CN100460358C - A kind of preparation method of high specific surface silicon oxygen carbon ceramic nanotube - Google Patents
A kind of preparation method of high specific surface silicon oxygen carbon ceramic nanotube 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
本发明公开了一种高比表面硅氧碳陶瓷纳米管的制备方法，包括下列步骤：a.选用多孔氧化铝作为模板浸入到聚硅氧烷液体中；b.浸过聚硅氧烷液体的模板在马弗炉中50～600℃温度下放置1～10小时；c.用酸去除氧化铝模板得到聚硅氧烷纳米管的前驱体；d.将前驱体置于高温管式炉中在惰性气体保护下以2～10℃/min的升温速度将温度升至1000～1500℃，然后恒温0.5～4小时得到产物。本发明以氧化铝作为模板制备硅氧碳陶瓷纳米管，制备出孔道分布均匀、形状高度均匀有序的纳米材料，该材料比表面高达700-2500m2/g，可作为功能材料或载体在光电、催化等方面得到广泛应用。
The invention discloses a preparation method of a silicon oxygen carbon ceramic nanotube with a high specific surface, which comprises the following steps: a. selecting porous alumina as a template and immersing it in a polysiloxane liquid; b. soaking the polysiloxane liquid The template is placed in a muffle furnace at a temperature of 50-600°C for 1-10 hours; c. Remove the alumina template with acid to obtain the precursor of polysiloxane nanotubes; d. Place the precursor in a high-temperature tube furnace in the Under the protection of inert gas, the temperature is raised to 1000-1500° C. at a heating rate of 2-10° C./min, and then the temperature is kept constant for 0.5-4 hours to obtain the product. The present invention uses alumina as a template to prepare silicon oxygen carbon ceramic nanotubes, and prepares nanomaterials with uniform pore distribution and highly uniform and orderly shape. , catalysis and other aspects have been widely used.
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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| CN100460358C true CN100460358C (en) | 2009-02-11 |
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| CN103833367B (en) * | 2013-11-22 | 2016-01-13 | 天津大学 | Titanium-containing silicon oxygen carbon fiber and its preparation method |
| 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 | A kind of preparation method of carbon nanotube material |
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| 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 | A kind of preparation method of carbon nanotube material |
Non-Patent Citations (2)
| Title |
|---|
| 模板法合成纳米结构材料. 王秀丽等.化学通报，第2005年第10期. 2005 |
| 模板法合成纳米结构材料. 王秀丽等.化学通报，第2005年第10期. 2005 * |
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