic is a pearl-like layered structure, in addition, it can be seen that the nickel metal layer is inserted into the pearl-like layered structure to form a flexible layer, and the flattened alumina ceramic microspheres are wrapped to form a net-like structure together, and no gap exists in the structure.
FIG. 6 is a scanning electron microscope image of alumina grains of an alumina-nickel composite ceramic according to an embodiment of the present invention.
As shown in fig. 6, the alumina grains are closely arranged, and the overall structure is dense, indicating that the alumina is completely sintered.
In order to further explore the strength performance of the alumina-nickel composite ceramics prepared in the steps (1) to (6), arbitrary 5 areas of the alumina-nickel composite ceramics are taken, and the alumina-nickel composite ceramics with the size of 2mm by 25mm are respectively cut as samples for stress-strain test.
FIG. 7 is a stress-strain curve of an alumina-nickel composite ceramic according to an embodiment of the present invention.
As shown in fig. 7, it can be seen that the strain curves of the 5 samples have high overlap ratio, which indicates that the strength of the alumina-nickel composite ceramic prepared in this embodiment is similar, and further indicates that the distribution of the nacre-like layered structure of the composite ceramic is more uniform. The average of the strength of these 5 samples was determined as the strength of the alumina-nickel composite ceramic prepared in this example, which was 285.18MPa.
Example 2: preparation of alumina-nickel advanced composite ceramic by gelatin-Tween 80 system
(1) Preparing alumina ceramic slurry according to a formula of 20% of alumina nano powder, 2% of sodium alginate and 78% of deionized water in mass ratio, and ball milling for 24 hours.
(2) The obtained alumina ceramic slurry is heated to 60 ℃ in water bath, mixed with a hot gelatin solution, tween-80 (surfactant) and diethyl succinate (organic solvent), and magnetically stirred and emulsified to obtain water-in-oil alumina ceramic emulsion, wherein the specific addition amount is shown in table 2.
Table 2: alumina ceramic slurry, gelatin solution, tween-80 and diethyl succinate
(3) And (3) dripping the alumina ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing the water-phase microspheres, separating the microspheres, washing and drying to obtain the alumina ceramic microspheres.
(4) Dispersing the alumina ceramic microspheres prepared in the step (3) in 150mL of 0.15mol/L nickel chloride aqueous solution, slowly dripping 0.15mol/L ammonium bicarbonate aqueous solution until bubbles are not generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, and filtering to obtain alumina ceramic microsphere metal salt precipitate. Adding 1-3 mL of chitosan with mass concentration of 2% into the precipitate, uniformly stirring, freeze-drying or supercritical drying after using absolute ethyl alcohol for exchange, and hot-pressing and tabletting after drying (the pressure used for hot pressing is 2-10 kN) to obtain an alumina-nickel carbonate composite material embryo body.
(5) Placing the alumina-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, treating for 2 hours at 700 ℃ by using the muffle furnace to remove organic matters of the alumina-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydride for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced aluminum oxide-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace (the time-varying curve of the temperature and the pressure in the sintering process is shown as figure 2) so as to obtain the flaky aluminum oxide-nickel composite ceramic by shaping.
Example 3: preparation of zirconia-nickel composite ceramic by agar-span 80 system
(1) Preparing ceramic slurry according to a formula of 19.8% of zirconia nano powder, 0.2% of magnesia, 2% of sodium alginate and 78% of deionized water in mass ratio, and ball milling for 24 hours.
(2) The obtained zirconia ceramic slurry was heated to 65 ℃ in a water bath, mixed with a hot agarose cellulose mixed solution, span-80 (surfactant), cyclohexane (organic solvent) and magnetically stirred and emulsified to obtain a water-in-oil zirconia ceramic emulsion, and the specific addition amounts are shown in table 3.
Table 3: zirconia ceramic slurry, agarose cellulose mixed solution, span-80 and cyclohexane adding amount
(3) Dripping the zirconia ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing water-phase microspheres, separating the microspheres, washing and drying to obtain zirconia ceramic microspheres;
(4) Dispersing the zirconia ceramic microspheres prepared in the step (3) in 300mL of 0.1mol/L nickel chloride aqueous solution, slowly dripping 0.1mol/L ammonium bicarbonate aqueous solution until no bubbles are generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, filtering to obtain zirconia ceramic microsphere metal salt precipitate, and adding 1 mL-3 mL of chitosan with mass concentration of 2% into the precipitate. And uniformly stirring, then freeze-drying or supercritical drying after absolute ethyl alcohol exchange, and hot-pressing and tabletting (the pressure used for hot pressing is 2-10 kN) after drying to obtain the zirconium oxide-nickel carbonate composite material blank.
(5) Placing the zirconia-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, treating the blank for 2 hours at 600 ℃ by using the muffle furnace to remove organic matters in the zirconia-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydride for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced alumina-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace to obtain the flaky zirconia-nickel advanced composite ceramic by shaping.
Example 4: preparation of zirconia-nickel advanced composite ceramic by gelatin-Tween 80 system
(1) Preparing ceramic slurry according to a formula of 20% of zirconia nano powder, 2% of sodium alginate and 78% of deionized water in mass ratio, and ball milling for 24 hours.
(2) The obtained zirconia ceramic slurry was heated to 60 ℃ in a water bath, mixed with a hot gelatin solution, span-80 (surfactant), cyclohexane (organic solvent), and magnetically stirred and emulsified to obtain a water-in-oil zirconia ceramic emulsion, and the specific addition amounts are shown in table 4.
Table 4: zirconia ceramic slurry, gelatin solution, tween-80 and diethyl succinate
(3) Dripping the zirconia ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing water-phase microspheres, separating the microspheres, washing and drying to obtain zirconia ceramic microspheres;
(4) Dispersing the zirconia ceramic microspheres prepared in the step (3) in 300mL of 0.1mol/L nickel chloride aqueous solution, slowly dripping 0.1mol/L ammonium bicarbonate aqueous solution until no bubbles are generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, filtering to obtain zirconia ceramic microsphere metal salt precipitate, and adding 1 mL-3 mL of chitosan with mass concentration of 2% into the precipitate. And uniformly stirring, then freeze-drying or supercritical drying after absolute ethyl alcohol exchange, and hot-pressing and tabletting (the pressure used for hot pressing is 2-10 kN) after drying to obtain the zirconium oxide-nickel carbonate composite material blank.
(5) Placing the zirconia-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, treating the blank for 2 hours at 700 ℃ by using the muffle furnace to remove organic matters in the zirconia-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydride for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced alumina-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace to obtain the flaky zirconia-nickel advanced composite ceramic by shaping.
Example 5: preparation of silicon dioxide-nickel advanced composite ceramic by agar-Tween 40 system
(1) Preparing silicon dioxide ceramic slurry according to a formula of 20% of silicon dioxide nano powder, 2% of sodium alginate and 78% of ultrapure water by mass ratio, and ball milling for 24 hours.
(2) The obtained silica ceramic slurry was heated to 50 ℃ in a water bath, mixed with a hot agarose solution, tween-40 (surfactant), cyclohexane (organic solvent), and magnetically stirred and emulsified to obtain a water-in-oil silica ceramic emulsion, and the specific addition amounts are shown in table 5.
Table 5: addition amount of silica ceramic slurry, agarose solution, tween-40 and cyclohexane
(3) And (3) dripping the silica ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing the water-phase microspheres, separating the microspheres, washing and drying to obtain the alumina ceramic microspheres.
(4) Dispersing the silica ceramic microspheres prepared in the step (3) in 150mL of 0.15mol/L nickel chloride aqueous solution, slowly dripping 0.15mol/L ammonium bicarbonate aqueous solution until bubbles are not generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, and filtering to obtain metal salt precipitates of the silica ceramic microspheres. Adding 1-3 mL of chitosan with mass concentration of 2% into the precipitate, uniformly stirring, freeze-drying or supercritical drying after absolute ethyl alcohol exchange, and hot-pressing and tabletting after drying (the pressure used for hot pressing is 2-10 kN) to obtain the silicon dioxide-nickel carbonate composite material embryo.
(5) Placing the silica-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, introducing air into the muffle furnace for 2 hours at 700 ℃ to remove organic matters of the silica-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydrogen for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced silicon dioxide-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace to obtain the flaky silicon dioxide-nickel composite ceramic by shaping.
Example 6: preparation of silicon dioxide-nickel advanced composite ceramic by gelatin-Tween 80 system
(1) Preparing silicon dioxide ceramic slurry according to a formula of 20% of silicon dioxide nano powder, 2% of sodium alginate and 78% of ultrapure water by mass ratio, and ball milling for 24 hours.
(2) The obtained silica ceramic slurry was heated to 60 ℃ in a water bath, mixed with a hot gelatin solution, tween-80 (surfactant), diethyl succinate (organic solvent), and magnetically stirred and emulsified to obtain a water-in-oil silica ceramic emulsion, the specific addition amounts of which are shown in table 6.
Table 6: silica ceramic slurry, gelatin solution, tween-80 and diethyl succinate
(3) And (3) dripping the silica ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing the water-phase microspheres, separating the microspheres, washing and drying to obtain the alumina ceramic microspheres.
(4) Dispersing the silica ceramic microspheres prepared in the step (3) in 150mL of 0.15mol/L nickel chloride aqueous solution, slowly dripping 0.15mol/L ammonium bicarbonate aqueous solution until bubbles are not generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, and filtering to obtain metal salt precipitates of the silica ceramic microspheres. Adding 1-3 mL of chitosan with mass concentration of 2% into the precipitate, uniformly stirring, freeze-drying or supercritical drying after absolute ethyl alcohol exchange, and hot-pressing and tabletting after drying (the pressure used for hot pressing is 2-10 kN) to obtain the silicon dioxide-nickel carbonate composite material embryo.
(5) Placing the silica-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, introducing air into the muffle furnace for 2 hours at 700 ℃ to remove organic matters of the silica-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydrogen for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced silicon dioxide-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace to obtain the flaky silicon dioxide-nickel composite ceramic by shaping.
Example 7: preparation of silicon dioxide-nickel advanced composite ceramic by gelatin-Tween 80 system
(1) Preparing silicon dioxide ceramic slurry according to a formula of 20% of silicon dioxide nano powder, 1% of magnesium dioxide, 2% of sodium alginate and 77% of deionized water by mass ratio, and ball milling for 24 hours.
(2) The obtained silica ceramic slurry was heated to 50 ℃ in a water bath, mixed with a hot gelatin solution, tween-80 (surfactant), diethyl succinate (organic solvent), and magnetically stirred and emulsified to obtain a water-in-oil silica ceramic emulsion, the specific addition amounts of which are shown in table 6.
(3) And (3) dripping the silica ceramic emulsion obtained in the step (2) into a cold nickel ethoxide solution, quickly condensing the water-phase microspheres, separating the microspheres, washing and drying to obtain the alumina ceramic microspheres.
(4) Dispersing the silica ceramic microspheres prepared in the step (3) in 150mL of 0.15mol/L nickel chloride aqueous solution, slowly dripping 0.15mol/L ammonium bicarbonate aqueous solution until bubbles are not generated in a large amount, coating nickel carbonate on the surfaces of the microspheres, and filtering to obtain metal salt precipitates of the silica ceramic microspheres. Adding 1-3 mL of chitosan with mass concentration of 2% into the precipitate, uniformly stirring, freeze-drying or supercritical drying after absolute ethyl alcohol exchange, and hot-pressing and tabletting after drying (the pressure used for hot pressing is 2-10 kN) to obtain the silicon dioxide-nickel carbonate composite material embryo.
(5) Placing the silica-nickel carbonate composite material blank prepared in the step (4) in a muffle furnace, introducing air into the muffle furnace for 2 hours at 700 ℃ to remove organic matters of the silica-nickel carbonate composite material blank, decomposing nickel carbonate to obtain nickel oxide, and then introducing argon hydrogen for 2 hours to reduce the nickel oxide into elemental nickel.
(6) And (3) sintering the reduced silicon dioxide-nickel carbonate composite material blanks obtained in the step (5) at 1300-1500 ℃ by using a hot-pressing sintering furnace to obtain the flaky silicon dioxide-nickel composite ceramic by shaping.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.
Claims (4)
1. A method of preparing a ceramic-metal composite comprising:
adding the ceramic powder, the binder A and the sintering aid into water for ball milling uniformly to obtain ceramic slurry;
uniformly stirring the ceramic slurry and the binder B, adding a surfactant and an organic solvent, and stirring and emulsifying to obtain ceramic emulsion;
adding the ceramic emulsion into a cross-linking agent solution, and then separating to obtain ceramic microspheres;
adding the ceramic microspheres into a solution of metal salt, performing surface modification treatment, and performing precipitation reaction to obtain ceramic-metal precursor composite microspheres;
carrying out hot pressing treatment on the ceramic-metal precursor composite microspheres to obtain ceramic-metal precursor composite material blanks;
reducing the ceramic-metal precursor composite material blank, and then sintering to obtain a ceramic-metal composite material;
wherein, after the ceramic slurry and the binder B are uniformly stirred, adding the surfactant and the organic solvent, stirring and emulsifying comprises the following steps:
uniformly stirring the ceramic slurry and the binder B to obtain a mixed solution;
adding a surfactant and an organic solvent into the mixed solution, heating and preserving heat for a period of time, and then preserving heat at the temperature, stirring and emulsifying;
wherein the volume ratio of the ceramic slurry to the binder B, the surfactant and the organic solvent is 5-10: 5-10: 2 to 5: 50-60, wherein the temperature range of heating and heat preservation is 50-90 ℃, the time range of heating and heat preservation is 10-20 minutes, and the time of heat preservation and stirring is 10-60 minutes;
the ceramic powder comprises at least one of alumina, zirconia, silicon oxide, silicon carbide and boron nitride; the adhesive A comprises at least one of polyvinyl alcohol, polyethylene glycol, chitosan, carboxymethyl cellulose sodium salt, hydroxypropyl cellulose, sodium polyacrylate, sodium alginate, bacterial cellulose and gelatin; the sintering aid comprises at least one of magnesium oxide, yttrium oxide, copper oxide, titanium oxide, calcium oxide and silicon oxide; the mass ratio of the ceramic powder to the binder A to the sintering aid to the water is 15-30: 1 to 3:0 to 2: 80-100, wherein the ball milling time is 12-24 hours;
the binder B comprises at least one of agarose, gelatin, cellulose and chitosan; the surfactant comprises at least one of span-40, span-80, tween-40, tween-80, cetyl trimethyl ammonium bromide and sodium dodecyl sulfate; the organic solvent comprises at least one of n-hexane, cyclohexane and diethyl succinate;
after the ceramic emulsion is added into the cross-linking agent solution, separation treatment is carried out, and the ceramic microsphere is obtained and comprises the following steps:
after the ceramic emulsion is dripped into the cross-linking agent solution, spherical sediment is separated out and washed;
freeze-drying the washed spherical precipitate to obtain ceramic microspheres with uneven particle size distribution ratio;
classifying and sieving the ceramic microspheres with uneven particle size distribution proportion to obtain ceramic microspheres with even particle size distribution proportion, so that the finally obtained ceramic-metal composite material has an even pearl-like layered structure;
wherein the cross-linking agent comprises at least one of nickel ethoxide and calcium ethoxide, and the concentration range of the cross-linking agent solution is 0.008 g/mL-0.01 g/mL;
the ceramic microsphere is added into a solution of metal salt for surface modification treatment, and after precipitation reaction, the ceramic-metal precursor composite microsphere is obtained, and the method comprises the following steps:
dispersing the ceramic microspheres into the solution of the metal salt to obtain ceramic microsphere metal salt dispersion;
slowly dropwise adding an ammonium bicarbonate solution into the ceramic microsphere metal salt dispersion liquid to obtain a ceramic microsphere metal salt precipitate;
adding the binder A into the ceramic microsphere metal salt precipitate, uniformly stirring, and drying to obtain ceramic-metal precursor composite microspheres;
wherein the metal salt comprises at least one metal salt with ductility and a melting point of 1400 ℃ or higher, the concentration range of the solution of the metal salt is 0.1 mol/L-0.15 mol/L, and the concentration range of the ammonium bicarbonate solution is 0.1 mol/L-0.15 mol/L;
wherein the metal salt comprises at least one of ferric salt, nickel salt and cobalt salt;
the ceramic-metal precursor composite material blank is reduced and then sintered to obtain the ceramic-metal composite material, which comprises the following steps:
introducing air into the ceramic-metal precursor composite material blank at a certain temperature to remove organic matters;
introducing hydrogen and argon into the ceramic-metal precursor composite material blank body from which the organic matters are removed, so as to reduce the surface of the ceramic-metal precursor composite material blank body to obtain a metal simple substance;
sintering the ceramic-metal precursor composite material blank after the reduction treatment under the protection of inert gas to obtain a ceramic-metal composite material;
wherein the temperature range at a certain temperature is 500-900 ℃, and the time range of air ventilation is 1-4 hours; the time range of introducing hydrogen and argon is 1-4 hours; the temperature range of the sintering treatment is 1300-1500 ℃ and the pressure range is 2-10 kN;
wherein the temperature holding time of the sintering treatment is 5 minutes to 30 minutes.
2. The method according to claim 1, wherein the pressure of the hot pressing treatment is in the range of 2kN to 10kN in the hot pressing treatment of the ceramic-metal precursor composite microsphere.
3. The method of claim 1, further comprising the step of obtaining the binder B by:
uniformly stirring the adhesive B and water under the water bath condition to obtain the adhesive B;
wherein the temperature range of the water bath condition is 50-95 ℃, and the stirring time range of the water bath condition is 1-3 hours; the concentration range of the binder B is 0.01 g/mL-0.05 g/mL.
4. A ceramic-metal composite material produced by the production method according to any one of claims 1 to 3.
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| WO2015079035A1 (en) * | 2013-11-29 | 2015-06-04 | Sandvik Intellectual Property Ab | A method of making a powder composition for production of a cubic boron nitride composite material |
| CN107326211A (en) * | 2017-07-13 | 2017-11-07 | 吉林大学 | A kind of high body part ceramet laminar composite and preparation method thereof |
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