CN1899960A - Method for preparing silicon carbide nano line - Google Patents
Method for preparing silicon carbide nano line Download PDFInfo
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- CN1899960A CN1899960A CN 200510028034 CN200510028034A CN1899960A CN 1899960 A CN1899960 A CN 1899960A CN 200510028034 CN200510028034 CN 200510028034 CN 200510028034 A CN200510028034 A CN 200510028034A CN 1899960 A CN1899960 A CN 1899960A
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Abstract
The process of preparing nano silicon carbide line includes the following steps: setting silane without oxygen inside corundum crucible or corundum boat, setting the corundum crucible or corundum boat on heat resist plate, setting the heat resist plate inside a high temperature furnace, removing oxygen from the furnace, introducing protecting inert gas at the rate of 6-15 sccm, raising the temperature at the rate of 5-15 deg.c/min to 1000-1100 deg.c, maintaining for 1-3 hr and final naturally cooling. The process can obtain relatively long nanometer silicon carbide line.
Description
Technical Field
The invention relates to the field of a preparation method of a silicon carbide nanowire.
Background
Since the advent of silicon carbide materials, silicon carbide materials have been used in various fields as various products with excellent high temperature resistance, abrasion resistance, corrosion resistance, high strength and high thermal conductivity. And has great potential in the application aspect of high-power and high-frequency devices due to the wide forbidden band, high breakdown electric field, high drift saturation velocity and high thermal conductivity. The one-dimensional SiC nanowires have higher mechanical properties such as elasticity, hardness and toughness than SiC blocks and SiC whiskers, and therefore, the one-dimensional SiC nanowires are extremely promising materials for reinforcing agents of ceramics, metals and polymer materials. The one-dimensional SiC nanowire is a semiconductor with excellent electrical performance, has high thermal conductivity (350-490 w/mk), wide band gap and excellent thermal stability, and is expected to become a semiconductor device material which is high in power and frequency and can work in severe environments. The current methods for preparing one-dimensional SiC nano-structures mainly comprise a carbon nano-tube template growth method, a reduction method and the like.
Documents z.w.pan, h.l.lai, f.c.k.au, x.f.duan, w.y.zhou, w.s.shi, n.wang, c.s.lee, n.b.wong, s.t.lee, s.s.xie, adv.mater 12(2000), 1186 report a method for preparing silicon carbide nanowires, using oriented C nanotubes to react with SiO to form oriented SiC nanowires, first they prepare oriented C nanotubes with a pyrolytic acetylene method, diameter of 10-40 nm, length of 2mm, grown perpendicular to an iron/SiO 2 substrate, and a gap between tubes of about 100nm, using prepared C nanotubes and SiO powderwith a purity of 99.9% as raw materials, heated in a furnace with argon (50cm3/min) protection for 14000C 2 hours to obtain SiC nanotubes similar to C, vertical to SiC nanowires grown in purity of 99.9%, prepared SiC nanowires with a length of 99.9% are expected to be used in microelectronic devices with high-emission stability of the C nanowires, and the length of β mm is expected to be used in microelectronic devices.
Documents j.q.hu, q.y.lu, k.b.tang, b.deng, r.r.jiang, y.t.qian, w.c.yu, g.e.zhou, x.m.liu, j.x.wu, j.phys.chem.b 104(2000), 5251. Hu et al report that SiC nanowires were prepared by the compound method using reduced carbon. The reaction equation is as follows:
the specific experimental process is as follows: taking appropriate amount of CCl4(50ml), Si powder (1.44g), Na(4.74g) the mixture was placed in a titanium alloy autoclave having a capacity of 50ml, heated to 700 ℃ and held for 10 to 48 hours, and then cooled to room temperature. At the beginning of the reaction, the pressure in the reactor is high, following CCl4Reducing the pressure with Na to obtain diluted HF and HNO3Removing unreactedThe reaction Si, then heating the product in air to 600 deg.C for 3 hours to remove C, which oxidizes the product to form amorphous SiO on the surface2So the product is then put into dilute HF to remove SiO2And then washed with deionized water to remove NaCl and other impurities to give the final product. The SiC nanowire with the sphalerite structure is analyzed, the diameter is 15-20 nm, and the length is 5-10 mu m. The SiC nanowires prepared by the method have uniform diameter distribution, serious stacking faults are caused by the pore structure of the SiC nanowires prepared by the method, and the light absorption band of the SiC nanowires has obvious blueshift.
The two methods are very complex, the adopted raw materials are expensive, and the requirement on equipment is high, the length of the nanowire prepared by the method depends on the length of the used nanotube, and the length of the nanowire synthesized by the method is only dozens of micrometers, so that the silicon carbide nanowire which is cheap and easy to obtain as the raw material, simple and easy to control in process, low in equipment requirement and capable of synthesizing longer silicon carbide nanowires is needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of silicon carbide nanowires, which has the advantages of cheap and easily-obtained raw materials, simple and easily-controlled process and low equipment requirement.
The silicon carbide nanowire provided by the invention is a crystallized SiC nanowire.
The preparation method of the silicon carbide nanowire comprises the following steps:
placing the oxygen-free silane in a corundum crucible or a corundum boat, placing the corundum crucible or the corundum boat on a high temperature resistant plate, pushing the high temperature resistant plate into a high temperature furnace, discharging oxygen in the furnace, introducing inert gas at the rate of 6-15sccm for protection, raising the temperature of the furnace to 1000-1100 ℃ at the speed of 5-15 ℃/min, preserving the temperature for 1-3 hours, and then naturally cooling to room temperature. White wool-like silicon carbide nanowires are generated above and below the high-temperature resistant plate.
The principle of the preparation method of the silicon carbide nanowire is as follows: at high temperatures the silicon-carbon bond is first broken, creating a methyl radical which is further cleaved to produce carbon and methane or carbon and hydrogen. The carbon reacts with Si to form silicon carbide nanowires.
In the method for preparing silicon carbide nanowires of the present invention, the silane containing no oxygen may be hexamethyl silazane, hexamethyl disilazane, or polydimethyl silane.
The preparation method of the silicon carbide nanowire can be used for preparing high-temperature resistant plates such as an aluminum oxide plate and a boron nitride plate. Preferably an alumina plate.
The preparation method of the silicon carbide nanowire is characterized in that the high-temperature furnace is a quartz tube furnace or an alumina tube furnace.
In the preparation method of the silicon carbide nanowire, the inert gas is preferably argon.
The invention has the beneficial effects that: the products obtained by the preparation method of the silicon carbide nanowires are the silicon carbide nanowires, the length of the silicon carbide nanowires is improved by 2 levels compared with the silicon carbide nanowires prepared by most of the existing methods, and the preparation method is simple, the raw materials are cheap and easy to obtain, the equipment requirement is simplified, and the cost is low.
Drawings
Fig. 1 is a scanning electron micrograph of a product of example 1 of the preparation method of silicon carbide nanowires according to the present invention.
Fig. 2 is a transmission electron micrograph of a product of example 1 of the preparation method of silicon carbide nanowires according to the present invention.
Fig. 3 isa scanning electron micrograph of a product of example 2 of the preparation method of silicon carbide nanowires according to the present invention.
Fig. 4 is a transmission electron micrograph of a product of example 2 of the preparation method of silicon carbide nanowires according to the present invention.
Fig. 5 is a scanning electron micrograph of a product of example 3 of the preparation method of silicon carbide nanowires according to the present invention.
Fig. 6 is a transmission electron micrograph of a product of example 3 of the preparation method of silicon carbide nanowires according to the present invention.
Detailed Description
Example 1
5ml of hexamethylsilazane was placed in a corundum crucible, the crucible was placed on a high temperature resistant alumina plate 20mm thick, and then the alumina plate was pushed flat into the center of a quartz tube furnace. Argon was passed through the quartz tube for a sufficient time to expel the oxygen. The furnace temperature is increased to 1000-1100 ℃ at the speed of 10 ℃/min, the temperature is kept for 2 hours and then is naturally reduced to the room temperature, the process is continuously protected by argon, and the introduction rate is about 6 sccm. White wool-like silicon carbide nanowires are generated above and below the alumina plate, the length of the nanowires reaches 3 mm at most, the average length of the nanowires exceeds 2mm, the nanowires are detected by a transmission electron microscope, the diameter of the nanowires is 7-100nm, and the silicon carbide is crystallized. The scanning electron microscope and transmission electron microscope photographs of the product are respectively shown in figures 1 and 2.
Example2
5mL of hexamethyldisilane was placed in a corundum crucible, the crucible was placed on a high temperature resistant alumina plate having a thickness of 20mm, and then the alumina plate was pushed flat into the center of the quartz tube furnace. Argon was passed through the quartz tube for a sufficient time to expel the oxygen. The furnace temperature is increased to 1000-1100 ℃ at the speed of 15 ℃/min, the temperature is preserved for 3 hours and then is naturally reduced to the room temperature, the process is continuously protected by argon, and the introduction rate is about 10 sccm. White wool-like silicon carbide nanowires were grown both above and below the alumina plate, with an average length of about 2 mm. The resulting product has a diameter of 10-120nm and the silicon carbide is crystalline. The scanning electron microscope and transmission electron microscope photographs of the product are respectively shown in FIGS. 3 and 4.
Example 3
Placing 5ml of polydimethylsilane in a corundum crucible, placing the crucible on a high-temperature-resistant alumina plate with the thickness of 20mm, and then horizontally pushing the alumina plate into the center of a quartz tube furnace. Argon was passed through the quartz tube for a sufficient time to expel the oxygen. The furnace temperature is increased to 1000-1100 ℃ at the speed of 5 ℃/min, the temperature is kept for 1 hour and then is naturally reduced to the room temperature, the argon is introduced for protection in the process, and the introduction rate is about 15 sccm. White wool-like silicon carbide nanowires are generated above and below the alumina plate, the length of the nanowires reaches 3 mm at most, the average length of the nanowires exceeds 2mm, the nanowires are detected by a transmission electron microscope, the diameter of the nanowires is 10-130nm, and the silicon carbide is crystallized. The scanning electron microscope and transmission electron microscope photographs of the product are respectively shown in FIGS. 5 and 6.
Claims (5)
1. A preparation method of silicon carbide nanowires comprises the following steps: placing the oxygen-free silane in a corundum crucible or a corundum boat, placing the corundum crucible or the corundum boat on a high temperature resistant plate, pushing the high temperature resistant plate into a high temperature furnace, discharging oxygen in the furnace, introducing inert gas at the rate of 6-15sccm for protection, raising the temperature of the furnace to 1000-1100 ℃ at the speed of 5-15 ℃/min, preserving the temperature for 1-3 hours, and then naturally cooling to room temperature.
2. The method for preparing silicon carbide nanowires according to claim 1, wherein the silane containing no oxygen is hexamethyl silazane, hexamethyl disilazane, or polydimethylsilane.
3. The method for preparing silicon carbide nanowires according to claim 1, wherein the high temperature resistant plate is an alumina plate or a boron nitride plate.
4. The method for preparing silicon carbide nanowires according to claim 1, wherein the high-temperature furnace is a quartz tube furnace or an alumina tube furnace.
5. The method for preparing silicon carbide nanowires according to claim 1, wherein the inert gas is argon gas.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306379B (en) * | 2008-07-01 | 2010-06-02 | 浙江理工大学 | Preparation method and use of silicon carbide nano-wire catalyst for making hydrogen |
| CN101311378B (en) * | 2008-03-24 | 2010-06-09 | 宁波工程学院 | Controllable doping of SiC single crystal low-dimensional nano material |
| CN101369473B (en) * | 2007-08-16 | 2011-12-07 | 同济大学 | Preparation of silicon carbide/silicon dioxide coaxial nanometer cable by floating catalysis method |
| CN102719029A (en) * | 2012-06-08 | 2012-10-10 | 扬州大学 | Preparation method of silicon carbide nanowire-base light-emitting film |
| CN103097283A (en) * | 2010-09-16 | 2013-05-08 | 格拉芬斯克公司 | Process for growth of graphene |
| CN108328617A (en) * | 2018-01-20 | 2018-07-27 | 南京航空航天大学 | A kind of silicon carbide nanometer line aeroge and preparation method thereof |
| CN109135356A (en) * | 2018-07-14 | 2019-01-04 | 南京航空航天大学 | A kind of silicon carbide nanometer line hydrophobic coating and preparation method thereof |
Family Cites Families (4)
| 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 |
| JP3709441B2 (en) * | 2003-03-26 | 2005-10-26 | 独立行政法人物質・材料研究機構 | Method for producing silicon carbide nanowire |
| JP2004360115A (en) * | 2003-06-04 | 2004-12-24 | Japan Science & Technology Agency | Method for producing silicon carbide-based nanofiber |
| CN1239758C (en) * | 2003-07-17 | 2006-02-01 | 上海交通大学 | Massive prepn process of nano beta-Sic crystal whisker |
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2005
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101369473B (en) * | 2007-08-16 | 2011-12-07 | 同济大学 | Preparation of silicon carbide/silicon dioxide coaxial nanometer cable by floating catalysis method |
| CN101311378B (en) * | 2008-03-24 | 2010-06-09 | 宁波工程学院 | Controllable doping of SiC single crystal low-dimensional nano material |
| CN101306379B (en) * | 2008-07-01 | 2010-06-02 | 浙江理工大学 | Preparation method and use of silicon carbide nano-wire catalyst for making hydrogen |
| CN103097283A (en) * | 2010-09-16 | 2013-05-08 | 格拉芬斯克公司 | Process for growth of graphene |
| CN102719029A (en) * | 2012-06-08 | 2012-10-10 | 扬州大学 | Preparation method of silicon carbide nanowire-base light-emitting film |
| CN108328617A (en) * | 2018-01-20 | 2018-07-27 | 南京航空航天大学 | A kind of silicon carbide nanometer line aeroge and preparation method thereof |
| CN109135356A (en) * | 2018-07-14 | 2019-01-04 | 南京航空航天大学 | A kind of silicon carbide nanometer line hydrophobic coating and preparation method thereof |
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