CN105819868A - Gel casting method for free radical system - Google Patents
Gel casting method for free radical system Download PDFInfo
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- CN105819868A CN105819868A CN201610165408.3A CN201610165408A CN105819868A CN 105819868 A CN105819868 A CN 105819868A CN 201610165408 A CN201610165408 A CN 201610165408A CN 105819868 A CN105819868 A CN 105819868A
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- slurry
- alcohol
- linking agent
- inhibition reagent
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- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000005266 casting Methods 0.000 title claims abstract description 21
- 150000003254 radicals Chemical class 0.000 title claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 60
- 239000000178 monomer Substances 0.000 claims abstract description 38
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 36
- 230000005764 inhibitory process Effects 0.000 claims abstract description 35
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 claims abstract description 10
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 claims abstract description 10
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims abstract description 8
- KJIOQYGWTQBHNH-UHFFFAOYSA-N undecanol Chemical compound CCCCCCCCCCCO KJIOQYGWTQBHNH-UHFFFAOYSA-N 0.000 claims abstract description 8
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 4
- 125000001165 hydrophobic group Chemical group 0.000 claims abstract description 4
- 229940057402 undecyl alcohol Drugs 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000004094 surface-active agent Substances 0.000 claims abstract 2
- 239000003999 initiator Substances 0.000 claims description 24
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- WGLLSSPDPJPLOR-UHFFFAOYSA-N 2,3-dimethylbut-2-ene Chemical group CC(C)=C(C)C WGLLSSPDPJPLOR-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 4
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- UMSVPCYSAUKCAZ-UHFFFAOYSA-N propane;hydrochloride Chemical compound Cl.CCC UMSVPCYSAUKCAZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 3
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 3
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 3
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 3
- FLCAEMBIQVZWIF-UHFFFAOYSA-N 6-(dimethylamino)-2-methylhex-2-enamide Chemical compound CN(C)CCCC=C(C)C(N)=O FLCAEMBIQVZWIF-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical compound [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 229920001427 mPEG Polymers 0.000 claims description 3
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 3
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims description 3
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001409 amidines Chemical class 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 13
- 239000010410 layer Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000006116 polymerization reaction Methods 0.000 abstract description 6
- 239000002344 surface layer Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 235000015895 biscuits Nutrition 0.000 description 21
- 238000007711 solidification Methods 0.000 description 12
- 230000008023 solidification Effects 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 239000007787 solid Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 238000001746 injection moulding Methods 0.000 description 7
- 229920001223 polyethylene glycol Polymers 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- GIEMHYCMBGELGY-UHFFFAOYSA-N 10-undecen-1-ol Chemical compound OCCCCCCCCCC=C GIEMHYCMBGELGY-UHFFFAOYSA-N 0.000 description 3
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- -1 reuse Substances 0.000 description 3
- YYPNJNDODFVZLE-UHFFFAOYSA-N 3-methylbut-2-enoic acid Chemical compound CC(C)=CC(O)=O YYPNJNDODFVZLE-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NDAJNMAAXXIADY-UHFFFAOYSA-N 2-methylpropanimidamide Chemical compound CC(C)C(N)=N NDAJNMAAXXIADY-UHFFFAOYSA-N 0.000 description 1
- BTYIFQSAIPDZQW-UHFFFAOYSA-N 2-propan-2-yl-4,5-dihydro-1h-imidazole Chemical compound CC(C)C1=NCCN1 BTYIFQSAIPDZQW-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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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
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention relates to a gel casting method for a free radical system.The method comprises the steps that slurry containing water, a dispersing agent, organic monomers, a cross-linking agent and ceramic powder is prepared; after an initiating agent is added into the slurry, the mixture is stirred, defoamed and injected into a mold, the surface of the slurry is covered with an anti-surface polymerization inhibition reagent, and then curing is conducted, wherein C5-C11 monohydric alcohol which has hydrophilic groups and hydrophobic chains and achieves the effect of a surfactant is adopted as the anti-surface polymerization inhibition reagent, the hydrophilic groups directly make contact with ceramic slurry, the hydrophobic groups tend to spread in air to form a film layer on the surface of the slurry to effectively isolate oxygen in the air, and the anti-surface polymerization inhibition reagent is one of or a combination of more than two of n-amyl alcohol, isoamyl alcohol, n-hexyl alcohol, n-heptanol, n-caprylic alcohol, n-nonyl alcohol, decanol and undecyl alcohol.Accordingly, the slurry and oxygen in the air can be effectively isolated, and curing of the slurry on the surface layer is guaranteed.
Description
The application is the divisional application of the application for a patent for invention of Application No. 201310190594.2, filing date on May 21st, 2013, invention entitled " a kind of method of free radical system gel casting forming ".
Technical field
A kind of method that the present invention relates to free radical system gel casting forming, is specifically related to a kind of method preventing free radical system gel casting forming pulp surface from inhibiting, and belongs to preparation technology and the application of pottery.
Background technology
Along with the development of modern science and technology, one of advanced technology of preparing emphasis and focus of becoming research of high-performance ceramic parts, particularly large scale, the technology of preparing of complicated shape goods.Ceramic material the most easily produces defect in forming process, and the defect formed often is difficult to be made up by subsequent technique and eliminate.Additionally, the high rigidity of ceramic material, high-wearing feature make following process relatively difficult, processing cost is expensive, and for the goods of complicated shape, processing problems seems particularly troublesome.Therefore forming technique is as a key link in preparation process, directly influences the sintering of material, processing and final performance.
Gel casting forming is a kind of new ceramics forming technique that Oak Ridge National Key Laboratory of the U.S. (OakRidgelaboratory) invented in early 1990s.It is a kind of near-net shape (nearnet-shape) forming method polymer chemistry, collochemistry and ceramic technology combined.The primary raw material that gel injection molding and forming technology uses has solvent, powder body, dispersant, organic monomer, cross-linking agent, initiator, catalyst and plastic agent etc..Its technology key is the stabiliser by the colloid system such as electrostatic stabilization or steric stabilization, prepares and has high solids content, low viscous slurry.This technique includes following process: is first dispersed in by powder body containing in organic monomer and the aqueous solution of cross-linking agent or nonaqueous solvent, adds initiator and catalyst, after stirring and deaerating, injected in mould by slurry before cast.Then under certain temperature conditions, cause organic monomer polymerization, make slurry viscosity abruptly increase, thus cause slurry solidification in situ, form wet base.After the wet base demoulding, it is dried at a certain temperature and humidity conditions, obtains high intensity base substrate, finally by dry body binder removal and sinter, obtain densification or porous member.
Gel injection molding and forming technology has significant advantage compared with other moulding process, and the additive used by this forming method can not have impurities left with all Organic substances after sintering.The green strength of this technological forming is the highest, can directly carry out machining, is a kind of more novel near-net shape in-situ solidifying forming technique, can make high-quality, complex-shaped parts.Provide effective method and approach for solving material molding and a processing difficult problem, thus obtained paying close attention to widely and obtaining significant progress.
Although gel casting forming has been successfully applied to oxide and non-oxide ceramics system, but yet suffers from a series of problem in preparation process.For free radical gel casting forming, directly contact with air due to pulp surface in the curing process, the Free Radical that the oxygen in air can produce with decomposition of initiator, generate stable peroxy radical, stop the generation of monomer polymerization reactions.Therefore, and the slurry of the surface portion of air contact remains in that flow regime because being polymerized, and the slurry of inside enters because of no oxygen, can be with normal cure.So, after solidification, biscuit surface forms one layer of uncured layer.It is dried rear surface uncured layer and is susceptible to cracking, and bottom normal cure part is layered, it is impossible to keep integrity and the complicated shape of sample.Traditional solution mainly has two kinds, and one is the evacuation when solidification, removes oxygen, it is to avoid oxygen causes surface to inhibit.Or it is passed through the noble gases such as nitrogen after evacuation, blanket of nitrogen solidifies (Jung-SooHa, EffectofatmospheretypeongelcastingbehaviorofAl2O3Andevaluationofgreenstrength, CeramicsInternational26 (2000) 251-254).But, this curing mode is due to needs vacuum equipment and noble gas, and not only equipment is complicated, poor operability, and relatively costly.It is unfavorable for industrialized production.Another kind of scheme is to add other chemical reagent, and such as Polyethylene Glycol, (Ceramic gel casting is selected the inhibitory action research of surface peeling by Li Fei, Zhai Changsheng, Wang Jun, Sun Baode, PEG.nullMaterial Leader，18[9]86-88(2004))，Polyvinyl pyrrolidone (JingtaoMa,ZhipengXie,HezhuoMiao,LongjieZhou,andYongHuang,YibingCheng,Eliminationofsurfacespallationofaluminagreenbodiespreparedbyacrylamide-basedgelcastingviapoly(vinylpyrrolidone),JournaloftheAmericanCeramicSociety,86 [2] 266-272 (2003)) etc..Such as Chinese patent CN1092168C discloses the non-oxygen polymerization-inhibiting gel injection process for preparing of a kind of ceramic component, by adding the water soluble polymer such as polyvinyl pyrrolidone, polyvinyl alcohol in monomer premixed liquid, it is possible to avoid the inhibition that in air, monomer is polymerized by oxygen.But, there is impact for composition, solid content and the gelation process of slurry in additive, is unfavorable for the control of gel injection molding and forming technology.The most unfavorable for follow-up unsticking and sintering.
Summary of the invention
The surface inhibition problem existed for above-mentioned free radical gel casting forming system, it is an object of the invention to propose the reagent system of a kind of resistance to surface inhibition, can cover in pulp surface, oxygen in air-isolation, guarantee that biscuit surface can be with normal cure, a kind of resistance to surface inhibition reagent directly covering in pulp surface and having no significant effect radically curing process is i.e. provided, it is thus possible to the oxygen being effectively isolated in slurry and air, guarantee that surface layer slurry can normal cure, it is to avoid the surface inhibition problem occurred in free radical gel casting forming.
Here, a kind of method that the present invention provides free radical system gel casting forming, described method includes: preparation is containing water, ceramic powder, organic monomer, cross-linking agent and the slurry of dispersant；And stir deaeration after described slurry is added initiator and inject mould, covering resistance to surface inhibition reagent on the surface of described slurry and solidify again, wherein said resistance to surface inhibition reagent is C5～C11Alcohol.
According to the present invention; resistance to surface inhibition reagent is at room temperature liquid, and before slurry curing, described resistance to surface inhibition reagent can directly overlay pulp surface and form protective layer; it is thus possible to the oxygen being effectively isolated in slurry and air, it is ensured that the solidification of surface layer slurry.And, this resistance to surface inhibition reagent has no significant effect for radically curing process, to slurry and biscuit without the control of obvious effect, beneficially gel injection molding and forming technology, and also has no significant effect for follow-up unsticking and sintering.Also, after elevated cure, can be reclaimed by this resistance to surface inhibition reagent, reuse, sample surfaces keeps good solid state, can obtain high-quality, without deformation, flawless gel injection-moulding biscuit.Described resistance to surface inhibition reagent adds simple, easily remove and reclaim, can with Reusability and and ceramic size and biscuit without obvious effect, and follow-up biscuit is dried, unsticking and sintering also have no significant effect, technical process is simply, easily operate, thus can effectively reduce the preparation cost of biscuit, for large scale and the sample of complicated shape, have very important significance.
Again, the method of the present invention need not add any auxiliary agent in the slurry, slurry composition and radically curing process will not be produced impact, simple and reliable process, low cost, easily operate, can quickly prepare surface texture high-performance biscuit complete, uniform, be suitable for the water-base gel casting of free radical system.
In the present invention, any one or the two or more combination during described resistance to surface inhibition reagent is preferably n-amyl alcohol, isoamyl alcohol, hexanol, n-heptanol, n-octyl alcohol, n-nonyl alcohol, Decanol and positive undecyl alcohol.
Described resistance to surface inhibition reagent be water-insoluble or close to water-insoluble, density be less than water, can cover in pulp surface, but will not or only pole be diffused into slightly in slurry, will not for slurry composition and radically curing process produce affect.Additionally, described resistance to surface inhibition reagent has hydrophilic group and hydrophobic chain, hydrophilic group directly can contact with ceramic size, and hydrophobic group then tends to stretch in atmosphere, can form a tunic layer, the oxygen being effectively isolated in air in pulp surface.Meanwhile, described resistance to surface inhibition reagent will not be had an effect with free radical, also will not capture free radical.Therefore, this resistance to surface is used to inhibit reagent, it is possible to be effectively formed film layer, it is ensured that the slurry of surface portion can be with normal cure.And after slurry curing, this reagent can simply reclaim, in pulp surface residual seldom.And residue can be removed in biscuit dry run completely, follow-up unsticking and sintering are had no significant effect.
In the present invention, described organic monomer can be acrylic acid, dimethylaminoethyl methacrylate, dimethylamino-propyl Methacrylamide, hydroxy ethyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl acrylate, Hydroxypropyl methacrylate, the monomethacrylates of methoxy poly (ethylene glycol), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacryiamidopropyl trimethyl ammonium chloride, methacrylic acid, Sodium styrene sulfonate, acrylamide, Methacrylamide, N, N-DMAA (DMAA), or vinyl pyrrolidone or their combination in any.
Also, described water is preferably deionized water.Described organic monomer can be 30:100～10:100 with the mass ratio of described water.
Also, described cross-linking agent can include that N, N '-methylene-bisacrylamide (MBAM) and poly-(vinyl alcohol) dimethacrylate [PEG (XXX) DMA] etc. are usually used in the cross-linking agent of gel casting forming.
The mass ratio of wherein said cross-linking agent and described organic monomer can be 1:15～1:1.
Also, described initiator can include that Ammonium persulfate ./tetramethyl-ethylene base diamidogen, azo [2-(2-imidazoline-2-base)] propane hydrochloride salt and azo (2 amidine propane) hydrochlorate etc. are usually used in the initiator of gel casting forming.
The addition of wherein said initiator can be the 1/10～1/20 of described organic monomer.
It is preferred that described solidification can be to solidify 10 minutes～3 hours at 40～80 DEG C.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that following embodiment is merely to illustrate the present invention below in conjunction with following embodiment, and the unrestricted present invention.
The present invention is directed to the surface inhibition problem that free radical gel casting forming system exists, a kind of method proposing free radical system gel casting forming, by introducing a kind of organic reagent, can directly overlay pulp surface, it is effectively isolated the oxygen in slurry and air, it is ensured that the solidification of surface layer slurry.This resistance to surface inhibition reagent has no significant effect for radically curing process.After elevated cure, this resistance to surface inhibition reagent can be reclaimed, reuse.Sample surfaces keeps good solid state.This resistance to surface inhibition reagent adds simple, easily reclaims, and ceramic size and biscuit are without obvious effect, and technical process is simply, easily operate.Thus can effectively reduce the preparation cost of biscuit.For large scale and the sample of complicated shape, have very important significance.
The method comprise the steps that preparation is containing water, ceramic powder, organic monomer, cross-linking agent and the slurry of dispersant；And stir deaeration after described slurry is added initiator and inject mould, covering resistance to surface inhibition reagent on the surface of described slurry and solidify again, wherein said resistance to surface inhibition reagent is C5～C11Alcohol.
Wherein the preparation of slurry can use known method, such as, can be to add ceramic powder in the premixed liquid comprising organic monomer, water, cross-linking agent and dispersant and carry out ball milling thus prepared slurry.
And, described slurry can use the conventional gel casting forming formula reported.Basic composition is: deionized water, ceramic powder, monomer, cross-linking agent, initiator and dispersant.Wherein monomer uses conventional monomer system.Including acrylic acid, dimethylaminoethyl methacrylate, dimethylamino-propyl Methacrylamide, hydroxy ethyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl acrylate, Hydroxypropyl methacrylate, the monomethacrylates of methoxy poly (ethylene glycol), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacryiamidopropyl trimethyl ammonium chloride, methacrylic acid, Sodium styrene sulfonate, acrylamide, Methacrylamide, N,N-DMAA (DMAA) and vinyl pyrrolidone and combinations thereof.The ratio of monomer and deionized water is between 30:100 and 10:100.Cross-linking agent includes N, N '-methylene-bisacrylamide (MBAM) and poly-(vinyl alcohol) dimethacrylate [PEG (XXX) DMA].The mass ratio of cross-linking agent and monomer is between 1:15-1:1.Conventional initiator includes Ammonium persulfate ./tetramethyl-ethylene base diamidogen (APS-TEMED), azo [2-(2-imidazoline-2-base)] propane HCl (azobis{2-(2-imidazolin-2-yl) propane}HCl [AZIP]) and azo (2-amidine propane) HCl (azobis (2-amidinopropane) HCl [AZAP]).Wherein the addition of initiator is the 1/10-1/20 of monomer.It is generally directed to different powder body and can select different dispersants.But the compound method of the slurry of the present invention and formula are not limited to this, gel casting forming slurry preparation method and formula that those skilled in the art commonly use all are contained in the present invention.
In the present invention, the powder body in ceramic size includes but not limited to carbide and the oxides such as aluminium oxide and zirconium oxide such as carborundum, titanium carbide, boron carbide.
The ceramic size prepared is injected in mould, pours C into5～C11Alcohol as resistance to surface inhibition reagent cover solidify again in pulp surface.
Also, any one or two or more combination that described resistance to surface inhibition reagent is preferably in n-amyl alcohol, isoamyl alcohol, hexanol, n-heptanol, n-octyl alcohol, n-nonyl alcohol, Decanol and positive undecyl alcohol.
Specifically, the present invention propose resistance to surface inhibition reagent have the characteristics that.First, this resistance to surface inhibition reagent be water-insoluble or close to water-insoluble, density be less than water, can cover in pulp surface, but will not or only pole be diffused into slightly in slurry, will not for slurry composition and radically curing process produce affect.Additionally, this resistance to surface inhibition reagent has hydrophilic group and hydrophobic chain, hydrophilic group directly can contact with ceramic size, and hydrophobic group then tends to stretch in atmosphere, can form a tunic layer, the oxygen being effectively isolated in air in pulp surface.Meanwhile, this resistance to surface inhibition reagent will not be had an effect with free radical, also will not capture free radical.Therefore, this resistance to surface is used to inhibit reagent, it is possible to be effectively formed film layer, it is ensured that the slurry of surface portion can be with normal cure.And after slurry curing, this reagent can simply reclaim, in pulp surface residual seldom.And residue can be removed in biscuit dry run completely, follow-up unsticking and sintering are had no significant effect.
Also, described solidification can be to solidify 10 minutes～3 hours in 40～80 DEG C of waters bath with thermostatic control.When sample is cooled to room temperature, open mould can get that surface cure is complete, the biscuit of even structure.Described biscuit can carry out dry, unsticking and sintering processes according to existing method.
The resistance to surface inhibition scheme that the present invention proposes, compares with the scheme of document report at present, it is not necessary to add any auxiliary agent in the slurry, slurry composition and radically curing process will not be produced impact.And simple and reliable process, easily operation and recovery, cost is the lowest, it is possible to quickly prepare surface texture high-performance biscuit complete, uniform.The present invention is applicable to the curing molding of water base free radical system gel injection-moulding ceramic size, it is possible to meet the requirement of each side such as industry, Aeronautics and Astronautics and national defence.
Citing embodiment is to describe the present invention in detail further below.It is also understood that; following example are served only for being further described the present invention; and it is not intended that limiting the scope of the invention, some nonessential improvement and adjustment that those skilled in the art makes according to the foregoing of the present invention belong to protection scope of the present invention.Reaction temperature that following example is concrete, time, inventory etc. are the most only examples in OK range, i.e., those skilled in the art can select in the range of being done suitably by explanation herein, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Monomeric acrylamide is dissolved the solution making 15wt% in deionized water, adds cross-linking agent N, N '-methylene-bisacrylamide (MBAM).The ratio of cross-linking agent and monomer is 1:6.It is subsequently adding dispersant Tetramethylammonium hydroxide (TMAH), prepares premixed liquid.Adding silicon carbide powder, ball milling obtains the slurry of solid content about 50vol%, and the viscosity of slurry is at about 300-600mPa.s.Add initiator azo [2-(2-imidazoline-2-base)] propane hydrochloride salt (AZIP 2HCl)), wherein the addition of initiator is the 1/10～1/15 of monomer.Strong agitation deaeration after interpolation.It is poured into the most as required in mould.Pour n-amyl alcohol into and cover pulp surface.Put into 45 degree of solidification 2h in water bath with thermostatic control.Mould is opened when being cooled to room temperature in sample.Obtain that surface cure is complete, the biscuit of even structure.
Embodiment 2
Monomer Methacrylamide is dissolved the solution making 15wt% in deionized water, adds cross-linking agent N, N '-methylene-bisacrylamide (MBAM).The ratio of cross-linking agent and monomer is 1:3.It is subsequently adding polyethylene of dispersing agent imines (PEI), prepares premixed liquid.Adding titanium carbide powder, ball milling obtains the slurry of solid content about 50vol%, and the viscosity of slurry is at about 300-600mPa.s.Adding Ammonium persulfate. (APS) is initiator, and wherein the addition of initiator is the 1/10～1/15 of monomer.Strong agitation deaeration after interpolation.It is poured into the most as required in mould.Pour hexanol into and cover pulp surface.Put into 50 degree of solidification 2h in water bath with thermostatic control.Mould is opened when being cooled to room temperature in sample.Obtain that surface cure is complete, the biscuit of even structure.
Embodiment 3
Monomer N,N-DMAA is dissolved the solution making 15wt% in deionized water, adds cross-linking agent N, N '-methylene-bisacrylamide (MBAM).The ratio of cross-linking agent and monomer is 1:6.It is subsequently adding dispersant Tetramethylammonium hydroxide, prepares premixed liquid.Adding boron carbide powder, ball milling obtains the slurry of solid content about 57vol%, and the viscosity of slurry is at about 400-600mPa.s.Adding azo (2-narrows base propane) hydrochlorate (AZAP 2HCl) is initiator, and wherein the addition of initiator is the 1/10～1/15 of monomer.Strong agitation deaeration after interpolation.It is poured into the most as required in mould.Pour n-heptanol into and cover pulp surface.Put into 55 degree of solidification 2h in water bath with thermostatic control.Mould is opened when being cooled to room temperature in sample.Obtain that surface cure is complete, the biscuit of even structure.
Embodiment 4
Monomeric acrylamide and polyethylene glycol acrylate are made the solution of 15wt% in deionized water according to the ratio dissolving of mass ratio 6:1, adds cross-linking agent PEG dimethylacrylate.The ratio of cross-linking agent and monomer is 1:3.It is subsequently adding dispersants ammonium polyacrylate, prepares premixed liquid.Adding alumina powder jointed, ball milling obtains the slurry of solid content about 50vol%, and the viscosity of slurry is at about 300-600mPa.s.Adding azo [2-(2-imidazoline-2-base)] propane hydrochloride salt (AZIP 2HCl) is initiator, and wherein the addition of initiator is the 1/10～1/15 of monomer.Strong agitation deaeration after interpolation.It is poured into the most as required in mould.Pour n-nonyl alcohol into and cover pulp surface.Put into 60 degree of solidification 2h in water bath with thermostatic control.Mould is opened when being cooled to room temperature in sample.Obtain that surface cure is complete, the biscuit of even structure.
Embodiment 5
Monomer N,N-DMAA is dissolved the solution making 15wt% in deionized water, adds cross-linking agent PEG dimethylacrylate.The ratio of cross-linking agent and monomer is 1:3.It is subsequently adding dispersants ammonium polyacrylate, prepares premixed liquid.Adding Zirconium powder, ball milling obtains the slurry of solid content about 50vol%, and the viscosity of slurry is at about 300-600mPa.s.Adding initiator azo (2-narrows base propane) hydrochlorate (AZAP 2HCl), wherein the addition of initiator is the 1/10～1/20 of monomer.Strong agitation deaeration after interpolation.It is poured into the most as required in mould.Pour Decanol into and cover pulp surface.Put into 65 degree of solidification 2h in water bath with thermostatic control.Mould is opened when being cooled to room temperature in sample.Obtain that surface cure is complete, the biscuit of even structure.
Industrial applicability: the method for the present invention need not add any auxiliary agent in the slurry, will not produce impact to slurry composition and radically curing process.And simple and reliable process, easily operation and recovery, cost is the lowest, it is possible to quickly prepare surface texture high-performance biscuit complete, uniform.The present invention is applicable to the curing molding of water base free radical system gel injection-moulding ceramic size, it is possible to meet the requirement of each side such as industry, Aeronautics and Astronautics and national defence.
Claims (8)
1. the method for a free radical system gel casting forming: it is characterized in that, described method includes:
Preparation is containing water, dispersant, organic monomer, cross-linking agent, the slurry of ceramic powder；
Being added by described slurry and stir deaeration after initiator and inject mould, then cover resistance to surface inhibition reagent on the surface of described slurry and solidify, wherein said resistance to surface inhibition reagent is to have a hydrophilic group and hydrophobic chain plays the C of Action of Surfactant5～C11Monohydric alcohol, described hydrophilic group directly contacts with ceramic size, hydrophobic group then tends to stretch in atmosphere to form a tunic layer thus the oxygen that is effectively isolated in air in pulp surface, and described resistance to surface inhibition reagent is any one or two or more combination in n-amyl alcohol, isoamyl alcohol, hexanol, n-heptanol, n-octyl alcohol, n-nonyl alcohol, Decanol and positive undecyl alcohol.
Method the most according to claim 1, it is characterized in that, described organic monomer is acrylic acid, dimethylaminoethyl methacrylate, dimethylamino-propyl Methacrylamide, hydroxy ethyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl acrylate, Hydroxypropyl methacrylate, the monomethacrylates of methoxy poly (ethylene glycol), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacryiamidopropyl trimethyl ammonium chloride, methacrylic acid, Sodium styrene sulfonate, acrylamide, Methacrylamide, N, N-DMAA, or vinyl pyrrolidone or their combination in any.
Method the most according to claim 1, it is characterised in that described organic monomer is 30:100～10:100 with the mass ratio of described water.
4. according to the method according to any one of claims 1 to 3, it is characterised in that described cross-linking agent includes N, N '-methylene-bisacrylamide and poly-(vinyl alcohol) dimethacrylate.
5. according to the method according to any one of Claims 1 to 4, it is characterised in that the mass ratio of described cross-linking agent and described organic monomer is 1:15～1:1.
6. according to the method according to any one of Claims 1 to 5, it is characterized in that, described initiator includes Ammonium persulfate ./tetramethyl-ethylene base diamidogen, azo [2-(2-imidazoline-2-base)] propane hydrochloride salt and azo (2 amidine propane) hydrochlorate.
7. according to the method according to any one of claim 1～6, it is characterised in that the addition of described initiator is the 1/10～1/20 of described organic monomer.
8. according to the method according to any one of claim 1～7, it is characterised in that described condition of cure is to solidify 10 minutes～3 hours at 40～80 DEG C.
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| CN101348376A (en) * | 2008-08-29 | 2009-01-21 | 中国科学院上海硅酸盐研究所 | Double-component monomer system for ceramic material gel pouring moulding and use method thereof |
| CN102060543A (en) * | 2010-11-29 | 2011-05-18 | 中国航空工业集团公司北京航空材料研究院 | Method for preventing oxygen inhibition in injection moulding process |
| CN102515776A (en) * | 2011-12-21 | 2012-06-27 | 中国科学院上海硅酸盐研究所 | Solidification method for gel injection molding slurry |
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| CN101348376A (en) * | 2008-08-29 | 2009-01-21 | 中国科学院上海硅酸盐研究所 | Double-component monomer system for ceramic material gel pouring moulding and use method thereof |
| CN102060543A (en) * | 2010-11-29 | 2011-05-18 | 中国航空工业集团公司北京航空材料研究院 | Method for preventing oxygen inhibition in injection moulding process |
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| CN112341184A (en) * | 2020-11-09 | 2021-02-09 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of waveguide structure laser transparent ceramic optical fiber based on Isobam gel state dip-coating technology |
| CN112341184B (en) * | 2020-11-09 | 2021-11-23 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of waveguide structure laser transparent ceramic optical fiber based on Isobam gel state dip-coating technology |
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