CN105541326B - Zirconia ceramics method for preparing slices - Google Patents
Zirconia ceramics method for preparing slices Download PDFInfo
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- CN105541326B CN105541326B CN201510981527.1A CN201510981527A CN105541326B CN 105541326 B CN105541326 B CN 105541326B CN 201510981527 A CN201510981527 A CN 201510981527A CN 105541326 B CN105541326 B CN 105541326B
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- Prior art keywords
- oxide powder
- powder
- zirconia ceramics
- solvent
- tetragonal phase
- Prior art date
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 168
- 239000000919 ceramic Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 170
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 42
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002002 slurry Substances 0.000 claims abstract description 37
- 239000002904 solvent Substances 0.000 claims abstract description 37
- 239000011812 mixed powder Substances 0.000 claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 15
- 238000002604 ultrasonography Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 13
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910001940 europium oxide Inorganic materials 0.000 claims description 6
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 6
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 6
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 6
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 6
- 229940075630 samarium oxide Drugs 0.000 claims description 6
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 6
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 6
- 229910003451 terbium oxide Inorganic materials 0.000 claims description 6
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims description 6
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 6
- 229940075624 ytterbium oxide Drugs 0.000 claims description 6
- UPEMFLOMQVFMCZ-UHFFFAOYSA-N [O--].[O--].[O--].[Pm+3].[Pm+3] Chemical compound [O--].[O--].[O--].[Pm+3].[Pm+3] UPEMFLOMQVFMCZ-UHFFFAOYSA-N 0.000 claims description 5
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 claims description 5
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 5
- 229940075613 gadolinium oxide Drugs 0.000 claims description 5
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 5
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 229960002415 trichloroethylene Drugs 0.000 claims description 4
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 238000005336 cracking Methods 0.000 description 7
- -1 for example Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 4
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000009514 concussion Effects 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical class CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- LJRSZGKUUZPHEB-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxypropoxy)propoxy]propyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COC(C)COC(=O)C=C LJRSZGKUUZPHEB-UHFFFAOYSA-N 0.000 description 1
- RIWRBSMFKVOJMN-UHFFFAOYSA-N 2-methyl-1-phenylpropan-2-ol Chemical compound CC(C)(O)CC1=CC=CC=C1 RIWRBSMFKVOJMN-UHFFFAOYSA-N 0.000 description 1
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- SHPBBNULESVQRH-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[Zr+4] Chemical compound [O-2].[O-2].[Ti+4].[Zr+4] SHPBBNULESVQRH-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QDHUQRBYCVAWEN-UHFFFAOYSA-N amino prop-2-enoate Chemical class NOC(=O)C=C QDHUQRBYCVAWEN-UHFFFAOYSA-N 0.000 description 1
- 230000002968 anti-fracture Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 229940106691 bisphenol a Drugs 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229940075616 europium oxide Drugs 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036651 mood Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
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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
- C04B35/632—Organic additives
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- 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
- C04B35/622—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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F120/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
A kind of zirconia ceramics method for preparing slices, includes the following steps：There is provided and stablize tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersant, ultraviolet initiator, photosensitive polymerization monomer and auxiliary agent；Tetragonal phase zirconium oxide powder, RE oxide powder and solvent are mixed, and carries out ultrasound and breaks up reunion operation, then is evaporated operation and removes solvent, obtains mixed powder；After mixed powder, dispersant, ultraviolet initiator, photosensitive polymerization monomer and auxiliary agent are mixed, ball milling and de-bubble operation are carried out, obtains zirconia ceramics slurry；Zirconia ceramics slurry is added into ceramic casting machine, then will carry zirconia ceramics slurry ceramic casting machine substrate by uv cure machine after, formed zirconia ceramics thin slice green compact；After zirconia ceramics thin slice green compact are sintered, zirconia ceramics thin slice is obtained.Above-mentioned preparation method can exempt traditional drying process, it is ensured that the product quality being prepared is more preferably.
Description
Technical field
The present invention relates to zirconia ceramics applied technical field, more particularly to a kind of zirconia ceramics thin slice preparation side
Method.
Background technology
At present, zirconia ceramics in industrial civil field using increasingly extensive, due to zirconia ceramics can in intensity and
Used under the high environmental condition of toughness reguirements, therefore, zirconia ceramics be often used in manufacture thin slice, substrate, pad or other
The less sheet material of thickness.
These sheet materials act not only as structure member use, are such as applied to craftwork and mechanical part field, and
Also it is incorporated in extensively in the electronic component of electronic equipment microminaturization, e.g., plate type oxygen sensor and circuit board substrate etc., and
In super large-scale integration, therefore, these zirconia ceramics sheet materials have boundless application prospect.
However, existing zirconia ceramics sheet manufacturing process, e.g., isostatic pressing, compression molding, injection moulding or solidifying
The step for glue casting is needed by drying in the preparation, i.e., in advance do zirconia ceramics green compact using drying box
It is dry to carry out crystallization operation, for follow-up sintering, still, since zirconia ceramics sheet material has the thickness lighter in structure
Characteristic thin, area is larger, surface is more smooth, it is easy in the drying process there arises a problem that：
1st, the green compact cracking phenomena that partially or fully surface is triggered because dry excessive, i.e. there is slight crack in surface；
2nd, there is excess shrinkage in dried green compact, can not meet the needs of near net-shape；
3rd, sinter after partial structurtes loosely；And other it is various the problem of, cause its sinter after quality do not reach
Industry requirement.When especially preparing ultra-thin zirconia ceramics sheet material, the defects of existing zirconia ceramics sheet manufacturing process more
It is prominent.
The content of the invention
Based on this, it is necessary to which providing a kind of can exempt drying process and the product being prepared more meets industry product
The zirconia ceramics method for preparing slices of matter demand.
A kind of zirconia ceramics method for preparing slices, includes the following steps：
There is provided and stablize tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersant, ultraviolet initiator, photosensitive
Polymerized monomer and auxiliary agent；
The tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed, and carries out ultrasound and beats
Operation of reuniting is dissipated, then is evaporated operation and removes the solvent, obtains mixed powder；
By the mixed powder, the dispersant, the ultraviolet initiator, the photosensitive polymerization monomer and the auxiliary agent
After being mixed, ball milling and de-bubble operation are carried out, obtains zirconia ceramics slurry；
The zirconia ceramics slurry is added into ceramic casting machine, then the zirconia ceramics slurry will be carried
After the substrate of ceramic casting machine is by uv cure machine, the life of zirconia ceramics thin slice is formed on the substrate of ceramic casting machine
Base；
After the zirconia ceramics thin slice green compact are sintered, the zirconia ceramics thin slice is obtained.
In one of the embodiments, by the tetragonal phase zirconium oxide powder, the RE oxide powder and described molten
When agent mixes, carry out ultrasound every preset time and break up reunion operation.
In one of the embodiments, the preset time is 5 seconds~10 seconds.
In one of the embodiments, the preset time is 7 seconds~10 seconds.
In one of the embodiments, the preset time is 8 seconds.
In one of the embodiments, by the tetragonal phase zirconium oxide powder, the RE oxide powder and described molten
In the operation of agent mixing, using magnetic agitation married operation.
In one of the embodiments, by the tetragonal phase zirconium oxide powder, the RE oxide powder and described molten
In the operation of agent mixing, specifically comprise the following steps：After the RE oxide powder is mixed with the solvent in advance, then add
Enter the tetragonal phase zirconium oxide powder.
Above-mentioned zirconia ceramics method for preparing slices realizes that in-situ solidifying is imitated using ultraviolet light-initiated cross-linking and curing reaction
Fruit, so as to exempt traditional drying process, so as to avoid the surface of green compact from showing because of dry cracking that is excessive and triggering
As excess shrinkage occur in, dried green compact, can not meet partial structurtes after the needs of near net-shape and sintering loosely
Problem, and then may insure the product quality being prepared more preferably, reach industry requirement.
Brief description of the drawings
Fig. 1 is the flow chart of the zirconia ceramics method for preparing slices of an embodiment.
Embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below in conjunction with the accompanying drawings to the present invention
Embodiment be described in detail.Many details are elaborated in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Referring to Fig. 1, the zirconia ceramics method for preparing slices of an embodiment includes the following steps：
S110：There is provided and stablize tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersant, ultraviolet light-initiated
Agent, photosensitive polymerization monomer and auxiliary agent.
In one embodiment, the D50 (median particle diameter) of the stable tetragonal phase zirconium oxide powder is 0.5 μm~2.5 μm, is adopted
Scattered zirconia ceramic slurry evenly can be prepared with the stabilization tetragonal phase zirconium oxide powder of above-mentioned median particle diameter,
So that the mechanical performance for the zirconia ceramics thin slice being prepared is more preferably, especially ultra-thin zirconia ceramics thin slice is such as thick
Spend the zirconia ceramics thin slice for 0.1~0.8mm, its mechanical performance more preferably, such as toughness, it is anti-fracture performance and hardness more preferably, and
Surface smoothness is also more preferably.
In one embodiment, the RE oxide powder includes yttrium oxide powder and other auxiliary rareearth oxidate powders
Body, for example, the stable tetragonal phase zirconium oxide powder, the yttrium oxide powder and other described auxiliary RE oxide powders
Mass ratio be (85~95)：(2~15)：(0.5~10), it is preferred that the stable tetragonal phase zirconium oxide powder, the oxidation
The mass ratio of yttrium powder body and other auxiliary RE oxide powders is 90：7：0.5, in this way, by stablizing four described
Square phase zircite powder adulterates the RE oxide powder, can further improve the mechanicalness of the zirconia ceramics thin slice
Can, moreover, it is also possible in follow-up sintering process, suppress growing up for crystal grain, crystal grain is tiny, consistency so as to obtain
The zirconia ceramics thin slice high, electric property is good.
Further, other described auxiliary RE oxide powders include lanthanum oxide powder, cerium oxide powder, praseodymium oxide powder
Body, neodymia powder, promethium oxide powder, samarium oxide powder, europium oxide powder, gadolinium oxide powder, terbium oxide powder, dysprosia powder
Body, holimium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, luteium oxide powder, scandium oxide powder, for example, oxygen
Change lanthanum powder, cerium oxide powder, praseodymium oxide powder, neodymia powder, promethium oxide powder, samarium oxide powder, europium oxide powder, oxygen
Change gadolinium powder, terbium oxide powder, dysprosia powder, holimium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, oxygen
Change lutetium powder, the mass ratio of scandium oxide powder is (1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1
~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~1.5)：(1~
1.5)：(1~1.5)：(1~1.5), it is preferred that lanthanum oxide powder, cerium oxide powder, praseodymium oxide powder, neodymia powder, oxygen
Change promethium powder, samarium oxide powder, europium oxide powder, gadolinium oxide powder, terbium oxide powder, dysprosia powder, holimium oxide powder, oxygen
It is 1.5 to change erbium powder, thulium oxide powder, ytterbium oxide powder, luteium oxide powder, the mass ratio of scandium oxide powder：1：1.5：1：1：
1.5：1.5：1：1.5：1：1：1.5：1.5：1：1.5：1, in this way, being more advantageous in follow-up sintering process, suppress crystal grain
Grow up, so as to obtain the zirconia ceramics thin slice that crystal grain is tiny, consistency is high, electric property is good.
It should be noted that the rare earth oxide refers to 15 kinds of group of the lanthanides members that period of element atom ordinal number is 57 to 71
Plain oxide, and the oxide of the scandium similar to lanthanide series chemical property (Sc) and yttrium (Y) totally 17 kinds of elements.It is i.e. described dilute
Native oxide includes lanthana, cerium oxide, praseodymium oxide, neodymia, promethium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, oxygen
Change dysprosium, holimium oxide, erbium oxide, thulium oxide, ytterbium oxide, luteium oxide, scandium oxide and yittrium oxide.
S120：The tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed, then steamed
Hair operation removes the solvent, obtains mixed powder.
In one embodiment, the relatively low solvent of boiling point is chosen.For example, the solvent includes binary azeotropic mixed solvent, institute
It is molten including ethanol/methyl ethyl ketone binary azeotropic mixed solvent, ethanol/trichloro ethylene binary azeotropic mixing to state binary azeotropic mixed solvent
At least one of agent, trichloro ethylene/methyl ethyl ketone binary azeotropic mixed solvent.For example, the binary azeotropic mixed solvent is second
Alcohol/methyl ethyl ketone binary azeotropic mixed solvent, both molar ratios are 1:1.Can be rear using above-mentioned binary azeotropic mixed solvent
In continuous Light Curing, there is low boiling point, easily evaporation to remove, i.e., volatilization is fast, drying time is short, solvent dosage is few, without dry
Dry process, follow-up de-bubble better simply advantage strong to powder wettability.
In addition, the solvent using above-mentioned binary azeotropic mixed solvent can reduce with the tetragonal phase zirconium oxide powder and
The surface tension of the RE oxide powder, so as to improve to the tetragonal phase zirconium oxide powder and the rare-earth oxidation
The wettability of powder.
In one embodiment, the mass ratio of the stable tetragonal phase zirconium oxide powder and the RE oxide powder is
(85~95)：(2.5~25), and for example, the stable tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent
Mass ratio be (85~95)：(2.5~25)：(15~20), it is preferred that the stable tetragonal phase zirconium oxide powder, described dilute
The mass ratio of native oxide powder and the solvent is 90：15：20, in this way, can both cause the stable tetragonal phase zirconium oxide
Powder is mixedly more uniform with the RE oxide powder, so as to get the mixed powder mixedly more uniformly, and
And using the solvent of above-mentioned mass ratio, it is more advantageous to evaporation and removes, obtain the mixed powder of drying.
In one embodiment, the tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed,
And carry out ultrasound and break up reunion operation.It is appreciated that the tetragonal phase zirconium oxide powder and the RE oxide powder are in life
When production or/and storage, reuniting effect can be produced, e.g., after making moist, the effect of its particle aggregation is more obvious, and by described super
Sound breaks up reunion operation, i.e., sends ultrasound to the tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent
Ripple, to break up the reunion bulky grain of the tetragonal phase zirconium oxide powder and the RE oxide powder, is more advantageous to described four
Square phase zircite powder and the RE oxide powder are uniformly mixed, so as to so that the zirconium oxide pottery subsequently obtained
Porcelain slurry mixedly more uniformly, and then can prevent bulky grain of reuniting in the zirconia ceramics slurry, is given birth to avoid influence
The flatness on base surface.
Further, when the tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent being mixed, often
Ultrasound is carried out every preset time and breaks up reunion operation, for example, the preset time is 5 seconds~10 seconds；And for example, the preset time
For 7 seconds~10 seconds, it is preferred that the preset time is 8 seconds, is broken up in this way, " impact type " can be produced to reunion bulky grain
Effect, e.g., " wave " or " intermittent " break up effect so that inside reunion bulky grain or/and outside is rushed be subject to sound wave
Power is hit, " dissipating group " phenomenon occurs, so as to obtain scattered more uniform the tetragonal phase zirconium oxide powder, the rare earth oxygen
Compound powder, and it is also possible that both more uniformly mix.
In one embodiment, the tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed
Operation in, using magnetic agitation married operation；And for example, the magnetic agitation married operation breaks up reunion operation with the ultrasound
It is carried out at the same time, in this way, the reunion that can preferably break up the tetragonal phase zirconium oxide powder and the RE oxide powder is big
Particle, is more advantageous to being uniformly mixed for the tetragonal phase zirconium oxide powder and the RE oxide powder, so as to so that after
The continuous obtained zirconia ceramics slurry is mixedly more uniformly, and then can prevent from reuniting in the zirconia ceramics slurry
Bulky grain, to avoid the flatness of green surface is influenced.
In one embodiment, the evaporation operation is handled using hot wind, in this way, the evaporation behaviour of " intrusive mood " can be carried out
Make, i.e. when the solvent volatilization on the surface of the mixed powder, utilize the gap between the dried mixed powder
Constantly hot wind is blown into the gap, and then preferably it is internally heated, promotes the solvent to volatilize, relative to
The box method of evaporating of traditional drying, uses hot wind processing to be evaporated operation, can improve evaporation efficiency, and in temperature
Relatively low situation can also produce the effect for preferably promoting the solvent volatilization.
Further, the hot wind is exported using multiple hot wind output ports；And for example, multiple hot wind output ports
Rectangular array is arranged；And for example, multiple hot wind output ports are arranged at intervals successively, in this way, covering using distribution and comprehensively
The hot wind processing of lid formula, can further improve evaporation efficiency, and can also be produced in the relatively low situation of temperature and preferably promote institute
State the effect of solvent volatilization.
In one embodiment, the tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed
Operation in, specifically comprise the following steps：After the RE oxide powder is mixed with the solvent in advance, add described
Tetragonal phase zirconium oxide powder, in this way, can prevent both while add the secondary agglomeration problem produced into the solvent, so that
Both powders are made more uniformly to mix.
In one embodiment, handled after carrying out the evaporation operation, also executed the following steps using hot wind：By the mixing
Powder stands cooling under vacuum, in this way, the mixed powder can be prevented while cooling, the vapor adhesion in air exists
On the mixed powder, so as to avoid the problem that condensed water occur in the mixed powder, to ensure the mixed powder
Quality.
In one embodiment, handled after carrying out the evaporation operation, also executed the following steps using hot wind：Carry out smashing behaviour to pieces
Make, and obtain the mixed powder, and for example, after smashing operation to pieces described in progress, be also ground operation, in this way, being beneficial to obtain grain
The uniform mixed powder in footpath.
S130：By the mixed powder, the dispersant, the ultraviolet initiator, the photosensitive polymerization monomer and institute
State after auxiliary agent mixed, carry out ball milling and de-bubble operation, obtain zirconia ceramics slurry.
In one embodiment, the mixed powder, the dispersant, the ultraviolet initiator, the photosensitive polymerization list
The mass ratio of body and the auxiliary agent is (87.5~120)：(15~20)：(10~12)：(4~6)：(27~34), it is and for example, described
Mixed powder, the dispersant, the ultraviolet initiator, the mass ratio of the photosensitive polymerization monomer and the auxiliary agent are (95
~120)：(15~19)：(11~12)：(5~6)：(27~30), it is preferred that the mixed powder, the dispersant, described
The mass ratio of ultraviolet initiator, the photosensitive polymerization monomer and the auxiliary agent is 115：16：11：6：28.
In one embodiment, the dispersant includes at least one of triethanolamine, terpinol and tributyl phosphate, again
Such as, the dispersant is the mixture of triethanolamine, the terpinol and the tributyl phosphate, and for example, in the mixture,
The mass ratio of the triethanolamine, the terpinol and the tributyl phosphate is (1~1.5)：(1~1.5)：(1~1.5),
Preferably, the dispersant is that the mass ratio of triethanolamine, the terpinol and the tributyl phosphate is 1：1.5：1.5, this
Sample, not only can preferably dissolve the mixed powder, the ultraviolet initiator, the photosensitive polymerization using above-mentioned dispersant
Monomer and the auxiliary agent, with obtain mixing evenly, zirconia ceramics slurry described in viscosity smaller and solid content bigger, it is and above-mentioned
With the mixed powder, the ultraviolet initiator, the photosensitive polymerization monomer and the auxiliary agent chemistry will not occur for dispersant
Fang Ying, it is ensured that the stability of the zirconia ceramics slurry.
In one embodiment, the ultraviolet initiator include 2,4,6- trimethylbenzoy-dipheny phosphine oxides and
At least one of 2- hydroxy-2-methyl -1- phenyl -1- acetone, and for example, the ultraviolet initiator are 2,4,6- trimethylbenzenes
The mixture of formoxyl-diphenyl phosphine oxide and 2- hydroxy-2-methyl -1- phenyl -1- acetone, and for example, in the mixture, institute
State the mass ratio of 2,4,6- trimethylbenzoy-dipheny phosphine oxides and the 2- hydroxy-2-methyls -1- phenyl -1- acetone
For (1~1.5)：(1~1.5), it is preferred that described 2,4,6- trimethylbenzoy-dipheny phosphine oxides and the 2- hydroxyls-
The mass ratio of 2- methyl isophthalic acids-phenyl -1- acetone is 1.5：1.
Wherein, the molecular structural formula of 2,4,6- trimethylbenzoy-dipheny phosphine oxides (DAROCUR TPO) is as follows：
Wherein, the molecular structural formula of 2- hydroxy-2-methyls -1- phenyl -1- acetone (DAROCUR 1173) is as follows：
In one embodiment, the photosensitive polymerization monomer includes methacrylic acid -2- hydroxy methacrylates, bisphenol-A epoxy propylene
In acid esters, urethane acrylate, amino acrylates, tri (propylene glycol) diacrylate and hydroxypropyl acrylate at least
It is a kind of.
Further, the ultraviolet initiator and the photosensitive polymerization monomer are using following compounding mode, it is for described
Zirconia ceramics slurry, which forms green compact, has fabulous in-situ solidifying effect, that is, is beneficial to whole groups of the zirconia ceramics slurry
Point carry out in-situ solidifying technique, to quickly complete shaping, can directly demould and without time-consuming complicated drying process, can be with
Dry contraction and cracking phenomena are avoided, improves production yield rate, for example, 2,4,6- trimethylbenzoy-dipheny phosphine oxides,
The mass ratio of 2- hydroxy-2-methyl -1- phenyl -1- acetone and methacrylic acid -2- hydroxy methacrylates is (1~1.5)：(1~
1.5)：(0.7~1.2), it is preferred that 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2- hydroxy-2-methyl -1- benzene
The mass ratio of base -1- acetone and methacrylic acid -2- hydroxy methacrylates is 1.5：1：0.7, in-situ solidifying be able to can be played compared with
Good facilitation effect.
In one embodiment, the auxiliary agent includes binding agent and plasticiser, for example, the binding agent includes polyacrylic acid first
At least one of fat and ethyl cellulose, in this way, can be in follow-up tape casting operation by adding the binding agent, it is ensured that
The zirconia ceramics slurry has suitable thermoplasticity, preferable dimensional stability and higher tensile strength, so as to
So that the tape casting operation carry out it is more smooth.And for example, the plasticiser includes diethyl oxalate ester, trietbhlene glycol
At least one of hexane dibutyl phthalate, dioctyl phthalate and polyethylene glycol.
Further, it is higher to ensure to have in order to strengthen the viscous holding force in the zirconia ceramics slurry between each component
Tensile strength and preferable dimensional stability, for example, the auxiliary agent further includes tackifying resin, the tackifying resin includes single third
At least one of olefin(e) acid resin and aliphatic polyurethane acrylic resin, in this way, the zirconium oxide pottery can be further enhanced
Viscous holding force in porcelain slurry between each component, to ensure there is higher tensile strength and preferable dimensional stability.Need
Bright, single acrylic resin and aliphatic polyurethane acrylic resin has the advantages that low viscosity and high viscous holding force, is increasing
While the zirconia ceramics slurry viscous holding force, it may also be ensured that the zirconia ceramics slurry has low viscosity, stream
The advantages of moving good property and high solids content.
In one embodiment, wherein, the de-bubble operation carries out under vacuum；And for example, the de-bubble operation uses
Concussion is handled；And for example, the de-bubble operation is using concussion up and down and left and right concussion alternate treatment, in this way, de-bubble effect can be improved
Fruit.
In one embodiment, the ball milling operation is operated using wet ball grinding；And for example, the ball milling operation uses titanium dioxide
Zirconium ball in this way, being conducive to improve the mixture homogeneity of the zirconia ceramics slurry, and will not introduce new as ball-milling medium
Impurity.
S140：The zirconia ceramics slurry is added into ceramic casting machine, then the zirconia ceramics will be carried
After the substrate of the ceramic casting machine of slurry is by uv cure machine, it is thin that zirconia ceramics is formed on the substrate of ceramic casting machine
Piece green compact.
By adding the zirconia ceramics slurry into ceramic casting machine, ceramic casting machine can make pottery the zirconium oxide
Porcelain slurry is cast in the ceramic casting machine substrate of itself, and e.g., ceramic casting machine has a substrate, i.e., substrate be ceramic casting machine from
The component of body, in this way, the zirconia ceramics slurry can be divided on the substrate of ceramic casting machine, and then will carrying
After having the substrate of the ceramic casting machine of the zirconia ceramics slurry by uv cure machine, uv cure machine is flowed to ceramics
Prolong the zirconia ceramics slurry emitting ultraviolet light line on the substrate of machine, under the irradiation of ultraviolet light, the ultraviolet initiator
It can trigger the photosensitive polymerization monomer that UV crosslinking curing reaction occurs, i.e. in-situ solidifying reacts, in this way, can quickly complete into
Type, can directly demould without time-consuming complicated drying process, can improve production to avoid dry contraction and cracking phenomena
Yield rate.That is, realizing in-situ solidifying effect using ultraviolet light-initiated cross-linking and curing reaction, traditional do can be exempted
Drying process, so as to avoid the surface of green compact from occurring excessively because of dry cracking phenomena, dried green compact excessive and trigger
Shrink, can not meet the problem of partial structurtes are loosely after the needs of near net-shape and sintering, product that it is prepared
Quality more preferably, reaches industry requirement.
In one embodiment, the zirconia ceramics slurry is heated to 50 DEG C~60 DEG C in advance, and while hot by the oxygen
Change zircon ceramic slurry add into ceramic casting machine, in this way, by advance by the zirconia ceramics slurry be heated to 50 DEG C~
60 DEG C, it can be ensured that the mobility of the zirconia ceramics slurry reaches the required requirement of curtain coating, i.e., in the same of high solids content
When be ensured that low viscosity.
In one embodiment, the uv cure machine is provided with the sequentially connected first default walking path, second pre-
If walking path, the 3rd default walking path, fourth line walk path and fifth line walks path, the described first default walking path,
Described second default walking path, the 3rd default walking path, the fourth line walks path and the fifth line walks path
Linear speed be sequentially increased, for example, the described first default walking path, the second default walking path, the 3rd default row
Walk path, the fourth line walks path and the fifth line walk path linear speed difference 10m/min~15m/min, 8m/min~
10m/min, 6m/min~8m/min, 4m/min~6m/min and 1m/min~2m/min, wherein, m/min expressions m/min, i.e.,
The linear speed unit that the substrate of the ceramic casting machine of the zirconia ceramics slurry is walked on uv cure machine is carried, into one
Step, the described first default walking path, the second default walking path, the 3rd default walking path, the described 4th
The ultraviolet light intensity that walking path and the fifth line walk path is respectively 260mw/cm2~320mw/cm2、350mw/cm2
~380mw/cm2、380mw/cm2~400mw/cm2、400mw/cm2~420mw/cm2And 450mw/cm2~500mw/cm2, this
Sample, using above-mentioned linear speed and ultraviolet light intensity, can be conducive to zirconia ceramics thin slice green compact and carry out in-situ solidifying reaction,
And the problem of excessive brittleness and cracking will not be produced.
S150：After the zirconia ceramics thin slice green compact are sintered, the zirconia ceramics thin slice is obtained.
After the zirconia ceramics thin slice green compact are sintered, the organic matter in it can be removed, and then obtain
The zirconia ceramics thin slice.
In one embodiment, the step of zirconia ceramics thin slice green compact are sintered, is as follows：Risen at 0 DEG C~120 DEG C
Warm speed is 0.5 DEG C/min, and heating rate is 0.4 DEG C/min between 120 DEG C~550 DEG C, and heating rate is between 550 DEG C~800 DEG C
0.5 DEG C/min, to ensure that various organic matters are all excluded without speed is too fast to be made because excluding in the zirconia ceramics thin slice
Into defect.Preferably, more than 800 DEG C 1450 DEG C are raised to respectively with the heating rate of 2 DEG C/min, 1500 DEG C, 1550 DEG C, and
At 1450 DEG C, 1500 DEG C, 1550 DEG C keep the temperature 5h, 3h, 2h respectively, so, it can be ensured that the quality of the zirconia ceramics thin slice.
For example, when at 1450 DEG C, insulation 5 is small, when at 1500 DEG C, insulation 3 is small, when at 1550 DEG C, insulation 2 is small.
Above-mentioned zirconia ceramics method for preparing slices realizes that in-situ solidifying is imitated using ultraviolet light-initiated cross-linking and curing reaction
Fruit, so as to exempt traditional drying process, so as to avoid the surface of green compact from showing because of dry cracking that is excessive and triggering
As excess shrinkage occur in, dried green compact, can not meet partial structurtes after the needs of near net-shape and sintering loosely
Problem, and then may insure the product quality being prepared more preferably, reach industry requirement.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (7)
1. a kind of zirconia ceramics method for preparing slices, it is characterised in that include the following steps：
There is provided and stablize tetragonal phase zirconium oxide powder, RE oxide powder, solvent, dispersant, ultraviolet initiator, photosensitive polymerization
Monomer and auxiliary agent；Wherein, the D50 of the stable tetragonal phase zirconium oxide powder is 0.5 μm~2.5 μm；
The tetragonal phase zirconium oxide powder, the RE oxide powder and the solvent are mixed, and carries out ultrasound and breaks up group
Poly- operation, then be evaporated operation and remove the solvent, obtain mixed powder；Wherein, the relatively low solvent of boiling point is chosen；It is described
Solvent includes binary azeotropic mixed solvent, the binary azeotropic mixed solvent include ethanol/methyl ethyl ketone binary azeotropic mixed solvent,
At least one of ethanol/trichloro ethylene binary azeotropic mixed solvent, trichloro ethylene/methyl ethyl ketone binary azeotropic mixed solvent；Institute
Stating RE oxide powder includes yttrium oxide powder and other auxiliary RE oxide powders, the stable tetragonal phase zirconium oxide
The mass ratio of powder, the yttrium oxide powder and other auxiliary RE oxide powders is 90：7：0.5；It is described other
Aid in RE oxide powder include lanthanum oxide powder, cerium oxide powder, praseodymium oxide powder, neodymia powder, promethium oxide powder,
Samarium oxide powder, europium oxide powder, gadolinium oxide powder, terbium oxide powder, dysprosia powder, holimium oxide powder, erbium oxide powder,
Thulium oxide powder, ytterbium oxide powder, luteium oxide powder and scandium oxide powder；The lanthanum oxide powder, the cerium oxide powder, institute
State praseodymium oxide powder, the neodymia powder, the promethium oxide powder, the samarium oxide powder, the europium oxide powder, described
Gadolinium oxide powder, the terbium oxide powder, the dysprosia powder, the holimium oxide powder, the erbium oxide powder, the oxygen
The mass ratio for changing thulium powder, the ytterbium oxide powder, the luteium oxide powder and the scandium oxide powder is 1.5：1：1.5：1：
1：1.5：1.5：1：1.5：1：1：1.5：1.5：1：1.5：1；By the mixed powder, dispersant, described ultraviolet light-initiated
After agent, the photosensitive polymerization monomer and the auxiliary agent are mixed, ball milling and de-bubble operation are carried out, obtains zirconia ceramics slurry
Material；
The zirconia ceramics slurry is added into ceramic casting machine, then the ceramics that the zirconia ceramics slurry will be carried
After the substrate of casting machine is by uv cure machine, zirconia ceramics thin slice green compact are formed on the substrate of ceramic casting machine；
After the zirconia ceramics thin slice green compact are sintered, the zirconia ceramics thin slice is obtained.
2. zirconia ceramics method for preparing slices according to claim 1, it is characterised in that by the tetragonal phase zirconium oxide
When powder, the RE oxide powder and the solvent mix, carry out ultrasound every preset time and break up reunion operation.
3. zirconia ceramics method for preparing slices according to claim 2, it is characterised in that the preset time is 5 seconds
~10 seconds.
4. zirconia ceramics method for preparing slices according to claim 3, it is characterised in that the preset time is 7 seconds
~10 seconds.
5. zirconia ceramics method for preparing slices according to claim 4, it is characterised in that the preset time is 8 seconds.
6. zirconia ceramics method for preparing slices according to claim 1, it is characterised in that by the tetragonal phase zirconium oxide
In the operation of powder, the RE oxide powder and solvent mixing, using magnetic agitation married operation.
7. zirconia ceramics method for preparing slices according to claim 1, it is characterised in that by the tetragonal phase zirconium oxide
In the operation of powder, the RE oxide powder and solvent mixing, specifically comprise the following steps：In advance by the rare earth
After oxide powder is mixed with the solvent, the tetragonal phase zirconium oxide powder is added.
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| US4957673A (en) * | 1988-02-01 | 1990-09-18 | California Institute Of Technology | Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof |
| CN101541708A (en) * | 2006-11-29 | 2009-09-23 | 康宁股份有限公司 | Plasticized mixture and method for stiffening |
| CN104788096A (en) * | 2015-03-31 | 2015-07-22 | 北京博曼迪汽车科技有限公司 | Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor |
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| US4957673A (en) * | 1988-02-01 | 1990-09-18 | California Institute Of Technology | Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof |
| CN101541708A (en) * | 2006-11-29 | 2009-09-23 | 康宁股份有限公司 | Plasticized mixture and method for stiffening |
| CN104788096A (en) * | 2015-03-31 | 2015-07-22 | 北京博曼迪汽车科技有限公司 | Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor |
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