CN107698262A - A kind of ceramic material - Google Patents
A kind of ceramic material Download PDFInfo
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- CN107698262A CN107698262A CN201710614789.3A CN201710614789A CN107698262A CN 107698262 A CN107698262 A CN 107698262A CN 201710614789 A CN201710614789 A CN 201710614789A CN 107698262 A CN107698262 A CN 107698262A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 claims abstract description 76
- 239000002002 slurry Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 39
- 230000008014 freezing Effects 0.000 claims abstract description 26
- 238000007710 freezing Methods 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 150000003384 small molecules Chemical class 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000007493 shaping process Methods 0.000 claims abstract description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 20
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 12
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 8
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011268 mixed slurry Substances 0.000 claims description 7
- 239000003507 refrigerant Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052788 barium Inorganic materials 0.000 claims 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 28
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 10
- 239000011229 interlayer Substances 0.000 abstract description 9
- 238000007711 solidification Methods 0.000 abstract description 5
- 230000008023 solidification Effects 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000004523 agglutinating effect Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 hydroxy alcohols Chemical class 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000012595 freezing medium Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000004421 molding of ceramic Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/007—Producing shaped prefabricated articles from the material by freezing the material
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/624—Sol-gel processing
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The present invention proposes a kind of ceramic material, with microcosmic layer structure, it is rod shaped ceramic crystal layer between layer and layer micro interface, described ceramic material is formed by being sintered after the chilled shaping of ceramic slurry, drying, described ceramic slurry adds ceramic powder and small molecule multi-hydroxy alcohol type organic using Ludox as liquid phase.The present invention is using successively freezing and the growth morphology of ice crystal in alcohol type organic control freezing solidification process, because water crystallization forms zigzag micro ice crystal structure between the frozen coating and frozen coating micro interface that make to be formed in successively refrigerating process in microstructure, base substrate interlayer is promoted to combine closely, it is ensured that ceramic layered good agglutinating property.
Description
Technical field
The present invention relates to a kind of ceramic material, belong to field of ceramic preparation technology.
Background technology
Ceramic material has high temperature resistant, wear-resistant, corrosion resistant feature, and intensity is high, the coefficient of expansion is low, thermal conductivity
It is good, more potential and advantage is used at high temperature.But its shortcoming is also it will be apparent that the fragility of ceramic material is larger, tough
Property it is relatively low, further development of these shortcomings for ceramic material and the large-scale application in engineering are a very big bottles
Neck.The fragility of ceramic material intuitively shows as absence of aura, the explosion type fracture under applied load, indirectly shows as resisting
Mechanical impact property's difference and thermal shocking are poor.Therefore, the toughness of ceramic material is increased, improving the use reliability of ceramic material is
The wide variety of key of structural ceramics.
At present, mutually mainly there is following four method to improve the toughness of ceramic material and intensity by adding toughness reinforcing:(1)
Grain dis-persion toughening；(2) transformation toughening；(3) long fibre toughness reinforcing；(4) it is crystal whisker toughened.Research shows that these methods have certain increasing
Tough effect, but still can not solve the fatal defects i.e. fracture suddenly of ceramic material.Importantly, the preparation technology of these methods
It is stricter with the requirement to experiment and use condition, therefore certain difficulty be present in terms of the engineer applied of reality.
Layered composite ceramic material makes ceramic material overcome non-layer compared to other toughness reinforcing modes, its unique structure
The defects of shape brittleness of ceramics is big, while the comprehensive mechanical performance of composition phase material is kept, increase substantially the fracture of material
Toughness, the higher field of safety coefficient is can apply to, the application field of ceramic material is expanded, layered composite ceramic is not
The shortcomings that fracture toughness being present in conventional ceramic is relatively low is only effectively improved, moreover, ceramic layered in preparation technology
Advantage is also obvious.Its production cycle is shorter, easy to spread and simple to operate.So it is designed with larger
The free degree, design and interlayer design in layer can be considered, by material selection and the aspect of structure design two come to material
Performance optimizes.
At present, the molding mode of laminated ceramic composite includes:(1) blank is laid compressing；(2) preformed layer stacks
Shaping；(3) again by laminated into type after slurry of the base layer by coating sandwich material；(4) phase between the slurry between raw material
Mutually deposition aftershaping.Wherein preformed layer stacks shaping and mainly includes two kinds of rolling formation and flow casting molding.Existing stratiform pottery
Macroscopical layer structure is presented in the ceramic material that porcelain production method makes, and improvement of this macroscopical layer structure to material property has
Certain limitation, while easily there is sintering delamination, and cause laminated structure ceramics to prepare failure.
The content of the invention
It is an object of the invention to overcome prior art insufficient, there is provided one kind has global formation and controllability is good, work
Skill is simple, Coating combination is good, the delamination free laminate ceramic of sintering.
The technical solution of the present invention：A kind of ceramic material, there is microcosmic layer structure, in microstructure layer and microcosmic stratum boundary
It is the bar-shaped crystal layer of ceramics between face, described ceramic material is formed by being sintered after the chilled shaping of ceramic slurry, drying, described
Ceramic slurry adds ceramic powder and small molecule multi-hydroxy alcohol type organic, described small molecule is more using Ludox as liquid phase
First hydroxy alcohols organic matter is 0.5~5% of the quality of liquid phase water in ceramic slurry.
Described refrigerating process is under the auxiliary of moulds of industrial equipment, and the moulds of industrial equipment for being filled with ceramic slurry are opened from one end
Beginning is successively freezed, refrigerating process employing mode one or mode two,
Mode one, the moulds of industrial equipment for being filled with ceramic slurry are placed in refrigerated container, are slowly noted from refrigerated container bottom
Enter≤- 80 DEG C of refrigerant, ceramic slurry is successively freezed since bottom, every layer of freezing thickness≤1 μm is that is, each
Height≤1 μm of the refrigerant of secondary injection, freezing soaking time are not less than 0.5 minute；
Mode two, according to freezing direction, the ceramic slurry being filled in moulds of industrial equipment persistently slowly enters≤- 80 DEG C
In refrigerant, admission velocity is no more than 1 μm/3min.
Using successively slowly control freezing, in conjunction with small molecule multi-hydroxy alcohol type organic to ceramic slurry freezing gel
During ice crystal crystal habit be controlled, microcosmic layer structure can be formed in microstructure, while freeze successively
During between the frozen coating and frozen coating micro interface that are formed because water crystallization process forms zigzag micro ice crystal structure, rear
In continuous sintering, the ceramic bar-shaped crystalline substance of formation can grow in the micropore that micro ice crystal structure leaves, and be formed in interlayer micro interface
The interlayer structure that the bar-shaped crystalline phase of ceramics mutually interweaves, so as to promote base substrate interlayer is microcosmic to combine closely and burning that stratified material is good
Tie performance.
Under the auxiliary of moulds of industrial equipment, ceramic slurry is under conditions of cryogenic temperature and freezing rate control, into freezing
Medium, successively freezing control is realized, realize the curing molding of ceramic slurry, form the ceramic body with some strength.
At low temperature can be with the characteristic of gel solidification present invention utilizes Ludox, the ceramic slurry to needing freeze forming
Progress slowly progressively freezes, and carries out the control of cryogenic temperature and freezing rate, makes during ceramic slurry freeze forming progressively
Form the microcosmic layer structure of the integrated molding of thin layer (≤1 μm)；It is simultaneously solid using the alcohol type organic control freezing of addition
The growth morphology of ice crystal during change, make because water crystallization forms zigzag micro ice crystal structure to promote between layer and layer micro interface
Enter base substrate interlayer to combine closely, it is ensured that ceramic layered good agglutinating property, high-performance stratiform structural ceramic material is finally made.
The molecular weight of described small molecule multi-hydroxy alcohol type organic is less than 10000.
The present invention is by adding small molecule multi-hydroxy alcohol type organic to the ice crystal during ceramic slurry freezing gel
Crystal size and form optimize control, and it is in microcrystalline form to make ice crystal, it is possible to reduce moisture removes the hole left to final pottery
The influence of ceramic material mechanical property and reliability.
The present invention is not particularly limited to the species of small molecule multi-hydroxy alcohol type organic, such as common glycerine, second
Glycol etc..The addition of small molecule multi-hydroxy alcohol type organic can not be too many, otherwise can be to the consistency of final ceramic material
Impact；Otherwise addition can not can not play very little and suppress freezing and expansion effect in follow-up freezing gel technique, with
Freezing gel technique does not have the synergy of control ice-crystal growth.The present invention gives small molecule multi-hydroxy alcohol type organic
Preferred addition, make its neither influence consistency and can play synergy；Under the same terms, small molecule multi-hydroxy alcohols
When the addition of organic matter changes within the above range, the combination property of final ceramic is slightly influenceed, during beginning with
Small molecule multi-hydroxy alcohol type organic addition increase, combination property slightly improve, addition reach 1% or so (1 ±
0.2%) when, combination property is optimal, and then, as addition increases, combination property is declined slightly.
The ceramic powder of the present invention can be conventional use of ceramic powder, such as silicon nitride powder, carborundum powder, aluminum oxide
Powder, silicon dioxide powder etc..It is preferred that following ceramic powder, may eventually form Si in sintering3N4/ BAS complex phase ceramics.
Silicon nitride powder, barium monoxide powder and alumina powder, wherein barium monoxide, the addition of aluminum oxide are with alkaline silica sol two
On the basis of the quality of silica, according to stoichiometric proportion BaO-A12O3-2SiO2Addition, silicon nitride powder quality are accounted in mixed slurry
(silicon nitride powder and BAS mass ratio are 55 for the 55~90% of solid phase gross mass:45~90:10), solid phase gross mass refers to silicon nitride
The silica containing quality sum of institute in powder, barium monoxide powder, alumina powder and Ludox；BAS mass refers to barium monoxide powder, oxidation
The silica containing quality sum of institute in aluminium powder and Ludox.
BAS compositions can not very little, on the one hand because BAS final content is by Ludox (contained titanium dioxide in mixed slurry
Silicon) determine, Ludox very little, is unfavorable for follow-up ceramic slurry freezing solidification, and BAS content can not be less than in mixed slurry
The 10% of solid phase gross mass；On the other hand, silicon nitride powder mass content can not be too low in mixed slurry, otherwise in blank sintering mistake
Cheng Zhong, a large amount of liquid phases can be formed due to the high sintering fusing of BAS contents, cause base substrate scorification, therefore, silicon nitride powder quality can not be lacked
The 55% of solid phase gross mass in slurry.When silicon nitride powder quality accounts for 55~90% of solid phase gross mass in mixed slurry, ability
Give full play to BAS and Si3N4Between mutual promoting action when sintering, and meet low temperature gel solidification, form Si3N4/ BAS is multiple
Phase ceramics.
Ludox can be generally 15~30% by commercially available acquisition, solid content in the present invention.Beta-silicon nitride powder, aluminum oxide
The requirement such as the particle diameter of the ceramic powders such as powder, barium monoxide powder and purity is known in the art technology, and those skilled in the art can be with
Selected according to specific requirement.
A small amount of dispersant can be added in described ceramic slurry according to needs of production, dispersant makes powder more preferable
Be dispersed in colloidal sol, ammonium polyacrylate or TMAH can be used, also can use to end article without unfavorable shadow
Other loud species dispersants, addition are 0.5~3% of solid powder gross mass in ceramic slurry.
Freezing solidifies obtained ceramic blank drying, sintering, obtains ceramic material.
Present invention drying is known in the art technology, and ceramic body can be dried at ambient pressure, and drying temperature does not have strict
Limitation, can be dried at normal temperatures, can also the optional temperature below 200 DEG C as needed, drying time is 2~48 hours,
Selected according to the degree of drying of drying temperature and ceramic body, ensure that base substrate is thoroughly dried.
Base substrate is sintered to techniques well known, can use pressureless sintering, gas pressure sintering or hot pressed sintering, sintering
Atmosphere is nitrogen.
The beneficial effect of the present invention compared with prior art：
(1) present invention is using successively freezing and the growth morphology of ice crystal in alcohol type organic control freezing solidification process, system
Standby high performance ceramic material, make in microstructure between the frozen coating and frozen coating micro interface that are formed in successively refrigerating process
Because water crystallization forms zigzag micro ice crystal structure, base substrate interlayer is promoted to combine closely, it is ensured that ceramic layered good agglutinating property；
(2) present invention energy global formation, technique is simple, controllability is good, Coating combination is good, sintering is without delamination.
Brief description of the drawings
Fig. 1 is the microcosmic stratiform structural representation of the present invention；
Fig. 2 is preparation flow figure of the present invention；
Fig. 3 a, b are the ceramic material microstructure that the embodiment of the present invention 1 is prepared.
Embodiment
With reference to instantiation and accompanying drawing, the present invention is described in detail.
The present invention is bar-shaped crystal structure layer between layer and layer micro interface as shown in figure 1, have microcosmic layer structure,
Ceramic material is sintered after successively freeze forming, drying by ceramic slurry and formed, and ceramic slurry is using Ludox as liquid phase, addition pottery
Porcelain powder and small molecule multi-hydroxy alcohol type organic, control every a layer thickness≤1 μm successively freezed.
Embodiment 1
Prepare Si3N4/ BAS diphase ceramic materials
Preparation process by following steps as shown in Fig. 2 realized：
1st, prepared by ceramic slurry
Slurry is formed by Ludox, silicon nitride powder, barium monoxide powder and alumina powder, and adds 1% tetramethyl hydroxide
Ammonium adds 1% (on the basis of the quality of liquid phase water in ceramic slurry) glycerine, wherein barium monoxide, aluminum oxide as dispersant
Addition on the basis of the quality of silica in Ludox, according to BaO-A12O3-2SiO2Stoichiometric proportion adds, nitridation
Silica flour and BAS mass ratio are 70:30；Ball mill mixing 5h in high speed ball mill.
2nd, successively freeze
Mould is injected after slurry degassing, under the auxiliary of moulds of industrial equipment, controls cryogenic temperature and freezing rate to lift
Mode is progressively slowly pushed into -80 DEG C of refrigerated container according to freezing direction, and fltting speed is 1 μm/3min, and realization successively freezes
Control, the integral solidifying of printout is realized, form the ceramic body with some strength, the demoulding, obtain base substrate.
3rd, drying and sintering
Base substrate is dried, dried sample (normal pressure) in nitrogen atmosphere is warming up to 5 DEG C/min speed
1780 DEG C are sintered, and are incubated 3h, finally give microcosmic stratiform S i3N4/ BAS diphase ceramic materials.Sintered body bending strength and
Work to break is respectively 430MPa and 350J/m2。
Microstructure such as Fig. 3 a, b can be seen that the material is comparatively dense, and Coating combination is good, have more in material
Obvious laminate structure, the bar-shaped crystalline substance of ceramics grow between adjacent layer and layer micro interface, and it is bar-shaped to form ceramics in microcosmic interlayer
Crystal structure layer, so as to promote the microcosmic interlayer of base substrate to combine closely.
Embodiment 2,3
Prepare Si3N4/ BAS complex phase ceramics, it is total to account for solid phase in mixed slurry respectively for silicon nitride powder quality during ceramic slurry matches
Quality is 55% and 90%, and ceramic slurry adds 1% (on the basis of the quality of liquid phase water in ceramic slurry) ethylene glycol, and slurry takes off
Mould is injected after gas, under the auxiliary of moulds of industrial equipment, is put into refrigerated container, refrigerant injects from refrigerated container bottom, often
Secondary injection rate ensures that ceramic slurry freezing thickness is 1 μm, freezes 1min, remaining step such as embodiment 1.Obtained Si3N4/ BAS is multiple
Phase ceramics are similar with Fig. 3 a, b in microstructure, and sintered body bending strength and fracture achievement are similar to Example 1.
Embodiment 4,5
Prepare Si3N4/ BAS complex phase ceramics, 0.5% and 5% is added respectively (using the quality of liquid phase water in ceramic slurry as base
It is accurate) glycerine, remaining step such as embodiment 1.Obtained Si3N4/ BAS complex phase ceramics are similar with Fig. 3 a, b in microstructure, burn
Knot body bending strength and work to break are slightly below embodiment 1.
Unspecified part of the present invention is known to the skilled person technology.
Claims (7)
- A kind of 1. ceramic material, it is characterised in that：It is ceramics between microstructure layer and microcosmic bed boundary with microcosmic layer structure Bar-shaped crystal layer, described ceramic material are formed by being sintered after the chilled shaping of ceramic slurry, drying, and described ceramic slurry is with silicon Colloidal sol is liquid phase, and adding ceramic powder and small molecule multi-hydroxy alcohol type organic, described small molecule multi-hydroxy alcohols has Machine thing is 0.5~5% of the quality of liquid phase water in ceramic slurry.
- A kind of 2. ceramic material according to claim 1, it is characterised in that：Described freeze forming technique is in frock mould Under the auxiliary of tool, the moulds of industrial equipment for being filled with ceramic slurry are successively freezed since one end, each layer successively freezed Thickness≤1 μm.
- A kind of 3. ceramic material according to claim 2, it is characterised in that：Described refrigerating process employing mode one or side Formula two,Mode one, the moulds of industrial equipment for being filled with ceramic slurry are placed in refrigerated container, be slowly injected into from refrigerated container bottom≤- 80 DEG C of refrigerant, ceramic slurry is successively freezed since bottom, every layer of freezing thickness≤1 μm, i.e., noted each time Height≤1 μm of the refrigerant entered, freezing soaking time are not less than 0.5 minute；Mode two, according to freezing direction, the ceramic slurry being filled in moulds of industrial equipment persistently slowly enters≤- 80 DEG C of freezing In medium, admission velocity is no more than 1 μm/3min.
- A kind of 4. ceramic material according to claim 1, it is characterised in that：Described ceramic powder is silicon nitride powder, oxygen Change barium powder and alumina powder, the wherein addition of barium monoxide, aluminum oxide on the basis of the quality of silica in alkaline silica sol, According to stoichiometric proportion BaO-A12O3-2SiO2Addition, silicon nitride powder quality account for solid gross mass in mixed slurry 55~ 90%.
- A kind of 5. ceramic material according to claim 1, it is characterised in that：A small amount of point is added in described ceramic slurry Powder, addition are 0.5~3% of solid gross mass in ceramic slurry.
- A kind of 6. ceramic material according to claim 1, it is characterised in that：Ceramic slurry is added in described ceramic slurry The small molecule multi-hydroxy alcohol type organic of the 1 ± 0.2% of the quality of middle liquid phase water.
- A kind of 7. ceramic material according to claim 1, it is characterised in that：Described small molecule multi-hydroxy alcohols is organic The molecular weight of thing molecular weight is less than 10000.
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