CN1172876C - Process for preparing ceramic sheet by water-base doctor blading method - Google Patents
Process for preparing ceramic sheet by water-base doctor blading method Download PDFInfo
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- CN1172876C CN1172876C CNB021252149A CN02125214A CN1172876C CN 1172876 C CN1172876 C CN 1172876C CN B021252149 A CNB021252149 A CN B021252149A CN 02125214 A CN02125214 A CN 02125214A CN 1172876 C CN1172876 C CN 1172876C
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- water
- latex
- add
- ceramic
- doctor blading
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- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000010345 tape casting Methods 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title description 4
- 239000004816 latex Substances 0.000 claims abstract description 30
- 229920000126 latex Polymers 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 25
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 19
- 239000000661 sodium alginate Substances 0.000 claims abstract description 19
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000000465 moulding Methods 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 239000004902 Softening Agent Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 10
- 239000004151 Calcium iodate Substances 0.000 claims description 9
- UHWJJLGTKIWIJO-UHFFFAOYSA-L calcium iodate Chemical group [Ca+2].[O-]I(=O)=O.[O-]I(=O)=O UHWJJLGTKIWIJO-UHFFFAOYSA-L 0.000 claims description 9
- 235000019390 calcium iodate Nutrition 0.000 claims description 9
- 230000001186 cumulative effect Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000007766 curtain coating Methods 0.000 claims description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 7
- VAJVDSVGBWFCLW-UHFFFAOYSA-N 3-Phenyl-1-propanol Chemical compound OCCCC1=CC=CC=C1 VAJVDSVGBWFCLW-UHFFFAOYSA-N 0.000 claims description 6
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 229920000193 polymethacrylate Polymers 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 5
- 239000003349 gelling agent Substances 0.000 abstract 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention discloses a method for preparing ceramic sheets through aqueous casting, which belongs to ceramic materials. In the method, a sodium alginate water solution and latex are firstly mixed and prepared into a premixing solution according to certain proportion; then, ceramic powder and a dispersing agent are added to the premixing solution, and a ceramic slurry material is prepared; after the ball milling and the mixture of the prepared ceramic slurry material are carried out, a gelling agent is added, and then, the vacuum pumping and the defoaming of the ceramic slurry material and the gelling agent are carried out; and the ceramic slurry material and the gelling agent are cast on a casting machine. The casting technology is easy to realize and is suitable for various ceramic powder materials, and the casting technology has quick drying speed. Molded block films have the advantages of high strength, good flexibility and uniformity.
Description
Technical field
The invention belongs to the stupalith field, particularly a kind of method of preparing ceramic sheet by water-base doctor blading.
Technical background
Flow casting molding is a kind of forming method that can obtain high quality, ultra-thin type ceramic substrate.The equipment that is characterized in is simple, process stabilizing, but operate continuously, and the production efficiency height can be realized increasingly automated.Divide by used solvent, casting technique can be divided into non-water system row and water-soluble serial two classes.From practical application, the casting technique comparative maturity of non-water system row, the ceramic sheet even structure of preparation, the intensity height, snappiness is good, is convenient to store and processing, is widely used.But since have in the solvent that non-water system row casting technique uses have a phenyl ring, have certain toxicity, contaminate environment, and cost is higher.And water-based tape casting adopts water as solvent, and organic content is low, and cost is low, and is harmless to HUMAN HEALTH, and Environmental compatibility is good.Therefore, research is subject to people's attention as solvent replace organic solvent system day by day with water.Present water-based flow casting technique patent is few, and great majority adopt water miscible polymer as binding agent.By the volatilization of aqueous solvent, make binding agent form network structure between ceramic particle during moulding, formation has certain intensity and flexible thin slice.But because evaporation of water speed is slower, dry difficulty, technological process is strong to dry link dependency, easily cause the base substrate shrinkage cracking in the drying process, and generation organic components Gradient distribution, solid load in the slurry is lower, and can not significantly reduce organic consumption in binding agent, the softening agent etc.At above-mentioned shortcoming, people's improved flow casting molding mechanism was once arranged, obtain the aqueous gel tape casting process moulding process of ceramic sheet by the superpolymer network structure of monomer polymerization reactions formation.This technology can avoid causing easily the dry link of moulding failure, obtains the curtain coating thin slice of better quality.Exist the monomer of oxygen inhibition and employing poisonous etc. but the main drawback of this technology is a monomer polymerization reactions, so the application of this technology is restricted.
Summary of the invention
The objective of the invention is to propose a kind of method of preparing ceramic sheet by water-base doctor blading, it is characterized in that: earlier the sodium alginate dissolving is sneaked in the casting slurry, add calcium iodate again, bring out sodium alginate gel as in mixing solutions, introducing calcium ion, thereby cause slurry in-situ solidifying film forming, moulding, and add an amount of latex, be used to improve the intensity of ceramic body.
Water-based tape casting prepares the moulding process of thin slice stupalith, mainly may further comprise the steps:
1). it is 1-3wt% solution that sodium alginate and water mixed dissolution are made concentration, adds an amount of latex and dispersion agent, and mixes; The latex consumption accounts for the 20-40vol% of sodium alginate soln and latex cumulative volume; The dispersant dosage that uses accounts for the 0.1-1wt% of ceramics powder; The Wt%=weight percent;
2). ceramic powder add contain dispersion agent the aqueous solution in, add an amount of softening agent then, prepare ceramic size.The ceramic powder volumn concentration is between 40-55% in the slurry; The softening agent add-on is the 1-3% of slurry cumulative volume;
3). with above-mentioned ceramic size mixing and ball milling 24-60 hour, add the gelifying agent of the 0.5-2wt% that accounts for ceramics powder and mix;
4). add defrother in the slurry that in 3, obtains, at room temperature vacuumize de-bubble then; The defrother add-on is the 1-2% of slurry cumulative volume;
5). the slurry curtain coating with after the de-bubble obtains casting films;
6). casting films is placed under 40-80 ℃, causes sodium alginate gel, can solidify demoulding through 30-90 minute.
Described latex be in complete third latex, phenylpropyl alcohol latex and second third latex three classes any one, two or three;
Described dispersion agent is a kind of in polyacrylic acid, ammonium polymethacrylate, ammonium citrate, the Tetramethylammonium hydroxide.
Described gelifying agent is a calcium iodate.
To be that in glycerine and the dibutyl phthalate one or both are compound be softening agent with described softening agent.
Described defrother is a tributyl phosphate, is used as film coalescence aid simultaneously to improve the quality of forming film of latex.
Beneficial effect of the present invention is:
1). make water as solvent, eliminated the problem of environmental pollution that with an organic solvent causes, can reduce production costs greatly and improve working conditions;
2). adopt nontoxic polymer as binding agent, can not damage human body;
3). the organism addition that is used for moulding is few, can exempt independent degreasing process, thereby shortens process cycle, reduces energy consumption and production costs;
4). slurry can reach higher solid load, and gained ceramic sheet density is higher;
5). because the in-situ solidifying of sodium alginate approaches the dead size moulding, almost there is not volumetric shrinkage;
6). reduced the dependence of technology, the ceramic body good uniformity to dry link;
7). demould time is shorter, has improved working efficiency;
Embodiment
The present invention is the method for preparing ceramic sheet by water-base doctor blading, it is earlier the sodium alginate dissolving to be sneaked in the casting slurry, add calcium iodate again, bring out sodium alginate gel as in mixing solutions, introducing calcium ion, thereby cause slurry in-situ solidifying film forming, moulding, and add an amount of latex, be used to improve the intensity of ceramic body.Moulding process of the present invention mainly may further comprise the steps:
1). it is 1-3wt% solution that sodium alginate and water mixed dissolution are made concentration, adds an amount of latex and dispersion agent, and mixes; The latex consumption accounts for the 20-40vol% of sodium alginate soln and latex cumulative volume; The dispersant dosage that uses accounts for the 0.1-1wt% of ceramics powder;
2). ceramic powder add contain dispersion agent the aqueous solution in, add an amount of softening agent then, prepare ceramic size.The ceramic powder volumn concentration is between 40-55% in the slurry; The softening agent add-on is the 1-3% of slurry cumulative volume;
3). with above-mentioned ceramic size mixing and ball milling 24-60 hour, add the gelifying agent of the 0.5-2wt% that accounts for ceramics powder and mix;
4). add defrother in the slurry that in 3, obtains, at room temperature vacuumize de-bubble then; The defrother add-on is the 1-2% of slurry cumulative volume;
5). the slurry curtain coating with after the de-bubble obtains casting films;
6). casting films is placed under 40-80 ℃, causes sodium alginate gel, can solidify demoulding through 30-90 minute.
In above-mentioned technology used latex be in complete third latex, phenylpropyl alcohol latex and second third latex three classes any one, two or three; Used dispersion agent is a kind of in polyacrylic acid, ammonium polymethacrylate, ammonium citrate, the Tetramethylammonium hydroxide; Used gelifying agent is a calcium iodate; Used softening agent is one or both the recombiner in glycerine and the dibutyl phthalate; Used defrother is a tributyl phosphate, is used as film coalescence aid simultaneously to improve the quality of forming film of latex.This casting technique is easy to realize, (comprises Al applicable to multiple ceramic powder
2O
3, ZrO
2, SiC, Si
3N
4Deng).The base sheet any surface finish of moulding, intensity height, snappiness are good, inner good uniformity.Further the present invention is illustrated for example below.
Embodiment 1
Add 1.2 gram sodium alginate stirring and dissolving in 40 ml waters and make solution, add 200 gram aluminum oxide powders and 1 gram polyacrylic acid dispersant after adding 10ml phenylpropyl alcohol latex, add glycerine 1.5ml, mixing and ball milling made ceramic size in 24 hours then; Add calcium iodate 2 grams, tributyl phosphate 1.5ml, curtain coating and curing under 60 ℃ obtain solidified base sheet after the de-bubble after 40 minutes.
Embodiment 2:
Add 0.3 gram sodium alginate stirring and dissolving in 30 ml waters and make solution, add phenylpropyl alcohol latex 20ml, 128 gram carborundum powder and 0.1 milliliter of Tetramethylammonium hydroxide dispersion agent then, add dibutyl phthalate 0.9ml, mixing and ball milling made ceramic size in 48 hours then; Add calcium iodate 2 grams, tributyl phosphate 1.8ml, curtain coating and curing under 40 ℃ obtain solidified base sheet after the de-bubble after 90 minutes.
Embodiment 3:
Add 0.6 gram sodium alginate stirring and dissolving in 30 ml waters and make solution, add 128 gram silicon nitride powder and 0.2 milliliter of Tetramethylammonium hydroxide dispersion agent after adding the complete third latex 20ml, add glycerine 1.2ml, mixing and ball milling made ceramic size in 60 hours then; Add calcium iodate 1 gram, tributyl phosphate 1.8ml, curtain coating and curing under 60 ℃ obtain solidified base sheet after the de-bubble after 60 minutes.
Embodiment 4:
Add 0.8 gram sodium alginate stirring and dissolving in 40 ml waters and make solution, add 300 gram zirconia powders and 1.5 gram ammonium citrate dispersion agents after adding phenylpropyl alcohol latex 10ml, add glycerine 2ml, mixing and ball milling made ceramic size in 36 hours; Add calcium iodate 2 grams, tributyl phosphate 1ml, curtain coating and curing under 80 ℃ obtain solidified base sheet after the de-bubble after 30 minutes.
Claims (6)
1. the method for a preparing ceramic sheet by water-base doctor blading, it is characterized in that: the moulding process that described water-based tape casting prepares the thin slice stupalith may further comprise the steps:
1). it is 1-3wt% solution that sodium alginate and water mixed dissolution are made concentration, adds latex and dispersion agent, and mixes; The latex consumption accounts for the 20-40vol% of sodium alginate soln and latex cumulative volume; The dispersant dosage that uses accounts for the 0.1-1wt% of ceramics powder;
2). ceramic powder adds and contains in the aqueous solution of dispersion agent, adds an amount of softening agent then, prepares ceramic size; The ceramic powder volumn concentration is between 40-55vol% in the slurry; The softening agent add-on is the 1-3vol% of slurry cumulative volume;
3). with above-mentioned ceramic size mixing and ball milling 24-60 hour, add the gelifying agent of the 0.5-2wt% that accounts for ceramics powder and mix;
4). add defrother in the slurry that in 3, obtains, at room temperature vacuumize de-bubble then; The defrother add-on is the 1-2vol% of slurry cumulative volume;
5). the slurry curtain coating with after the de-bubble obtains casting films;
6). casting films is placed under 40-80 ℃, causes sodium alginate gel, through 30-90 minute curing demoulding.
2. according to the method for the described a kind of preparing ceramic sheet by water-base doctor blading of claim 1, it is characterized in that: described latex be in complete third latex, phenylpropyl alcohol latex and second third latex three classes any one, two or three.
3. according to the method for the described a kind of preparing ceramic sheet by water-base doctor blading of claim 1, it is characterized in that: described dispersion agent is a kind of in polyacrylic acid, ammonium polymethacrylate, ammonium citrate, the Tetramethylammonium hydroxide.
4. according to the method for the described a kind of preparing ceramic sheet by water-base doctor blading of claim 1, it is characterized in that: described gelifying agent is a calcium iodate.
5. according to the method for the described a kind of preparing ceramic sheet by water-base doctor blading of claim 1, it is characterized in that: to be that in glycerine and the dibutyl phthalate one or both are compound be softening agent with described softening agent.
6. according to the method for the described a kind of preparing ceramic sheet by water-base doctor blading of claim 1, it is characterized in that: described defrother is a tributyl phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021252149A CN1172876C (en) | 2002-07-17 | 2002-07-17 | Process for preparing ceramic sheet by water-base doctor blading method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021252149A CN1172876C (en) | 2002-07-17 | 2002-07-17 | Process for preparing ceramic sheet by water-base doctor blading method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1390808A CN1390808A (en) | 2003-01-15 |
| CN1172876C true CN1172876C (en) | 2004-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021252149A Expired - Fee Related CN1172876C (en) | 2002-07-17 | 2002-07-17 | Process for preparing ceramic sheet by water-base doctor blading method |
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| Country | Link |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321091C (en) * | 2004-04-09 | 2007-06-13 | 中国航空工业第一集团公司北京航空材料研究院 | Solid-phase reacting synthesis of composite ceramic powder non-toxic gel |
| CN102745995A (en) * | 2011-04-22 | 2012-10-24 | 比亚迪股份有限公司 | Ceramics substrate preparation method |
| CN112209705A (en) * | 2020-10-27 | 2021-01-12 | 唐山恭成科技有限公司 | Water-based tape casting method of ceramic green tape |
| CN117303914B (en) * | 2023-11-30 | 2024-03-15 | 山东合创明业精细陶瓷有限公司 | Preparation method of plastic ceramic biscuit |
-
2002
- 2002-07-17 CN CNB021252149A patent/CN1172876C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1390808A (en) | 2003-01-15 |
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