CN101792327A - Preparation method of alumina oxide matrix porous ceramic material - Google Patents
Preparation method of alumina oxide matrix porous ceramic material Download PDFInfo
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- CN101792327A CN101792327A CN201010112097A CN201010112097A CN101792327A CN 101792327 A CN101792327 A CN 101792327A CN 201010112097 A CN201010112097 A CN 201010112097A CN 201010112097 A CN201010112097 A CN 201010112097A CN 101792327 A CN101792327 A CN 101792327A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011159 matrix material Substances 0.000 title description 22
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000000465 moulding Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 230000004224 protection Effects 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229920002050 silicone resin Polymers 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 4
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000007873 sieving Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000011800 void material Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 235000015895 biscuits Nutrition 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000004523 agglutinating effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
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Abstract
本发明提供的氧化铝基多孔陶瓷材料的制备方法，具体是：将有机硅树脂与氧化铝陶瓷粉料均匀混合，二者之体积配比为1∶1～4∶1；将混合粉体在100～150℃处理3～24小时蒸发溶剂，同时脱去有机硅中的自由水，获得氧化铝陶包覆粉体，研磨过筛后采用阶梯升温模压工艺制度将氧化铝陶包覆粉体成型，得到素坯试样；将素坯在800～1200℃惰性气氛保护下裂解，控制反应速率为100～300℃/小时，保温时间1～10小时，即得到一种氧化铝基多孔陶瓷材料。本发明裂解温度低、可重复性好、成本低廉，而且所制备的氧化铝基多孔陶瓷材料具有孔隙分布均匀、孔径尺度小、孔隙率较高和力学强度较高等优异性能。
The preparation method of the alumina-based porous ceramic material provided by the present invention is specifically: uniformly mixing the organosilicon resin and the alumina ceramic powder, and the volume ratio of the two is 1:1 to 4:1; mixing the powder in Treat at 100-150°C for 3-24 hours to evaporate the solvent and remove the free water in the organosilicon at the same time to obtain the alumina ceramic coated powder. After grinding and sieving, the alumina ceramic coated powder is formed by using the step-up temperature molding process system , to obtain a green body sample; crack the green body under the protection of an inert atmosphere at 800-1200°C, control the reaction rate at 100-300°C/hour, and hold the temperature for 1-10 hours, and obtain an alumina-based porous ceramic material. The invention has low cracking temperature, good repeatability and low cost, and the prepared alumina-based porous ceramic material has excellent properties such as uniform pore distribution, small pore size, high porosity and high mechanical strength.
Description
Technical field
The present invention relates to the stupalith field, particularly relate to the preparation method of a kind of silicone resin as the alumina oxide matrix porous ceramic material of binding agent.
Background technology
Porous ceramics is a kind ofly to burn till, form in the material bodies new ceramic material of a large amount of pores through high temperature in moulding and sintering process, can be used as uses such as biomaterial, catalyst support material, filtering material, heat exchanger material.
Alumina-ceramic is with its preferred material that becomes porous ceramics cheap for manufacturing cost.Aluminum oxide is except characteristics such as wide material sources, relative low price, technology of preparing maturation, and also have following good characteristic: (1) is high temperature resistant; (2) chemical stability is good; (3) abrasion resistance properties is good; (4) corrosion-resistant; (5) physical strength height; (6) thermal conductivity is low; (7) hardness is big.Alumina oxide matrix porous pottery is as a kind of excellent performance, the porous ceramic film material that has a extensive future, and its potential application can be distributed widely in melted metal filtering, hot gas filtration, microporous membrane, transmitter, diaphragm material and industries such as fixed enzyme vector and heat insulating.
The main preparation methods of alumina porous ceramic has following several method: 1) add pore-forming material, volatile substances technology; 2) extruding shaping technique; 3) particle packing moulding process; 4) foam process; 5) organic foam body impregnation technology; 6) sol-gel technology etc.The porous ceramics preparation method that these are traditional except a large amount of sintering aid of needs, has also improved sintering temperature, the difficult higher alumina porous ceramic material of purity that obtains.
Summary of the invention
Technical problem to be solved by this invention is: a kind of more easy method is provided, preparation has the alumina oxide matrix porous ceramic material of excellent performance under lower temperature, and develops the novel method that a kind of novel silicone resin cracking prepares alumina oxide matrix porous ceramic material.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of alumina oxide matrix porous ceramic material provided by the invention is to utilize silicone resin to prepare alumina oxide matrix porous ceramic material as binding agent, specifically is to be undertaken by following step:
(1) mix: with silicone resin as binding agent directly and alumina-ceramic powder uniform mixing, the volume proportion of the two is 1: 1～4: 1.Described volume proportion is meant the volume proportion of pure silicone resin and alumina-ceramic powder; When using the solvent-type organosilicon resin, should silicone resin content be converted into pure silicone resin according to its solid content and prepare burden again.
Described silicone resin can adopt the SOLID ORGANIC silicone resin that can be dissolved in organic solvent, perhaps adopts the solvent-type organosilicon resin.Can also be with hydroxy-end capped condensed type resin, with phenyl and methyl as side chain, molecular weight 〉=2000.
(2) pre-treatment: mixed powder is handled 3～24 hours evaporating solvents at 100～150 ℃, slough the free water in the organosilicon simultaneously, obtain aluminum oxide pottery coated powder;
(3) ladder-elevating temperature compression molding: the method that adopts the moulding of ladder-elevating temperature mould pressing process system obtains biscuit with the aluminum oxide coated powder moulding of making pottery; The volume content of silicone resin is 50～80% in the biscuit.Ladder-elevating temperature mould pressing process system is meant: axial pressure 10～60Mpa, and temperature schedule is 100～120 ℃ of insulation 0.5～1h; Be warming up to 130～150 ℃ of insulation 0.5～2h again; Be warming up to 170～190 ℃ of insulation 0.5～2h again; Be warming up to 200～210 ℃ of insulation 0.5～1h at last again.
(4) thermal treatment and cracking: with biscuit cracking under 800～1200 ℃ of inert atmosphere protections, the control speed of reaction is 100～300 ℃/hour and soaking time 1～10 hour, promptly obtains described alumina oxide matrix porous ceramic material.
Described inert atmosphere is meant nitrogen or argon gas.
The particle diameter of the alumina-ceramic powder of the present invention's preparation is 1～20 μ m.
The present invention utilizes the cohesiveness of silicone resin highly effectively to form coated powder with alumina particle, and impels the alumina particle bonding, makes biscuit have mechanical property preferably.Along with the rising of temperature, the silicone resin molecular chain in the base substrate is constantly reset and is produced a large amount of glassy phases, plays the agglutinating effect, with Al
2O
3The particle dissolving is wrapped in wherein, and the adjacent particle center is approached mutually, increases contact area, take place bondingly between the particle, improved matrix strength, form some sealed porositys simultaneously, the silicone resin molecular rupture forms the successive spilehole simultaneously, has improved porosity.In whole process, silicone resin plays to have arrived simultaneously binding agent and pore-forming material, has saved cost effectively.
The present invention utilizes the organosilicon cracking to prepare alumina oxide matrix porous ceramic material and compares with traditional method and also have following advantage:
One. thereby the silicone resin cracking can produce the purpose that gas reaches pore-creating, can reach controlled, the controlled porosity of perforate/closed pore by the control experimental technique, obtains the aperture size of relative broad range, does not need to add other pore-forming materials.
They are two years old. and silicone resin is to be the organic polymer of main chain with Si-O-Si, and cracking temperature is lower and have cohesiveness, need not to add other binding agents in the ceramic process of preparation.
They are three years old. and silicone resin had not only played the effect of binding agent but also had played the effect of pore-forming material in whole process of preparation, this has saved the use of sintering aid greatly, reduce the introducing of impurity, can obtain purer alumina-ceramic, and also reduced production cost.Simultaneously, silicone resin forms a large amount of liquid phases in cracking process, has reduced the sintering temperature of aluminum oxide.
They are four years old. and favorable repeatability, cost are low, and prepared alumina oxide matrix porous ceramic material has even pore distribution, the aperture yardstick is little, porosity is high and the more high excellent properties of mechanical strength.
In sum: the present invention utilizes the silicone resin cracking to prepare alumina oxide matrix porous pottery, can reach 40% apparent porosity, ratio by control silicone resin and aluminum oxide can reach the controlled requirement of apparent porosity, and have plurality of advantages such as moulding process is simple, firing temperature is low, meet the demand of modern industry.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is the XRD figure of embodiment 1 product.
Fig. 3 is the SEM figure of embodiment 1 product.
Embodiment
The invention provides the preparation method of a kind of silicone resin as the alumina oxide matrix porous ceramic material of binding agent, its technical process as shown in Figure 1: comprise mixing, pre-treatment, compression molding, thermal treatment and sintering circuit.
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1:
(1) be 4: 1 to carry out uniform mixing less than the alumina powder of 20 μ m according to weight ratio with silicone resin and particle diameter;
(2) the method moulding by ladder-elevating temperature mould pressing process system, axial pressure 60Mpa, temperature schedule is 120 ℃, 0.5h → 150 ℃, 1h → 180 ℃, 1h → 200 ℃, 0.5h;
(3) nitrogen atmosphere protection is carried out normal pressure-sinteredly down in 1200 ℃, and temperature rise rate is 120 ℃/hour, is incubated 2 hours.Can obtain void content 25%, bending strength is 57MPa, and density is 2.03g/cm
3Alumina oxide matrix porous ceramic material.
Analytical test shows (see figure 2): the main thing of product is Alpha-alumina and gama-alumina mutually, has still kept the main thing phase of raw material, does not take place to change mutually.But, can find out significantly that silicone resin has formed the amorphous state material of a kind of Si-C-O in cracking process, weakened the diffraction peak of aluminum oxide.The material of this amorphous state provides liquid phase, has reduced the sintering temperature of aluminum oxide, makes this alumina oxide matrix porous ceramic material have higher mechanical strength simultaneously.The alumina oxide matrix porous ceramic material void distribution for preparing by this method is more even, and porosity is higher, and the aperture yardstick is less.
Analytical test shows (see figure 3): the alumina oxide matrix porous ceramic material porosity for preparing is higher, and void distribution is more even, and the aperture yardstick is little.
Embodiment 2:
(1) be 3.3: 1 to carry out uniform mixing less than the alumina powder of 20 μ m according to weight ratio with silicone resin and particle diameter;
(2) the method moulding by ladder-elevating temperature mould pressing process system, axial pressure 40Mpa, temperature schedule is 120 ℃, 1h → 150 ℃, 1h → 180 ℃, 1h → 200 ℃, 1h;
(3) nitrogen atmosphere protection is carried out cracking in 1200 ℃ down, and temperature rise rate is 120 ℃/hour, is incubated 2 hours.Can obtain void content 31%, bending strength is 43MPa, and density is 2.01g/cm
3Alumina oxide matrix porous ceramic material.
Embodiment 3:
(1) be 3.6: 1 to carry out uniform mixing less than the alumina powder of 10 μ m according to weight ratio with silicone resin and particle diameter;
(2) the method moulding by ladder-elevating temperature mould pressing process system, axial pressure 30Mpa, temperature schedule is 120 ℃, 0.5h → 150 ℃, 1h → 180 ℃, 1h → 200 ℃, 1h;
(3) nitrogen atmosphere protection is carried out cracking in 1100 ℃ down, and temperature rise rate is 140 ℃/hour, is incubated 2 hours.Can obtain void content 33%, bending strength is 36MPa, and density is 1.98g/cm
3Alumina oxide matrix porous ceramic material.
Embodiment 4:
(1) be 1.6: 1 to carry out uniform mixing less than the alumina powder of 10 μ m according to weight ratio with silicone resin and particle diameter;
(2) the method moulding by ladder-elevating temperature mould pressing process system, axial pressure 10Mpa, temperature schedule is 120 ℃, 0.5h → 150 ℃, 0.5h → 180 ℃, 1h → 200 ℃, 1h;
(3) nitrogen atmosphere protection is carried out cracking in 1000 ℃ down, and temperature rise rate is 240 ℃/hour, is incubated 2 hours.Can obtain void content 36%, bending strength is 29MPa, and density is 1.96g/cm
3Alumina oxide matrix porous ceramic material.
Embodiment 5:
(1) be 4: 1 to carry out uniform mixing less than the alumina powder of 20 μ m according to weight ratio with silicone resin and particle diameter;
(2) the method moulding by ladder-elevating temperature mould pressing process system, axial pressure 20Mpa, temperature schedule is 120 ℃, 0.5h → 150 ℃, 0.5h → 180 ℃, 1h → 200 ℃, 1h;
(3) nitrogen atmosphere protection is carried out cracking in 800 ℃ down, and temperature rise rate is 240 ℃/hour, is incubated 2 hours.Can obtain void content 34%, bending strength is 32MPa, and density is 1.96g/cm
3Alumina oxide matrix porous ceramic material.
The analytical test result of the foregoing description 2-5 is with embodiment 1.
Claims (8)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351563A (en) * | 2011-07-06 | 2012-02-15 | 武汉理工大学 | Preparation method for silicon nitride porous ceramic with multilevel pore size structure and high porosity |
| CN102795885A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method of aluminum oxide-zirconium oxide composite porous ceramic for high-temperature filtration |
| CN102795884A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method for synthesizing porous magnesium aluminate spinel by reacting |
| CN103887054A (en) * | 2012-12-19 | 2014-06-25 | 中磁科技股份有限公司 | Preparation method of large-sized neodymium-iron-boron magnetic steel |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
| CN107200599A (en) * | 2017-06-16 | 2017-09-26 | 深圳市商德先进陶瓷股份有限公司 | Porous alumina ceramic and its preparation method and application |
| CN111892385A (en) * | 2020-08-18 | 2020-11-06 | 重庆奥福精细陶瓷有限公司 | Preparation method of large-size diesel particle filter |
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-
2010
- 2010-02-09 CN CN201010112097A patent/CN101792327A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351563A (en) * | 2011-07-06 | 2012-02-15 | 武汉理工大学 | Preparation method for silicon nitride porous ceramic with multilevel pore size structure and high porosity |
| CN102795885A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method of aluminum oxide-zirconium oxide composite porous ceramic for high-temperature filtration |
| CN102795884A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method for synthesizing porous magnesium aluminate spinel by reacting |
| CN102795884B (en) * | 2012-09-11 | 2014-06-11 | 江苏格业新材料科技有限公司 | Preparation method for synthesizing porous magnesium aluminate spinel by reacting |
| CN102795885B (en) * | 2012-09-11 | 2015-01-28 | 江苏格业新材料科技有限公司 | Preparation method of aluminum oxide-zirconium oxide composite porous ceramic for high-temperature filtration |
| CN103887054A (en) * | 2012-12-19 | 2014-06-25 | 中磁科技股份有限公司 | Preparation method of large-sized neodymium-iron-boron magnetic steel |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
| CN107200599A (en) * | 2017-06-16 | 2017-09-26 | 深圳市商德先进陶瓷股份有限公司 | Porous alumina ceramic and its preparation method and application |
| CN111892385A (en) * | 2020-08-18 | 2020-11-06 | 重庆奥福精细陶瓷有限公司 | Preparation method of large-size diesel particle filter |
| CN111892384A (en) * | 2020-08-18 | 2020-11-06 | 重庆奥福精细陶瓷有限公司 | Wall-flow cordierite gasoline particle filter and preparation method thereof |
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Application publication date: 20100804 |