CN100445206C - Method for preparing Nano composite material of amorphous carbon / silicon dioxide - Google Patents
Method for preparing Nano composite material of amorphous carbon / silicon dioxide Download PDFInfo
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- CN100445206C CN100445206C CNB2006101510613A CN200610151061A CN100445206C CN 100445206 C CN100445206 C CN 100445206C CN B2006101510613 A CNB2006101510613 A CN B2006101510613A CN 200610151061 A CN200610151061 A CN 200610151061A CN 100445206 C CN100445206 C CN 100445206C
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Abstract
This invention relates to method for preparing amorphous carbon/silica nanocomposite. The method solves the problems of complex process, low yield, high impurity content and ununiform particle size distribution faced by the present methods in preparing carbon/silica nanocomposite. The method comprises: (1) mixing silica sol, sucrose and deionized water; (2) stirring; (3) gelatinizing the sol; (4) heat-treating the gel; (5) cooling to obtain amorphous carbon/silica nanocomposite. The method has simple process, and does not need any catalyst. The ratio of carbon to silica in the product can be easily controlled. Carbon and silica both exist in the amorphous states, and combine to form uniform particles on nanometer scale. The product has high reactivity, and can be used as the raw material for SiC nanomaterial, SiC-containing composite and Si-O-C-containing composite.
Description
Technical field
The present invention relates to a kind of preparation method of nano composite material.
Technical background
The material that complicated process of preparation, the productive rate of original carbon/silicon dioxide nano composite material is low, needs are introduced additive or catalyzer, raw material and product are easy to generate pollution, make often contains impurity, wherein carbon and SiO
2The uniform particles degree poor, not of uniform size.
Summary of the invention
The present invention be for the complicated process of preparation that solves original carbon/silicon dioxide nano composite material, low, the impure composition of productive rate is more and the uneven problem of granularity.The present provides a kind of preparation method of amorphous carbon/silicon dioxide nano composite material, and this method realizes by following steps: (one) gets silicon sol and sucrose, and wherein the mol ratio of silicon and carbon is 1: 6～6: 1; (2) use magnetic stirring apparatus in beaker, to stir at ambient temperature 3～6 hours, be mixed with uniform sol; (3) beaker that colloidal sol is housed is put into water-bath heater, temperature is controlled at carries out gelation processing 5～20 hours between 50 ℃～95 ℃, obtains white or slightly is faint yellow transparent gel; (4) gel that obtains is put into crucible and placed tubular oven, flow with 800～1600ml/min feeds nitrogen in tubular oven, tubular oven is heated to 600～900 ℃ with the rate of heating of 5～20 ℃/min simultaneously, keeps temperature 0.5～5 hour; (5) continue in tubular oven, to feed nitrogen, under protection of nitrogen gas, be cooled to room temperature, promptly obtain amorphous carbon/silicon dioxide nano composite material with the flow of 800～1600ml/min.The preparation technology of a kind of amorphous carbon/silicon dioxide nano composite material of the present invention's preparation is simple, do not need catalyzer in the process of preparation, the product inclusion-free, the atomic ratio of Si and C can be controlled in 6: 1～1: 6 the scope in the product, and the atomic ratio of Si and O constant be 1: 2, uniform granularity, mainly be distributed in 20-50nm, product is amorphous nano-powder, wherein carbon and silicon-dioxide all exist with the non-crystalline state form, granularity is a nanometer scale, has very strong reactive behavior, just can generate the SiC nano wire by sintering reaction under the condition of not adding catalyzer, while product of the present invention can also be used as the SiOC matrix material or contain the preparation raw material of the matrix material of silica carbon.The actual yield height, what use among the present invention is to contain 30%SiO
2Silicon sol, the carbon content of sucrose is 40%, the total mass of theoretical yield=(in the raw material 40% of the 30%+ sucrose quality of silicon sol quality)/raw material, actual yield can reach more than 90% of theoretical yield among the present invention, raw materials used is common environment-friendly material, reaction process does not produce pollution, is beneficial to industrialization production.
Embodiment
Embodiment one: present embodiment realizes by following steps: (one) gets silicon sol and sucrose, and wherein the mol ratio of silicon and carbon is 1: 6～6: 1; (2) use magnetic stirring apparatus in beaker, to stir at ambient temperature 3～6 hours, be mixed with uniform sol; (3) beaker that colloidal sol is housed is put into water-bath heater, temperature is controlled at carries out gelation processing 5～20 hours between 50 ℃～95 ℃, obtains white or slightly is faint yellow transparent gel; (4) gel that obtains is put into crucible and placed tubular oven, flow with 800～1600ml/min feeds nitrogen in tubular oven, tubular oven is heated to 600～900 ℃ with the rate of heating of 5～20 ℃/min simultaneously, keeps temperature 0.5～5 hour; (5) continue in tubular oven, to feed nitrogen, under protection of nitrogen gas, be cooled to room temperature, promptly obtain amorphous carbon/silicon dioxide nano composite material with the flow of 800～1600ml/min.
Embodiment two: the difference of present embodiment and embodiment one is in the step () molar ratio when carbon and silicon above 3, and in per 2 portions of quality sucrose: the ratio of 1 part of quality deionized water adds deionized water.Other step is identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is to get silicon sol and sucrose in the step (), and wherein the mol ratio of silicon, carbon is 2: 5～5: 2.Other step is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is that water-bath heater is controlled at 90 ℃ with temperature in the step (three).Other step is identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is that the time that gelation is handled in the step (three) is 6 hours.Other step is identical with embodiment one.
Embodiment six: the difference of present embodiment and embodiment one is that tubular oven is with the rate of heating heating of 10 ℃/min in the step (four).Other step is identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is that tubular oven is heated to 800 ℃ in the step (four).Other step is identical with embodiment one.
Embodiment eight: the difference of present embodiment and embodiment one is that the flow with 1000ml/min feeds nitrogen in the step (four) in tubular oven.Other step is identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is that the flow with 1500ml/min feeds nitrogen in the step (four) in tubular oven.Other step is identical with embodiment one.
Embodiment ten: the difference of present embodiment and embodiment one is that tubular oven kept temperature 2 hours in the step (four).Other step is identical with embodiment one.
Claims (9)
1, a kind of preparation method of amorphous carbon/silicon dioxide nano composite material, it is characterized in that the preparation method realizes by following steps: (one) gets JN30 type silicon sol and sucrose, and wherein the mol ratio of silicon and carbon is 1: 6～6: 1; (2) under 15～30 ℃ of conditions, use magnetic stirring apparatus in beaker, to stir 3～6 hours, be mixed with uniform sol; (3) beaker that colloidal sol is housed is put into water-bath heater, temperature is controlled at carries out gelation processing 5～20 hours between 50 ℃～95 ℃, obtains white or slightly is faint yellow transparent gel; (4) gel that obtains is put into crucible and placed tubular oven, flow with 800～1600ml/min feeds nitrogen in tubular oven, tubular oven is heated to 600～900 ℃ with the rate of heating of 5～20 ℃/min simultaneously, keeps temperature 0.5～5 hour; (5) continue in tubular oven, to feed nitrogen, under protection of nitrogen gas, be cooled to room temperature, promptly obtain amorphous carbon/silicon dioxide nano composite material with the flow of 800～1600ml/min; Wherein in the step () when the molar ratio of carbon and silicon above 3, in per 2 portions of quality sucrose: the ratio of 1 part of quality deionized water adds deionized water.
2, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that getting silicon sol and sucrose in the step (), and wherein the mol ratio of silicon, carbon is 2: 5～5: 2.
3, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that water-bath heater is controlled at 90 ℃ with temperature in the step (three).
4, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that the time that gelation is handled in the step (three) is 6 hours.
5, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that tubular oven is with the rate of heating heating of 10 ℃/min in the step (four).
6, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that tubular oven is heated to 800 ℃ in the step (four).
7, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that the flow with 1000ml/min feeds nitrogen in the step (four) in tubular oven.
8, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that the flow with 1500ml/min feeds nitrogen in the step (four) in tubular oven.
9, the preparation method of a kind of amorphous carbon/silicon dioxide nano composite material according to claim 1 is characterized in that tubular oven kept temperature 2 hours in the step (four).
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101510613A CN100445206C (en) | 2006-11-24 | 2006-11-24 | Method for preparing Nano composite material of amorphous carbon / silicon dioxide |
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| CNB2006101510613A CN100445206C (en) | 2006-11-24 | 2006-11-24 | Method for preparing Nano composite material of amorphous carbon / silicon dioxide |
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| CN101003373A CN101003373A (en) | 2007-07-25 |
| CN100445206C true CN100445206C (en) | 2008-12-24 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030506B (en) * | 2010-11-16 | 2012-08-29 | 哈尔滨工业大学 | Preparation method of SiO2-based porous composite block material |
| CN103896282B (en) * | 2012-12-25 | 2015-09-30 | 北京有色金属研究总院 | The silicon carbide powder pressed compact preparation method of silica white nano-wire |
| CN104176725B (en) * | 2014-09-02 | 2016-08-24 | 陈大明 | Carbon in a kind of immobilized saccharide material the method for high purity carbon (graphite) material |
| CN105293500B (en) * | 2015-11-06 | 2018-01-12 | 天津大学 | A kind of preparation method of silica carbon aerogels |
| CN113666375B (en) * | 2021-09-06 | 2023-10-27 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6387531B1 (en) * | 1998-07-27 | 2002-05-14 | Nanogram Corporation | Metal (silicon) oxide/carbon composite particles |
| EP1352930A2 (en) * | 2002-02-07 | 2003-10-15 | Toda Kogyo Corporation | Black composite particles for semiconductor sealing material, and semiconductor sealing material using the same |
| US6695986B1 (en) * | 2002-09-25 | 2004-02-24 | The United States Of America As Represented By The Secretary Of The Navy | Electrocatalytic enhancement with catalyst-modified carbon-silica composite aerogels |
| CN1821182A (en) * | 2006-01-26 | 2006-08-23 | 复旦大学 | Method for preparing mesoporous carbon material |
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- 2006-11-24 CN CNB2006101510613A patent/CN100445206C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6387531B1 (en) * | 1998-07-27 | 2002-05-14 | Nanogram Corporation | Metal (silicon) oxide/carbon composite particles |
| EP1352930A2 (en) * | 2002-02-07 | 2003-10-15 | Toda Kogyo Corporation | Black composite particles for semiconductor sealing material, and semiconductor sealing material using the same |
| US6695986B1 (en) * | 2002-09-25 | 2004-02-24 | The United States Of America As Represented By The Secretary Of The Navy | Electrocatalytic enhancement with catalyst-modified carbon-silica composite aerogels |
| CN1821182A (en) * | 2006-01-26 | 2006-08-23 | 复旦大学 | Method for preparing mesoporous carbon material |
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