CN1821073A - Process for preparing test tube brush type silicon carbide - Google Patents
Process for preparing test tube brush type silicon carbide Download PDFInfo
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- CN1821073A CN1821073A CN 200610049683 CN200610049683A CN1821073A CN 1821073 A CN1821073 A CN 1821073A CN 200610049683 CN200610049683 CN 200610049683 CN 200610049683 A CN200610049683 A CN 200610049683A CN 1821073 A CN1821073 A CN 1821073A
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- CN
- China
- Prior art keywords
- silicon carbide
- carbon fiber
- crucible
- silicon
- test tube
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 21
- 239000004917 carbon fiber Substances 0.000 claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 23
- 241000209456 Plumbago Species 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000002826 coolant Substances 0.000 claims description 3
- 239000007858 starting material Substances 0.000 claims description 3
- 238000009827 uniform distribution Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 abstract description 3
- 229910002804 graphite Inorganic materials 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000498 cooling water Substances 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 17
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 229910003910 SiCl4 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- RNRZLEZABHZRSX-UHFFFAOYSA-N diiodosilicon Chemical compound I[Si]I RNRZLEZABHZRSX-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000003407 synthetizing effect Effects 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The preparation process of test tube brush shaped silicon carbide includes the following steps: setting silicon inside graphite crucible, distributing polyacrylonitrile-base carbon fiber on the crucible and covering with one graphite crucible in the same size to increase contact between carbon fiber and silicon vapor; setting the crucible without direct contact between the Si powder and carbon fiber inside vacuum high temperature sintering furnace under Ar atmosphere, heating in the temperature raising rate of 10-30deg.c/min to 1450-1650deg.c and maintaining for 3-9 hr; and turning off the power supply after finishing reaction while maintaining circular cooling water until cooling completely to obtain grey silicon carbide.
Description
Technical field
The present invention relates to a kind of preparation method of test tube brush type silicon carbide.
Background technology
The silicon carbide fiber material has huge application potential at aspects such as high temperature, high frequency, high-power, high-voltage photoelectron and anti-irradiation.Thereby silicon carbide fiber enhancing ceramic matric composite has excellent mechanical behavior under high temperature and is widely used as high-temperature structural components, as rocket pipe, guided missile nose cone, leading edge and brake facing etc.; Silicon carbide fiber, becomes and makes short-wavelength light electron device, high-temperature device, anti-irradiation device and the most important semiconductor material of high-power/high-frequency electron device with its good physics-chem characteristic and electrical characteristic as a kind of novel semiconductor material.Silicon carbide fiber will be 21 century one of the most noticeable high-tech material.At present, the main method of preparation silicon carbide fiber has three kinds: the precursor method: make the method for silicon carbide fiber by the invention of Japanese carbon element company as precursor with Polycarbosilane; Activated carbon fiber conversion method: utilize the reaction of gasiform silicon monoxide and gac to transform and generate silicon carbide fiber; Chemical Vapor deposition process.Because the continuous carbofrax fibre of precursor method preparation more is applicable to suitability for industrialized production than the low and production efficiency height of preparation cost of CVD method, but oxygen, the too high performance that influences fiber of carbon massfraction in the silicon carbide fiber.The performance of activated carbon fiber conversion method silicon carbide fiber and chemical Vapor deposition process, precursor conversion method make silicon carbide fiber and compare a certain distance is still arranged.Though the activated carbon fiber conversion method reduces the silicon carbide fiber production cost greatly, make that silicon carbide fiber is in enormous quantities, suitability for industrialized production and to be applied to be possible on a large scale.But its performance also needs further to improve.Prepare silicon carbide fiber with chemical Vapor deposition process, precursor conversion method and activated carbon fiber conversion method its relative merits are respectively arranged.Chemical Vapor deposition process is eliminated gradually owing to can't realize industrialization; The precursor conversion method is present comparative maturity, realizes the method for suitability for industrialized production, is the main flow direction of silicon carbide fiber preparation research; The activated carbon fiber conversion method is to realize the popular optimal path of silicon carbide fiber application, further improves the research direction that its performance is this method.
Silicon carbide nano bar (nano wire) can be used as toughner and be used for polymer-based, ceramic base, metal matrix is made matrix material.The silicon carbide nano bar of orientations (nano wire) also has field emission effect in addition, and the microelectronic device of this against vacuum also is that a potential is used.Therefore people have poured into very big effort for making silicon carbide nano bar.Successful first in the world synthetizing silicon carbide nano rods is to be realized in nineteen ninety-five by the C.M.Lieber research group of Harvard University.Its method is to utilize prepared in reaction silicon carbide nano bar between carbon nanotube and SiO or the SiI2.Afterwards, the carbonaceous preparation of silica gel silicon carbide nano bar that has the people to make by the carbothermic reduction collosol and gel.Also utilize chemical Vapor deposition process on the silicon substrate, to obtain silicon carbide nano bar.The Qian Yitai research group of Chinese University of Science and Technology then uses SiCl4 and CCl4 as reactant, and sodium Metal 99.5 has been realized the growth of silicon carbide nano bar as catalyzer in autoclave.In the synthetic method of numerous known silicon carbide nano bars, owing to exist many deficiencies and defective, silicon carbide nano bar to fail to realize industrialization so far.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of test tube brush type silicon carbide.
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 silk uniform distribution is on the crucible, in order to increase contacting of carbon fiber and silicon steam as far as possible, the plumbago crucible of being inverted same diameter is on the crucible that silicon is housed; Do not contact between Si powder and the carbon fiber, whole then crucible is placed in the vacuum high-temperature sintering stove, is warmed up to 1450～1650 ℃, soaking time 3～9 hours with the temperature rise rate of 10～30 ℃/min always; Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior; Reaction is turned off heating power supply after finishing, and water coolant circulates always and cools off fully until whole device.Reaction finishes, and the carbon fiber of black becomes canescence.
The useful effect that the present invention has is:
The present invention is source of the gas with the silicon vapor, adopts vapour to ooze the method carbon fiber and is converted into test tube brush type silicon carbide.Also do not meet at present the report of this pattern silicon carbide.This test tube brush type silicon carbide not only can be used as toughner and be used for polymer-based, ceramic base, metal matrix is made matrix material.The silicon carbide nano bar of orientations (nano wire) also has field emission effect in addition, and the microelectronic device of against vacuum is that a potential is used.Being of high quality of test tube brush type silicon carbide product, defectives such as product impurity, fault are few, and silicon carbide nano bar is very straight, and diameter Distribution is more even; Conversion unit is simple, and method is simple, the technology easy handling.
Description of drawings
Accompanying drawing is the sem photograph of test tube brush type silicon carbide.
Embodiment
Raw material: carbon fiber, silicon.
Conversion unit: vacuum high-temperature sintering stove, plumbago crucible
Silicon at first is placed in the plumbago crucible as initial starting material, then PAN-based carbon fiber silk uniform distribution is on the crucible, and in order to increase contacting of carbon fiber and silicon steam as far as possible, the crucible of being inverted same diameter is on the crucible that silicon is housed.Certain distance is arranged between Si powder and the carbon fiber.Whole then crucible is placed in the vacuum high-temperature sintering stove, is warmed up to 1450～1650 ℃, soaking time 3-9 hour with the temperature rise rate of 10～30 ℃/min always.Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior.Reaction is turned off heating power supply after finishing, and water coolant circulates always and cools off fully until whole device.Reaction finishes, and the carbon fiber of black becomes canescence.
The applicant is being converted into carbon fiber in the experiment of silicon carbide fiber, and the surface growth of discovery silicon carbide fiber has the silicon carbide nano bar of orientations.Because this special construction seems to be test-tube brush, so be named as test tube brush type silicon carbide.
Embodiment 1:
The crucible that installs raw material is positioned 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.Reaction finishes, and the PAN-based carbon fiber of black becomes linen test tube brush type silicon carbide, as shown in drawings.
Embodiment 2:
The crucible that installs raw material is positioned in the vacuum high-temperature sintering stove, is warmed up to 1450 ℃, 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.Reaction finishes, and the carbon fiber of black becomes linen test tube brush type silicon carbide.
Embodiment 3:
The crucible that installs raw material is positioned 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.Reaction finishes, and the PAN-based carbon fiber of black becomes linen test tube brush type silicon carbide.
Claims (1)
1, a kind of preparation method of test tube brush type 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 silk uniform distribution is on this plumbago crucible, in order to increase contacting of carbon fiber and silicon steam as far as possible, the plumbago crucible of being inverted same diameter is on the crucible that silicon is housed; Do not contact between silicon and the carbon fiber, crucible is placed in the vacuum high-temperature sintering stove then, is warmed up to 1450～1650 ℃, soaking time 3～9 hours with the temperature rise rate of 10～30 ℃/min always; Whole device carries out under the atmosphere of Ar, takes place to avoid any oxidation behavior; Reaction is turned off heating power supply after finishing, and water coolant circulates always and cools off fully until whole device.Reaction finishes, and the carbon fiber of black becomes canescence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100496835A CN1331743C (en) | 2006-03-02 | 2006-03-02 | Process for preparing test tube brush type silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100496835A CN1331743C (en) | 2006-03-02 | 2006-03-02 | Process for preparing test tube brush type silicon carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1821073A true CN1821073A (en) | 2006-08-23 |
| CN1331743C CN1331743C (en) | 2007-08-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100496835A Expired - Fee Related CN1331743C (en) | 2006-03-02 | 2006-03-02 | Process for preparing test tube brush type silicon carbide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1331743C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102828249A (en) * | 2012-04-27 | 2012-12-19 | 中国人民解放军第二炮兵工程学院 | Method for preparing monocrystalline silicon carbide nano-wires on flexible carbon fiber substrate |
| CN104828825A (en) * | 2015-05-19 | 2015-08-12 | 山东大学 | Low-cost method for synthesizing silicon carbide powder at low temperature |
| CN104988658A (en) * | 2015-07-13 | 2015-10-21 | 浙江理工大学 | SiC nanometer fiber non-woven material preparation method |
| CN109179419A (en) * | 2018-09-05 | 2019-01-11 | 哈尔滨工业大学 | A kind of preparation method of New test tube brush SiC nanowire |
| CN114735703A (en) * | 2022-04-28 | 2022-07-12 | 中电化合物半导体有限公司 | Synthesis method and application of silicon carbide fiber |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0744390B1 (en) * | 1995-05-22 | 1999-04-07 | Nippon Carbon Co., Ltd. | Process for producing silicon carbide fibers |
| US5720933A (en) * | 1996-03-11 | 1998-02-24 | Srinivasan; Makuteswara | Process for preparing ceramic fibers |
| DE19739881A1 (en) * | 1997-09-11 | 1999-03-18 | Andreas Gabriel | Production of crystalline silicon carbide |
| CN1260124C (en) * | 2004-04-29 | 2006-06-21 | 中国科学院山西煤炭化学研究所 | Method of preparing nano-silicon carbide fiber |
| CN1292986C (en) * | 2005-06-16 | 2007-01-03 | 哈尔滨工业大学 | Process for preparing silicon carbide nano fibre |
-
2006
- 2006-03-02 CN CNB2006100496835A patent/CN1331743C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102828249A (en) * | 2012-04-27 | 2012-12-19 | 中国人民解放军第二炮兵工程学院 | Method for preparing monocrystalline silicon carbide nano-wires on flexible carbon fiber substrate |
| CN104828825A (en) * | 2015-05-19 | 2015-08-12 | 山东大学 | Low-cost method for synthesizing silicon carbide powder at low temperature |
| CN104988658A (en) * | 2015-07-13 | 2015-10-21 | 浙江理工大学 | SiC nanometer fiber non-woven material preparation method |
| CN104988658B (en) * | 2015-07-13 | 2017-10-20 | 浙江理工大学 | A kind of preparation method of SiC micro/nano-fibre non-woven materials |
| CN109179419A (en) * | 2018-09-05 | 2019-01-11 | 哈尔滨工业大学 | A kind of preparation method of New test tube brush SiC nanowire |
| CN109179419B (en) * | 2018-09-05 | 2021-11-16 | 哈尔滨工业大学 | Preparation method of test tube brush-shaped SiC nanowire |
| CN114735703A (en) * | 2022-04-28 | 2022-07-12 | 中电化合物半导体有限公司 | Synthesis method and application of silicon carbide fiber |
| CN114735703B (en) * | 2022-04-28 | 2024-09-06 | 中电化合物半导体有限公司 | Synthesis method and application of silicon carbide fiber |
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| Publication number | Publication date |
|---|---|
| CN1331743C (en) | 2007-08-15 |
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Granted publication date: 20070815 |