CN1233593C - Water-based gel casting forming method for thin ceramic blank sheet - Google Patents
Water-based gel casting forming method for thin ceramic blank sheet Download PDFInfo
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- CN1233593C CN1233593C CN 02153278 CN02153278A CN1233593C CN 1233593 C CN1233593 C CN 1233593C CN 02153278 CN02153278 CN 02153278 CN 02153278 A CN02153278 A CN 02153278A CN 1233593 C CN1233593 C CN 1233593C
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Abstract
The present invention belongs to the technical field of inorganic nonmetallic materials, and relates to a new water base gelatinization casting molding method for a thin ceramic blank sheet. The method of the present invention comprises the technology steps of material preparation, ball milling, addition of an organic monomer, a crosslink agent, a binding agent and a plasticizing agent, stirring, gelatinization, casting operation and gelatinization drying. In the method of the present invention, the advantages of low pollution and low cost of water base casting and the advantages of rapid film formation, rapid drying, less organic substance dosage, etc. of gelatinization casting are combined, and the industrialized production of water base gelatinization casting is realized.
Description
Technical field.
The invention belongs to technical field of inorganic nonmetallic materials.Relate to a kind of thin ceramic base sheet aqueous gel tape casting process novel molding method.
Background technology.
Flow casting molding (Tape Casting) is a kind of forming method that can prepare high quality, ultra-thin type ceramic substrate.Through the development of decades, it has realized increasingly automatedly at present, and technical maturity is stable, highly efficient in productivity, can successfully be used for the moulding that thickness is 0.025～1.27mm ceramic green sheet.But what traditional casting molding processes adopted is to have certain toxic organic solvent (benzene,toluene,xylene), to serious environment pollution and production cost is improved, and still have a large amount of organism in the base substrate after the moulding, shrinkage strain is big in follow-up skimming processes, cause base sheet cracking easily, limited its some application.Therefore, people's water-based tape casting system that begins one's study replaces organic curtain coating system.The water system curtain coating have hypotoxicity, nonflammable, environmental pollution is little, low cost and other advantages.Laboratory study has now obtained bigger progress, has developed corresponding tackiness agent, dispersion agent, softening agent etc., and the technological processs such as preparation, curtain coating, drying and sintering of slip have been carried out systematic research.But because the volatilization of the aqueous solvent of water system curtain coating is too slow, thus can only be used for the very moulding of thin stock sheet at present, and also production efficiency is very low, becomes the major cause of restriction water system curtain coating widespread use.In addition, the spendable adhesive strength of water system curtain coating is lower, and the crack sensitivity of base sheet is higher, and slip bubbles easily and gets rid of difficulty, and these all await further improving perfect.The aqueous gel tape casting process method of forming, in the organic monomer aqueous solution, add solid powder and dispersion agent, the slip of making high solid loading and having certain flowability, add initiator and catalyzer again, carry out flow casting molding, 40 ℃～80 ℃ trigger monomer polyreactions, the polymer formation network structure makes the slip film-forming, reaches the moulding purpose.But this technology can not realize that on general casting machine gas shield has also increased technology difficulty and production cost because oxygen inhibition need carry out protection of inert gas.So far, water system curtain coating technology still mainly is in the laboratory study stage, and suitability for industrialized production is still needed and will further be worked.
Summary of the invention.
The objective of the invention is: propose a kind of thin ceramic base sheet aqueous gel tape casting process forming method that is suitable for suitability for industrialized production, overcome the shortcoming that traditional water-based tape casting and aqueous gel tape casting process method exist, and with water-based tape casting low pollute, cheaply advantage, fast drying fast, organism consumption with the gel casting film-forming less etc. advantages get up, realized the suitability for industrialized production of aqueous gel tape casting process.
Technical scheme of the present invention is: a kind of thin ceramic base sheet aqueous gel tape casting process forming method is characterized in that this method adopts following processing step:
(1) batching and ball milling add ceramic powder and dispersion agent and are made into the water slip in the entry and carry out ball milling, and ratio of grinding media to material is: 1: 1～5: 1, the add-on of water was 10～100% of a ceramic powder weight, and the ball milling time is 2～100 hours;
(2) add organic monomer and linking agent, preceding 0.5～15 hour of discharging, in slip, add organic monomer and linking agent, organic monomer is acrylamide, Methacrylamide or n-vinyl arsenic pyrrolidone, linking agent is methylene-bisacrylamide or many ethylene glycol dimethyl acrylamide, total add-on of organic monomer and linking agent is 2～10% of a ceramic powder weight, and the weight ratio of organic monomer and linking agent is 5: 1～40: 1;
(3) add binding agent, softening agent, in slip, add water-based tape casting after the discharging with binding agent and mix, binding agent is polyvinyl alcohol, ether of cellulose or ACRYLIC EMULSION, the consumption of binding agent is 1～40% of a ceramic powder weight, for the snappiness that increases the base sheet is adding softening agent in slip after the discharging, softening agent is glycerine, polyoxyethylene glycol, polyether glycol and phthalate or their combination, and the add-on of softening agent is 0.1～10% of a slip weight;
(4) stir, slip put into agitator, stir 2～30 hours with 30～150 rev/mins speed after, vacuumize or vibrated de-bubble 10～30 minutes;
(5) gel, one of them makes the slip after the degasification realize gel to adopt following two kinds of methods,
Party A's method: in slip, add initiator and catalyzer, initiator is one of following material: ammonium persulphate, Potassium Persulphate or tetrazo [ether propane] hydrochloric acid, the aqueous solution that initiator is made into 5～20% weight ratios uses, and the add-on of initiator solution is 0.5～15% of an organic monomer weight; Catalyzer is a Tetramethyl Ethylene Diamine, and add-on is 0.1～4% of an organic monomer weight;
Party B's method: in slip, add the oxidation-reduction solution of preparation in advance, the add-on of oxidation-reduction solution is 0.1～10% of an organic monomer weight, oxidation-reduction solution is solvent with water, oxygenant is one of the following material or the mixture of two kinds of materials wherein: ammonium persulphate, Potassium Persulphate, Sodium Persulfate, reductive agent is one of them or wherein several mixture of following material: ammonium sulphite, S-WAT, potassium sulfite, sodium bisulfite, Sulfothiorine, the gross weight of reductive agent and oxygenant be water weight 2～20%, wherein the weight ratio of reductive agent and oxygenant is 1: 5～5: 1;
(6) curtain coating operation is injected casting machine with slip and is carried out the curtain coating operation;
(7) gel oven dry, slip becomes ceramic green sheet after 40～80 ℃ of following gels and oven dry.
Advantage of the present invention is: on traditional water-based tape casting basis, in slip, add the organic monomer that home position polymerization reaction can take place, in the curtain coating process, realize the curing molding of base sheet by the effect polymerization reaction take place of initiator and catalyzer, shortened time of drying greatly, improve production efficiency, also avoided the distortion, the problems of crack that occur easily in traditional curtain coating drying process.And the existence of water-based tape casting binding agent guaranteed the film forming of base sheet surface in drying process, overcome gelation process oxygen inhibition problem, do not need protection of inert gas, simplified technology and also reduced cost.Simultaneously, the introducing of polyreaction has significantly reduced the consumption of organic binder bond, has reduced production cost, also can improve base sheet density, helps the raising of base tablet quality.
Below the present invention is described in further details.At first the technology according to the traditional ceramics slip is made into slip with required ceramic powder and water, guarantees abundant dispersion and the suspension and the suitable rheological characteristics of powder under enough ball millings.Stir adding organic monomer and linking agent after the discharging, and the curtain coating binding agent.Ball milling can influence the usefulness of binding agent, equally also should avoid long-time vigorous stirring.For increasing the snappiness of base sheet, can in slip, add softening agent.The bubble in the slip is discharged in vacuum stirring or vibration degasification then, avoids forming defective in the base sheet after moulding, influences its performance.In ready slip, add initiator, catalyzer or redox solution, carry out the curtain coating operation after mixing, slip is film-forming under monomeric polyreaction, be subjected to oxygen influence the inadequate surface of polymerization in drying process subsequently by also film forming gradually under the assistance of binding agent.By gelation rate and bake out temperature, the control of time, can guarantee the coupling of the speed of polymerization film formation and drying and forming-film, obtain not having layering, the complete base sheet of no strain cracking.
Embodiment.
The moulding of embodiment 1:96 alumina ceramic substrate aqueous gel tape casting process
In 60 ml waters, add 450 grams, 96 alumina ceramics raw materials, add the ammonium polyacrylate dispersion agent of 1 gram, be made into ceramic water slip.Slurry ball-milling is mixed 36 hours.In discharging preceding 5 hours, add 18 gram acrylamide monomers and 0.6 gram methylene-bisacrylamide.After the discharging, add polyvinyl alcohol water solution (solid content 15%) 40 grams, stirring at low speed final vacuum de-bubble in 8 hours.In slip, add 0.4 milliliter of ammonium persulfate aqueous solution and 0.2 milliliter of Tetramethyl Ethylene Diamine solution.70 ℃ of following gel formings are also dried and are obtained the base sheet that thickness range is 0.2～2mm on casting machine.
Embodiment 2: the moulding of zirconia ceramics substrate aqueous gel tape casting process
In 60 ml waters, add 360 gram yttrium oxide PSZ porcelains, add 1.2 milliliters JA281 dispersion agent, be made into ceramic water slip.Slurry ball-milling is mixed 25 hours.In discharging preceding 6 hours, add 14 gram acrylamide monomers and 1 gram methylene-bisacrylamide.After the discharging, add ACRYLIC EMULSION (solid content 50%) 60 grams, glycerine 8.0g, stirring at low speed final vacuum de-bubble in 10 hours.In slip, add 0.3 milliliter of ammonium persulfate aqueous solution and 0.2 milliliter of Tetramethyl Ethylene Diamine solution.80 ℃ of following gel formings are also dried and are obtained the base sheet that thickness is 0.4mm on casting machine.
Embodiment 3: the moulding of cyanines green stone ceramic substrate aqueous gel tape casting process
With talcum, aluminum oxide and silicon oxide is raw material, and formulated pottery porcelain 500 grams according to cyanines green stone ceramic substrate join in 75 ml waters, add 2.0 milliliters D3021 dispersion agent, are made into ceramic water slip.Slurry ball-milling is mixed 60 hours.In discharging preceding 10 hours, add 20 gram methyl acrylamide monomers and 0.8 gram methylene-bisacrylamide.After the discharging, add hydroxy ethyl fiber cellulose solution (solid content 15%) 80 grams, stirring at low speed final vacuum de-bubble in 12 hours.In slip, add 0.5 milliliter of Diisopropyl azodicarboxylate and 0.2 milliliter of Tetramethyl Ethylene Diamine solution.60 ℃ of following gel formings are also dried and are obtained the base sheet that thickness is 0.3mm on casting machine.
Embodiment 4: the moulding of lead zirconate-titanate ceramic substrate aqueous gel tape casting process
Take by weighing Pb-based lanthanumdoped zirconate titanates powder 300 gram, add the D3021 dispersion agent of 68 ml waters and 1.4 milliliters, be made into ceramic water slip.Slip was carried out ball milling mixed 48 hours with zirconia ball.In discharging preceding 4 hours, add 18 gram acrylamide monomers and 1.8 gram methylene-bisacrylamides.After the discharging, add Duramax B-1070 solution (solid content 44%) 26 grams, polyoxyethylene glycol 2.0g, stirring at low speed final vacuum de-bubble in 18 hours.In slip, add oxidation-reduction and cause 0.2 milliliter of solution.60 ℃ of following gel formings are also dried and are obtained the base sheet that thickness is 0.6mm on casting machine.
Claims (1)
1, a kind of thin ceramic base sheet aqueous gel tape casting process forming method is characterized in that this method adopts following processing step:
(1) batching and ball milling add ceramic powder and dispersion agent and are made into the water slip in the entry and carry out ball milling, and ratio of grinding media to material is: 1: 1～5: 1, the add-on of water was 10～100% of a ceramic powder weight, and the ball milling time is 2～100 hours;
(2) add organic monomer and linking agent, preceding 0.5～15 hour of discharging, in slip, add organic monomer and linking agent, organic monomer is acrylamide, Methacrylamide or n-vinyl arsenic pyrrolidone, linking agent is methylene-bisacrylamide or many ethylene glycol dimethyl acrylamide, total add-on of organic monomer and linking agent is 2～10% of a ceramic powder weight, and the weight ratio of organic monomer and linking agent is 5: 1～40: 1;
(3) add binding agent, softening agent, in slip, add water-based tape casting after the discharging with binding agent and mix, binding agent is polyvinyl alcohol, ether of cellulose or ACRYLIC EMULSION, the consumption of binding agent is 1～40% of a ceramic powder weight, for increasing the snappiness of base sheet, adding softening agent after the discharging in slip, softening agent is glycerine, polyoxyethylene glycol, polyether glycol and phthalate or their combination, and the add-on of softening agent is 0.1～10% of a slip weight;
(4) stir, slip put into agitator, stir 2～30 hours with 30～150 rev/mins speed after, vacuumize or vibrated de-bubble 10～30 minutes;
(5) gel, one of them makes the slip after the degasification realize gel to adopt following two kinds of methods,
Party A's method: in slip, add initiator and catalyzer, initiator is one of following material: ammonium persulphate, Potassium Persulphate or tetrazo [ether propane] hydrochloric acid, the aqueous solution that initiator is made into 5～20% weight ratios uses, and the add-on of initiator solution is 0.5～15% of an organic monomer weight; Catalyzer is a Tetramethyl Ethylene Diamine, and add-on is 0.1～4% of an organic monomer weight;
Party B's method: in slip, add the oxidation-reduction solution of preparation in advance, the add-on of oxidation-reduction solution is 0.1～10% of an organic monomer weight, oxidation-reduction solution is solvent with water, oxygenant is one of the following material or the mixture of two kinds of materials wherein: ammonium persulphate, Potassium Persulphate, Sodium Persulfate, reductive agent is one of them or wherein several mixture of following material: ammonium sulphite, S-WAT, potassium sulfite, sodium bisulfite, Sulfothiorine, the gross weight of reductive agent and oxygenant be water weight 2～20%, wherein the weight ratio of reductive agent and oxygenant is 1: 5～5: 1;
(6) curtain coating operation is injected casting machine with slip and is carried out the curtain coating operation;
(7) gel oven dry, slip becomes ceramic green sheet after 40～80 ℃ of following gels and oven dry.
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| CN 02153278 CN1233593C (en) | 2002-11-26 | 2002-11-26 | Water-based gel casting forming method for thin ceramic blank sheet |
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| CN 02153278 CN1233593C (en) | 2002-11-26 | 2002-11-26 | Water-based gel casting forming method for thin ceramic blank sheet |
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Cited By (1)
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| TWI747694B (en) * | 2020-12-31 | 2021-11-21 | 遠東科技大學 | Method for fabricating zirconia ceramics by aqueous gel-casting technology |
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| CN1317234C (en) * | 2005-10-26 | 2007-05-23 | 北京科技大学 | Ceramic part gel injection moulding forming method realized by cellulose ether heat gel reaction |
| CN100387679C (en) * | 2005-12-13 | 2008-05-14 | 刘伟 | Antifreezing type filtrate reducer and its preparation method |
| CN100398491C (en) * | 2006-11-28 | 2008-07-02 | 武汉理工大学 | Silicon nitride non-aqueous tape-casting slurry and its preparation method |
| CN101265086B (en) * | 2008-04-11 | 2011-01-19 | 华中科技大学 | Method for forming water-base casting of sheet-type positive temperature coefficient thermal sensitive ceramic |
| CN101302117B (en) * | 2008-05-20 | 2011-05-11 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation of ordered big hole porous ceramic film material |
| US20100028674A1 (en) * | 2008-07-31 | 2010-02-04 | Fredrick O Ochanda | Nanofibers And Methods For Making The Same |
| CN102085688B (en) * | 2010-11-29 | 2013-02-20 | 中国航空工业集团公司北京航空材料研究院 | Method for precisely shaping non-water-base injection molding gel of ceramic body |
| CN102173821A (en) * | 2011-01-25 | 2011-09-07 | 景德镇陶瓷学院 | Method for performing in-situ polymerization on surfaces of yttria-stabilized zirconia (YSZ) particles to obtain water system tape-casting slurry with high solid content by adopting initiator |
| CN102219516A (en) * | 2011-03-17 | 2011-10-19 | 景德镇陶瓷学院 | Preparation method for high solid content aqueous tape-casting slurry of cerium oxide-based ceramic particles |
| CN103056958A (en) * | 2012-12-29 | 2013-04-24 | 贵州振华红云电子有限公司 | Method for preparing piezoelectric ceramic piece green compact by using aqueous tape casting |
| BR112015023159A2 (en) * | 2013-03-15 | 2017-07-18 | Gen Electric | fluid paste composition, malleable non-flammable tape and process of using fluid paste composition |
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| CN106699192B (en) * | 2017-02-24 | 2020-08-28 | 中南大学 | Functional ceramic gel casting slurry and preparation method thereof |
| CN108793144B (en) * | 2018-06-13 | 2020-10-20 | 中国航发北京航空材料研究院 | Graphene porous membrane gel casting preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI747694B (en) * | 2020-12-31 | 2021-11-21 | 遠東科技大學 | Method for fabricating zirconia ceramics by aqueous gel-casting technology |
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