CN103979967A - Method for preparing micron-scale worm-like SiCO ceramics - Google Patents
Method for preparing micron-scale worm-like SiCO ceramics Download PDFInfo
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Abstract
The invention discloses a method for preparing micron-scale worm-like SiCO ceramics and relates to micron ceramics. The method comprises the following steps: adding a thermal cross-linking agent, dicumyl peroxide, into 0.8g of template agent F127, then, dissolving into 5ml of xylene solution, and stirring so as to obtain mixed liquid A; dissolving 0.8g of ceramic precursor, polyvinyl silazane, into 5ml of ethanol, and stirring so as to obtain mixed liquid B; mixing the mixed liquid A and the mixed liquid B, and stirring so as to obtain mixed liquid C; pouring the mixed liquid C on a glass substrate, carrying out heat preservation in a baking oven at the temperature of 50 DEG C, then, cross-linking at the temperature of 140 DEG C so as to obtain a yellowish transparent film, taking out, stripping, and then, pyrolyzing the film in an inert atmosphere, thereby obtaining the micron-scale worm-like SiCO ceramics on the surface of the film. The prepared micron-scale worm-like SiCO ceramics have the length of 0.5-2 microns, are good in stability and are applied to the fields of composite materials, high-temperature device design and the like; the method has the advantages that the equipment investment is small, the operation is easy, the process is simple, and the repeatability is good.
Description
Technical field
The present invention relates to a kind of micrometer ceramics, especially relate to a kind of preparation method of SiCO micron order vermiform pottery.
Background technology
The preparation of micro-nano structure is difficult point and the focus in current application field.The method of microstage structured material is received in preparation two kinds: a kind of is method from top to bottom, reduces as possible structure of matter dimension, as: mechanical mill comminuting method and unconventional optical etching technology; Another is method from bottom to top, as the self-assembly by molecule builds nano material.The method of wherein preparing nano material based on Self-Assembling of Block Copolymer causes investigator's very big interest, this is that the kinetic stability of its self-assembly and structural stability are all greater than small molecules tensio-active agent because segmented copolymer can self-assembly form abundant ordered micro structure.In addition, the regular microstructure that self-assembly forms can not only exist in solution, and can also form at solid state, and to becoming, really to have the material of Practical significance most important for this.
Segmented copolymer has been studied widely and has been paid attention at organic polymer and electrochemical field etc., and Chinese patent CN101914191A discloses a kind of preparation method of polyoxometallate-polymer hybridized segmented copolymer nanotube.Chinese patent CN101244818 discloses a kind ofly take polyurethane sponge as skeleton support body, take nonionic surface active agent as structure directing agent, take polymer presoma as carbon source, take inorganic silicon source etc. is additive, through high temperature hot polymerization and carbonization, preparation has in order mesoporous polymer, carbon material and the matrix material of mesopore orbit, high-specific surface area, macropore volume continuously.Chinese patent CN101059472 discloses the method for assembling block copolymer for preparing gold nano array electrode in a kind of water, by the poly-four vinyl pyridines-polystyrene block copolymer of assembling in water, utilize the electrostatic interaction between cationic micelle and electronegative golden nanometer particle to prepare gold-nano array electrode.This making method is fast and convenient, does not introduce organic solvent, and electrode surface can upgrade to be reused, and has reduced cost.Although the self-assembling technique of segmented copolymer is as a kind of very potential ordered structure assemble method, yet be applied in inorganic aspect or a newer field.It is simple that Chinese patent CN103073297A discloses a kind of preparation process, can prepare efficiently the method for SiCO nanometer ball.And the preparation of SiCO micrometer ceramics cross bar have not been reported.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of SiCO micron order vermiform pottery.
The present invention includes following steps:
1) at 0.8g template F127 (PEO
106-pPO
70-PEO
106, add thermal cross-linking agent dicumyl peroxide in Mw=12600g/mol), then be dissolved in 5ml xylene solution, after stirring, obtain mixed liquor A;
2) by the ceramic precursor Polyvinylsilazane of 0.8g, be dissolved in 5ml ethanol, after stirring, obtain mixed liquid B;
3) mixed liquor A and mixed liquid B are mixed, after stirring, obtain mixed solution C;
4) mixed solution C is poured on glass substrate, in the baking oven of 50 ℃, is incubated, then 140 ℃ crosslinked after, obtain faint yellow transparent film, take out rear demoulding, then pyrolysis film in inert atmosphere, obtains SiCO micron order vermiform pottery at film surface.
In step 1) in, described in be dissolved in 5ml xylene solution after, the sealing of the most handy sealed membrane; The time of described stirring can be 30~60min.
In step 2) in, described in be dissolved in 5ml ethanol after, the sealing of the most handy sealed membrane; Described stirring can adopt magnetic agitation 30~60min.
In step 3) in, after described mixing, the most handy sealed membrane sealing; The time of described stirring can be 12~36h.
In step 4) in, the time of described insulation can be 24~96h; The described crosslinked time can be 60~80min; The program of described pyrolysis can be: with 1 ℃/min, rise to 130 ℃ of insulation 1h, with 0.5 ℃/min, rise to 300 ℃ of insulation 3h, with 0.5 ℃/min, rise to 400 ℃ of insulation 3h, with 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.
The present invention adopts ceramic precursor Polyvinylsilazane and template F127 (PEO
106-PPO
70-PEO
106, Mw=12600g/mol) blend in the mixed solvent of dimethylbenzene and ethanol, after self-assembly, in inert atmosphere, SiCO micron order vermiform pottery is prepared in pyrolysis.
The method of the SiCO of preparation micron order vermiform pottery provided by the invention has the following advantages:
1) length of the SiCO micron order vermiform pottery that prepared by the present invention is between 0.5~2 μ m, and good stability.
2) the SiCO micron order vermiform pottery that prepared by the present invention has important using value in fields such as matrix material and high-temperature device designs.
3) the present invention adopts Polyvinylsilazane and template F127 (PEO
106-PPO
70-PEO
106, the method for common assembling Mw=12600g/mol) is prepared SiCO micron order vermiform pottery, and its great advantage is that facility investment is few, processing ease, technical process is simpler, reproducible.
Accompanying drawing explanation
Fig. 1 is the SEM photo (scale is 10 μ m) of the prepared SiCO micron order vermiform pottery of the embodiment of the present invention 1.
Fig. 2 is the SEM photo (scale is 5 μ m) of the prepared SiCO micron order vermiform pottery of the embodiment of the present invention 1.
Embodiment
Below by embodiment, the present invention will be further described by reference to the accompanying drawings.
Embodiment 1:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 24h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 48h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 70min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.As illustrated in fig. 1 and 2, can clear view arrive SiCO micron order vermiform pottery.
Embodiment 2:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 12h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 24h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 70min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
Embodiment 3:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 24h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 96h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 80min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
Embodiment 4:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 36h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 36h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 80min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
Embodiment 5:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 12h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 72h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 60min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
Embodiment 6:
Glass substrate is cleaned and supersound process with ethanol and acetone, put into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 36h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 24h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 60min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
Embodiment 7:
Glass substrate cleans and supersound process with ethanol and acetone, puts into subsequently baking oven dry for standby.Take in the container of the dimethylbenzene that is dissolved in 5ml after the F127 of 0.8g and the dicumyl peroxide of 0.032g mix and sealing, stir 30min and obtain mixed liquor A.The Polyvinylsilazane that adds 0.8g in another container, is dissolved in 5ml ethanol, and sealing rapidly, and magnetic agitation 30min, obtains mixed liquid B.Subsequently the solution in two containers is mixed and sealing rapidly, container is avoided irradiate light, continues churning time 12h, obtains mixed solution C.Mixed solution C is laid in to glass baseplate surface, moves in 50 ℃ of insulation cans and be incubated 48h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 80min of 140 ℃, film becomes faint yellow from water white transparency, takes out demoulding.After demoulding, film is placed on graphite paper.Subsequently, put into the tube furnace sintering of protection of inert gas.
Following heating schedule is set: from room temperature, with the temperature rise rate of 1 ℃/min, rise to 130 ℃ and be incubated 1h, with the temperature rise rate of 0.5 ℃/min, rise to 300 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃, rise to 400 ℃ and be incubated 3h, with the temperature rise rate of 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.Take out graphite paper, obtain the film sample of black, on its surface, obtain SiCO micron order vermiform pottery.
First the present invention is dissolved in ethanolic soln by ceramic forerunner Polyvinylsilazane, simultaneously by template F127 (PEO
106-PPO
70-PEO
106mw=12600g/mol) and thermal cross-linking agent dicumyl peroxide be dissolved in xylene solution, stir respectively 30~60min, again two solution are mixed, obtain mixing solutions, subsequently mixing solutions is laid on face glass, molten insulation evaporation, crosslinked in 50 degree thermostat containers, the demoulding again, thermal treatment obtain SiCO micron order vermiform pottery, and length is between 0.5~μ m.The method preparation technology is simple, and preparation condition is gentle, can prepare efficiently micron order vermiform pottery.
Claims (10)
1. a preparation method for SiCO micron order vermiform pottery, is characterized in that comprising the following steps:
1) at 0.8g template F127 (PEO
106-PPO
70-PEO
106, add thermal cross-linking agent dicumyl peroxide in Mw=12600g/mol), then be dissolved in 5ml xylene solution, after stirring, obtain mixed liquor A;
2) by the ceramic precursor Polyvinylsilazane of 0.8g, be dissolved in 5ml ethanol, after stirring, obtain mixed liquid B;
3) mixed liquor A and mixed liquid B are mixed, after stirring, obtain mixed solution C;
4) mixed solution C is poured on glass substrate, in the baking oven of 50 ℃, is incubated, then 140 ℃ crosslinked after, obtain faint yellow transparent film, take out rear demoulding, then pyrolysis film in inert atmosphere, obtains SiCO micron order vermiform pottery at film surface.
2. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 1) in, described in be dissolved in 5ml xylene solution after, with sealed membrane, seal.
3. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 1) in, the time of described stirring is 30~60min.
4. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 2) in, described in be dissolved in 5ml ethanol after, with sealed membrane, seal.
5. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 2) in, described stirring adopts magnetic agitation 30~60min.
6. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 3) in, after described mixing, with sealed membrane, seal.
7. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 3) in, the time of described stirring is 12~36h.
8. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 4) in, the time of described insulation is 24~96h.
9. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, is characterized in that in step 4) in, the described crosslinked time is 60~80min.
10. a kind of preparation method of SiCO micron order vermiform pottery as claimed in claim 1, it is characterized in that in step 4) in, the program of described pyrolysis is: with 1 ℃/min, rise to 130 ℃ of insulation 1h, with 0.5 ℃/min, rise to 300 ℃ of insulation 3h, with 0.5 ℃/min, rise to 400 ℃ of insulation 3h, with 0.5 ℃/min, rise to 500 ℃ and be incubated 4h, finally naturally cool to room temperature.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105205316A (en) * | 2015-09-10 | 2015-12-30 | 温州大学 | Simulation method for predicting performance of SiCO anode material |
CN106554205A (en) * | 2016-11-25 | 2017-04-05 | 厦门大学 | A kind of preparation method of the micrometer level porous hollow ceramic ball of SiCO |
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CN103022434A (en) * | 2012-11-23 | 2013-04-03 | 中国科学院宁波材料技术与工程研究所 | Precursor ceramic-carbon nano tube composite material and preparation method thereof |
CN103073297A (en) * | 2013-02-22 | 2013-05-01 | 厦门大学 | Preparation method of SiCO ceramic nanospheres |
CN103466590A (en) * | 2013-09-13 | 2013-12-25 | 厦门大学 | Preparation method of SiCO hollow nanospheres |
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2014
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Patent Citations (3)
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CN103022434A (en) * | 2012-11-23 | 2013-04-03 | 中国科学院宁波材料技术与工程研究所 | Precursor ceramic-carbon nano tube composite material and preparation method thereof |
CN103073297A (en) * | 2013-02-22 | 2013-05-01 | 厦门大学 | Preparation method of SiCO ceramic nanospheres |
CN103466590A (en) * | 2013-09-13 | 2013-12-25 | 厦门大学 | Preparation method of SiCO hollow nanospheres |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105205316A (en) * | 2015-09-10 | 2015-12-30 | 温州大学 | Simulation method for predicting performance of SiCO anode material |
CN105205316B (en) * | 2015-09-10 | 2017-09-29 | 温州大学 | One kind prediction SiCO negative material performance simulation methods |
CN106554205A (en) * | 2016-11-25 | 2017-04-05 | 厦门大学 | A kind of preparation method of the micrometer level porous hollow ceramic ball of SiCO |
CN106554205B (en) * | 2016-11-25 | 2019-09-10 | 厦门大学 | A kind of preparation method of the micrometer level porous hollow ceramic ball of SiCO |
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