CN1861521A - Synthesis process of needle shape nano silicon carbide - Google Patents
Synthesis process of needle shape nano silicon carbide Download PDFInfo
- Publication number
- CN1861521A CN1861521A CNA2006100517051A CN200610051705A CN1861521A CN 1861521 A CN1861521 A CN 1861521A CN A2006100517051 A CNA2006100517051 A CN A2006100517051A CN 200610051705 A CN200610051705 A CN 200610051705A CN 1861521 A CN1861521 A CN 1861521A
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- China
- Prior art keywords
- silicon
- carbon fiber
- whole device
- crucible
- silicon carbide
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- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 14
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 13
- 239000005543 nano-size silicon particle Substances 0.000 title claims description 8
- 230000015572 biosynthetic process Effects 0.000 title 1
- 238000003786 synthesis reaction Methods 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 11
- 239000004917 carbon fiber Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 28
- 229910052710 silicon Inorganic materials 0.000 claims description 28
- 239000010703 silicon Substances 0.000 claims description 28
- 241000209456 Plumbago Species 0.000 claims description 15
- 238000002791 soaking Methods 0.000 claims description 10
- 239000002826 coolant Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007858 starting material Substances 0.000 claims description 5
- 238000010189 synthetic method Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract 2
- 229910002804 graphite Inorganic materials 0.000 abstract 2
- 229920002239 polyacrylonitrile Polymers 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000003763 carbonization Methods 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000005424 photoluminescence Methods 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Ceramic Products (AREA)
- Inorganic Fibers (AREA)
Abstract
A process for synthesizing the SiC nanoneedles includes such steps as putting Si in graphite crucible, putting the polyacrylonitrile carbon fibers or activated carbon fiber on the crucible, covering them by another graphite crucible, putting them in Ar atmosphere in vacuum high-temp sintering furnace, sintering at 1500-1650 deg.C for 3-9 hr, cooling to 1200 deg.C, and cooling by water.
Description
Technical field
The present invention relates to a kind of synthetic method of needle shape nano silicon carbide.
Background technology
Silicon carbide has very excellent mechanical property, thermodynamics and chemical stability, very high thermal conductivity and very big bandwidth as third generation wide bandgap semiconductor materials, is widely used under the rugged environments such as high temperature, high frequency, superpower.Compare with the single-crystal silicon carbide of bulk, silicon carbide nano bar has outstanding electricity and mechanical property.1-dimention nano carbonization silicon can be used as toughner and is used to make matrix material.The silicon carbide nano bar of orientations (nano wire) also has field emission effect in addition, photoluminescence effect etc.The Lieber research group of Harvard University utilizes carbon nanotube and SiO or SiI
2Between reaction prepare 1-dimention nano carbonization silicon rod first.After this, the carbonaceous preparation of silica gel 1-dimention nano carbonization silicon that makes by the carbothermic reduction collosol and gel of people.Also utilize chemical Vapor deposition process on the silicon substrate, to obtain 1-dimention nano carbonization silicon.The Qian Yitai research group of Chinese University of Science and Technology then uses SiCl
4And CCl
4As reactant, sodium Metal 99.5 has been realized the growth of 1-dimention nano carbonization silicon as catalyzer in autoclave.Report for needle shape nano silicon carbide is less, and professor Xu Ningsheng of Zhongshan University adopts commercial SiC powder, under the effect of catalyzer, has prepared acicular nanometer silicon carbide, and has studied its emission and photoluminescence performance.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of needle shape nano silicon carbide, is to be carbon source with the carbon fiber, and silicon steam prepares needle-like 1-dimention nano carbonization silicon for the silicon source, and this needle-like 1-dimention nano carbonization silicon is the divergent shape growth at carbon base body.
The technical solution adopted for the present invention to solve the technical problems is: silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber or the distribution of activated carbon fiber silk are on the plumbago crucible, the crucible of being inverted same diameter again is on the plumbago crucible that the silicon source is housed, above-mentioned whole device is placed in the vacuum high-temperature sintering stove, temperature rise rate with 10～30 ℃/min is warmed up to 1500～1650 ℃ always, soaking time 3～9 hours.Whole device carries out under the atmosphere of Ar, after soaking time finishes, cools to 1200 ℃ with the rate of temperature fall of 5～20 ℃/min, turns off heating power supply then, and water coolant circulates always and cools off fully until whole device.
The beneficial effect that the present invention has is: it is carbon source with the carbon fiber, and silicon steam has prepared needle-like 1-dimention nano carbonization silicon for the silicon source.This needle-like 1-dimention nano carbonization silicon is the divergent shape growth at carbon base body.The needle-like 1-dimention nano carbonization silicon of growing on carbon base body has certain application prospect in fields such as field emission effect, photoluminescence and electroluminescent.
Description of drawings
Accompanying drawing is the sem photograph of needle shape nano silicon carbide.
Embodiment
Embodiment 1:
Silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber or activated carbon fiber silk uniform distribution are on the plumbago crucible, in order to increase contacting of carbon fiber or activated carbon fiber and silicon steam as far as possible, the crucible of being inverted same diameter again is on the plumbago crucible that the silicon source is housed.Above-mentioned whole device is placed in the vacuum high-temperature sintering stove, is warmed up to 1600 ℃, soaking time 9 hours always with the temperature rise rate of 30 ℃/min.Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior.After soaking time finishes, cool to 1200 ℃ with the rate of temperature fall of 5 ℃/min, turn off heating power supply then, water coolant circulates always and cools off fully until whole device, and accompanying drawing is the sem photograph of needle shape nano silicon carbide.
Embodiment 2:
Silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber or activated carbon fiber silk uniform distribution are on the plumbago crucible, in order to increase contacting of carbon fiber or activated carbon fiber and silicon steam as far as possible, the crucible of being inverted same diameter again is on the plumbago crucible that the silicon source is housed.Above-mentioned whole device is placed in the vacuum high-temperature sintering stove, is warmed up to 1650 ℃, soaking time 3 hours always with the temperature rise rate of 10 ℃/min.Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior.After soaking time finishes, cool to 1200 ℃ with the rate of temperature fall of 10 ℃/min, turn off heating power supply then, water coolant circulates always and cools off fully until whole device.
Embodiment 3:
Silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber or activated carbon fiber silk uniform distribution are on the plumbago crucible, in order to increase contacting of carbon fiber or activated carbon fiber and silicon steam as far as possible, the crucible of being inverted same diameter again is on the plumbago crucible that the silicon source is housed.Above-mentioned whole device is placed in the vacuum high-temperature sintering stove, is warmed up to 1500 ℃, soaking time 6 hours always with the temperature rise rate of 20 ℃/min.Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior.After soaking time finishes, cool to 1200 ℃ with the rate of temperature fall of 20 ℃/min, turn off heating power supply then, water coolant circulates always and cools off fully until whole device.
Claims (1)
1. the synthetic method of a needle shape nano silicon carbide is characterized in that the step of this method is as follows:
Silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber or the distribution of activated carbon fiber silk are on the plumbago crucible, the crucible of being inverted same diameter again is on the plumbago crucible that the silicon source is housed, above-mentioned whole device is placed in the vacuum high-temperature sintering stove, temperature rise rate with 10～30 ℃/min is warmed up to 1500～1650 ℃ always, soaking time 3～9 hours.Whole device carries out under the atmosphere of Ar, after soaking time finishes, cools to 1200 ℃ with the rate of temperature fall of 5～20 ℃/min, turns off heating power supply then, and water coolant circulates always and cools off fully until whole device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100517051A CN1330568C (en) | 2006-05-30 | 2006-05-30 | Synthesis process of needle shape nano silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100517051A CN1330568C (en) | 2006-05-30 | 2006-05-30 | Synthesis process of needle shape nano silicon carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1861521A true CN1861521A (en) | 2006-11-15 |
| CN1330568C CN1330568C (en) | 2007-08-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100517051A Expired - Fee Related CN1330568C (en) | 2006-05-30 | 2006-05-30 | Synthesis process of needle shape nano silicon carbide |
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| Country | Link |
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| CN (1) | CN1330568C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749357A (en) * | 2012-07-05 | 2012-10-24 | 浙江理工大学 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
| CN103065907A (en) * | 2012-12-28 | 2013-04-24 | 青岛爱维互动信息技术有限公司 | Preparation method for field emission materials |
| CN104828825A (en) * | 2015-05-19 | 2015-08-12 | 山东大学 | Low-cost method for synthesizing silicon carbide powder at low temperature |
| CN105088182A (en) * | 2015-08-19 | 2015-11-25 | 宁波工程学院 | N-doped SiC nanoneedle and application thereof |
| CN108987215A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-carbon nano-tube array composite material field emission performance |
| CN108987218A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-silicon nanowire array composite material field emission performance |
| CN108987214A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting carbon nano pipe array field emission performance |
| CN108987217A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene sheet-carbon nanotube film flexible composite field emission performance |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112466C (en) * | 1999-07-21 | 2003-06-25 | 中国科学院山西煤炭化学研究所 | Preparation method of nanometer silicon carbide whiskers |
| CN1164488C (en) * | 2001-07-25 | 2004-09-01 | 中山大学 | Process for preparing nm-class silicon carbide material |
-
2006
- 2006-05-30 CN CNB2006100517051A patent/CN1330568C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749357A (en) * | 2012-07-05 | 2012-10-24 | 浙江理工大学 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
| CN102749357B (en) * | 2012-07-05 | 2014-05-14 | 浙江理工大学 | Method of preparing gas sensor with silicon carbide nanowires used as gas sensitive material |
| CN103065907A (en) * | 2012-12-28 | 2013-04-24 | 青岛爱维互动信息技术有限公司 | Preparation method for field emission materials |
| CN104828825A (en) * | 2015-05-19 | 2015-08-12 | 山东大学 | Low-cost method for synthesizing silicon carbide powder at low temperature |
| CN105088182A (en) * | 2015-08-19 | 2015-11-25 | 宁波工程学院 | N-doped SiC nanoneedle and application thereof |
| CN105088182B (en) * | 2015-08-19 | 2017-04-19 | 宁波工程学院 | N-doped SiC nanoneedle and application thereof |
| CN108987215A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-carbon nano-tube array composite material field emission performance |
| CN108987218A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene film-silicon nanowire array composite material field emission performance |
| CN108987214A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting carbon nano pipe array field emission performance |
| CN108987217A (en) * | 2018-01-31 | 2018-12-11 | 天津师范大学 | A method of promoting graphene sheet-carbon nanotube film flexible composite field emission performance |
| CN108987215B (en) * | 2018-01-31 | 2019-12-31 | 天津师范大学 | Method for improving field emission performance of graphene sheet-carbon nanotube array composite material |
| CN108987217B (en) * | 2018-01-31 | 2019-12-31 | 天津师范大学 | Method for improving field emission performance of graphene sheet-carbon nanotube film flexible composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1330568C (en) | 2007-08-08 |
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Granted publication date: 20070808 |