CN103936425A - Preparation method of ceramic plate - Google Patents
Preparation method of ceramic plate Download PDFInfo
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- CN103936425A CN103936425A CN201410024496.6A CN201410024496A CN103936425A CN 103936425 A CN103936425 A CN 103936425A CN 201410024496 A CN201410024496 A CN 201410024496A CN 103936425 A CN103936425 A CN 103936425A
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Abstract
The invention relates to a preparation method of a ceramic plate, which comprises the following steps: providing a ceramic slurry, wherein the ceramic slurry comprises ceramic powder, an organic monomer, a dispersant, a cross-linking agent, an initiator and a solvent; providing a metal alloy in a molten state, wherein the concentration of metal alloy is greater than the concentration of the ceramic slurry, casting the ceramic slurry to the surface of the metal alloy to obtain a ceramic slurry layer; insulating the metal alloy and the ceramic slurry layer, polymerizing the organic monomer, forming a ceramic gel layer on the surface of the metal alloy; continuously insulating the ceramic gel layer on the surface of the metal alloy and drying to obtain a ceramic base substrate; and then sintering the ceramic base substrate to obtain the ceramic plate.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic plate, relate in particular to a kind of preparation method of large-sized ceramic plate.
Background technology
Along with high-performance ceramics is in the widespread use of engineering field, usually need large-sized fine ceramics sheet material of some different thickness, and the ceramic method of existing preparation as forming method etc., casting method, dry pressure formed method, cold isostatic compaction method and gel cannot solve.
Ordinary gel injection formation technology can prepare high-density, evenly, the ceramic body of complicated shape, but in the time of the tabular base substrate of moulding large size, the volumetric shrinkage of gel, drying process easily causes subsurface defect and buckling deformation.
Summary of the invention
In view of this, the necessary preparation method that a kind of large-sized and smooth ceramic plate is provided.
A preparation method for ceramic plate, it comprises the following steps: a ceramic size is provided, and described ceramic size comprises ceramic powder, organic monomer, dispersion agent, linking agent, initiator and solvent; The metal alloy of one molten state is provided, and the density of the metal alloy of described molten state is greater than the density of described ceramic size, and the surface that described ceramic size is poured into the metal alloy of described molten state obtains a ceramic slurry bed of material; By the metal alloy of described molten state and the insulation of the ceramic slurry bed of material, make described organic monomer polymerization reaction take place, form a ceramic gel coat on the surface of the metal alloy of described molten state; Described ceramic gel coat is continued to insulation to be dried on the surface of the metal alloy of described molten state, obtain a ceramic body; And ceramic body described in sintering, obtains a ceramic plate.
Compared with prior art, the preparation method of ceramic plate of the present invention has the following advantages: the process that forms described ceramic gel coat and dry described ceramic gel coat due to polymerization is carried out on the surface of the metal alloy of molten state, the metal alloy of this molten state is in a liquid state, surface is extremely smooth, thereby greatly reduce polymerization and form the resistance while there is volumetric shrinkage after described ceramic gel coat and described ceramic gel coat dry out, obtain smooth, indeformable ceramic body, and then make the ceramic plate defect that obtains little.And, by the metal alloy in molten state, polyreaction and drying process are all carried out under levitated state, the method is not subject to the restriction of size, can form large-sized ceramic plate.
Brief description of the drawings
Fig. 1 is the schema of the preparation method of ceramic plate described in the embodiment of the present invention.
Fig. 2 be in the preparation method of the ceramic plate described in Fig. 1 each raw material schematic diagram is set.
Fig. 3 be described in the embodiment of the present invention ceramic plate sintering process graphic representation.
Main element nomenclature
| The ceramic slurry bed of material | 10 |
| The metal alloy of molten state | 20 |
| Isolated film | 30 |
| Container | 40 |
Following specific embodiment further illustrates the present invention in connection with above-mentioned accompanying drawing.
Embodiment
The preparation method of the ceramic plate embodiment of the present invention being provided below with reference to accompanying drawing is further described.
Refer to Fig. 1 and Fig. 2, the preparation method of the ceramic plate providing for first embodiment of the invention, this preparation method comprises the following steps:
Step S1, provides a ceramic size, and described ceramic size comprises ceramic powder, organic monomer, dispersion agent, linking agent, initiator and solvent;
Step S2, provides the metal alloy 20 of a molten state, and the surface that described ceramic size is poured into the metal alloy 20 of described molten state obtains a ceramic slurry bed of material 10, and the density of the metal alloy 20 of described molten state is greater than the density of described ceramic size;
Step S3, is incubated for some time by the metal alloy of described molten state 20 and the ceramic slurry bed of material 10, makes described organic monomer polymerization reaction take place, forms a ceramic gel coat on the surface of the metal alloy 20 of described molten state;
Step S4, continues insulation for some time to be dried by described ceramic gel coat on the surface of the metal alloy 20 of described molten state, obtains a ceramic body; And
Step S5, ceramic body described in sintering, obtains a ceramic plate.
In step S1, described formation ceramic size carries out at low temperatures, and preferred, temperature is 2 degrees Celsius ~ 20 degrees Celsius, to avoid described organic monomer that polymerization occurs in advance.Specifically comprising the following steps of described formation ceramic size:
Step S11, provides a monomer solution that comprises organic monomer, dispersion agent, linking agent and aqueous solvent, and ceramic powder is added in described monomer solution and by mill Jie ball and stirred;
Step S12, isolates mill Jie ball, obtains a monomer ceramic size; And
Step S13, adds initiator, and continues to stir for some time, obtains homodisperse ceramic size.
In step S11, describedly ceramic powder is added to monomer solution and stir and undertaken by a stirring mill by mill Jie ball.Concrete, first, stirring a certain amount of mill Jie ball adding in mill, ready monomer solution is joined and stirred in mill, start and stir mill, its rotating speed is controlled at 80 ~ 150 revs/min; Then lentamente a certain amount of ceramic powder is joined and stir the abundant dispersed with stirring of fluffing, in whipping process, can suitably supplement some solvent deionized water, to make up the moisture of vaporization losses; Finally form the mixed slurry of uniform ceramic powder and monomer.Described mill Jie ball plays and makes ceramic powder be well-dispersed in the object in monomer solution.Because ceramic powder is of a size of micro/nano level, the surface free energy of described ceramic powder is larger, disperses and be difficult to realize, and by adding mill Jie's ball and continuing to stir, can make ceramic powder be infiltrated gradually, and be dispersed in monomer solution.
Described monomer solution is configured than for 40vol% ~ 50vol% according to the solid volume of described ceramic powder, to ensure that the described ceramic plate finally obtaining is as fine and close solid.Described organic monomer can be acrylamide, dimethylaminoethyl methacrylate, vinylformic acid, dimethylamino-propyl Methacrylamide etc., can carry out polyreaction at 60 degrees Celsius ~ 90 degrees Celsius as long as ensure.Described dispersion agent plays the homodisperse effect of described ceramic powder that makes.Described dispersion agent can be citric acid ammonia, ammonium polyacrylate, polymine, Tetramethylammonium hydroxide etc.Described linking agent can promote covalent linkage between linear molecule or the formation of ionic linkage, makes linear molecule that the crosslinked polymkeric substance that obtains network structure occur.Described linking agent can be methylene-bisacrylamide, Vinylstyrene or vulcabond etc.
Described ceramic powder can be oxide compound (as Al
2o
3, ZrO
2deng), nitride is (as Si
3n
4, AlN etc.), carbide (as BC, TiC etc.), refractory materials (as mullite, zircon etc.), or its matrix material.The particle diameter of described ceramic powder is 100 nanometer ~ 500 micron.
In the present embodiment, described mill Jie ball is zirconium white, and described ceramic powder is Al
2o
3, Al
2o
3purity be 99.5%, described organic monomer is acrylamide, described dispersion agent is citric acid ammonia, described linking agent is methylene-bisacrylamide, in described ceramic size, the solid volume of ceramic powder ratio is about 50vol%.
In step S12, described separation mill Jie ball can separate described mill Jie ball by a screen cloth, obtains monomer ceramic size.This monomer ceramic size low temperature seal is preserved.In the present embodiment, by one 60 object screen clothes, described zirconium white (mill Jie ball) is separated.
In step S13, by stirring, described initiator is dispersed in described monomer ceramic size.By add initiator in described monomer ceramic size, to improve the reaction efficiency of polyreaction of organic monomer.The easy decomposes of described initiator becomes the compound with free radical.Should can further cause with the compound of free radical radical polymerization and the copolymerization of alkene class, two vinyl monomers, and the crosslinking curing of unsaturated polyester and polymer crosslinking reaction.Described initiator can be ammonium persulfate, peroxidation toluoyl, tertbutyl peroxide, 2,2'-Azobis(2,4-dimethylvaleronitrile), ammonium persulfate/sodium bisulfite etc.In the present embodiment, described initiator can be ammonium persulfate.
Further, can after adding initiator, carry out the step of a vacuum stripping bubble.By remove bubble under vacuum, solid phase and liquid phase in described ceramic size are evenly mixed, and exist without larger bubble, distribute thereby solid is fine and close in finally obtaining ceramic plate.Concrete, first described ceramic size is positioned in an airtight container, then, in vacuumizing, stir described ceramic size.
In step S2, the metal alloy of described molten state 20 is positioned in a container 40, the surperficial size of the metal alloy 20 of described molten state is consistent with the size of the bottom of described container 40.Described container 40 plays the effect of mould, in the time ceramic size being poured into metal alloy surperficial of described molten state, described in the size of the ceramic slurry bed of material that obtains consistent with the size of the bottom of described container 40.Thereby the shape and size of ceramic plate that can be according to specific needs, select the shape and size of described container 40.In the present embodiment, the bottom of described container 40 be shaped as square, the length of side of bottom is 1340 millimeters, the height of described container is 50 millimeters.
The fusing point of the metal alloy 20 of described molten state is 60 degrees Celsius ~ 95 degrees Celsius.The material of the metal alloy 20 of described molten state can be tin-bismuth alloy electroplating, bismuth-Sn-In alloy or bismuth-lead-Xi-cadmium alloy etc.Described in the density ratio of the metal alloy 20 of described molten state, the density of ceramic size is large, to ensure that described ceramic size floats over the surface of the metal alloy 20 of the described molten state of molten state.Preferably, the density of the metal alloy 20 of described molten state can be 1.5 times ~ 5 times of density of described ceramic size.In the present embodiment, the material of the metal alloy 20 of described molten state is tin-bismuth alloy electroplating, and its density is 9g/cm
3, the density of the metal alloy 20 of described molten state is about 4 times of density of described ceramic size.
Be appreciated that, before the described ceramic size of cast, can lay in advance an isolated film 30 on the surface of the metal alloy 20 of described molten state, infiltrate through in ceramic size at the metal alloy 20 of the metal alloy 20 of described molten state and the interface partial melting state of described ceramic size avoiding.Described isolated film 30 is a continuous laminate structure, and the density of described isolated film 30 is less than the density of the metal alloy 20 of described molten state, thereby described isolated film 30 is held between the two.The chemical property of described isolated film 30 is more stable, with ensure not can with the metal alloy of described molten state 20 and ceramic size in each component generation chemical reaction.Be appreciated that the variation of physical condition can not occur on the surface of the metal alloy 20 of molten state described isolated film 30, such as gasification or liquefaction.The material of described isolated film 30 can be flexible plastic film or silicone oil.The material of described flexible plastic film can be polycarbonate (PC), polymethylmethacrylate (PMMA), polyethersulfone (PES), cellulose ester, polyvinyl chloride (PVC), benzocyclobutene (BCB), acrylic resin, acrylonitrile-butadiene-styrene copolymer (ABS), polyethylene terephthalate (PET), polycarbonate/acrylonitrile-butadiene-phenylethene copolymer blend (PC/ABS), polycarbonate/polybutylene terephthalate blend (PC/PBT), polycarbonate/polyethylene terephthalate blend (PC/PET), the materials such as polycarbonate/polymethylmethacrylate blend (PC/PMMA) or polyamide (PA).In the present embodiment, the material of described isolated film 30 is a plastics film, and the material of described plastics film is PET.
In step S3, described the insulation of the metal alloy of molten state and the ceramic slurry bed of material is referred to the heat that provides certain makes metal alloy continue to keep molten state, thereby the described ceramic slurry bed of material is also remained at this temperature, so that the polymerization reaction take place under the effect of initiator of the organic monomer in the described ceramic slurry bed of material.Described organic monomer is polymerization reaction take place under the effect of initiator and catalyzer, obtains the polymkeric substance that comprises side chain.Because this polymkeric substance is water insoluble, thereby this polyreaction can be carried out on the ceramic powder of solid phase.When described initiator adds fashionablely, organic monomer carries out pre-polymerization and obtains performed polymer, the further polymerization of performed polymer; After performed polymer polymerization size progressively increases, can be deposited on the surface of ceramic powder, thus three-dimensional net structure ceramic powder is coated and that formation one is stable, to realize gelation.
Described polyreaction can be carried out under rough vacuum environment or inert atmosphere.This is because oxygen has two unpaired electrons that spin direction is identical, and this unpaired electron can be at war with and consume the free radical of part with the free radical that needs in polyreaction, affects the efficiency of polyreaction.Described rough vacuum environment can be the environment with certain vacuum degree, such as normal atmosphere is-0.1MPa, or passes into rare gas element, as nitrogen, argon gas, neon.
The temperature of reaction of described polyreaction can be 25 degrees Celsius ~ 95 degrees Celsius, preferred, 60 degrees Celsius ~ 95 degrees Celsius.By the metal alloy of described molten state 20 and the ceramic slurry bed of material 10 are incubated, can ensure the needed temperature of reaction of described polyreaction.Owing to adopting the metal alloy 20 of molten state as the supply source of heat, the metal alloy 20 of this molten state can evenly and fast transfer heat to the described ceramic slurry bed of material 10, thereby ensures carrying out smoothly of polyreaction.And because described polyreaction is carried out on the surface of the metal alloy 20 of described molten state, the metal alloy 20 of this molten state is in a liquid state, make the surface of metal alloy 20 of described molten state extremely smooth; When floating on the described ceramic slurry bed of material 10 polymerization reaction take places on metal alloy 20 surfaces of molten state, it is very little that the deflation resistance of generation can become, and makes the smooth and smooth surface of the described ceramic gel coat that obtains.
In the present embodiment, under the environment of low vacuum, the metal alloy of described molten state 20 and the ceramic slurry bed of material 10 are kept 1 hour at about 85 degrees Celsius.
In step S4, described ceramic gel coat continues insulation for some time on the surface of the metal alloy 20 of molten state, to remove moisture.Described insulation is to instigate the metal alloy of molten state 20 to continue to keep molten state.Because the moisture in described ceramic gel coat volatilizees gradually, can there is at least 2% linear shrinkage on its surface in described ceramic gel coat.And because the metal alloy 20 of molten state is in a liquid state, make the surface of metal alloy 20 of described molten state extremely smooth; In the time floating on the described ceramic gel coat on metal alloy 20 surfaces of molten state and shrink, it is very little that the resistance running into can become, and makes the smooth and smooth surface of the described ceramic body that obtains, avoided the excessive cracking causing of resistance and distortion when shrinking.
In the present embodiment, described ceramic gel coat is continued under 85 degrees Celsius to insulation 72 hours, obtain described ceramic body.
In step S5, refer to Fig. 3, described ceramic body is transferred in a sintering oven and carries out high temperature sintering, obtain described ceramic plate.Concrete, along with temperature raises, in described ceramic body, there is specific surface greatly and surperficial powder that can be higher, change to the direction of falling low surface energy gradually, constantly carry out crystal boundary and move, pore is progressively got rid of, and finally obtains having the fine and close ceramic plate of some strength.In the present embodiment, the length of described ceramic plate is 1000mm, and width is 1000mm, and thickness is 20mm.
In the preparation method of ceramic plate of the present invention, the process that forms described ceramic gel coat and dry described ceramic gel coat due to polymerization is carried out on the surface of the metal alloy 20 of molten state, the metal alloy 20 of this molten state is in a liquid state, surface is extremely smooth, thereby greatly reduce polymerization and form the resistance while there is volumetric shrinkage after described ceramic gel coat and described ceramic gel coat dry out, obtain smooth, indeformable ceramic body, and then make the ceramic plate defect that obtains little.And, by the metal alloy 20 in molten state, polyreaction and drying process are all carried out under levitated state, this preparation method is not subject to the restriction of size, can form large-sized ceramic plate.This preparation method is simple, is beneficial to industrialization.
In addition, those skilled in the art also can do other and change in spirit of the present invention, and these variations of doing according to spirit of the present invention certainly, all should be included in the present invention's scope required for protection.
Claims (10)
1. a preparation method for ceramic plate, it comprises the following steps:
One ceramic size is provided, and described ceramic size comprises ceramic powder, organic monomer, dispersion agent, linking agent, initiator and solvent;
The metal alloy of one molten state is provided, and the density of the metal alloy of described molten state is greater than the density of described ceramic size, and the surface that described ceramic size is poured into the metal alloy of described molten state obtains a ceramic slurry bed of material;
By the metal alloy of described molten state and the insulation of the ceramic slurry bed of material, make described organic monomer polymerization reaction take place, form a ceramic gel coat on the surface of the metal alloy of described molten state;
Described ceramic gel coat is continued to insulation to be dried on the surface of the metal alloy of described molten state, obtain a ceramic body; And
Ceramic body described in sintering, obtains a ceramic plate.
2. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, described ceramic size is prepared by following steps:
One monomer solution that comprises organic monomer, dispersion agent, linking agent and aqueous solvent is provided, ceramic powder is added in described monomer solution and by mill Jie ball and stirred;
Isolate mill Jie ball, obtain a monomer ceramic size; And
Add initiator, and continue to stir, obtain a ceramic size.
3. the preparation method of ceramic plate as claimed in claim 2, is characterized in that, described formation ceramic size is to carry out under 2 degrees Celsius ~ 20 degrees Celsius in temperature.
4. the preparation method of ceramic plate as claimed in claim 2, is characterized in that, further after separating described mill Jie ball, carries out the step of a vacuum stripping bubble.
5. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, the material of described metal alloy is tin-bismuth alloy electroplating, bismuth-Sn-In alloy or bismuth-lead-Xi-cadmium alloy.
6. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, the fusing point of the metal alloy of described molten state is 60 degrees Celsius ~ 95 degrees Celsius.
7. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, 1.5 times ~ 5 times of the density that the density of the metal alloy of described molten state is described ceramic size.
8. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, described polyreaction is carried out under rough vacuum environment or inert atmosphere.
9. the preparation method of ceramic plate as claimed in claim 1, is characterized in that, further before the described ceramic size of cast, lays an isolated film in advance on the surface of the metal alloy of described molten state.
10. the preparation method of ceramic plate as claimed in claim 9, is characterized in that, described isolated film is arranged between the described ceramic slurry bed of material and the alloyed metal of described molten state, and the material of described isolated film is flexible plastic film or silicone oil.
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| CN201410024496.6A CN103936425B (en) | 2014-01-20 | 2014-01-20 | A kind of preparation method of ceramic plate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630717A (en) * | 2015-02-27 | 2015-05-20 | 河北大学 | Preparation method of P type NaXCoO2 transparent conductive thin film |
| CN115321954A (en) * | 2022-08-09 | 2022-11-11 | 广东环波新材料有限责任公司 | Preparation method of ceramic substrate and low-temperature co-fired ceramic substrate |
Citations (1)
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| CN102351526A (en) * | 2011-06-11 | 2012-02-15 | 江苏尚易新材料科技有限公司 | Method for preparing AZO target materials by adopting gel injection molding forming |
-
2014
- 2014-01-20 CN CN201410024496.6A patent/CN103936425B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351526A (en) * | 2011-06-11 | 2012-02-15 | 江苏尚易新材料科技有限公司 | Method for preparing AZO target materials by adopting gel injection molding forming |
Non-Patent Citations (1)
| Title |
|---|
| 张敏等: "钛酸铝陶瓷水基注凝成型工艺", 《材料科学与工程学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630717A (en) * | 2015-02-27 | 2015-05-20 | 河北大学 | Preparation method of P type NaXCoO2 transparent conductive thin film |
| CN115321954A (en) * | 2022-08-09 | 2022-11-11 | 广东环波新材料有限责任公司 | Preparation method of ceramic substrate and low-temperature co-fired ceramic substrate |
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| CN103936425B (en) | 2015-08-12 |
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