CN117164349A - Alumina ceramic casting slurry, preparation method thereof and alumina ceramic green ceramic tape - Google Patents
Alumina ceramic casting slurry, preparation method thereof and alumina ceramic green ceramic tape Download PDFInfo
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- CN117164349A CN117164349A CN202311139535.2A CN202311139535A CN117164349A CN 117164349 A CN117164349 A CN 117164349A CN 202311139535 A CN202311139535 A CN 202311139535A CN 117164349 A CN117164349 A CN 117164349A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000002002 slurry Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005266 casting Methods 0.000 title claims description 60
- 239000000919 ceramic Substances 0.000 title abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 104
- 239000011521 glass Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 27
- 239000004014 plasticizer Substances 0.000 claims abstract description 22
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims description 39
- 239000011230 binding agent Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 18
- 239000011268 mixed slurry Substances 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 6
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920006217 cellulose acetate butyrate Polymers 0.000 claims description 6
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 239000001923 methylcellulose Substances 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052810 boron oxide Inorganic materials 0.000 claims description 5
- 229920006184 cellulose methylcellulose Polymers 0.000 claims description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 4
- JKFRYNBULZZKHW-UHFFFAOYSA-N C(C)(=O)O.C(C)(=O)O.C(C(=O)O)(=O)O Chemical compound C(C)(=O)O.C(C)(=O)O.C(C(=O)O)(=O)O JKFRYNBULZZKHW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 4
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 125000005456 glyceride group Chemical group 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 abstract description 18
- 238000010345 tape casting Methods 0.000 abstract description 18
- 238000005245 sintering Methods 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000005452 bending Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 5
- 235000010981 methylcellulose Nutrition 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009849 vacuum degassing Methods 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- -1 phosphate ester Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- UGZICOVULPINFH-UHFFFAOYSA-N acetic acid;butanoic acid Chemical compound CC(O)=O.CCCC(O)=O UGZICOVULPINFH-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides an alumina ceramic tape casting slurry, a preparation method thereof and an alumina ceramic green ceramic tape, and belongs to the technical field of ceramic materials. According to the invention, the alumina ceramic powder and the glass powder are used as powder materials, and the alumina ceramic powder and the glass powder are used as powder materials together, so that the density of the ceramic powder after sintering and the mechanical property of the ceramic can be improved; according to the invention, the powder is wrapped in the adhesive, and the powder is solidified to form a framework with a three-dimensional structure, so that the strength, plasticity, flexibility and smoothness of the green porcelain belt can be improved by limiting the types of the adhesive; according to the invention, the agglomeration of the powder particles is restricted and the powder particles can be uniformly dispersed in the slurry by adding the dispersing agent, so that the anti-sedimentation performance and uniformity of the slurry are enhanced; the invention improves the flexibility and the bending strength of the green porcelain belt by adding the plasticizer, and can lubricate ceramic particles and play a bridging role, so that the slurry is stable and uniform.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to an alumina ceramic tape casting slurry, a preparation method thereof and an alumina ceramic green ceramic tape.
Background
Along with the continuous miniaturization and the precision of electronic equipment such as mobile phones, computers and the like, higher requirements are put forward on the precision and the high performance of corresponding electronic components in the electronic equipment, so that equipment for packaging and protecting the electronic components also improves corresponding standards. The alumina ceramic packaging base gradually replaces the traditional packaging material due to the good performances of dielectric property, high temperature resistance, corrosion resistance, dimensional stability and the like.
The tape casting technology has been widely used for the stable batch production of alumina ceramic materials at present because of the advantages of continuous molding, simple operation, stable process, small defects of substrate performance and the like. The tape casting process mainly comprises the preparation of the early-stage slurry and the adjustment of the later-stage process parameters. The composition components of the casting slurry determine specific technological parameters of the subsequent casting process and the performances of appearance quality, strength toughness, sintering shrinkage and the like of the green body.
The tape casting technology is a standard wet forming technology, can prepare a ceramic green tape of 50-1000 mu m, and forms a ceramic sheet through further lamination, degreasing and sintering, and has the advantages of wider application range, smaller defect size of the prepared green body, higher production efficiency, stable product performance and the like. The binder and the solvent in the tape casting technology determine the fluidity and volatility in the slurry, but when the binder and the solvent are not used properly, the prepared raw porcelain tape is easy to generate defects of dark crack, curling, agglomeration, uneven thickness and the like, so that the raw porcelain tape has the problems of poor toughness, low strength and poor bonding strength between the raw porcelain tapes. Accordingly, there is a need to provide an alumina ceramic casting slurry capable of solving the problems of poor toughness, low strength and poor bonding strength between green tapes.
Disclosure of Invention
The invention aims to provide an alumina ceramic casting slurry capable of improving the strength of an alumina ceramic green tape and the bonding strength between the green tapes.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an alumina ceramic casting slurry, which comprises the following components in percentage by mass:
the powder consists of alumina ceramic powder and glass powder;
the binder includes one or more of polyvinyl butyral, acrylic resin, cellulose acetate-butyrate, and methylcellulose.
Preferably, the mass ratio of the alumina porcelain powder to the glass powder is (90-95): 5-10.
Preferably, the purity of the alumina porcelain powder is greater than or equal to 99%.
Preferably, the particle size of the alumina porcelain powder is 1.5-4.8 mu m; the particle size of the glass powder is 2-5 mu m.
Preferably, the glass frit comprises one or more of boron oxide, silicon oxide, calcium oxide, titanium oxide, zirconium oxide, lanthanum oxide, and magnesium oxide.
Preferably, the dispersant comprises one or more of phosphate esters, glycerol esters, sodium silicate, sodium carbonate, ammonium polyphosphate, polymethacrylic acid and castor oil.
Preferably, the plasticizer comprises one or more of oxalic acid diacetic acid, polyethylene glycol, dibutyl phthalate and butyl benzyl phthalate.
The invention also provides a preparation method of the alumina ceramic tape casting slurry, which comprises the following steps:
mixing powder, an organic solvent, a dispersing agent and a plasticizer, and performing one-stage ball milling to obtain mixed slurry; and mixing the mixed slurry with a binder, and performing two-stage ball milling to obtain the alumina ceramic casting slurry.
Preferably, the rotating speed of the first-stage ball milling is 20-40 r/min, and the time of the first-stage ball milling is 10-16 h; the rotating speed of the secondary ball milling is 20-40 r/min, and the time of the secondary ball milling is 20-26 h.
The invention also provides an alumina ceramic green ceramic tape, which is prepared from the alumina ceramic casting slurry prepared by the technical scheme or the alumina ceramic casting slurry prepared by the preparation method by casting molding.
The invention provides an alumina ceramic casting slurry, which is prepared from the following raw materials: 55-63% of powder, 12-18% of organic solvent, 23-29% of binder, 0.05-1% of dispersing agent and 1-10% of plasticizer; the powder consists of alumina ceramic powder and glass powder; the binder includes one or more of polyvinyl butyral, acrylic resin, cellulose acetate-butyrate, and methylcellulose. According to the invention, the alumina ceramic powder and the glass powder are used as powder materials, the alumina ceramic powder has good high-temperature stability, excellent electrical property and good mechanical property, and the glass powder has a function of reducing the melting temperature of ceramic powder, can be used as a sintering aid, and improves the density of the sintered ceramic powder and the mechanical property and mechanical property of ceramic; according to the invention, the powder is wrapped in the adhesive, and the skeleton with a three-dimensional structure can be formed after curing, and the strength, plasticity, flexibility and smoothness of the green porcelain belt can be improved by limiting the types of the adhesive; according to the invention, the agglomeration of the powder particles is restricted and the powder particles can be uniformly dispersed in the slurry by adding the dispersing agent, so that the anti-sedimentation performance and uniformity of the slurry are enhanced; the invention improves the flexibility and the bending strength of the green porcelain belt by adding the plasticizer, and can lubricate ceramic particles and play a bridging role, so that the slurry is stable and uniform. The example results show that the alumina ceramic tape prepared from the alumina ceramic tape casting slurry provided by the invention has excellent strength.
Detailed Description
The invention provides an alumina ceramic casting slurry, which comprises the following components in percentage by mass:
the powder consists of alumina ceramic powder and glass powder;
the binder includes one or more of polyvinyl butyral, acrylic resin, cellulose acetate-butyrate, and methylcellulose.
In the present invention, the reagents used in the present invention are commercially available products well known to those skilled in the art unless specified otherwise.
The alumina ceramic casting slurry provided by the invention comprises 55-63% of powder by mass, preferably 60-63%. In the invention, the powder consists of alumina porcelain powder and glass powder. In the invention, the alumina ceramic powder has good high-temperature stability, excellent electrical property and good mechanical property, and the glass powder has a function of reducing the melting temperature of ceramic powder, can be used as a sintering aid, and improves the density of the ceramic powder after sintering and the mechanical property and mechanical property of ceramic.
In the present invention, the purity of the alumina porcelain powder is preferably 99% or more, more preferably 99.86%. In the invention, when the purity of the alumina ceramic powder is in the above range, the alumina ceramic powder has better high-temperature stability, electrical property and mechanical property.
In the present invention, the particle size of the alumina porcelain powder is preferably 1.5 to 4.8. Mu.m, more preferably 2 to 3. Mu.m. In the invention, when the particle size of the alumina ceramic powder is in the range, the particle size of the alumina ceramic powder can be matched with that of the glass powder, and when the alumina ceramic casting slurry is prepared, the powder distribution can be more uniform.
In the present invention, the glass frit preferably includes one or more of boron oxide, silicon oxide, calcium oxide, titanium oxide, zirconium oxide, lanthanum oxide, and magnesium oxide, more preferably boron oxide, silicon oxide, calcium oxide, or titanium oxide. In the invention, when the glass powder is of the type, the glass powder is matched with alumina ceramic powder, which is more beneficial to improving the density of ceramic powder after sintering and the mechanical property and mechanical property of ceramic.
In the present invention, the particle size of the glass frit is preferably 2 to 5. Mu.m, more preferably 3 to 4. Mu.m. In the invention, when the particle size of the glass powder is in the range, the glass powder can be matched with the particle size of the alumina ceramic powder, and when the alumina ceramic casting slurry is prepared, the powder distribution can be more uniform.
In the invention, the mass ratio of the alumina porcelain powder to the glass powder is preferably (90-95): (5-10), more preferably (92-95): (8-10). In the invention, when the mass ratio of the alumina ceramic powder to the glass powder is in the above range, the ceramic powder is more beneficial to improving the density after sintering and the mechanical property and mechanical property of the ceramic.
The alumina ceramic casting slurry provided by the invention comprises 12-18% of organic solvent, preferably 15-18% of organic solvent by mass. In the present invention, the organic solvent preferably includes one or more of toluene, xylene, butanone, ethanol, and ethyl acetate. In the invention, when the organic solvent is of the type, the components can be fully dispersed, the fluidity of the alumina ceramic casting slurry is improved, and the alumina ceramic casting slurry has better volatility.
The alumina ceramic casting slurry provided by the invention comprises 23-29% of binder by mass, and preferably 25-29%. In the present invention, the binder includes one or more of polyvinyl butyral, acrylic resin, cellulose acetate-butyrate and methyl cellulose, more preferably polyvinyl butyral, acrylic resin or cellulose acetate-butyrate. In the invention, the adhesive can wrap the powder therein and is solidified to form a framework with a three-dimensional structure, so that the strength, the plasticity, the flexibility and the smoothness of the green porcelain belt can be improved; when the binder is of the type, the adhesive has the advantages of good collocation, high plasticity, easy adhesive discharge and the like. In addition, the present invention improves the strength and toughness of the green body and the bonding force between the green bodies by limiting the amount of the binder to the above range.
The alumina ceramic casting slurry provided by the invention comprises 0.05-1% of dispersing agent by mass, and preferably 0.08-1%. In the present invention, the dispersant preferably includes one or more of phosphate, glyceride, sodium silicate, sodium carbonate, ammonium polyphosphate, polymethacrylic acid and castor oil, more preferably phosphate, glyceride, sodium silicate, sodium carbonate or ammonium polyphosphate. In the invention, the particle size of the powder particles is smaller, the surface energy is higher, the powder particles have a polymerization trend, so that the slurry is unstable; when the dispersing agent is of the type, the surface of the powder particles is more favorably wetted, the surface potential energy is reduced, and the dispersibility of the powder is improved.
The alumina ceramic casting slurry provided by the invention comprises 1-10% of plasticizer, preferably 5-8% of plasticizer by mass. In the present invention, the plasticizer preferably includes one or more of oxalic acid diacetic acid, polyethylene glycol, dibutyl phthalate and butyl benzyl phthalate, more preferably oxalic acid diacetic acid, polyethylene glycol or dibutyl phthalate. In the invention, the plasticizer can reduce the glass transition temperature of the binder in the slurry, so that the molecular chain curling and stretching deformation of the binder are increased under the low-temperature condition, the flexibility and bending strength of the green ceramic tape can be improved, ceramic particles can be lubricated and have a bridging effect, and the slurry is stable and uniform; when the plasticizer is of the above type, it has good compatibility with the binder used, a high boiling point, a low vapor pressure, a high plasticizing efficiency, good flexibility at low temperature, and stable chemical and physical properties.
According to the invention, the density of the ceramic powder after sintering and the mechanical property and mechanical property of the ceramic are improved by adopting the alumina ceramic powder and the glass powder as the powder; according to the invention, the powder is wrapped in the ceramic tape through the binder and is solidified to form a framework with a three-dimensional structure, so that the strength, the plasticity, the flexibility and the smoothness of the green ceramic tape can be improved; according to the invention, the agglomeration of the powder particles is restricted and the powder particles can be uniformly dispersed in the slurry by adding the dispersing agent, so that the anti-sedimentation performance and uniformity of the slurry are enhanced; the invention improves the flexibility and the bending strength of the green porcelain belt by adding the plasticizer, and can lubricate ceramic particles and play a bridging role, so that the slurry is stable and uniform.
The invention also provides a preparation method of the alumina ceramic tape casting slurry, which comprises the following steps:
mixing powder, an organic solvent, a dispersing agent and a plasticizer, and performing one-stage ball milling to obtain mixed slurry; and mixing the mixed slurry with a binder, and performing two-stage ball milling to obtain the alumina ceramic casting slurry.
The invention mixes the powder, the organic solvent, the dispersing agent and the plasticizer, and then carries out one-stage ball milling to obtain mixed slurry.
The method for mixing the powder, the organic solvent, the dispersing agent and the plasticizer is not particularly limited, and the above components are uniformly mixed by a mixing method well known to those skilled in the art.
In the invention, the rotating speed of the one-stage ball milling is preferably 20-40 r/min, more preferably 34-36 r/min; the one-stage ball milling time is preferably 10 to 16 hours, more preferably 12 to 16 hours. In the invention, the one-stage ball milling can fully open and disperse the agglomerated powder particles, and the dispersing agent can be uniformly coated on the powder particles in the process, so that the surface energy of the particles is reduced; when the rotation speed and time of the ball mill are in the above ranges, the powder can be fully dispersed.
After the mixed slurry is obtained, the mixed slurry is mixed with the binder, and then the two-stage ball milling is carried out to obtain the alumina ceramic casting slurry.
The method for mixing the mixed slurry and the binder is not particularly limited, and the above components are uniformly mixed by a mixing method well known to those skilled in the art.
In the invention, the rotating speed of the two-stage ball milling is preferably 20-40 r/min, more preferably 34-36 r/min; the time of the secondary ball milling is preferably 20 to 26 hours, more preferably 24 to 26 hours. In the invention, the two-stage ball mill can fully disperse the binder in the mixed slurry, and can also prevent the adsorption and wrapping performance of the polymer chain of the binder from being damaged.
After the secondary ball milling is finished, the invention preferably carries out vacuum defoaming on the slurry obtained after the secondary ball milling to obtain the alumina ceramic casting slurry.
In the present invention, the temperature of the vacuum degassing is preferably 24 to 35 ℃, more preferably 28 to 30 ℃; the time for the vacuum degassing is preferably 20 to 60 minutes, more preferably 30 to 50 minutes. In the invention, a large amount of bubbles are arranged in the slurry obtained after the two-stage ball milling, and the existence of the bubbles can lead the slurry to bulge, crack and the like in the casting molding process; when the temperature and time of the vacuum degassing are within the above ranges, bubbles can be sufficiently removed.
According to the invention, through a two-stage ball milling mode, on one hand, powder can be fully dispersed, and the adsorption and wrapping performances of a polymer chain of a binder can be prevented from being damaged, so that the toughness and strength of a raw porcelain belt can be improved.
The invention also provides an alumina ceramic green ceramic tape, which is prepared from the alumina ceramic casting slurry prepared by the technical scheme or the alumina ceramic casting slurry prepared by the preparation method by the scheme through casting molding.
The method of casting according to the present invention is not particularly limited, and a casting method known to those skilled in the art may be used. The parameters of the casting molding are not particularly limited, and the casting molding process is carried out according to the required size of the alumina ceramic green ceramic tape.
According to the invention, the intensity and toughness of the green body can be improved by regulating and controlling the consumption of each component in the alumina ceramic casting slurry; meanwhile, the preparation method of the alumina ceramic tape casting slurry provided by the invention can prevent the adsorption and wrapping performance of the polymer chain of the binder from being damaged under the condition of uniformly mixing the components by two-stage ball milling, thereby improving the toughness and strength of the green ceramic tape. Therefore, the alumina ceramic tape casting slurry provided by the invention can improve the strength and toughness of the alumina ceramic green ceramic tape obtained by tape casting.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The alumina ceramic casting slurry consists of the following components in percentage by mass:
57% of alumina porcelain with purity of 99% and grain diameter of 2.5-3.0 μm;
the glass powder with the grain diameter of 2.0-2.5 mu m is boron oxide 5%;
the organic solvent is absolute ethyl alcohol, 12.65%;
the binder is polyvinyl butyral, 23.9%;
the dispersant is phosphate ester, 0.05%;
the plasticizer is dibutyl phthalate, 1.4%;
the preparation method of the alumina ceramic tape casting slurry comprises the following steps:
mixing alumina ceramic powder, glass powder, an organic solvent, a dispersing agent and a plasticizer, performing ball milling for 12 hours at 34r/min, and performing one-stage ball milling to obtain mixed slurry;
and mixing the mixed slurry with a binder, performing ball milling for 24 hours at 34r/min, performing secondary ball milling, and performing vacuum defoaming for 30 minutes at 25 ℃ to obtain the alumina ceramic casting slurry.
Example 2
The alumina ceramic casting slurry consists of the following components in percentage by mass:
55.7% of alumina ceramic powder with the purity of 99% and the grain diameter of 2.5-2.7 mu m;
4.95 percent of glass powder silicon oxide with the grain diameter of 2.3 to 2.7 mu m;
the organic solvent is toluene, 13%;
the binder is cellulose acetate-butyric acid and 24.88%;
the dispersant is glyceride, 0.07%; the plasticizer is polyethylene glycol, 1.4%;
the preparation method of the alumina ceramic tape casting slurry comprises the following steps:
mixing alumina ceramic powder, glass powder, an organic solvent, a dispersing agent and a plasticizer, performing ball milling for 12 hours at 34r/min, and performing one-stage ball milling to obtain mixed slurry;
and mixing the mixed slurry with a binder, performing ball milling for 24 hours at 34r/min, performing secondary ball milling, and performing vacuum defoaming for 30 minutes at 25 ℃ to obtain the alumina ceramic casting slurry.
Example 3
The alumina ceramic casting slurry consists of the following components in percentage by mass:
alumina ceramic powder 56% with purity of 99% and grain diameter of 2.7-2.8 μm;
5% of glass powder zirconia with the grain diameter of 2.8-2.7 mu m;
the organic solvent is absolute ethyl alcohol and 12%;
the binder is methyl cellulose, 25%;
the dispersant is phosphate ester, 0.7%;
the plasticizer is dibutyl phthalate, 1.3%;
the preparation method of the alumina ceramic tape casting slurry comprises the following steps:
mixing alumina ceramic powder, glass powder, an organic solvent, a dispersing agent and a plasticizer, performing ball milling for 12 hours at 34r/min, and performing one-stage ball milling to obtain mixed slurry;
and mixing the mixed slurry with a binder, performing ball milling for 24 hours at 34r/min, performing secondary ball milling, and performing vacuum defoaming for 30 minutes at 25 ℃ to obtain the alumina ceramic casting slurry.
Example 4
The alumina ceramic casting slurry prepared in the example 1 is injected into a casting machine trough, the height of a knife is adjusted to 720mm, the speed of a conveyor belt is set to be 0.6m/min, and the temperature area is 50-65 ℃, so that the solvent in the slurry can be uniformly evaporated, and the alumina ceramic green ceramic belt is obtained.
Example 5
The alumina ceramic casting slurry prepared in the example 2 is injected into a casting machine trough, the height of a knife is adjusted to 720mm, the speed of a conveyor belt is set to be 0.6m/min, and the temperature area is 50-65 ℃, so that the solvent in the slurry can be uniformly evaporated, and the alumina ceramic green ceramic belt is obtained.
Example 6
The alumina ceramic casting slurry prepared in the example 3 is injected into a casting machine trough, the height of a knife is adjusted to 720mm, the speed of a conveyor belt is set to be 0.6m/min, and the temperature area is 50-65 ℃, so that the solvent in the slurry can be uniformly evaporated, and the alumina ceramic green ceramic belt is obtained.
Test case
The alumina ceramic green tape prepared in example 6 was cut into 7 green sheets of a set length of 10cm and a set width of 1cm, and a thickness of 0.25 μm, and each of which was numbered 1 to 7, and tested. The testing method comprises the following steps: the cut green sheet was hung on a tester, the tensile force was gradually increased until the casting sheet was broken, and the maximum tensile force applied by the tester before the break was recorded as the affordable ultimate strength of the green sheet, and the results of the obtained strength are shown in table 1.
TABLE 1 test results of alumina ceramic green tapes prepared in example 6
| Numbering device | Acceptable value of tensile force |
| 1 | 3.5N |
| 2 | 3.6N |
| 3 | 3.6N |
| 4 | 3.2N |
| 5 | 3.2N |
| 6 | 3.4N |
| 7 | 3.4N |
From the test results, the invention can prevent the adsorption and wrapping performance of the polymer chain of the adhesive from being damaged under the condition of uniformly mixing the components by regulating and controlling the consumption of each component of the alumina ceramic tape casting slurry and performing two-stage ball milling, thereby improving the strength of the green ceramic tape. Therefore, the alumina ceramic tape casting slurry provided by the invention can improve the strength of the alumina ceramic green ceramic tape obtained by tape casting.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. An alumina ceramic casting slurry comprises the following components in percentage by mass:
the powder consists of alumina ceramic powder and glass powder;
the binder includes one or more of polyvinyl butyral, acrylic resin, cellulose acetate-butyrate, and methylcellulose.
2. The alumina ceramic casting slurry according to claim 1, wherein the mass ratio of the alumina ceramic powder to the glass frit is (90 to 95): 5 to 10.
3. The alumina ceramic casting slurry according to claim 1 or 2, wherein the purity of the alumina ceramic powder is 99% or more.
4. The alumina ceramic casting slurry according to claim 1 or 2, wherein the alumina ceramic powder has a particle size of 1.5 to 4.8 μm; the particle size of the glass powder is 2-5 mu m.
5. The alumina ceramic casting slurry according to claim 1 or 2, wherein the glass frit comprises one or more of boron oxide, silicon oxide, calcium oxide, titanium oxide, zirconium oxide, lanthanum oxide, and magnesium oxide.
6. The alumina ceramic casting slurry according to claim 1, wherein the dispersant comprises one or more of phosphate esters, glycerides, sodium silicate, sodium carbonate, ammonium polyphosphate, polymethacrylic acid, and castor oil.
7. The alumina ceramic casting slurry according to claim 1, wherein the plasticizer comprises one or more of oxalic acid diacetic acid, polyethylene glycol, dibutyl phthalate, and butyl benzyl phthalate.
8. The method for preparing an alumina ceramic casting slurry according to any one of claims 1 to 7, comprising the steps of:
mixing powder, an organic solvent, a dispersing agent and a plasticizer, and performing one-stage ball milling to obtain mixed slurry; and mixing the mixed slurry with a binder, and performing two-stage ball milling to obtain the alumina ceramic casting slurry.
9. The method for preparing alumina ceramic casting slurry according to claim 8, wherein the rotational speed of the one-stage ball milling is 20-40 r/min, and the time of the one-stage ball milling is 10-16 h; the rotating speed of the secondary ball milling is 20-40 r/min, and the time of the secondary ball milling is 20-26 h.
10. An alumina ceramic green tape prepared from the alumina ceramic casting slurry according to any one of claims 1 to 7 or the alumina ceramic casting slurry prepared by the preparation method according to any one of claims 8 to 9 by casting molding.
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