CN104402522A - Method and device for preparing porous ceramic by heavy gas-protective direct-foaming technology - Google Patents
Method and device for preparing porous ceramic by heavy gas-protective direct-foaming technology Download PDFInfo
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Abstract
The invention belongs to the field of inorganic non-metallic materials and relates to a method and device for preparing porous ceramic by a heavy gas-protective direct-foaming technology. The method comprises preparing suspension slurry, carrying out vacuum bubble-removal, removing environment air by heavy gas, carrying out heavy gas-protective stirring foaming, carrying out pouring, carrying out demolding, carrying out drying and carrying out sintering. The foamed ceramic is prepared by heavy gas (such as argon or carbon dioxide)-protective stirring foaming and the water-based ceramic slurry foaming special-purpose device is designed. The method for preparing the foamed ceramic adopts a stirring foaming method adopting heavy gas to extrude air upward, utilizes simple equipment and is convenient for operation. The foamed ceramic slurry undergoes a free radical polymerization reaction for gelation curing, has a fast gelation rate, has uniform blank aperture distribution and is suitable for preparation of a porous ceramic material with apertures of 50-300 microns.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to method and device that the direct foaming of a kind of heavy gas shield prepares porous ceramics.
Background technology
Earlier 1990s, the Gelcasting Technique of ceramic body has been invented by Oak Ridge National Key Laboratory of the U.S., traditional organic base substrate injection forming technology combines with high molecular theory by this technology, the organic monomer of gelinite and linking agent and organic solvent or water can be formed and be configured to premixed liquid, ceramic slurry is mixed with after mixing with ceramic powder, be poured in the mould without infiltration and also make it in-situ polymerization under certain condition, form the gelinite of cross key structure and ceramic body is shaped, be applicable to the precise forming of the ceramic body of various complicated shape.But as a kind of Raolical polymerizable, contact with air due to during monomer polymerization, the oxygen in air can hinder polyreaction, therefore ceramic slurry is difficult to polymerization in air filled cavity.The problem of polyreaction is hindered in order to overcome Surface Oxygen; have patent to adopt nitrogen protection radical polymerization foaming to prepare porous ceramics, the method requires that gelation process is heating and curing (60 ~ 150 DEG C), and the gelation process time is long; cause the productive experiment cycle long, equipment requirements is high.
Summary of the invention
The object of the invention is to propose a kind of equipment requirements low, gelation process temperature is low, and the gelation process time short direct foaming of heavily gas shield prepares the method and apparatus of porous ceramics.
Technical scheme of the present invention is: according to the composition proportion of the porous ceramics of required preparation, and precise ceramic powder, takes deionized water, and the weight of deionized water accounts for 8 ~ 30% of ceramic powder weight; Take dispersion agent, the add-on of dispersion agent is 0.5% ~ 2% of ceramic powder weight; Take conditioning agent, the add-on of conditioning agent is 0.5% ~ 2% of ceramic powder weight; Take organic monomer and linking agent, the add-on of organic monomer is 0.5 ~ 4% of ceramic powder weight, the ratio of organic monomer and linking agent is between 10:1 ~ 30:1, ceramic slurry is formed by after above-mentioned component mixing, this ceramic slurry is put into ball grinder and carries out ball milling, ball milling 1h ~ 30h, ratio of grinding media to material is within the scope of 1:1 ~ 5:1; After discharging, aqueous-based ceramic slip under vacuum stirring condition bubble removing to bubble-free effusion; Then in slip, add tensio-active agent, its add-on is 0.1 ~ 10% of slip weight; Described slip is put into the cavity of heavily gas shield foam device, heavy gas passes in environmental chamber by ventpipe, gas flow > 500ml/min, time length >1min; Afterwards, regulate the under meter of heavily gas shield foam device, control gas flow >100ml/min<500ml/min, regulate the stirrer adjustment of rotational speed of heavily gas shield foam device to be 500 ~ 3000r/min, foamed time controls at 20 ~ 120 minutes; By tetramethyl-two aqueous ammoniums and ammonium persulfate aqueous solution from the feeding mouth instillation foamed ceramics slip of heavy gas shield foam device, after stirring 1 ~ 10min, in the mould that described foamed ceramics slip casting is made in the non-anti-coagulating action material of non-infiltration; Foamed ceramics slip completes gel solidification in envrionment temperature <40 DEG C, 5 ~ 60 minutes; Be positioned on screen cloth penetrating up and down after the foamed ceramics base substrate demoulding that gel solidification is completed, place and carry out drying in 5 ~ 30 days; Drying foamed ceramics base substrate shove charge is completely sintered, adopts the sintering schedule of slowly continuous warming stage by stage, ceramic body is sintered; Described heavily gas shield foam device comprises stirrer, agitator arm, slip container, CO
2gas cylinder or Ar gas cylinder, reducing valve, ventpipe, rubber seal, environmental chamber and environmental chamber upper cover, slip container is placed in environmental chamber, environmental chamber upper cover is obturaged by rubber seal, environmental chamber upper cover leaves give vent to anger gap and plup inlet, the agitator arm of stirrer is inserted in slip container by gap of giving vent to anger, CO
2the air outlet of gas cylinder or Ar gas cylinder is communicated with environmental chamber, and plup inlet is placed on environmental chamber and covers.
Described ceramic powder is one of following material: aluminum oxide, zirconium white, silicon nitride, silicon carbide, Mo Laishi; Dispersion agent is one of following material: polyacrylate, poly-methyl acrylate; Conditioning agent is one of following material: ammoniacal liquor, Tetramethylammonium hydroxide; Organic monomer is acrylamide or Methacrylamide, and linking agent is N, N methylene-bisacrylamide or many ethyleneglycol dimethacrylates; Tensio-active agent is alkyl benzene sulfonate anionic, plant proteins or animal proteinum class tensio-active agent, and various surfactants is compound.
The gap of giving vent to anger that the environmental chamber of described heavy gas shield foam device covers is annular, stirrer agitator arm and the gap L EssT.LTssT.LT0.2mm--1mm given vent to anger between gap.
Described catalyzer adopts the aqueous solution of tetramethyl-two ammoniums 20 ~ 100%, and initiator adopts the aqueous solution of ammonium persulphate 5 ~ 40%.
The mould that the non-anti-coagulating action material of described non-infiltration is made is metal, glass, dense plastics material.
The advantage that the present invention has and beneficial effect, the present invention adopt heavy gas upwards air-discharging method get rid of the air in slip environment, utilize gap between stirrer revolving bar and upper cover as production well cleverly, simplify the device of technological operation, ceramic slurry foamable gel in argon gas or carbon dioxide environment prepares porous ceramics base substrate, and the investigation and application for porous ceramic film material proposes new method.The present invention propose a kind of adopt heavy gas (molecular weight is greater than air molecular-weight average) argon gas, carbonic acid gas etc. upwards air-discharging method remove the method for the air-making in slip environment for porous ceramic film material; gelation process envrionment temperature requires <40 DEG C (temperature too high bubble unstable), this be different from before nitrogen protection method prepare the patented method (requiring temperature 60 ~ 150 DEG C) of porous ceramics.In foamed ceramics slip solidification process; heavy gas density is greater than the density of air, and not easily overflow from foam slurry surface, foam slurry is more stable for this reason; mould gelation process does not need additional shielding gas, and this is different from the method preparing porous ceramics with nitrogen protection method foaming.Therefore, the direct foaming of heavy gas is prepared porous ceramics method and is had the advantages such as gelling temp is low, gelation rate fast, foam stabilization, device are simple, easy to operate.
Accompanying drawing explanation
Fig. 1 is the structural representation of the heavy gas shield foam device of the present invention.
Below the present invention is described in further detail.The present invention is integrated with following Technology: heavy gas upwards air-discharging collection technique; Aqueous-based ceramic slip containing tensio-active agent stirs foaming technique; Foamed ceramics slip radical polymerization technique in an inert atmosphere.
Principle is as follows: density is greater than the gas of air (as argon gas, CO
2), adopt upwards air-discharging method to collect, the gas (as hydrogen) that density is less than air adopts downward air-discharging method to collect, and the oxygen close with density of air, nitrogen can only adopt drainage to collect.The present invention adopt heavy gas upwards air-discharging remove the gas of environment, device is simple, easy to operate; In gelation process, foamed ceramics slip upper layer bubble not easily floats, and more stable, mould is positioned in air ambient and does not need protection of inert gas; There is Raolical polymerizable gel solidification in short period of time in water-based foam ceramic slurry, realize the preparation of porous ceramics base substrate under the room temperature environment of temperature lower than 40 DEG C.Operation step is played as follows:
1. prepare burden: according to required composition proportion, the various ceramic powder of precise, it can be one of following material: aluminum oxide, zirconium white, silicon nitride, silicon carbide, Mo Laishi etc.; Take deionized water, deionized water weight accounts for 8 ~ 30% of ceramic powder weight; Take dispersion agent, it is one of following material: polyacrylate, poly-methyl acrylate, and dispersion agent add-on is 0.5% ~ 2% of ceramic powder weight; Take conditioning agent, it is one of following material: the alkaline reagents such as ammoniacal liquor, Tetramethylammonium hydroxide, and conditioning agent add-on is 0.5% ~ 2% of ceramic powder weight; Take organic monomer and linking agent, organic monomer add-on is 0.5 ~ 4% of ceramic powder weight, the ratio of organic monomer and linking agent is between 10:1 ~ 30:1, organic monomer is acrylamide or Methacrylamide, linking agent is N, N methylene-bisacrylamide or many ethyleneglycol dimethacrylates;
2. ball milling: ceramic slurry is put into ball grinder and carries out ball milling, Ball-milling Time is 1h ~ 30h, and ratio of grinding media to material is 1:1 ~ 5:1;
3. froth in vacuum: after discharging, aqueous-based ceramic slip is put into vacuum environment stirring degassing bubble and overflow to bubble-free;
4. add tensio-active agent: add tensio-active agent in slip, its add-on is 0.1 ~ 10% of slip weight; Surfactant character is alkyl benzene sulfonate aniorfic surfactant, plant proteins or animal proteinum class tensio-active agent, and various surfactants is compound, can select according to required frothing percentage with to the requirement of froth stability;
5. except air: above-mentioned slip to be put into heavily gas shield foam device, pass into heavy gas afterwards, heavy gas flow > 500ml/min, time length >1min; As shown in Figure 1, this device is made up of 12 parts foaming special purpose device feature: stirrer 1, agitator arm 2, slip container 3, CO
2gas cylinder or Ar gas cylinder 4, reducing valve 5, ventpipe 6, rubber seal 7, environmental chamber 8, environmental chamber upper cover 9, gap 10 of giving vent to anger, gas meter 11 and plup inlet 12, slip container 3 is placed in environmental chamber 8, environmental chamber upper cover 9 is obturaged by rubber seal 7, environmental chamber upper cover 9 leaves give vent to anger gap 10 and plup inlet 12, the agitator arm 2 of stirrer 1 inserts slip container 3, CO by gap 10 of giving vent to anger
2the air outlet of gas cylinder or Ar gas cylinder 4 is communicated with environmental chamber 8, and plup inlet 12 is placed on environmental chamber upper cover 9.Gas cylinder 4 is argon gas or carbon dioxide, and giving vent to anger and forming width between gap 10 and agitator arm is 0.2 ~ 1mm gap.
6. stir foaming: adjusting gas flow >100ml/min<500ml/min, stirrer adjustment of rotational speed is 500 ~ 3000r/min, and churning time controls in 20 ~ 120 minutes;
7. drip catalyzer, initiator: be 20 ~ 100% tetramethyl-s, two aqueous ammoniums by concentration, concentration is 5 ~ 40% ammonium persulfate aqueous solutions from feeding mouth instillation foamed ceramics slip, and the add-on of tetramethyl-two aqueous ammoniums and ammonium persulfate aqueous solution is 0.5 ~ 20% of monomer weight amount.
8. inject mould: the mould made in the non-anti-coagulating action material of non-infiltration by above-mentioned foamed ceramics slip casting, envrionment temperature <40 DEG C, foamed ceramics slip completed gel in 5 ~ 60 minutes; Moulding stock can be the non-anti-coagulating action materials of unwetted such as metal, glass, dense plastic.
9. the demoulding, drying are positioned on screen cloth penetrating up and down by after the gel solidification completely demoulding of foamed ceramics base substrate, place 5 ~ 30 days;
10. sinter: ceramic body drying completed enters stove sintering, adopt the sintering schedule of slowly continuous warming stage by stage to sinter ceramic body.Oxide ceramics adopts air furnace sintering; Silicon nitride ceramics adopts nitrogen protective sintering, and sintering temperature is between 1600 DEG C ~ 1800 DEG C; Silicon carbide ceramics adopts Ar-sintering, and sintering temperature is between 1500 DEG C ~ 2200 DEG C.
Embodiment 1
Take the alumina ceramic powder that 500g median size is 0.5 μm, add 80ml deionized water, the ammonium acrylate dispersion agent of 10ml, 10ml ammoniacal liquor (10%), 1g magnesium basic carbonate powder, 12g acrylamide organic monomer, 0.8g methylene-bisacrylamide; Said mixture is put into cylinder abrading-ball and grind 15 hours; After discharging, measure 150ml slip and pour in beaker, slip stirs de-bubble in vacuum environment and overflows to bubble-free; Add tensio-active agent 0.5g, put into foaming specific equipment, and keep Ar airshed 500ml/min; After 2min, adjustment stirrer rotor speed 1000r/min, slip foaming is to 500ml; Instillation ammonium persulfate aqueous solution (10%) 1.5g, four first class second two ammonium (50%) aqueous solution 1.5g; By above-mentioned foamed ceramics slip implantation glass mould; After 1 hour, the demoulding of porous ceramics base substrate to be positioned on screen cloth penetrating up and down freely dry 10 days; Drying completely base substrate, through air furnace 1600 DEG C calcining 2h sintering, obtains the Alumina Foam Ceramics that void content is 65%.
Embodiment 2
Take the silicon nitride ceramics powder that 500g median size is 0.5 μm, 7g alumina-ceramic powder, 7g yttrium oxide powder, measure 150ml deionized water, the ammonium acrylate dispersion agent of 15ml, 15ml ammoniacal liquor (10%), 20g acrylamide organic monomer, 1g methylene-bisacrylamide; Said mixture is put into ball grinder, ball milling 15 hours; Measure 100ml ceramic suspension slip; Slip overflows to bubble-free through vacuum stirring degasification, adds tensio-active agent 0.5g; Slip is put into foaming specific equipment, pass into Ar gas 2min with 500ml/min, adjustment stirrer rotating speed 1000r/min, slip foaming is to 500ml, instillation ammonium persulfate aqueous solution (10%) 2ml, four first class second two ammonium (50%) aqueous solution 3ml; By in above-mentioned slip implantation glass mould; After 1h, base substrate is taken out from mould, to be positioned on screen cloth penetrating up and down dry 10 days; Drying completely porous silicon nitride base substrate, through 1750 DEG C of nitrogen protection 2h pressureless sintering, obtains the silicon nitride ceramics that void content is 71%.
Claims (5)
1. heavily the direct foaming of gas shield prepares a method for porous ceramics, it is characterized in that, according to the composition proportion of the porous ceramics of required preparation, precise ceramic powder, takes deionized water, and the weight of deionized water accounts for 8 ~ 30% of ceramic powder weight; Take dispersion agent, the add-on of dispersion agent is 0.5% ~ 2% of ceramic powder weight; Take conditioning agent, the add-on of conditioning agent is 0.5% ~ 2% of ceramic powder weight; Take organic monomer and linking agent, the add-on of organic monomer is 0.5 ~ 4% of ceramic powder weight, the ratio of organic monomer and linking agent is between 10:1 ~ 30:1, ceramic slurry is formed by after above-mentioned component mixing, this ceramic slurry is put into ball grinder and carries out ball milling, Ball-milling Time is 1h ~ 30h, and ratio of grinding media to material is between 1:1 ~ 5:1; After discharging, aqueous-based ceramic slip under vacuum stirring condition bubble removing to bubble-free effusion; Then in slip, add tensio-active agent, the add-on of tensio-active agent is 0.1 ~ 10% of slip weight; Described slip is put into the cavity of heavily gas shield foam device, heavy gas passes in environmental chamber by ventpipe, gas flow > 500ml/min, time length >1min; Afterwards, regulate the under meter of heavily gas shield foam device, control gas flow >100ml/min<500ml/min, regulate the stirrer rotating speed of heavily gas shield foam device, rotating speed is 500 ~ 3000r/min, and churning time controls within the scope of 20 ~ 120min; By tetramethyl-two aqueous ammoniums and ammonium persulfate aqueous solution from the feeding mouth instillation foamed ceramics slip of heavy gas shield foam device, after stirring 1 ~ 10min, in the mould that described foamed ceramics slip casting is made in the non-anti-coagulating action material of non-infiltration; Foamed ceramics slip completes gel solidification in envrionment temperature <40 DEG C, 5 ~ 60 minutes; Be positioned on screen cloth penetrating up and down after the foamed ceramics base substrate demoulding that gel solidification is completed, place and carry out drying in 5 ~ 30 days; Foamed ceramics base substrate shove charge sintering drying completed, adopts the sintering schedule of slowly continuous warming stage by stage, sinters ceramic body; Described heavily gas shield foam device comprises stirrer, agitator arm, slip container, CO
2gas cylinder or Ar gas cylinder, reducing valve, ventpipe, rubber seal, environmental chamber and environmental chamber upper cover, slip container is placed in environmental chamber, the agitator arm of stirrer is inserted in slip container by gap of giving vent to anger, environmental chamber upper cover is obturaged by rubber seal, environmental chamber upper cover leaves give vent to anger gap and plup inlet, CO
2the air outlet of gas cylinder or Ar gas cylinder is communicated with environmental chamber, and plup inlet is placed on environmental chamber and covers.
2. the direct foaming of a kind of heavy gas shield according to claim 1 prepares the method for porous ceramics, it is characterized in that, described ceramic powder is one of following material: aluminum oxide, zirconium white, silicon nitride, silicon carbide, Mo Laishi; Dispersion agent is one of following material: polyacrylate, poly-methyl acrylate; Conditioning agent is one of following material: ammoniacal liquor, Tetramethylammonium hydroxide; Organic monomer is acrylamide or Methacrylamide, and linking agent is N, N methylene-bisacrylamide or many ethyleneglycol dimethacrylates; Tensio-active agent is alkyl benzene sulfonate anionic, plant proteins or animal proteinum class tensio-active agent, and various surfactants is compound.
3. the direct foaming of a kind of heavy gas shield according to claim 1 prepares the method for porous ceramics; it is characterized in that; the gap of giving vent to anger that the environmental chamber of described heavy gas shield foam device covers is annular, the gap L EssT.LTssT.LT0.2mm ~ 1mm in stirrer agitator arm and gap of giving vent to anger.
4. the direct foaming of a kind of heavy gas shield according to claim 1 prepares the method for porous ceramics, it is characterized in that, described catalyzer adopts tetramethyl-two aqueous ammoniums of 20 ~ 100%, and initiator adopts the ammonium persulfate aqueous solution of 5 ~ 40%.
5. the direct foaming of a kind of heavy gas shield according to claim 1 prepares the method for porous ceramics, it is characterized in that, the mould that the non-anti-coagulating action material of described non-infiltration is made is metal, glass, dense plastics material.
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CN105036788A (en) * | 2015-09-01 | 2015-11-11 | 中国科学院重庆绿色智能技术研究院 | Preparation method of foamed ceramic |
CN107052352A (en) * | 2017-04-01 | 2017-08-18 | 北京康普锡威科技有限公司 | A kind of CO2The apparatus for preparing metal powder and method of gas shield |
EP3514122A1 (en) | 2018-01-23 | 2019-07-24 | FRAUNHOFER-GESELLSCHAFT zur Förderung der angewandten Forschung e.V. | Method for producing porous inorganic shaped articles and articles obtained therewith and their use |
CN112811931A (en) * | 2020-12-31 | 2021-05-18 | 中国建筑材料科学研究总院有限公司 | Ceramic material and preparation method and application thereof |
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CN113477343A (en) * | 2021-05-26 | 2021-10-08 | 张洪军 | Carbon-ceramic material production equipment and production process thereof |
CN113477343B (en) * | 2021-05-26 | 2023-01-03 | 烟台奥森制动材料有限公司 | Carbon-ceramic material production equipment and production process thereof |
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