CN100460358C - Method of preparing high specific surface siloxicon ceramic nano-tube - Google Patents
Method of preparing high specific surface siloxicon ceramic nano-tube Download PDFInfo
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- CN100460358C CN100460358C CNB2007100411051A CN200710041105A CN100460358C CN 100460358 C CN100460358 C CN 100460358C CN B2007100411051 A CNB2007100411051 A CN B2007100411051A CN 200710041105 A CN200710041105 A CN 200710041105A CN 100460358 C CN100460358 C CN 100460358C
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Abstract
The invention discloses a making method of high specific surface area siloxcarbon ceramic nanometer pipe, which comprises the following steps: a. selecting porous alumina as mould to immerse in the polysiloxane liquid; b. placing the mould immersed in the polysiloxane into Muffle furnace under 50-600 deg. c for 1-10h; c. removing aluminium mould through acid to obtain the predecessor of polysiloxane nanometer pipe; d. heating the predecessor in the high-temperature pipe typed furnace protected by inert gas with heating speed at 2-10deg. c/min to 1000-1500 deg. c; insulating 0. 5-4h to obtain the product. The invention can produce the nanometer material with even pore passage distribution and shape with specific surface area to 700-2500m2/g, which can be used in the photoelectric and catalytic domains as functional material or carrier.
Description
Technical field
The present invention relates to a kind of preparation ceramic nano tube side method, more particularly relate to a kind of method for preparing high specific surface siloxicon ceramic nano-tube by template.
Background technology
Stupalith has numerous particular performances, as the mechanical behavior under high temperature of structural ceramics excellence, and effects such as the distinctive light of function ceramics, sound, electricity, magnetic, heat, stupalith extensively is used in fields such as information communication, military industrial technology, environmental protection.The silicon-oxygen-carbon ceramic material has good thermostability, light stability, high hardness and thermal conductivity; have wide being with and high specific refraction simultaneously; be developed and be used as supercoat, ceramic matrix, high temperature resistance material, optics etc.; the preparation research that a lot of silicon-oxygen-carbon ceramic films are arranged at present, but the silicon-oxygen-carbon ceramic nano-array is synthetic still rare.Template is one of important method of nano materials, and one of wherein the most frequently used template is an alumina formwork, and this template has that pore space structure is orderly, pore size is controlled, the advantage of controllable thickness.In addition, the preparation condition of alumina formwork is simple, cost is low, the duct is evenly distributed, and is the desirable template of the uniform sequential nano material of preparation shape height.The still unexposed synthetic method of crossing siloxicon ceramic nano-tube in existing document particularly has the preparation method that high-specific surface area can be used as the high specific surface siloxicon ceramic nano-tube that functional materials uses very much.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that adopts template to prepare high specific surface siloxicon ceramic nano-tube, and the specific surface area of the siloxicon ceramic nano-tube material that is obtained can reach 700-2500m
2/ g.
The technical solution used in the present invention: a kind of preparation method of high specific surface siloxicon ceramic nano-tube comprises the following steps:
A. selecting mean pore size for use is that 200nm, thickness are that the porous alumina of 60um specification is as template, then above-mentioned template is immersed in the polyorganosiloxane fluid, described polyorganosiloxane fluid is selected from the mixing solutions of single polyphenyl methyl siloxane solution or hydrogen methyl-silicone oil and vinyl polysiloxane;
B. will soak the alumina formwork of polyorganosiloxane fluid and in retort furnace, place 1～10 hour under 50～600 ℃ of temperature, make the polysiloxane thermofixation in the template;
C. remove the presoma that alumina formwork obtains the polysiloxane nanotube with acid;
D. the presoma with above-mentioned polysiloxane nanotube places high temperature process furnances under protection of inert gas; heat-up rate with 2～10 ℃/min rises to 1000～1500 ℃ with temperature; constant temperature promptly got siloxicon ceramic nano pipe in 0.5～4 hour then, and the specific surface area of this siloxicon ceramic nano-tube is 700～2500m
2/ g.
The beneficial effect of the invention, the present invention prepares siloxicon ceramic nano-tube with aluminum oxide as template, the pore space structure that has utilized alumina formwork to have is orderly, pore size is controlled, the advantage of controllable thickness, prepare the nano material that the duct is evenly distributed, shape height is uniform sequential, this material specific surface reaches 700-2500m
2/ g is expected to be used widely at aspects such as photoelectricity, catalysis as functional materials or carrier.
Description of drawings
Fig. 1 is the stereoscan photograph of the siloxicon ceramic nano-tube for preparing of the present invention.
Embodiment
Below by embodiment the present invention is described in further detail, a kind of preparation method of high specific surface siloxicon ceramic nano-tube comprises the following steps:
A. selecting mean pore size for use is that 200nm, thickness are that the porous alumina of 60um specification is as template, then above-mentioned template is immersed in the polyorganosiloxane fluid, described polyorganosiloxane fluid is selected from the mixing solutions of single polyphenyl methyl siloxane solution or hydrogen methyl-silicone oil and vinyl polysiloxane;
B. will soak the alumina formwork of polyorganosiloxane fluid and in retort furnace, place 1～10 hour under 50～600 ℃ of temperature, make the polysiloxane thermofixation in the template;
C. remove the presoma that alumina formwork obtains the polysiloxane nanotube with acid;
D. the presoma with above-mentioned polysiloxane nanotube places high temperature process furnances under protection of inert gas; heat-up rate with 2～10 ℃/min rises to 1000～1500 ℃ with temperature; constant temperature promptly got siloxicon ceramic nano pipe in 0.5～4 hour then, and the specific surface area of this siloxicon ceramic nano-tube is 700～2500m
2/ g, its concrete pattern as shown in Figure 1.
Embodiment 1
1, selecting specification for use is mean pore size 200nm, and thickness is that the porous alumina of 60um is as template;
2, alumina formwork is immersed in the polyphenyl methyl siloxane solution;
3, the alumina formwork that is soaked with polysiloxane was placed 10 hours under 50 ℃ the temperature in retort furnace, polysiloxane is solidified;
4, remove alumina formwork with phosphoric acid and chromic acid solution and obtain the polysiloxane precursor body of Nano tube;
5, the polysiloxane precursor body of Nano tube is placed high temperature process furnances, the heat-up rate with 5 ℃/min under rare gas element (as argon gas) protection rises to 1200 ℃ with temperature, and constant temperature 1 hour promptly gets siloxicon ceramic nano pipe.Use the specific surface area of the siloxicon ceramic nano-tube material of this method acquisition to be 850m
2/ g.
Embodiment 2
1, selecting specification for use is mean pore size 200nm, and thickness is that the porous alumina of 60um is as template;
2, alumina formwork is immersed in hydrogeneous methyl-silicone oil and the vinyl polysiloxane mixing solutions;
3, the alumina formwork that is soaked with polysiloxane was placed 2 hours under 200 ℃ the temperature in retort furnace, polysiloxane is solidified;
4, remove alumina formwork with phosphoric acid and chromic acid solution and obtain the polysiloxane precursor body of Nano tube;
5, the polysiloxane precursor body of Nano tube is placed high temperature process furnances, the heat-up rate with 5 ℃/min under rare gas element (as argon gas) protection rises to 1300 ℃ with temperature, and constant temperature 2 hours promptly gets siloxicon ceramic nano pipe.Use the specific surface area of the siloxicon ceramic nano-tube material of this method acquisition to be 2370m as specific surface area
2/ g.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (1)
1. the preparation method of a high specific surface siloxicon ceramic nano-tube comprises the following steps:
A. selecting mean pore size for use is that 200nm, thickness are that the porous alumina of 60um specification is as template, then above-mentioned template is immersed in the polyorganosiloxane fluid, described polyorganosiloxane fluid is selected from the mixing solutions of single polyphenyl methyl siloxane solution or hydrogen methyl-silicone oil and vinyl polysiloxane;
B. will soak the alumina formwork of polyorganosiloxane fluid and in retort furnace, place 1～10 hour under 50～600 ℃ of temperature, make the polysiloxane thermofixation in the template;
C. remove the presoma that alumina formwork obtains the polysiloxane nanotube with acid;
D. the presoma with above-mentioned polysiloxane nanotube places high temperature process furnances under the rare gas element argon shield; heat-up rate with 2～10 ℃/min rises to 1000～1500 ℃ with temperature; constant temperature promptly got siloxicon ceramic nano pipe in 0.5～4 hour then, and the specific surface area of this siloxicon ceramic nano-tube is 700～2500m
2/ g.
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| CNB2007100411051A CN100460358C (en) | 2007-05-23 | 2007-05-23 | Method of preparing high specific surface siloxicon ceramic nano-tube |
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| CN100460358C true CN100460358C (en) | 2009-02-11 |
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| CN103833367B (en) * | 2013-11-22 | 2016-01-13 | 天津大学 | Silica carbon fiber of titaniferous and preparation method thereof |
| CN112194379A (en) * | 2020-09-09 | 2021-01-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | Medical glass bottle with low liquid medicine residue and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004001107A2 (en) * | 2002-06-19 | 2003-12-31 | The Board Of Regents Of The University Of Oklahoma | Carbon nanotube-filled composites |
| CN1600683A (en) * | 2004-10-26 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for preparing material of nano carbon tube |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004001107A2 (en) * | 2002-06-19 | 2003-12-31 | The Board Of Regents Of The University Of Oklahoma | Carbon nanotube-filled composites |
| CN1600683A (en) * | 2004-10-26 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for preparing material of nano carbon tube |
Non-Patent Citations (2)
| Title |
|---|
| 模板法合成纳米结构材料. ***等.化学通报，第2005年第10期. 2005 |
| 模板法合成纳米结构材料. ***等.化学通报，第2005年第10期. 2005 * |
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Effective date of registration: 20110607 Address after: 338 No. 423400 Hunan province Zixing Jiangbei Industrial Park Avenue Shanshan Patentee after: Binzhou Shanshan New Material Co., Ltd. Address before: 200235 Xuhui District, Caobao Road, No. 120, Patentee before: Shanghai Institute of Technology |