CN1775708A - Method for precission shaping ceramic blank by semi-water-base injection-moulding gel process - Google Patents
Method for precission shaping ceramic blank by semi-water-base injection-moulding gel process Download PDFInfo
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Abstract
The invention belongs to the field of inorganic material, relating to the improvement of a ceramic blank precision molding technique. The steps of the invention includes: mixing, blending and ball-milling, eliminating gas, adding in catalyst or reducing agent, adding in initiator, injection molding and gelating, and demolding and drying. The invention uses less water, thoroughly eliminates organic matter, reduces the blank shrinkage and avoids larger-sized ceramic blanks from cracking in the drying course. Besides, the gelated blanks have better machining property before glycol, glycerine, and other solvents are eliminated.
Description
Technical field
The invention belongs to field of inorganic materials, relate to a kind of improvement of ceramic body precision molding technology.
Background technology
Earlier 1990s, organic slip gel-casting forming technique (U.S Patent 4894194 of ceramic body has successively invented in U.S. Oak Ridge National Key Laboratory, 1990) and aqueous slurries gel-casting forming technique (U.S Patent 5028362,1991).This technology combines traditional ceramic body injection forming technology with the polymer chemistry theory, can form the organic monomer of gelinite and linking agent and organic solvent or water and be mixed with premixed liquid, with be mixed with ceramic slurry after ceramic powder mixes, be poured in the mould of ne-leakage and make it in-situ polymerization under certain condition, form the gelinite of cross key structure and make the ceramic body typing, therefore applicable to the precise forming of the ceramic body of various complicated shapes.Comparatively speaking, organic slip gel-casting forming technique is because of adopting dibutyl phthalate as solvent.Itself viscosity is higher, is difficult to make the ceramic slurry of high solid loading and good fluidity, and the solvent price is higher in addition, does not see the report of successful Application so far.And aqueous slurries is solvent with water, and not only cost is low, and is low in the pollution of the environment, and because the invention of multiple efficient water soluble dispersion agent application in recent years, be easy to make the slip of high ceramic powder volume component, therefore get more and more people's extensive concerning, and obtained successful Application in some field.
Yet the ceramic body of aqueous slurries gel-casting moulding certainly leads to certain shrinking percentage in the process of dehydrating.When the base substrate size is big, because the moisture of gel billet surface volatilizees at first, the space that the contraction result will originally be communicated with is from the billet surface shutoff, cause the moisture of base substrate inside to be difficult to remove smoothly, the way that patent U.S.Patent 5028362 provides is that the base substrate behind the gel is placed warm and humid loft drier, reduce the relative humidity of loft drier gradually, the moisture in the base substrate is removed from inside to outside gradually.Practice shows that this process is quite slow, and still is difficult to guarantee that the moisture of base substrate inside fully deviates from when low for larger-size base substrate or ceramic powder volume component, so that causes base substrate spalling damage in dry and the sintering process.This also is that aqueous slurries gel-casting forming technique is difficult to one of major obstacle of using in the achieving success of large-size ceramic part always in recent years.
Summary of the invention
The present invention seeks to: propose a kind of half water base gel-casting forming ceramic base substrate new technology, by in aqueous slurries, adding a certain amount of and the water not volatilization simultaneously and the alcohol organic solvent of infinitely dissolving each other with water, under the situation that does not influence slip solid load and gelation, realize the gel-casting precise forming of base substrate, simplify the process that dehydrates of base substrate, guarantee fully removing of moisture and organic solvent in the base substrate, avoid rimose danger in the dry and sintering process of large-size ceramic part.
Technical scheme of the present invention is: a kind of half water base gel-casting method method for precisely forming of ceramic body, it is characterized in that,
1, batching: according to the moulding requirement of the ceramic body that is disposed, the accurate various ceramic powders of weighing; Weighing water and water-miscible organic solvent to scale, this organic solvent is the mixing of one or several material of following material: methyl alcohol, ethanol, ethylene glycol, glycerol, the ratio of itself and water is 0.05: 1～1: 1; Take by weighing dispersion agent, it is one of following material: polyacrylate, poly-methyl acrylate, carboxylate salt, Citrate trianion, its add-on are 0.2～2% of ceramic powder weight; Take by weighing organic monomer and linking agent, organic monomer is water miscible acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of water and an alcoholic solvent total amount;
2, mixing and ball milling: above-mentioned ceramic powder, water and alcohol organic solvent, dispersion agent, organic monomer and linking agent are put into ball mill thorough mixing ball milling, form half water base ceramic slurry, the ball milling time is 2～30 hours, ratio of grinding media to material: 1: 1～4: 1;
3, degasification: the half water base ceramic slurry that mixing and ball milling is good takes out the back and carries out degasification by vacuum stirring or method for oscillating, and the time is 1～10 minute;
4, add catalyzer or reductive agent: add the reductive agent ammonium sulphite aqueous solution of catalyzer Tetramethyl Ethylene Diamine or 5～50% in half water base ceramic slurry, stir, catalyzer or the sharp add-on of reduction are 0.05～1% of organic monomer weight;
5, add initiator: add the initiator ammonium persulfate aqueous solution in above-mentioned slip, concentration is 5～20%, stirs, and the add-on of initiator is 0.2～0.8% of an organic monomer weight;
6, gel-casting: above-mentioned slip is injected ready mould, and mould should use to impermeable metal, glass, plastics or the manufacturing of wax material material, at room temperature places 3～30 minutes, and slip can be finalized the design by gel in the mould;
7, demoulding drying: after the slurry gel process was finished, ceramic gel base substrate was taken out in die sinking, places air, and seasoning at ambient temperature places baking oven further to dry under 150～200 ℃ of conditions then and gets final product.
Advantage of the present invention is: solved large-size ceramic blank drying process problem easy to crack, and made the simplification that becomes of its drying process, its advantage mainly shows as:
1. compare with patent U.S Patent 4894194 organic slip gel-casting forming ceramic base substrate technology.Because adopting water and alcohols material is solvent, its viscosity is far below dibutyl phthalate, substantially the characteristics that kept water base ceramic slurry are easy to dispose half water base ceramic slurry of high ceramic powder volume component and good fluidity, and cost of material is also relatively cheap simultaneously.
2. compare with patent U.S.patent 5028362 aqueous slurries gel-casting forming ceramic base substrate technology, owing to introduced with the viscosity of water is basic identical but the alcohols material that volatilization point is different, under the situation of the half water base ceramic slurry that does not influence high ceramic powder volume component of preparation and good fluidity, because of the consumption of water reduces relatively, make also minimizing relatively of shrinking percentage in the ceramic blank drying process, can guarantee that moisture can fully be got rid of in the base substrate, it is dangerous and simplify drying process to have avoided large-size ceramic blank drying process to be easy to rimose.
3. because alcohols material partly replaces water, the surface force of bubble is reduced and be easy to and remove, so need not add defoamer in the slip again and can easier eliminate bubble, the ceramic body defective that obtains behind the gel still less.
4. when adopting the volatilization point temperature to be higher than the alcohols material of water such as ethylene glycol, glycerol (its volatilization point temperature is near 200 ℃), after moisture in the wet gel ceramic body is got rid of, has the favorable mechanical processibility, further processing obtains the more complicated ceramic part base substrate of shape as need, can carry out mechanical workout at this moment, place baking oven to remove ethylene glycol or glycerol equal solvent then.Mould design processing can be simplified like this, and the more complicated accurate ceramic part base substrate of shape can be prepared.
5. contain in the employed ceramic powder and be easy to hydrolysis and increase the raw material of viscosity such as magnesiumcarbonate, magnesium basic carbonate, during materials such as lanthanum trioxide, aluminium nitride, wolfram varbide, can be with the ball milling refinement in alcoholic solvent of these raw materials, and will be not ball milling refinements in water solvent such as the raw material of facile hydrolysis such as aluminum oxide, zirconium white, yttrium oxide, strontium titanate, silicon carbide, silicon nitride, being blended together in short-term at last, ball milling mixes and can use, avoided being easy to the problem that hydrolysis material increases slip viscosity, this has just enlarged raw-material use range.
Embodiment
Below the present invention is described in further details.Processing step of the present invention is as follows:
1, batching: according to the moulding requirement of the ceramic body that is disposed, the accurate various ceramic powders of weighing; Weighing water and water-miscible organic solvent to scale, this organic solvent is the mixing of one or several material of following material: methyl alcohol, ethanol, ethylene glycol, glycerol, the ratio of itself and water is 0.05: 1～1: 1, and these materials and water infinitely dissolve each other, low viscosity and do not influence the gelation of slip; Take by weighing dispersion agent, it is one of following material: polyacrylate, poly-methyl acrylate, carboxylate salt, Citrate trianion, its add-on are 0.2～2% of ceramic powder weight; Take by weighing organic monomer and linking agent, organic monomer is water miscible acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of water and an alcoholic solvent total amount.
2, mixing and ball milling: above-mentioned ceramic powder, water and alcohol organic solvent, dispersion agent, organic monomer and linking agent are put into ball mill thorough mixing ball milling, form half water base ceramic slurry, the ball milling time is 2～30 hours, ratio of grinding media to material: 1: 1～4: 1.
When mixing and ball milling, in employed ceramic powder, contain raw material such as the magnesiumcarbonate that is easy to hydrolysis and increases slip viscosity, magnesium basic carbonate, lanthanum trioxide, aluminium nitride, during materials such as wolfram varbide, can be with the independent mixing and ball milling refinement of said pure type organic in these raw materials and 1.1, with the not raw material such as the aluminum oxide of facile hydrolysis, zirconium white, silicon oxide, yttrium oxide, barium titanate, silicon carbide, silicon nitride etc. place and contain dispersion agent, organic monomer, ball milling refinement in the aqueous solution of linking agent mixes two kinds of slips in short-term that mix grinding evenly gets final product then, and the mix grinding time is no more than 1 hour.
3, degasification: the half water base ceramic slurry that mixing and ball milling is good takes out the back and carries out degasification by vacuum stirring or method for oscillating, and the time is to get final product in 1～10 minute.
4, add catalyzer or reductive agent: the reductive agent ammonium sulphite aqueous solution that in half water base ceramic slurry, adds catalyzer Tetramethyl Ethylene Diamine or 5～50%, its concentration is, stir, the add-on of catalysis profit or reductive agent is 0.05～1% of an organic monomer weight.
5, add initiator: add the initiator ammonium persulfate aqueous solution in above-mentioned slip, concentration is 5～20%, stirs, and the add-on of initiator is 0.2～0.8% of an organic monomer weight.
6, gel-casting: above-mentioned slip is injected ready mould, and mould should use to impermeable metal, glass, plastics or the manufacturing of wax material material, at room temperature places 3～30 minutes, and slip can the gel typing in the mould.
7, demoulding drying: after the slurry gel process is finished, ceramic gel base substrate is taken out in die sinking, place air, seasoning at ambient temperature, the alcoholic solvent of eliminating low volatilization point is methyl alcohol and ethanol etc. and part moisture for example, place baking oven further oven dry under 150～200 ℃ of conditions then, get rid of all moisture and high volatilization point kind solvents in the ceramic body, obtain solvent-free ceramic body at last.
Embodiment
Embodiment 1, large size 95% alumina-ceramic blank forming.
Take by weighing 1000g by α-Al
2O
3, the 95% alumina-ceramic powder formed of kaolin and lime carbonate, add the 100ml deionized water, 40ml ethylene glycol, 10ml ethanol, 10ml ammonium polyacrylate dispersion agent, 1.5g acrylamide organic monomer, 25g methylene-bisacrylamide linking agent, place the roller milling machine, add the 1200g abrading-ball simultaneously, mix grinding took out slip after 18 hours, after vibration removes bubble, the ammonium persulfate initiator aqueous solution that adds 8% pre-configured concentration of 2ml Tetramethyl Ethylene Diamine catalyzer and 4ml, stir, the cast forward (FWD) has in Φ 80 * 80mm nylon mould of cast gate.Placed slurry gelization 10 minutes.The gel base substrate is taken out from mould, fall cast gate, be placed under the air natural condition dry 24 hours, place baking oven then, vapor away ethylene glycol in 200 ℃ of insulations 8 hours with graduating with cutter.This moment base substrate shrinking percentage diametric(al) be 0.8%, short transverse 0.9%.1560 ℃ of sintering 3 hours, density reach 3.77g/cm in air furnace
3, the complete nothing cracking of sample.
Embodiment 2, the precise forming of large-scale silicon nitride ceramic body.
Take by weighing the beta-silicon nitride powder that the 300g median size is 1.4um, add the 80ml deionized water, 4.5ml ammonium polymethacrylate dispersion agent, 9g acrylamide organic monomer, 0.5g the methylene-bisacrylamide linking agent is adjusted slip pH=9 with Tetramethylammonium hydroxide, places ball grinder 1, add the 500g abrading-ball simultaneously, 10 hours ball milling time; Take by weighing 24g yttrium oxide and 24g lanthanum trioxide powder in addition, add 10ml ethylene glycol, 1ml ammonium polymethacrylate dispersion agent is put into ball grinder 2, adds the 100g abrading-ball simultaneously, ball milling 10 hours.Then the slip in the ball grinder 2 is poured in the ball grinder 1, continued to mix 0.5 hour.This moment the slip good fluidity, take out after the vacuum stirring degasification, add the ammonium sulphite reductive agent aqueous solution 2ml of 20% pre-configured concentration and the ammonium persulfate initiator aqueous solution 1.5ml of 8% concentration, the back cast forward (FWD) that stirs has in Φ 50 * 80mm nylon mould of cast gate, placed slurry gelization 15 minutes.The gel base substrate is taken out from mould,, be placed in the air seasoning 24 hours, place baking oven then, vapor away ethylene glycol in 200 ℃ of insulations 8 hours with the cast gate that lancinates.This moment, the base substrate shrinking percentage was a diametric(al) 1.0%, short transverse 1.0%, and the sample base substrate is intact.
Simultaneous test takes by weighing same silicon nitride, yttrium oxide, lanthanum trioxide powder.Add 90ml deionized water, 5.5ml ammonium polymethacrylate dispersion agent simultaneously.9g acrylamide organic monomer, 0.5g methylene-bisacrylamide linking agent, and adjust slip pH=9 with the Tetramethylammonium hydroxide adjustment, place ball grinder, add the 600g ball milling simultaneously, ball milling 10 hours, because the hydrolysis of lanthanum trioxide, slip is thickness very, replenishes to add the 20ml deionized water, continued ball milling 0.5 hour, take out slip through the vacuum stirring degasification, add same reductive agent and initiator, the back cast that stirs is advanced in the same mould, placed slurry gelization 22 minutes.Slip is taken out from mould, with the cast gate that lancinates, be positioned in the air seasoning 72 hours, this moment, the base substrate shrinking percentage was a diametric(al) 1.2%, and short transverse is 1.3%.But green body end face has depressed phenomenon, shows its inside defectiveness.
Embodiment 3, the precise forming of large size zirconia ball base substrate.
Taking by weighing the 200g median size is the partial stabilization zirconium oxide ceramic powder of 1.8um, adding 12ml goes from water, 8ml ethylene glycol, 1ml methyl alcohol, 3ml vinylformic acid and Sipacril 2739OF disperse sharp, 5g acrylamide organic monomer, 0.3g methylene-bisacrylamide linking agent is regulated pH=10 with ammoniacal liquor.Place the roller milling machine, add the 600g abrading-ball simultaneously.Ball milling took out slip after 15 hours, the ammonium persulfate aqueous solution initiator that adds 5% pre-configured concentration of 0.5ml Tetramethyl Ethylene Diamine catalyzer and 1ml after the vacuum stirring degasification, stir, cast is advanced in the Φ 60mm spherical set mould that has cast gate and production well of steel, placed slurry gelization 5 minutes.Ceramic Balls gel base substrate is taken out in die sinking, slices off cast gate and production well, is positioned under the air natural condition dry 24 hours, places baking oven to keep 2 hours in 150 ℃ then, is warming up to 200 ℃ again and keeps 5 hours, vapors away ethylene glycol.Base substrate shrinks evenly, and diametric(al) average line shrinking percentage is 0.6%, calcines 3 hours the complete nothing cracking of spheroid in air furnace for 1550 ℃.
The contrast experiment, other condition is identical, but adds the 21ml deionized water and do not add ethylene glycol and methyl alcohol.Base substrate is taken out in die sinking after the gelation, is placed under the air natural condition dry 72 hours base substrates and shrinks the part, back depression is arranged, and diametric(al) average line shrinking percentage is 1.1%, and 1550 ℃ of calcinings are 3 hours in air furnace, and spheroid damages from the recess cracking.
Embodiment 4, the precise forming of barium-strontium titanate ceramic thin slice base substrate.
Take by weighing 100g median size 0.5um strontium-barium titanate superfine powder, add the 12ml deionized water, 4ml ethylene glycol, the 1ml glycerol, 2ml vinylformic acid and Sipacril 2739OF dispersion agent, 3g acrylamide organic monomer, 0.1g methylene-bisacrylamide linking agent, regulate slip pH=9 with Tetramethylammonium hydroxide, place planetary ball mill, add the 200g abrading-ball simultaneously, ball milling took out slip after 4 hours, and vibration adds 0.1ml Tetramethyl Ethylene Diamine catalyzer and 5% pre-configured concentration ammonium persulfate aqueous solution initiator of 0.2ml after removing bubble, stir, cast is advanced in the mould of being made up of sheet glass that has the 0.2mm gap, places slurry gelization 8 minutes.The gel ceramic green sheet is taken in die sinking off, is put under the nylon cloth screen cloth air natural condition dry 10 hours, and this moment, the base sheet was smooth indeformable, and snappiness is good, can carry out Punching Technology.
The contrast experiment, other condition is identical, adds the 17ml deionized water and does not add ethylene glycol and glycerol.Take the gel ceramic green sheet after the gelation off and be put in equally under the nylon cloth screen cloth air natural condition dry 10 hours, this moment, the buckling deformation of base sheet was serious, and it is hard and crisp to become, and it is promptly broken to exert pressure a little.
Claims (2)
1, a kind of half water base gel-casting method method for precisely forming of ceramic body is characterized in that,
1.1, batching: according to the moulding requirement of the ceramic body that is disposed, accurate various ceramic powders of weighing; Weighing water and water-miscible organic solvent to scale, this organic solvent is the mixing of one or several material of following material: methyl alcohol, ethanol, ethylene glycol, glycerol, the ratio of itself and water is 0.05: 1～1: 1; Take by weighing dispersion agent, it is one of following material: polyacrylate, poly-methyl acrylate, carboxylate salt, Citrate trianion, its add-on are 0.2～2% of ceramic powder weight; Take by weighing organic monomer and linking agent, organic monomer is water miscible acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of water and an alcoholic solvent total amount;
1.2, mixing and ball milling: above-mentioned ceramic powder, water and alcohol organic solvent, dispersion agent, organic monomer and linking agent are put into ball mill thorough mixing ball milling, form half water base ceramic slurry, the ball milling time is 2～30 hours, ratio of grinding media to material: 1: 1～4: 1;
1.3, degasification: the half water base ceramic slurry that mixing and ball milling is good takes out the back and carries out degasification by vacuum stirring or method for oscillating, and the time is 1～10 minute;
1.4, add catalyzer or reductive agent: in half water base ceramic slurry, add catalyzer Tetramethyl Ethylene Diamine or concentration and be 5～50% the reductive agent ammonium sulphite aqueous solution, stir, the add-on of catalyzer or reductive agent is 0.05～1% of an organic monomer weight;
1.5, add initiator: add the initiator ammonium persulfate aqueous solution in above-mentioned slip, concentration is 5～20%, stirs, and the add-on of initiator is 0.2～0.8% of an organic monomer weight;
1.6, gel-casting: above-mentioned slip is injected ready mould, and mould should use to impermeable metal, glass, plastics or the manufacturing of wax material material, at room temperature places 3～30 minutes, and slip can the gel typing in the mould;
1.7, demoulding drying: after the slurry gel process was finished, ceramic gel base substrate was taken out in die sinking, places air, seasoning at ambient temperature, place then baking oven under 150～200 ℃ of conditions further oven dry get final product.
2, half water base gel-casting method accurate forming method according to claim 1, it is characterized in that, when mixing and ball milling, in employed ceramic powder, contain raw material such as the magnesiumcarbonate that is easy to hydrolysis and increases slip viscosity, magnesium basic carbonate, lanthanum trioxide, aluminium nitride, during materials such as wolfram varbide, can be with the independent mixing and ball milling refinement of the pure type organic of indication in these raw materials and 1.1, with the not raw material such as the aluminum oxide of facile hydrolysis, zirconium white, silicon oxide, yttrium oxide, barium titanate, silicon carbide, silicon nitride etc. place and contain dispersion agent, organic monomer, ball milling refinement in the aqueous solution of linking agent mixes two kinds of slips in short-term that mix grinding evenly gets final product then, and the mix grinding time is no more than 1 hour.
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| CN108975908A (en) * | 2018-08-29 | 2018-12-11 | 济南大学 | A kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder |
| CN110937895A (en) * | 2019-12-26 | 2020-03-31 | 淄博奥诺新材料科技有限公司 | Preparation method of zirconia sheet ceramic |
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