CN101348253A - Method for preparing twin structure silicon carbide nanowire by heat evaporation method - Google Patents
Method for preparing twin structure silicon carbide nanowire by heat evaporation method Download PDFInfo
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- CN101348253A CN101348253A CNA2008101204636A CN200810120463A CN101348253A CN 101348253 A CN101348253 A CN 101348253A CN A2008101204636 A CNA2008101204636 A CN A2008101204636A CN 200810120463 A CN200810120463 A CN 200810120463A CN 101348253 A CN101348253 A CN 101348253A
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Abstract
The invention discloses a method for preparing a silicon carbide nano line with a twin crystal structure by a heat evaporation method. Firstly, silica resources are put at the bottom of a graphite pot, at the top of which carbon materials are put, the silica resources do not contact the carbon materials which are taken as carbon resources of the reaction as well as the substrate formed by the reaction products; the pot loaded with materials are placed in a high-temperature vacuum sintering furnace and vacuumized to be between 0.1 and 20Pa, and argon shielding gases are filled in the pot; and, the pot is heated up to a temperature of between 1200 and 1650 DEG C and kept warm for 0.5 to 10h, the power is cut, the pot is cooled down and taken out, and the carbon materials on which a layer of light green, light blue or gray products are arranged are obtained. The method of the invention has the advantages of low production cost, high purity of the nano line and simple and convenient process.
Description
Technical field
A kind of thermal evaporation of preparation prepares the method for twin structure silicon carbide nanowire in the carbonaceous material substrate of the present invention.
Background technology
Silicon carbide (SiC) nano wire all is better than block materials at aspect of performances such as optics, electricity and machineries, is the ideal material of preparation blue light-emitting diode and nano-photons such as laser diode, high power transistor, opto-electronic device.Simultaneously, research shows that also the elasticity of single SiC nano wire or nanometer rod and intensity are far longer than bulk SiC crystalline intensity, and near theoretical value, thereby the SiC nano wire also is applied in metal matrix, ceramic base and the polymer matrix composite as the wild phase material widely.
Twin is by the caused a kind of plane defect of the stacking fault of solid matter face, is lattice defect common in the metallic substance.Find in the spinels inorganic materials that at first the back is observed in zincblende lattce structure and face-centred cubic structure compound crystal.Report in recent years shows that twinning is prevalent in the nano wire of materials such as GaP, GaAs, Si, ZnSe, Zn2TiO4, Zn2SnO4, ZnO, ZnS, Cu and Au.Because the photoelectric properties of semiconductor nanowires depend primarily on the pattern and the microstructure of nano wire, the twin structure nano wire has broad application prospects in the sub-field of nano photoelectric.Twining plane defective equally also existence widely has in the beta-SiC nano-wire/whisker of zincblende lattce structure.R.D.Jong etc. have early reported silicon carbide whisker (the Growth of twinned β-silicon carbide whiskers by thevapor-liquid-solid process that adopts gas-liquid-solid method to prepare twin structure, J.Am.Ceram.Soc., (1987), 70 (11): C-338-C-341.); H.F.Zhang etc. have reported SiO
2Coat spiral twin structure SiC nano wire (Helical crystalline SiC/SiO2core-shell nanowires, Nano Lett., (2002), 2 (9): 941-944.), H.W.Shim etc. adopt the iron powder catalyzer, based on gas-liquid-solid growth mechanism, deposition has prepared the transformable twin structure silicon carbide nanowire of diameter (Three-stage transition during silicon carbide nanowire growth on alumina substrate, Appl.Phys.Lett., (2007), 90:083106 (1-3)) employing CNT (carbon nano-tube) such as .R.Wu twin structure silicon carbide nanoneedle (the Twinned SiC zigzag nanoneedles that has been feedstock production, J.Phys.Chem.C, (2007), 111:6233-6237.) Guo Xiangyun etc. reported with nitrate (iron nitrate, Xiao Suangu or nickelous nitrate) be catalyzer, prepared silicon carbide nanometer line (patent publication No.: CN101186297) by the silica xerogel that heats carbonaceous sources with periodical twin crystal structure.Above preparation method adopts metal catalyst by gas-liquid-solid growth mechanism or carbon nanotube template growing silicon carbide nano wire more, contains more impurity in the product, and nano wire is intertwined easily, is not easy to disperse.
Summary of the invention
The object of the present invention is to provide a kind of thermal evaporation to prepare the method for twin structure silicon carbide nanowire.Directly evaporate various siliceous sources by elevated temperature heat, deposition growing has twin structure silicon carbide nanowire in the carbonaceous material substrate.
The step of the technical solution used in the present invention is as follows:
At first the silicon source is put into graphite earthenware bottom; shelve carbonaceous material at the crucible top; be not in contact with one another between silicon source and the carbonaceous material; carbonaceous material is the carbon source of reaction; serve as the substrate that reaction product forms again; put into the high-temperature vacuum sintering oven adorning excellent crucible device, be evacuated down to 0.1～20Pa, charge into argon shield gas then.Then, heat temperature raising to 1200～1650 ℃ were incubated after 0.5～10 hour, turned off power supply, and plumbago crucible is taken out in the cooling back, obtained that just one deck light green is arranged on the carbonaceous material, light blue or gray product.
Described silicon source is the mixture or the carbon containing silica xerogel of pure silicon, silicon-dioxide and carbon.
Described carbonaceous material is graphite substrate, carbon black, carbon fiber or activated carbon fiber.
To be grown in the phase composite of the product employing X-ray diffraction analysis product on the carbonaceous material, it is elementary composition to observe its pattern and analysis with the field emission scanning electron microscope (SEM) of band energy spectrometer, and (TEM) analyzes its microstructure etc. with transmission electron microscope.Product on the analysis revealed graphite base is for having twin structure silicon carbide nanowire.
The beneficial effect that the present invention has:
1. adopt the preparation of elevated temperature heat method of evaporation to have twin structure silicon carbide nanowire and have production cost advantage low, simple for process.
2. adopt carbonaceous material to induce substrate, induce the growth of SiC nanowire deposition as graphite substrate, the SiC nano wire is grown directly upon graphite and induces substrate surface, does not have impurity particle, can not pollute the SiC nano wire, has guaranteed the high purity of SiC nano wire.
Description of drawings
Fig. 1 is silicon carbide nanometer line SEM figure.
Fig. 2 is twin structure silicon carbide nanowire TEM figure.
Embodiment
Embodiment 1:
At first the pure silicon powder is put into graphite earthenware bottom, shelved graphite substrate, be not in contact with one another between silicon and the graphite substrate at the crucible top.Put into the high-temperature vacuum sintering oven adorning excellent crucible device, be evacuated down to 0.1Pa, charge into argon shield gas then.Then, heat to 1500 ℃, constant temperature was turned off power supply after 5 hours.Plumbago crucible is taken out in the cooling back, on the visible graphite substrate one deck light green product is arranged.To be grown in the phase composite of the product employing X-ray diffraction analysis product on the graphite substrate, product consists of β-SiC as can be known.(SEM) observes its pattern with field emission scanning electron microscope, and visible β-SiC is a nano wire, as shown in Figure 1.(TEM) analyzes its microstructure with transmission electron microscope, and the product on the analysis revealed graphite base is for having twin structure silicon carbide nanowire, and nanowire surface indention facet is formed by the psuedo-periodicity twin as shown in Figure 2.
Embodiment 2:
At first the mixture of silicon-dioxide and carbon black (silicon-dioxide is 1: 1～3 with carbon black amount of substance ratio) is put into graphite earthenware bottom, shelved carbon fiber, be not in contact with one another all the time between mixture and the carbonaceous material at the crucible top.Put into the high-temperature vacuum sintering oven adorning excellent crucible device, be evacuated down to 20Pa, charge into argon shield gas then.Then, 1650 ℃ of heat temperature raisings after 10 hours for some time of insulation, are turned off power supply.Plumbago crucible is taken out in the cooling back, and just can see has one deck light green product on the carbon fiber.The phase composite of the product employing X-ray diffraction analysis product on the carbonaceous material will be grown in, its pattern of use emission scan electron microscopic observation and analyze that it is elementary composition, analyze its microstructure with transmission electron microscope and high-resolution-ration transmission electric-lens, the product on the analysis revealed graphite base is for having twin structure silicon carbide nanowire.
Embodiment 3:
Being raw material with tetraethoxy, dehydrated alcohol and deionized water earlier, is catalyzer with hydrochloric acid, preparation SiO
2Colloidal sol before collosol and gel, adds the nano active carbon black particle, ultra-sonic dispersion, and the ageing gel handled for 1 week for 90 ℃ with gel then, obtained to contain the SiO of C
2Xerogel with putting into plumbago crucible after this xerogel pulverizing, is shelved activated carbon fiber at the crucible top.Put into the high-temperature vacuum sintering oven adorning excellent crucible device, be evacuated down to 10Pa, charge into argon shield gas then.Be warming up to 1200 ℃, be incubated 3 hours.SiO in the experiment
2Can be respectively 1: 1,1: 1.5,1: 2,1: 2.5 and 1: 3 with the molar mass ratio of C.The product of one deck green is collected in the reaction back on the activated carbon fiber that places on the crucible, product is for having twin structure SiC nano wire by analysis.
Claims (3)
1, a kind of thermal evaporation prepares the method for twin structure silicon carbide nanowire; the step that it is characterized in that this method is as follows: at first the silicon source is put into graphite earthenware bottom; shelve carbonaceous material at the crucible top; be not in contact with one another between silicon source and the carbonaceous material; carbonaceous material is the carbon source of reaction, serves as the substrate that reaction product forms again, puts into the high-temperature vacuum sintering oven adorning excellent crucible device; be evacuated down to 0.1～20Pa, charge into argon shield gas then.Then, heat temperature raising to 1200～1650 ℃ were incubated after 0.5～10 hour, turned off power supply, and plumbago crucible is taken out in the cooling back, obtained that just one deck light green is arranged on the carbonaceous material, light blue or gray product.
2, a kind of thermal evaporation according to claim 1 prepares the method for twin structure silicon carbide nanowire, it is characterized in that: described silicon source is the mixture or the carbon containing silica xerogel of pure silicon, silicon-dioxide and carbon.
3, a kind of thermal evaporation according to claim 1 prepares the method for twin structure silicon carbide nanowire, it is characterized in that: described carbonaceous material is graphite substrate, carbon black, carbon fiber or activated carbon fiber.
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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 |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| 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 |
| CN106278267A (en) * | 2016-08-10 | 2017-01-04 | 大连理工大学 | A kind of growth in situ silicon carbide nanometer line strengthens the preparation method of porous carbon composite |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011166B (en) * | 2012-12-27 | 2014-10-15 | 哈尔滨工业大学 | Synthesis method of SiC/SiO2 nanowire reinforcement body |
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Cited By (7)
| 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 |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| CN102850087B (en) * | 2012-09-29 | 2014-10-29 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| 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 |
| CN106278267A (en) * | 2016-08-10 | 2017-01-04 | 大连理工大学 | A kind of growth in situ silicon carbide nanometer line strengthens the preparation method of porous carbon composite |
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