CN117209272B - Ceramic slurry and preparation method and application thereof - Google Patents
Ceramic slurry and preparation method and application thereof Download PDFInfo
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- CN117209272B CN117209272B CN202311053269.1A CN202311053269A CN117209272B CN 117209272 B CN117209272 B CN 117209272B CN 202311053269 A CN202311053269 A CN 202311053269A CN 117209272 B CN117209272 B CN 117209272B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 120
- 239000002002 slurry Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000007613 slurry method Methods 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 32
- UGPWRRVOLLMHSC-UHFFFAOYSA-N 2-[3-(2-hydroxypropan-2-yl)phenyl]propan-2-ol Chemical compound CC(C)(O)C1=CC=CC(C(C)(C)O)=C1 UGPWRRVOLLMHSC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 26
- 150000001639 boron compounds Chemical class 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims description 22
- 239000011230 binding agent Substances 0.000 claims description 18
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 150000002009 diols Chemical class 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 229910002971 CaTiO3 Inorganic materials 0.000 claims description 2
- 229910002976 CaZrO3 Inorganic materials 0.000 claims description 2
- 229910003781 PbTiO3 Inorganic materials 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000000304 alkynyl group Chemical group 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
- 229910021523 barium zirconate Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910014031 strontium zirconium oxide Inorganic materials 0.000 claims description 2
- 238000001879 gelation Methods 0.000 abstract description 26
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 239000003985 ceramic capacitor Substances 0.000 abstract description 11
- 230000007547 defect Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 24
- -1 boric acid ester compound Chemical class 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 239000004327 boric acid Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000001298 alcohols Chemical class 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000000693 micelle Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- 229940035437 1,3-propanediol Drugs 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 150000000180 1,2-diols Chemical class 0.000 description 1
- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical compound CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-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
- 229910052691 Erbium Inorganic materials 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
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 125000005233 alkylalcohol group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect 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
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 125000000468 ketone group Chemical group 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
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses ceramic slurry, a preparation method and application thereof, wherein the ceramic slurry comprises the following components: ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent; the inorganic auxiliary agent comprises a boron compound; the organic aid comprises polyvinyl butyral; the organic alcohol includes meta-diol. The ceramic slurry provided by the invention adopts specific organic alcohol, so that the gelation phenomenon of the ceramic slurry can be effectively improved, the internal defects of a ceramic capacitor prepared from the ceramic slurry are reduced, the carbon content in the ceramic capacitor is reduced, and the performance requirement of the high-frequency ceramic capacitor on the ceramic slurry is further met.
Description
Technical Field
The invention belongs to the field of ceramics, and particularly relates to ceramic slurry, and a preparation method and application thereof.
Background
The multilayer ceramic capacitor is a laminated electronic component in which a plurality of ceramic dielectric layers and internal electrode layers are alternately laminated. Among them, the material used for the internal electrode is ag—pb alloy, but Cu metal having a low resistivity is currently used as a substitute because of its high price. However, cu has a low melting point of 1085 ℃ and is easily melted during sintering, so that the sintering temperature of the ceramic dielectric layer is lower than the melting point of Cu.
Researchers have added glass materials containing boron compounds (e.g., B 2O3) as sintering aids to ceramic powders to reduce the sintering temperature of the ceramic dielectric layer. In order to increase the strength of the ceramic green sheet, a resin binder containing free hydroxyl groups, such as polyvinyl butyral (PVB), is generally added to the slurry, but such ceramic slurry is prone to gelation due to the reaction of B (OH) 4 - ions generated by hydrolysis of the boron compound with the side chain hydroxyl groups in the resin binder to form a three-dimensional network gel structure.
In the prior art, the water content of the porcelain powder is reduced by drying the porcelain powder at 400 ℃, and the generation of B (OH) 4 - ions can be reduced, but the method only considers the water in the porcelain powder, ignores the water in an organic solvent and has a certain proportion, and the method can not completely remove the water, so that the gelation problem can not be thoroughly solved. Researchers also use chelating agents to react with B (OH) 4 - to form chelates, so as to avoid the reaction of B (OH) 4 - with the side chain hydroxyl of the resin binder, and thus avoid the gelation of the slurry, but in organic systems, the mutual solubility of the chelating agents and organic solvents is low, so that the dispersibility of the slurry is affected, and the dispersion of the semi-finished product is not facilitated, and serious defects may occur in the product.
Disclosure of Invention
In order to overcome the problems of the prior art, it is an object of the present invention to provide a ceramic slurry.
The second object of the present invention is to provide a method for preparing ceramic slurry.
The invention further provides an application of the ceramic slurry in electronic products.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
In a first aspect, the present invention provides a ceramic slurry comprising the following components: ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent; the inorganic auxiliary agent comprises a boron compound; the organic aid includes a resin binder containing free hydroxyl groups; the organic alcohol includes meta-diol.
In the ceramic slurry, when the boron compound in the inorganic auxiliary agent is hydrolyzed, the generated B (OH) 4 - is subjected to crosslinking reaction with hydroxyl side chains in the resin binder to generate a three-dimensional network structure, for example, when the boron compound is B 2O3 and the resin binder is polyvinyl butyral (PVB), the crosslinking reaction in the slurry is shown in reaction equations (1), (2) and (3):
B2O3+3H2O→2H3BO3 (1)
H3BO3+2H2O→B(OH)4 -+H3O+… (2)
B(OH)4 -+4ROH→B(OR)4 -+4H2O… (3)
In the formula (3): r represents a carbon chain structure connected with hydroxyl in PVB.
Through researches, organic alcohol can form cyclic or chain boric acid ester compound with H 3BO3 generated by hydrolysis of boron compound, and B (OH) 4 - is prevented from reacting with side chain hydroxyl of resin binder, so that gelation of ceramic slurry is improved. In the alcohol compound, the polyhydric alcohol and H 3BO3 form a cyclic compound, and the chain compound formed by the monohydric alcohol and H 3BO3 is more stable than the chain compound formed by the monohydric alcohol and H 3BO3, so that the hydrolysis of the lipid compound can be avoided, and the gelation can be further improved. In the polyol, the meta-diol and H 3BO3 form six-membered ring boric acid ester, which is more stable than five-membered ring, seven-membered ring and other boric acid esters formed by other diols, and the six-membered ring boric acid ester is not easy to hydrolyze in the ceramic slurry, so that gelation can be further avoided.
The "meta diol" in the present invention means a compound having a structure represented by formula (I). In formula (I), R 1、R2、R3 is selected from any substituents. Two alcohol hydroxyl groups in meta-diol and H 3BO3 form stable six-membered ring boric acid ester, and the six-membered ring boric acid ester is not easy to hydrolyze in ceramic slurry, so that the gelation phenomenon of the ceramic slurry can be obviously improved.
Preferably, the meta diol is selected from at least one of compounds represented by formula (I), wherein in formula (I), R 1、R2、R3 is independently selected from any one of H and a hydrocarbon group, and the hydrocarbon group may be selected from alkyl, alkenyl, alkynyl, and aryl of C 1～C8.
Through researches, when the R 1、R2、R3 has a hydrocarbon group, the six-membered ring formed by the meta-diol structure and boric acid can be stabilized, and the hydrolysis of borate is avoided, so that the gelation is further avoided. However, if the number of hydrocarbon groups is too large or the number of carbon atoms of the groups is too large, the stability of the hexacyclic borate is affected by steric hindrance, and gelation is not advantageously avoided. R 1、R2、R3 may be the same or different, for example R 1、R2、R3 are all hydrogen atoms. Stabilizing groups other than hydrocarbyl groups, such as carbonyl, aldehyde groups, etc., are not preferred because such groups may react with boric acid. For example, R 1、R2、R3, if carboxyl or other hydroxyl groups are present, can affect the crosslinking of the meta-diol with boric acid, affecting the structure of the product borate; aldehyde, ketone groups may react with boric acid to form succinic compounds.
Preferably, the total number of carbon atoms of the compound shown in the formula (I) is 3-16; further preferably, the total number of carbon atoms of the compound represented by the formula (I) is 6 to 10. The compound shown in the formula (I) with the carbon chain length of 6-10 carbon atoms is easier to dissolve and disperse in ceramic slurry, is easier to be removed in the green body glue discharging process, avoids a large number of defects of a ceramic dielectric layer after glue discharging, and can also avoid carbon deposition of products caused by insufficient glue discharging.
Preferably, the mass ratio of the ceramic powder to the inorganic auxiliary agent to the organic alcohol to the organic solvent is 100: (0.1-3): (8-15): (0.1-3): (80-150).
Preferably, the organic alcohol further comprises at least one of monohydric alcohol, ortho dihydric alcohol, and trihydric alcohol.
Preferably, the monohydric alcohol is selected from the group consisting of C 1～C16 alkyl alcohols; further preferably, the monohydric alcohol comprises at least one of methanol, ethanol, butanol, propanol, pentanol, heptanol, hexanol, octanol.
Preferably, in the organic alcohol, the mass percentage of meta-diol is 60-100%.
If the organic alcohol is only one meta-diol compound, the mutual solubility with the organic solvent is incomplete, the dispersion of B element in the ceramic slurry is easy to be uneven, the sintering of the ceramic slurry is affected, the meta-diol is mixed and added or the meta-diol and the monohydric alcohol are mixed and added, the mutual solubility of the meta-diol and the organic solvent in the slurry can be promoted through the synergistic effect of the two alcohols, and the binding capacity to H 3BO3 can be obviously enhanced, so that the ceramic slurry has almost no free B (OH) 4 - or has a trace amount of free B (OH) 4 - before the resin binder containing free hydroxyl is added, and the crosslinking reaction of the free hydroxyl in the resin binder is avoided.
Preferably, the molar ratio of the compound represented by the formula (I) to the boron atom in the boron compound is 1: (0.2-1).
Preferably, the weight average molecular weight of the resin binder containing free hydroxyl groups is 20000 to 40000. When the molecular weight of the PVB resin is 20000 to 40000, even if a small amount of free B (OH) 4 - exists in the ceramic slurry, the generation of a three-dimensional network structure with extremely large molecular weight can be avoided, so that the gelation problem of the ceramic slurry can be relieved.
Preferably, the ceramic powder includes at least one of BaTiO3、BaTiZrO3、PbTiO3、CaTiO3、CaZrO3、SrZrO3、BaZrO3、ZrO2.
Preferably, the boron compound comprises at least one of B 2O3, borate, borosilicate.
Preferably, the resin binder containing free hydroxyl groups includes at least one of polyvinyl butyral and polyvinyl formal.
Preferably, the inorganic auxiliary further comprises at least one of a compound of Si, a compound of Al, a compound of an alkaline earth metal, a compound of a transition metal, and a compound of a rare earth element.
Preferably, the compound of Si comprises SiO 2.
Preferably, the compound of Al includes Al 2O3.
Preferably, the alkaline earth metal comprises at least one of magnesium, calcium, strontium, barium.
Preferably, the transition metal comprises at least one of chromium, manganese, iron, cobalt, nickel, copper, zinc, zirconium.
Preferably, the rare earth element comprises at least one of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium.
Preferably, the organic auxiliary agent further comprises at least one of a binder, a plasticizer and a dispersant.
Preferably, the binder comprises at least one of ethylcellulose, acrylic resin.
Preferably, the plasticizer comprises at least one of dibutyl phthalate and dioctyl phthalate.
Preferably, the dispersant comprises at least one of alkyl imidazolines, polyesteramide ammonium salts.
Preferably, the organic solvent comprises at least one of toluene, ethanol, isopropanol, xylene, acetone, and ethyl acetate.
The second aspect of the present invention provides a method for preparing the ceramic slurry provided in the first aspect of the present invention, comprising the steps of:
Drying the ceramic powder to ensure that the water content of the ceramic powder is less than or equal to 0.3 percent; mixing ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent for reaction, and then mixing with the organic auxiliary agent to prepare the ceramic slurry.
Preferably, the drying temperature is 600-700 ℃.
Preferably, the drying time is 12-14 h.
When the water content of the ceramic powder is less than or equal to 0.3%, the hydrolysis of the boron compound can be effectively reduced, and the crosslinking reaction is avoided. On the other hand, the ceramic powder, the inorganic auxiliary agent, the meta-diol and the organic solvent are mixed first, and then the organic auxiliary agent is mixed, so that B (OH) 4 - can be fully reacted with the meta-diol first, and B (OH) 4 - is prevented from reacting with PVB.
A third aspect of the present invention provides the use of the ceramic slurry provided in the first aspect of the present invention in an electronic product.
Preferably, the electronic product comprises a ceramic capacitor.
Preferably, the ceramic capacitor comprises more than two ceramic dielectric layers and electrode layers; the ceramic dielectric layer is made from the ceramic slurry provided in the first aspect of the invention.
Preferably, the preparation method of the ceramic capacitor comprises the following steps: casting ceramic slurry into a ceramic film, printing conductive slurry containing copper powder on the surface of the ceramic film to form conductive patterns, and performing lamination forming, isostatic pressing and cutting on the ceramic film with the conductive patterns to obtain a laminated green body; and discharging glue from the laminated body green body, and sintering to obtain the ceramic capacitor.
The beneficial effects of the invention are as follows: the ceramic slurry provided by the invention adopts specific organic alcohol, so that the gelation phenomenon of the ceramic slurry can be effectively improved, the internal defects of a ceramic capacitor prepared from the ceramic slurry are reduced, the carbon content in the ceramic capacitor is reduced, and the performance requirement of the high-frequency ceramic capacitor on the ceramic slurry is further met.
The preparation method of the ceramic slurry is simple and easy to operate, and the gelation phenomenon of the ceramic slurry can be further improved by strictly controlling the water content of the ceramic powder.
Detailed Description
Specific implementations of the invention are described in further detail below with reference to examples, but the practice and protection of the invention is not limited thereto. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The ceramic slurry in this example comprises ceramic powder, inorganic auxiliary agent containing boron compound, organic auxiliary agent containing PVB (polyvinyl butyral), meta-glycol and organic solvent; ceramic powder, inorganic auxiliary agent containing boron compound, organic auxiliary agent containing PVB, meta-diol and organic solvent in the mass ratio of 100:3:8:3:80;
Wherein the ceramic powder is Ca 0.7Sr0.3ZrO3, the boron compound is B 2O3, the inorganic auxiliary agent contains SiO 2、Al2O3、ZrO2 besides the boron compound, and the mass ratio of B 2O3、SiO2、Al2O3、ZrO2 is 1:0.5:2:0.1. The weight average molecular weight of PVB is 20000, the organic auxiliary agent contains dibutyl phthalate besides PVB, and the mass ratio of PVB to dibutyl phthalate is 1:2. The meta-diol is in particular 1, 3-propanediol. The organic solvent is acetone and toluene, and the mass ratio of the acetone to the toluene is 1:1. The molar ratio of 1, 3-propanediol to boron atoms was 1:0.31.
The ceramic slurry in this example is prepared by the following preparation method, and specifically comprises the following steps:
Drying the ceramic powder at 600 ℃ for 12 hours to ensure that the water content of the ceramic powder is less than or equal to 0.3%; then mixing the ceramic powder with the inorganic auxiliary agent containing boron compound, meta-diol and organic solvent according to a certain proportion, adding the organic auxiliary agent containing polyvinyl butyral, and mixing to obtain the ceramic slurry in this example.
Examples 2 to 7
The ceramic slurries in examples 2 to 7 differ from example 1 only in that: the meta diol was different in kind, and the kinds and amounts of the remaining components in examples 2 to 7 were the same as in example 1. The meta-diol types in examples 2 to 7 are shown in Table 1 below:
table 1 examples 1 to 7 and comparative examples 1 to 3 types of intermediate diols
* : When the meta diol is more than one, the average carbon number C is obtained by the following formula (4):
Where n 1、n2、n3 … is the amount of the substance of several alcohols and C 1、C2、C3 … is the number of carbon atoms of several alcohols.
Examples 8 to 11
The meta-diol in the ceramic slurries of examples 8 to 11 was 2, 4-trimethyl-1, 3-pentanediol, and the preparation method was the same as that of example 1. The ceramic slurries in examples 8 to 11 differ from example 2 in that: the ceramic slurry other than meta-diol has different components and the ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent have different mass ratios. The components and proportions of the ceramic slurries in examples 8 to 11 are shown in Table 2:
table 2 Components and proportions of the ceramic slurries of examples 8 to 11
Example 12
The ceramic slurry in example 12 differs from example 2 only in that: the PVB had a weight average molecular weight of 50000, the other components of example 12 were the same in kind and amount as in example 2, and the preparation method of example 12 was the same as in example 1.
Comparative examples 1 to 3
The components and proportions of the ceramic slurries in comparative examples 1 to 3 are recorded in table 1, and the comparative examples 1 to 3 differ from example 2 in that: comparative example 1 does not contain meta diol, the alcohol added in comparative example 2 is a monohydric alcohol, the alcohol added in comparative example 3 is a1, 2-dihydric alcohol, and the remaining components of comparative examples 1 to 3 are the same as in example 2.
The ceramic slurries of comparative examples 1 to 3 were prepared in the same manner as in example 1.
Comparative example 4
The ceramic slurry in comparative example 4 was identical in composition and proportion to example 2, and comparative example 4 was different from example 2 only in that: in the preparation of the ceramic slurry, the ceramic powder is dried for 2 hours at the temperature of 400 ℃ and the water content of the ceramic powder is 0.5 percent.
Performance test:
1. Degree of gelation of the slurry
The degree of gelation of the slurry is determined by macroscopic or microscopic observation, which is an observation of the green body after casting by a scanning electron microscope. The extent of slurry gelation was compared by grades a-E, where:
A represents heavy gel, at this time, the slurry macroscopically presents jelly shape, and microscopic observation can see gel groups with the size of more than 5 mu m, and the volume ratio is more than 70%;
b represents medium gel, the slurry is in paste shape macroscopically, the micelle with the volume more than 5 mu m can be seen by microscopic observation, and the volume ratio is more than 50%;
C represents light gel, the slurry has high macroscopic viscosity, and the microscopic observation can see the micelle with the volume more than 5 mu m, and the volume ratio is more than 20%;
D represents microgel, the macroscopic state of the sizing agent is normal, the microscopic observation can be performed on the micelle with the size of more than 5 mu m, and the volume ratio is more than 1 percent;
E represents a qualified slurry. The macroscopic state of the slurry is normal, large micelles cannot be observed under the microscopic state, or the volume ratio of the micelles with the size of more than 5 μm is less than 1%.
2. Slurry viscosity
The viscosity of the slurry was measured by a viscometer, the test procedure being: a viscometer measurement probe was inserted into the slurry, measurement was started, and the viscosity value at 30 ℃ was read out.
3. Ceramic cracking ratio: and carrying out high Wen Jileng operation on the sintered sample, testing whether the product has cracking or not by using a metallographic microscope and testing the cracking proportion by using an SAT (ultrasonic scanner). A cracking rate of less than 5% of a batch of products is regarded as being qualified.
4. Ceramic carbon content: the sample was tested for carbon content using a carbon sulfur instrument. The carbon content of a batch of products is within 2 percent and is regarded as qualified.
Test sample:
The samples used in the measurement of the degree of gelation of the ceramic and the viscosity of the slurry were the ceramic slurries of examples 1 to 12 and comparative examples 1 to 4, respectively;
The preparation method of the sample for testing the cracking proportion and the carbon content of the ceramic comprises the following steps:
Casting the ceramic slurries of examples 1 to 12 and comparative examples 1 to 4 into ceramic films, printing conductive slurry containing copper powder on the surface of the ceramic films to form conductive patterns, and performing lamination forming, isostatic pressing and cutting on the ceramic films with the conductive patterns to obtain a laminated green body; and (3) discharging glue and sintering the laminated green body to obtain a ceramic dielectric material, and then testing and recording the ceramic cracking proportion and the ceramic carbon content of the ceramic dielectric layer, wherein each batch is tested for 1000 sample wafers, and the obtained experimental result is the average value of 1000 samples.
The ceramic slurries of examples 1 to 12 and comparative examples 1 to 4 were tested for properties according to the above test methods, and the specific test results are shown in table 3:
TABLE 3 results of Performance test of ceramic slurries in examples 1 to 12 and comparative examples 1 to 4
As is clear from Table 3, the gelation problem of the ceramic slurry obtained by using the meta diol in examples 1 to 12 of the present invention was greatly alleviated compared with comparative examples 1 to 3. The comparative example 1 was free from the addition of meta-diol and other alcohols, and the water content of the ceramic powder was controlled, but the gelation problem of the ceramic slurry obtained was still serious, and the use requirements could not be satisfied, whereas the comparative examples 2 to 3 were free from the addition of other alcohols, such as monohydric alcohol or 1, 2-diol, and the effect of avoiding gelation was not ideal, and the ceramic slurry obtained still could not satisfy the use requirements. Comparative example 4 was conducted in the same manner as in example 2, except that the water content of the ceramic powder was not strictly controlled, and the gelation phenomenon of the ceramic slurry obtained was improved, but gelation reaction still occurred, indicating that the water content of the ceramic powder was controlled to be advantageous in avoiding gelation.
Comparative examples 1 to 2 show that when R 1、R2、R3 in the meta diol compound has a hydrocarbon group, the six-membered ring formed by the meta diol compound and boric acid can be stabilized, and the hydrolysis of the borate is avoided, and the gelation is prevented. Comparative examples 2 and 5 to 6 show that the increase in the number of carbon atoms in the meta-diol compound causes insufficient removal of the binder, and the amount of carbon deposition in the product increases, which results in easy occurrence of defects in the ceramic dielectric layer after the binder removal. Comparative example 3 and example 7 show that the effect of avoiding gelation is better by the synergistic effect of the two meta diols. As is clear from comparative example 12 and example 1, when the weight average molecular weight of the polyvinyl butyral is too large, it is also disadvantageous to avoid gelation of the ceramic slurry.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (8)
1. A ceramic slurry characterized by: the composition comprises the following components: ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent; the inorganic auxiliary agent comprises a boron compound; the organic aid includes a resin binder containing free hydroxyl groups; the organic alcohol comprises two meta diols; the mass ratio of the ceramic powder to the inorganic auxiliary agent to the organic alcohol to the organic solvent is 100: (0.1 to 3): (8-15): (0.1 to 3): (80-150); the molar ratio of meta diol to boron atom in the boron compound is 1: (0.2-1); the weight average molecular weight of the resin binder containing free hydroxyl groups is 20000-40000.
2. The ceramic slurry according to claim 1, wherein: the meta diol is at least one selected from compounds shown in a formula (I):
Formula (I)
In the formula (I), R 1、R2、R3 is independently selected from any one of H and a hydrocarbon group, and the hydrocarbon group is selected from alkyl, alkenyl, alkynyl and aryl of C 1~C8.
3. The ceramic slurry according to claim 1, wherein: and the total number of carbon atoms of the meta-diol is 3-16.
4. The ceramic slurry according to claim 1, wherein: and the total number of carbon atoms of the meta-diol is 6-10.
5. The ceramic slurry according to claim 1, wherein: the organic alcohol also comprises at least one of monohydric alcohol, ortho-dihydric alcohol and trihydric alcohol; in the organic alcohol, the mass percentage of meta-diol is 60-100%.
6. The ceramic slurry according to claim 1, wherein: the ceramic powder comprises at least one of BaTiO3、BaTiZrO3、PbTiO3、CaTiO3、CaZrO3、SrZrO3、BaZrO3、ZrO2; the boron compound comprises at least one of B 2O3, borate and borosilicate; the inorganic auxiliary agent also comprises at least one of a compound of Si, a compound of Al, a compound of alkaline earth metal, a compound of transition metal and a compound of rare earth element; the organic aid further comprises at least one of a binder, a plasticizer and a dispersant.
7. The method for preparing the ceramic slurry according to any one of claims 1 to 6, characterized in that: the method comprises the following steps:
Drying the ceramic powder to ensure that the water content of the ceramic powder is less than or equal to 0.3 percent; mixing ceramic powder, inorganic auxiliary agent, organic alcohol and organic solvent for reaction, and then mixing with the organic auxiliary agent to prepare the ceramic slurry.
8. Use of the ceramic slurry according to any one of claims 1 to 6 in electronic products.
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