CN103979540A - Method for preparing micron-scale strawberry-shaped SiCO ceramic balls - Google Patents
Method for preparing micron-scale strawberry-shaped SiCO ceramic balls Download PDFInfo
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- CN103979540A CN103979540A CN201410230575.2A CN201410230575A CN103979540A CN 103979540 A CN103979540 A CN 103979540A CN 201410230575 A CN201410230575 A CN 201410230575A CN 103979540 A CN103979540 A CN 103979540A
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Abstract
The invention discloses a method for preparing micron-scale strawberry-shaped SiCO ceramic balls and relates to micron ceramics. The method comprises the following steps: dissolving 0.8g of template agent F127 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, adding 0.032g of thermal cross-linking agent, dicumyl peroxide, 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; and pouring the mixed liquid C on a polytetrafluoroethylene tray, carrying out heat preservation in a baking oven at the temperature of 80 DEG C, then, cross-linking at the temperature of 130 DEG C so as to form a yellowish transparent film, taking out, stripping, and then, pyrolyzing the film in an inert atmosphere, thereby obtaining the micron-scale strawberry-shaped SiCO ceramic balls on the surface of the film. The prepared micron-ceramic SiCO balls have the diameter of 2-10 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 strawberry shape Ceramic Balls.
Background technology
The preparation of micro-nano structure is difficult point and the focus in current application field.The self-assembling technique of segmented copolymer, as a kind of very potential ordered structure assemble method from bottom to top, has become one of focus of fabrication technical field over nearly 20 years.Segmented copolymer is connected and is formed by chemical bond by mutual exclusive segment on thermodynamics, and this constructional feature causes segmented copolymer that micron-scale phase separation can only occur, and forms colourful ordered phase form on meso-scale.These microcosmic ordered phase forms have good Modulatory character and relatively easy preparation method, by change segmented copolymer composition, chain length, apply outfield or change preparation method etc. and can make segmented copolymer by self-assembly, produce the microscopic pattern of various high-sequentials.
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 pyridine ?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 strawberry shape Ceramic Balls.
The present invention includes following steps:
1) by 0.8g template F127 (PEO
106-PPO
70-PEO
106) be dissolved in 5ml xylene solution, after stirring, obtain mixed liquor A;
2) the ceramic precursor Polyvinylsilazane of 0.8g is dissolved in 5ml ethanol, adds the thermal cross-linking agent dicumyl peroxide of 0.032g, after stirring, obtain mixed liquid B;
3) mixed liquor A and mixed liquid B are mixed, after stirring, mixed solution C;
4) mixed solution C is poured in polytetrafluoroethyldisk disk, in the baking oven of 80 ℃, is incubated, then 130 ℃ crosslinked after, become faint yellow transparent film, take out rear demoulding, then pyrolysis film in inert atmosphere, obtains SiCO micron order strawberry shape Ceramic Balls at film surface.
In step 1) in, the time of described stirring can be 1～2h.
In step 2) in, described in add after the thermal cross-linking agent dicumyl peroxide of 0.032g, preferably seal lucifuge; Described stirring can adopt magnetic agitation 1～2h.
In step 3) in, after described mixing, preferably 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 30～50min; 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) blend in the mixed solvent of dimethylbenzene and Virahol, after assembling altogether, in inert atmosphere, SiCO micron order strawberry shape Ceramic Balls is prepared in pyrolysis.
The method of the SiCO of preparation micron order strawberry shape Ceramic Balls provided by the invention has the following advantages:
1) diameter of the SiCO micron order strawberry shape Ceramic Balls that prepared by the present invention is between 2～10 μ m, and good stability.
2) the SiCO micron order strawberry shape Ceramic Balls 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 prepare SiCO micron order strawberry shape Ceramic Balls, 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 strawberry shape Ceramic Balls of the embodiment of the present invention 1.
Fig. 2 is the SEM photo (scale is 4 μ m) of the prepared SiCO micron order strawberry shape Ceramic Balls 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:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 1h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 1h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 48h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 40min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.As illustrated in fig. 1 and 2, can clear view arrive SiCO micron order strawberry shape Ceramic Balls.
Embodiment 2:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 2h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 2h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 48h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 50min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.
Embodiment 3:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 1h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 1h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 24h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 50min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.
Embodiment 4:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 2h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 2h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 72h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 40min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.
Embodiment 5:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 1h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 1h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 96h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 30min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.
Embodiment 6:
By ethanol cleaning ultrasonic for polytetrafluoroethyldisk disk, put into subsequently baking oven dry for standby.The F127 that takes 0.8g is dissolved in the container of dimethylbenzene of 5ml and sealing, stirs 1h and obtains mixed liquor A.In another container, add the Polyvinylsilazane of 0.8g and the dicumyl peroxide of 0.032g, be dissolved in 5ml ethanol, and sealing rapidly, magnetic agitation 1h, 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 poured in the polytetrafluoroethyldisk disk of 80 ℃ of insulations and be incubated 72h, after solvent evaporation, obtain transparent film.Film is put into the baking oven heat cross-linking 40min of 130 ℃, 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 program is set: temperature program(me) is, 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 strawberry shape Ceramic Balls.
First the present invention is dissolved in ethanolic soln by ceramic forerunner Polyvinylsilazane and thermal cross-linking agent dicumyl peroxide, simultaneously by template F127 (PEO
106-PPO
70-PEO
106mw=12600g/mol) be dissolved in xylene solution, stir respectively 30～60min, again two solution are mixed, obtain mixing solutions, subsequently mixing solutions is laid on tetrafluoroethylene panel, be placed in evaporation in 80 ℃ of thermostat containers, crosslinked, through the demoulding, high-temperature heat treatment, obtain SiCO micron order strawberry shape Ceramic Balls again, diameter is between 2～10 μ m.The method preparation technology is simple, and preparation condition is gentle, can prepare efficiently SiCO micron order strawberry shape Ceramic Balls.
Claims (9)
1. a preparation method for SiCO micron order strawberry shape Ceramic Balls, is characterized in that comprising the following steps:
1) by 0.8g template F127 (PEO
106-PPO
70-PEO
106) be dissolved in 5ml xylene solution, after stirring, obtain mixed liquor A;
2) the ceramic precursor Polyvinylsilazane of 0.8g is dissolved in 5ml ethanol, adds the thermal cross-linking agent dicumyl peroxide of 0.032g, after stirring, obtain mixed liquid B;
3) mixed liquor A and mixed liquid B are mixed, after stirring, mixed solution C;
4) mixed solution C is poured in polytetrafluoroethyldisk disk, in the baking oven of 80 ℃, is incubated, then 130 ℃ crosslinked after, become faint yellow transparent film, take out rear demoulding, then pyrolysis film in inert atmosphere, obtains SiCO micron order strawberry shape Ceramic Balls at film surface.
2. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 1) in, the time of described stirring is 1～2h.
3. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 2) in, described in add after the thermal cross-linking agent dicumyl peroxide of 0.032g, sealing lucifuge.
4. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 2) in, described stirring adopts magnetic agitation 1～2h.
5. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 3) in, after described mixing, sealing.
6. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 3) in, the time of described stirring is 12～36h.
7. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 4) in, the time of described insulation is 24～96h.
8. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls as claimed in claim 1, is characterized in that in step 4) in, the described crosslinked time is 30～50min.
9. a kind of preparation method of SiCO micron order strawberry shape Ceramic Balls 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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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103137968A (en) * | 2011-11-30 | 2013-06-05 | 北京有色金属研究总院 | Positive electrode composite material for lithium ion batteries and preparation method thereof |
| CN103466590A (en) * | 2013-09-13 | 2013-12-25 | 厦门大学 | Preparation method of SiCO hollow nanospheres |
-
2014
- 2014-05-28 CN CN201410230575.2A patent/CN103979540B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103137968A (en) * | 2011-11-30 | 2013-06-05 | 北京有色金属研究总院 | Positive electrode composite material for lithium ion batteries and preparation method thereof |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| YUXI YU: "A Facile Route to Construct SiCO Nanospheres with Tunable Sizes", 《INT. J. APPL. CERAM. TECHNOL.》 * |
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