CN1330796C - Method of synthetizing two kinds of different shaped silicon carbid nano wire - Google Patents
Method of synthetizing two kinds of different shaped silicon carbid nano wire Download PDFInfo
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- CN1330796C CN1330796C CNB2006100496820A CN200610049682A CN1330796C CN 1330796 C CN1330796 C CN 1330796C CN B2006100496820 A CNB2006100496820 A CN B2006100496820A CN 200610049682 A CN200610049682 A CN 200610049682A CN 1330796 C CN1330796 C CN 1330796C
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- silicon carbide
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- alumina crucible
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000002070 nanowire Substances 0.000 title claims abstract description 9
- 230000003407 synthetizing effect Effects 0.000 title claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 12
- 229910052710 silicon Inorganic materials 0.000 title claims description 12
- 239000010703 silicon Substances 0.000 title claims description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 34
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 17
- 239000002826 coolant Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 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
- 239000007858 starting material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000005543 nano-size silicon particle Substances 0.000 abstract 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 2
- 239000000498 cooling water Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 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
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000642 polymer Polymers 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
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The present invention discloses a method for synthetizing two kinds of silicon carbide nano wires in different shapes. Si powder and multi-walled carbon nanotubes are used as raw materials and are placed into an aluminum oxide crucible, then the crucible is placed into a vacuum high-temperature sintering furnace, the temperature is increased to 1410 to 1600 DEG C at the temperature rise rate of 10 to 30 DEG C per min, and the holding time is from 3 to 9 hours; the whole device is in the Ar atmosphere; after the reaction is finished, a heating power supply is switched off, and cooling water circulation is carried out until the whole device is cooled completely. Finally, a large quantity of offwhite products are produced in the aluminum oxide crucible, and the mixed liquor of hydrofluoric acid and nitric acid is used for removing excess unreacted Si to obtain the powder of the silicon carbide nano wires, wherein the volume ratio of the hydrofluoric acid to the nitric acid is 1: 2. Besides, the gourd-shaped nano silicon carbide also exists on the cover of the crucible. The present invention has the advantages of higher product quality, no defects such as stacking fault, straight silicon carbide nano wire, uniform diameter distribution, simple reaction device, simple method and easy process operation, and a small amount of gourd-shaped nano silicon carbide is prepared.
Description
Technical field
The present invention relates to a kind of method of synthetizing two kinds of different shaped silicon carbid nano wire.
Background technology
Silicon carbide has very excellent mechanical property, thermodynamics and chemical stability, very high thermal conductivity and very big bandwidth as third generation semiconductor material, is widely used under the rugged environments such as high temperature, high frequency, superpower.Compare with the single-crystal silicon carbide of bulk: one silicon carbide nanometer line has outstanding electricity and mechanical property.Be used for polymer-based, ceramic base because these excellent properties of unidimensional silicon carbide nano material, silicon carbide nanometer line (nano wire) can be used as toughner, metal matrix is made matrix material.The silicon carbide nanometer line 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 nanometer line.Successful first in the world synthesizing silicon carbide nano wire is to be realized in nineteen ninety-five by the C.M.Lieber research group of Harvard University.Its method is to utilize carbon nanotube and SiO or SiI
2Between the prepared in reaction silicon carbide nanometer line.Afterwards, the carbonaceous preparation of silica gel silicon carbide nanometer line 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 nanometer line.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 silicon carbide nanometer line as catalyzer in autoclave.In the synthetic method of numerous known silicon carbide nanometer lines, owing to exist many deficiencies and defective, silicon carbide nanometer line to fail to realize industrialization so far.
Summary of the invention
The object of the present invention is to provide a kind of method of synthetizing two kinds of different shaped silicon carbid nano wire.
The technical solution adopted for the present invention to solve the technical problems is:
Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, cover lid, crucible is positioned in the vacuum high-temperature sintering stove then, temperature rise rate with 10～30 ℃/min is warmed up to 1410～1600 ℃ always, soaking time 3～9 hours, 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, finds that at last a large amount of linen products is in alumina crucible; Taking out behind the product with volume ratio is 1: 2 hydrofluoric acid and nitric acid mixed solution, removes unnecessary unreacted silicon and obtains the silicon carbide nanometer line powder; In addition, also there is skim cucurbit shape nanometer silicon carbide covering of alumina crucible.
The useful effect that the present invention has is:
1, the quality of nanometer silicon carbide line products is higher, defectives such as no fault, and silicon carbide nanometer line is very straight, and diameter Distribution is more even;
2, prepared a small amount of cucurbit shape nanometer silicon carbide;
3, conversion unit is simple, and method is simple, the technology easy handling; Silicon carbide nanometer line product production height, preparation cost is lower.
Description of drawings
Fig. 1 is the sem photograph of silicon carbide nanometer line;
Fig. 2 is the sem photograph of cucurbit shape nanometer silicon carbide.
Specific implementation method
Experimental procedure:
Raw material: multi-walled carbon nano-tubes, Si powder.
Conversion unit: vacuum high-temperature sintering stove, alumina crucible
Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, cover lid.Then crucible is positioned in the vacuum high-temperature sintering stove, is warmed up to 1410～1600 ℃, soaking time 3～9 hours always with the temperature rise rate of 10～30 ℃/min.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.Find that at last a large amount of linen products is in alumina crucible.Remove unnecessary unreacted silicon with the mixed solution (volume ratio is 1: 2) of hydrofluoric acid and nitric acid behind the taking-up product and obtain the silicon carbide nanometer line powder, see shown in Figure 1.In addition, also there is the skim nanometer silicon carbide, under scanning electron microscope, observes, find that this nanometer silicon carbide is the cucurbit shape, sees shown in Figure 2 covering of alumina crucible.
Embodiment 1:
Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, then crucible are positioned in the vacuum high-temperature sintering stove, are warmed up to 1450 ℃, soaking time 6 hours with the temperature rise rate of 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.Find that at last a large amount of linen products is in alumina crucible.Remove unnecessary unreacted silicon with the mixed solution (volume ratio is 1: 2) of hydrofluoric acid and nitric acid behind the taking-up product and obtain the silicon carbide nanometer line powder, see shown in Figure 1.Also there is the skim nanometer silicon carbide covering of alumina crucible, under scanning electron microscope, observes, find that this nanometer silicon carbide is the cucurbit shape, sees shown in Figure 2.
Embodiment 2:
Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, then crucible are positioned in the vacuum high-temperature sintering stove, are warmed up to 1410 ℃, soaking time 9 hours with the temperature rise rate of 10 ℃/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.Find that at last a large amount of linen products is in alumina crucible.Remove unnecessary unreacted silicon with the mixed solution (volume ratio is 1: 2) of hydrofluoric acid and nitric acid behind the taking-up product and obtain the silicon carbide nanometer line powder.
Embodiment 3:
Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, then crucible are positioned in the vacuum high-temperature sintering stove, are warmed up to 1600 ℃, soaking time 5 hours with the temperature rise rate of 20 ℃/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.Find that at last a large amount of linen products is in alumina crucible.Remove unnecessary unreacted silicon with the mixed solution (volume ratio is 1: 2) of hydrofluoric acid and nitric acid behind the taking-up product and obtain the silicon carbide nanometer line powder.
Claims (1)
1, a kind of method of synthetizing two kinds of different shaped silicon carbid nano wire, the step that it is characterized in that this method is as follows: Si powder and multi-walled carbon nano-tubes place in the alumina crucible as initial starting material, cover lid, crucible is positioned in the vacuum high-temperature sintering stove then, temperature rise rate with 10～30 ℃/min is warmed up to 1410～1600 ℃ always, soaking time 3～9 hours, 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, finds that at last a large amount of linen products is in alumina crucible; Taking out behind the product with volume ratio is 1: 2 hydrofluoric acid and nitric acid mixed solution, removes unnecessary unreacted silicon and obtains the silicon carbide nanometer line powder; In addition, also there is skim cucurbit shape nanometer silicon carbide covering of alumina crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100496820A CN1330796C (en) | 2006-03-02 | 2006-03-02 | Method of synthetizing two kinds of different shaped silicon carbid nano wire |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100496820A CN1330796C (en) | 2006-03-02 | 2006-03-02 | Method of synthetizing two kinds of different shaped silicon carbid nano wire |
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| Publication Number | Publication Date |
|---|---|
| CN1834309A CN1834309A (en) | 2006-09-20 |
| CN1330796C true CN1330796C (en) | 2007-08-08 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718217B (en) * | 2012-05-18 | 2014-01-15 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN102689904B (en) * | 2012-05-25 | 2013-10-30 | 太原理工大学 | Method for preparing SiC nanowire and array thereof |
| CN103835181B (en) * | 2014-03-03 | 2016-01-27 | 浙江理工大学 | A kind of preparation method of SiC nanofiber paper |
| CN109110763A (en) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | A kind of Sic nanotube and its preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222495A (en) * | 1997-11-14 | 1999-07-14 | 中国科学院固体物理研究所 | Nanometer silicon carbide rod with or without silicon dioxide coated surface and its preparation |
| CN1327944A (en) * | 2001-07-25 | 2001-12-26 | 中山大学 | Process for preparing nm-class silicon carbide material |
| CN1436724A (en) * | 2003-03-14 | 2003-08-20 | 清华大学 | Prepn process of nanometer silicon carbide rod |
| JP2004307299A (en) * | 2003-04-10 | 2004-11-04 | Japan Atom Energy Res Inst | Nano-size silicon carbide tube and its manufacturing method |
| JP2006001779A (en) * | 2004-06-16 | 2006-01-05 | National Institute For Materials Science | Method for producing sic nanoparticles by nitrogen plasma |
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2006
- 2006-03-02 CN CNB2006100496820A patent/CN1330796C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222495A (en) * | 1997-11-14 | 1999-07-14 | 中国科学院固体物理研究所 | Nanometer silicon carbide rod with or without silicon dioxide coated surface and its preparation |
| CN1327944A (en) * | 2001-07-25 | 2001-12-26 | 中山大学 | Process for preparing nm-class silicon carbide material |
| US20040202599A1 (en) * | 2001-07-25 | 2004-10-14 | Ningsheng Xu | Method of producing nanometer silicon carbide material |
| CN1436724A (en) * | 2003-03-14 | 2003-08-20 | 清华大学 | Prepn process of nanometer silicon carbide rod |
| JP2004307299A (en) * | 2003-04-10 | 2004-11-04 | Japan Atom Energy Res Inst | Nano-size silicon carbide tube and its manufacturing method |
| JP2006001779A (en) * | 2004-06-16 | 2006-01-05 | National Institute For Materials Science | Method for producing sic nanoparticles by nitrogen plasma |
Non-Patent Citations (6)
| Title |
|---|
| Growth of SiC nanorod prepared by carbonnanotubes-confined reaction Tang C C et.al,J.Cryst.Growth,Vol.210 2000 * |
| Growth of SiC nanorod prepared by carbonnanotubes-confined reaction Tang C C et.al,J.Cryst.Growth,Vol.210 2000;碳化硅纳米晶须的制备研究进展 吴艳军等，电子元件与材料，第22卷第9期 2003;哑铃形碳化硅晶须的微观结构分析 白朔等，材料研究学报，第14卷第5期 2000;哑铃形碳化硅晶须的制备与表征 白朔等，材料研究学报，第13卷第3期 1999;哑铃形碳化硅晶须生长的机理 白朔等，材料研究学报，第16卷第2期 2002 * |
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| 碳化硅纳米晶须的制备研究进展 吴艳军等，电子元件与材料，第22卷第9期 2003 * |
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| CN1834309A (en) | 2006-09-20 |
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