CN103896589B - Method for preparing silicon-boron-carbon-nitrogen porous ceramic with nano pore structure - Google Patents
Method for preparing silicon-boron-carbon-nitrogen porous ceramic with nano pore structure Download PDFInfo
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- CN103896589B CN103896589B CN201410079851.XA CN201410079851A CN103896589B CN 103896589 B CN103896589 B CN 103896589B CN 201410079851 A CN201410079851 A CN 201410079851A CN 103896589 B CN103896589 B CN 103896589B
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Abstract
The invention relates to a method for preparing silicon-boron-carbon-nitrogen porous ceramic with a nano pore structure. The method comprises the following steps: uniformly mixing boron trichloride, aniline and simethicone according to a ratio of 1:1:2.5, and heating to react to prepare an organic precursor; then dipping nano polyacrylonitrile fibers in the organic precursor and performing heat preservation at a certain temperature; finally sintering the mixture in a high-purity nitrogen atmosphere, and cooling the mixture to room temperature with the furnace after the heat preservation is finished, wherein after the high temperature nitrogen treatment, the nano polyacrylonitrile fibers are corroded to form silicon-boron-carbon-nitrogen (Si-B-C-N) porous ceramic with the nano pore structure. The aperture of the obtained silicon-boron-carbon-nitrogen (Si-B-C-N) porous ceramic is 150-300 nm, the porosity is up to 78-90%, the silicon-boron-carbon-nitrogen (Si-B-C-N) porous ceramic is high temperature resistant, oxidation resistant, free of obvious oxidation at 950 DEG C in an air atmosphere, and free of obvious loss of mechanical property at 1100 DEG C. The silicon-boron-carbon-nitrogen (Si-B-C-N) porous ceramic can be applied to a diesel exhaust particulate filter (DPF) carrier.
Description
Technical field
The present invention relates to a kind of composite ceramic material preparation method, specifically a kind of nano-pore structure Si-B-C-N porous ceramics preparation method.
Background technology
Along with environmental ecology is polluted more and more serious, city haze phenomenon is also increasingly serious, has a strong impact on life and the health of people, purifying air problem thus cause the extensive concern of society.Porous ceramics as a kind of good filtration supports, industry-by-industry purifying air, filter play an important role.The preparation method of nowadays conventional porous ceramics has: Polymeric sponge method, foaming, template synthesis method etc.Polymeric sponge method utilizes porous support (as porous plastics) absorbent ceramic slip, then at high temperature after-flame solid support material and form hole mechanism, its shortcoming is raw materials used and operation is loaded down with trivial details, made porous ceramics duct and aperture wayward, and porosity is not high.Foaming is the chemical substance adding organic or inorganic in ceramic composition, during processing, produce volatile gases, thus produces foam, then through super-dry and burn till obtained porous ceramics.Although the porous ceramics that foaming obtains can have complicated shape, the porous state of different structure, its porosity lower (being generally no more than 50%).Template synthesis method utilizes the pore passage structure contained in template, ceramic precursor is injected template, sintering, original pore passage structure is made to remain and prepare the porous ceramics identical with shape with formwork structure, but the porous ceramics mechanical property difference obtained by different templates is large, is subject to having a strong impact on of templating species.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method and simply, easily operates, and production cost is low, ceramic porous nickel, high temperature resistant, oxidation resistant nano-pore structure Si-B-C-N porous ceramics preparation method.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of nano-pore structure Si-B-C-N porous ceramics preparation method, is characterized in that: it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 40 ~ 65
oc reacts 4 ~ 5h, makes Si-B-C-N organic precursor method stand-by;
(2) by nano polypropylene nitrile fiber impregnation in above-mentioned Si-B-C-N organic precursor method, and at 50-70
o1 ~ 2h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 0.3 ~ 1.5g; Nano polypropylene nitrile Fibre diameter is 150-200nm;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 1.5 ~ 2.5h; Sintering oven passes into high pure nitrogen (purity is 99.999%) and does shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, and after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.
The present invention is with dimethyl silicone oil, boron trichloride, aniline for raw material monomer synthesis Si-B-C-N organic precursor method, and this precursor is the main raw material of Si-B-C-N porous ceramics, and nano polypropylene nitrile fiber is pore-creating raw material.After high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.Against existing technologies, the inventive method simply, easily operates, reproducible, production cost is low, ceramic porous nickel, high temperature resistant, anti-oxidant.Si-B-C-N (Si-B-C-N) the porous ceramics aperture of preparation is 150-300nm, and porosity is up to 78 ~ 90% after tested, high temperature resistant, anti-oxidant.Under air atmosphere 950
oc is not obviously oxidized, and 1100
oduring C, mechanical property does not have significantly sacrificing.Can be used for diesel exhaust particulate trap (DPF) carrier.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
A kind of nano-pore structure Si-B-C-N porous ceramics preparation method, is characterized in that: it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 40 ~ 65
oc reacts 4 ~ 5h, makes Si-B-C-N organic precursor method stand-by;
(2) by nano polypropylene nitrile fiber impregnation in above-mentioned Si-B-C-N organic precursor method, and at 50-70
o1 ~ 2h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 0.3 ~ 1.5g; Nano polypropylene nitrile Fibre diameter is 150-200nm;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 1.5 ~ 2.5h; Sintering oven pass into purity be 99.999% high pure nitrogen do shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, and after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.
The present invention is with dimethyl silicone oil, boron trichloride, aniline for raw material monomer synthesis Si-B-C-N organic precursor method, and this precursor is the main raw material of Si-B-C-N porous ceramics, and nano polypropylene nitrile fiber is pore-creating raw material.Under the mixture of Si-B-C-N (Si-B-C-N) organic precursor method and nano polypropylene nitrile fiber is placed in protective atmosphere, high temperature sintering prepares nano-pore structure Si-B-C-N porous ceramics.After high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.Si-B-C-N (Si-B-C-N) porous ceramics prepared by the present invention is observed microscopic appearance, and can see that porous nickel distributes, aperture is 150-300nm, and porosity is up to 78 ~ 90% after tested.High temperature resistant, anti-oxidant.Under air atmosphere 950
oc is not obviously oxidized, and 1100
oduring C, mechanical property does not have significantly sacrificing.Can be used for diesel exhaust particulate trap (DPF) carrier.
Embodiment 1: a kind of nano-pore structure Si-B-C-N porous ceramics preparation method, it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 40
oc reacts 5h, makes Si-B-C-N organic precursor method stand-by;
(2) nano polypropylene nitrile fiber (Fibre diameter 150-200nm) be impregnated in above-mentioned Si-B-C-N organic precursor method, and 50
o1h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 1.0g;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 2h; Sintering oven passes into high pure nitrogen (purity is 99.999%) and does shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, and after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.
Embodiment 2: a kind of nano-pore structure Si-B-C-N porous ceramics preparation method, it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 50
oc reacts 4.5h, makes Si-B-C-N organic precursor method stand-by;
(2) nano polypropylene nitrile fiber (Fibre diameter 150-200nm) be impregnated in above-mentioned Si-B-C-N organic precursor method, and 60
o1.5h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 1.5g;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 1.5h; Sintering oven passes into high pure nitrogen (purity is 99.999%) and does shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, and after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.
Embodiment 3: a kind of nano-pore structure Si-B-C-N porous ceramics preparation method, it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 65
oc reacts 4h, makes Si-B-C-N organic precursor method stand-by;
(2) nano polypropylene nitrile fiber (Fibre diameter 150-200nm) be impregnated in above-mentioned Si-B-C-N organic precursor method, and at 50-70
o2h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 0.3g;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 1.5h; Sintering oven passes into high pure nitrogen (purity is 99.999%) and does shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, and after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, and forms Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure.
Si-B-C-N (Si-B-C-N) porous ceramics prepared by the present invention can be used for diesel exhaust particulate trap (DPF) carrier.
Claims (1)
1. a nano-pore structure Si-B-C-N porous ceramics preparation method, is characterized in that: it comprises the following steps:
(1) Si-B-C-N organic precursor method is first prepared by boron trichloride, aniline, dimethyl silicone oil 1:1:2.5 Homogeneous phase mixing in molar ratio, and 40 ~ 65
oc reacts 4 ~ 5h, makes Si-B-C-N organic precursor method stand-by;
(2) by nano polypropylene nitrile fiber impregnation in above-mentioned Si-B-C-N organic precursor method, and at 50-70
o1 ~ 2h is incubated under C; Wherein in every 100gSi-B-C-N organic precursor method the add-on of nano polypropylene nitrile fiber for adding 0.3 ~ 1.5g; Described nano polypropylene nitrile Fibre diameter is 150-200nm;
(3) the Si-B-C-N organic precursor method of above-mentioned preparation and nano polypropylene nitrile fibre blend are cooled to room temperature and put into gas-protecting sintering stove; Sintering oven is with 3 ~ 5
othe temperature rise rate of C/min is warming up to 1200
oc, and 1200
oc is incubated 1.5 ~ 2.5h; Sintering oven pass into purity be 99.999% high pure nitrogen do shielding gas;
(4) insulation cools to room temperature with the furnace after terminating, after high-temperature ammonolysis process, nano polypropylene nitrile fiber is wherein etched away, form Si-B-C-N (Si-B-C-N) porous ceramics of nano-pore structure, Si-B-C-N (Si-B-C-N) the porous ceramics aperture obtained is 150-300nm, and porosity is up to 78 ~ 90% after tested.
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| US6444006B1 (en) * | 2000-05-18 | 2002-09-03 | Fleetguard, Inc. | High temperature composite ceramic filter |
| CN101700978A (en) * | 2009-11-11 | 2010-05-05 | 哈尔滨工业大学 | Method for preparing SiBCN(O) ceramic material |
| CN103396125B (en) * | 2013-08-01 | 2014-07-02 | 哈尔滨工业大学（威海） | Preparation method for boron-carbon-nitrogen porous ceramic |
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