CN102432012A - Method for synthesizing silicon carbide nanometer needle without catalysts - Google Patents
Method for synthesizing silicon carbide nanometer needle without catalysts Download PDFInfo
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- CN102432012A CN102432012A CN2011102985786A CN201110298578A CN102432012A CN 102432012 A CN102432012 A CN 102432012A CN 2011102985786 A CN2011102985786 A CN 2011102985786A CN 201110298578 A CN201110298578 A CN 201110298578A CN 102432012 A CN102432012 A CN 102432012A
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Abstract
The invention relates to a method for synthesizing a silicon carbide nanometer needle without catalysts. In the method, a double graphite tube crucible is used for quickly synthesizing a needle tip-shaped silicon carbide nanometer material, namely a high-frequency induction coil is used for heating a graphite tube to provide required temperatures during evaporation of raw materials and growth of the nanometer needle; the catalysts are not used at all, only silicon monoxide powder and coke powder are used as the raw materials, the high-frequency induction coil is used as a quick heating source, and a process form evaporation to deposition can be finished within 10 minutes; a large number of attached light green substances can be collected from carbon fibers filled in the graphite tube after the preparation process is finished; and by representation analysis, the light green substances are the needle-shaped silicon carbide nanometer material. Compared with the prior art, the method for quickly preparing the needle-shaped silicon carbide nanometer material without the catalysts is provided.
Description
Technical field
The present invention relates to the technical field of nano material preparation, especially relate to a kind of method of catalyst-free synthetizing silicon carbide nano pin.
Background technology
Carbofrax material has HS, high firmness, wear-resistant, high temperature resistant, anti-oxidant, resistance to chemical attack, thermal expansivity is little and premium properties such as high thermoconductivity, therefore is widely used in engineering fields such as Aeronautics and Astronautics, machinery and petrochemical industry.Simultaneously; Silit is as third generation semiconductor material; Therefore have characteristics such as the bandwidth of broad, high disruptive critical voltage, high carrier saturation drift velocity, be with a wide range of applications at high frequency, high-power, high temperature, radiation-resistant semiconducter device and aspects such as ultraviolet detector and short-wave LED.
Monodimension nanometer material has more superior performance than the body material.The one dimension carbofrax material is because quantum size effect, small-size effect and surface effects have the more luminescent properties of excellence, electric property, an emission characteristic and photocatalytic effect.In addition, the silit monodimension nanometer material all has wide practical use in the fields such as probe of storage hydrogen and AFM.
Based on the above-described performance of silit, a large amount of researchers have carried out extensive studies to it.Through existing literature search is found that the report of catalyst-free synthetizing silicon carbide nano pin seldom.Renbing Wu; Yi Pan, Guangyi Yang, Mingxia Gao; People such as Jing Lin in 2007 at The Journal of Physical Chemistry C (physical chemistry magazine C; 2007,111, delivered the article that is entitled as " Twinned SiC Zigzag Nanoneedles " (twin zigzag nanometer silicon carbide pin) on 6233-6237).Adopt silicon fragment and multi-walled carbon nano-tubes as raw material in the literary composition, adopt high temperature process furnances to carry out the thermal evaporation reaction, be incubated 30 minutes and 8 hours at 1000 degrees centigrade and 1500 degrees centigrade respectively, prepared silicon carbide nano material with tip-like form.This method preparation time is longer.
Summary of the invention
The object of the invention is exactly to provide a kind of for the defective that overcomes above-mentioned prior art existence to use two carbon tube crucibles to synthesize the silicon carbide nano material with needle-like form fast, i.e. raw materials evaporate and nanoneedle growth all uses radio-frequency induction coil heating carbon tube that required temperature is provided.The present invention does not use any catalyzer; Only use silicon monoxide powder and coke powder as raw material; Use radio-frequency induction coil as the rapid heating source; Can in 10 minutes, accomplish the sedimentary process that is evaporated to, collect the light green material that adheres in a large number on the carbon fiber wire that preparation can be filled after accomplishing in carbon tube, phenetic analysis is indicated as the needle-like silicon carbide nano material.
The object of the invention can be realized through following technical scheme:
A kind of method of catalyst-free synthetizing silicon carbide nano pin as raw material, uses the hollow graphite pipe as charging crucible and heating element with silicon monoxide powder and coke powder; Use high-frequency induction equipment as the rapid heating source; The growth district of the hollow graphite pipe of fluffy carbon fiber wire as nanoneedle is equipped with in use, do not use any catalyzer, obtains being attached with the carbon fiber wire of light green material after reaction finishes; The light green material is the nanometer silicon carbide pin, specifically may further comprise the steps:
(1) weighs in the balance and get silicon monoxide powder and coke powder, use agate mortar two kinds of abundant ground and mixed of powder;
(2) powder of mixture is put into the first hollow graphite pipe, and this carbon tube is placed silica tube, silica tube is in the reach of radio-frequency coil;
(3) with filling in carbon fiber wire in the second hollow graphite pipe, and the second hollow graphite pipe is put into silica tube, near the first hollow graphite pipe;
(4) close the valve at silica tube two ends, charge into argon gas after vacuumizing, bleeding regulating amount and air input, it is stable that quartzy intraductal pressure is kept;
(5) open cooling circulating water, open the high-frequency induction device power supply (DPS), the temperature of mixture is risen to rapidly more than 1600 degrees centigrade;
(6) spray from the hollow carbon tube from the visible a large amount of smog of silica tube form, continue heating and disappear until smog;
(7) close the high-frequency induction device power supply (DPS), naturally cool to room temperature, on carbon fiber wire, can collect the light green material, be the nanometer silicon carbide pin.
The mol ratio of silicon monoxide powder described in the step (1) and coke powder is 1: 1.
Device required for the present invention and equipment are divided into following 6 parts: recirculating cooling water system, vacuum system, high frequency induction power supply and can lead to the ruhmkorff coil of water coolant, high temperature resistant silica tube, two hollow graphite pipe, gas circuit and air-path control systems that size is different.Wherein the geometrical dimension of high temperature resistant silica tube is long 1.4 meters, 80 millimeters of external diameters, 72 millimeters of internal diameters.Wherein the specification of the hollow graphite pipe of two different sizes is respectively: the first hollow graphite Guan Weiyi holds open, and end sealing is of a size of long 12 centimetres, 22 millimeters of internal diameters, 30 millimeters of external diameters; The second hollow graphite pipe is a both ends open, is of a size of long 12 centimetres, 32 millimeters of internal diameters, 40 millimeters of external diameters.
Described carbon fiber wire is rubbed into puffy, and this carbon fiber wire is a growth substrate, the gaseous substance that from the first hollow graphite pipe, sprays attachment reaction and grow into one-dimensional material on thomel.
Quartzy intraductal pressure described in the step (4) is 40-60 kPa.
The temperature of mixture was raised to more than 1600 degrees centigrade in 2 minutes in the step (5).
The time of continuing heating in the step (6) look blowing what and decide, be no more than 5 minutes.
Compared with prior art; The present invention does not use any catalyzer, only uses high-frequency induction equipment to heat, and can make mixed powder be raised to comparatively high temps at the utmost point in the short period of time; Silicon monoxide powder and coke powder in the first hollow graphite pipe at high temperature can react rapidly; The gas ejection that reaction produces arrives the second hollow graphite pipe from the first hollow graphite pipe, and this carbon tube is similarly high-frequency induction heating; Inside has comparatively high temps, and the fluffy carbon fiber wire of filling can play the effect that is similar to substrate.When the atmosphere in the second hollow graphite pipe is fit to, a large amount of nanometer silicon carbide pins can be on carbon fiber wire apposition growth.The silicon carbide nano material of gained has tangible tip-like structure, and diameter is between the 50-100 nanometer, and the cross section has the regular hexagon structure.
Description of drawings
Fig. 1 is the electron scanning micrograph of tip-like silicon carbide nano material;
Fig. 2 is the electron scanning micrograph of tip-like silicon carbide nano material;
Fig. 3 is the transmission electron microscope photo of tip-like silicon carbide nano material.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment 1
Weigh in the balance and get silicon monoxide powder 11 grams, take by weighing coke powder 3 grams, use agate mortar to grind 30 minutes, guarantee that two kinds of powder thorough mixing are even; Ground mixed powder is put into the first hollow graphite pipe; Carbon tube places silica tube; And be in the reach of radio-frequency coil, place preceding need of carbon tube and carbon tube and silica tube are separated with high temperature insulating material, at high temperature burnt out to prevent silica tube; With filling in an amount of carbon fiber wire in the second hollow graphite pipe, the second hollow graphite pipe is put into silica tube, and, likewise need the second hollow graphite pipe and silica tube to be separated with high temperature thermal insulation material near the first hollow graphite pipe; Close the valve at silica tube two ends, vacuumize, treat that vacuum tightness acquires a certain degree, charge into an amount of argon gas, bleeding regulating amount and air input are kept quartzy intraductal pressure and are stabilized between 40-60 kPa; Open cooling circulating water, open the high-frequency induction device power supply (DPS), mixture temperature is risen to rapidly more than 1600 degrees centigrade, use high-frequency induction heating only to need about 2 minutes; Spray from the hollow carbon tube from the visible a large amount of smog of silica tube form, continue heating and disappear until smog; Close the high-frequency induction device power supply (DPS), naturally cool to room temperature, on carbon fiber wire, can obtain the light green material, be the nanometer silicon carbide pin, its electron scanning micrograph is shown in Fig. 1-2, and the transmission electron microscope photo is as shown in Figure 3.
Embodiment 2
A kind of method of catalyst-free synthetizing silicon carbide nano pin as raw material, uses the hollow graphite pipe as charging crucible and heating element with silicon monoxide powder and coke powder; Use high-frequency induction equipment as the rapid heating source; The growth district of the hollow graphite pipe of fluffy carbon fiber wire as nanoneedle is equipped with in use, do not use any catalyzer, obtains being attached with the carbon fiber wire of light green material after reaction finishes; The light green material is the nanometer silicon carbide pin, specifically may further comprise the steps:
(1) weigh in the balance and get silicon monoxide powder and coke powder, the mol ratio of silicon monoxide powder and coke powder is 1: 1, uses agate mortar with two kinds of abundant ground and mixed of powder;
(2) powder of mixture is put into the first hollow graphite pipe, and this carbon tube is placed silica tube, silica tube is in the reach of radio-frequency coil;
(3) with filling in carbon fiber wire in the second hollow graphite pipe; And the second hollow graphite pipe put into silica tube; Near the first hollow graphite pipe; Carbon fiber wire is rubbed into puffy, and this carbon fiber wire is a growth substrate, the gaseous substance that from the first hollow graphite pipe, sprays attachment reaction and grow into one-dimensional material on thomel;
(4) close the valve at silica tube two ends, charge into argon gas after vacuumizing, bleeding regulating amount and air input are kept quartzy intraductal pressure and are stabilized in 40-60 kPa, and pressure is 50 kPas in the present embodiment;
(5) open cooling circulating water, open the high-frequency induction device power supply (DPS), the temperature of mixture is being risen to rapidly within 2 minutes more than 1600 degrees centigrade;
(6) spray from the hollow carbon tube from the visible a large amount of smog of silica tube form, look blowing what and decide, continue heating to be no more than 5 minutes and to disappear until smog, the time of continuing among the application to heat is 2 minutes;
(7) close the high-frequency induction device power supply (DPS), naturally cool to room temperature, on carbon fiber wire, can collect the light green material, be the nanometer silicon carbide pin.
Device required for the present invention and equipment are divided into following 6 parts: recirculating cooling water system, vacuum system, high frequency induction power supply and can lead to the ruhmkorff coil of water coolant, high temperature resistant silica tube, two hollow graphite pipe, gas circuit and air-path control systems that size is different.Wherein the geometrical dimension of high temperature resistant silica tube is long 1.4 meters, 80 millimeters of external diameters, 72 millimeters of internal diameters.Wherein the specification of the hollow graphite pipe of two different sizes is respectively: the first hollow graphite Guan Weiyi holds open, and end sealing is of a size of long 12 centimetres, 22 millimeters of internal diameters, 30 millimeters of external diameters; The second hollow graphite pipe is a both ends open, is of a size of long 12 centimetres, 32 millimeters of internal diameters, 40 millimeters of external diameters.
Claims (9)
1. the method for a catalyst-free synthetizing silicon carbide nano pin; It is characterized in that this method as raw material, uses the hollow graphite pipe as charging crucible and heating element with silicon monoxide powder and coke powder; High-frequency induction equipment is as the rapid heating source; The growth district of the hollow graphite pipe of fluffy carbon fiber wire as nanoneedle is housed, obtains being attached with the carbon fiber wire of light green material after reaction finishes, the light green material is the nanometer silicon carbide pin.
2. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 1 is characterized in that, this method specifically may further comprise the steps:
(1) weighs in the balance and get silicon monoxide powder and coke powder, use agate mortar two kinds of abundant ground and mixed of powder;
(2) powder of mixture is put into the first hollow graphite pipe, and this carbon tube is placed silica tube, silica tube is in the reach of radio-frequency coil;
(3), and the second hollow graphite pipe is put into silica tube near the first hollow graphite pipe with filling in carbon fiber wire in the second hollow graphite pipe;
(4) close the valve at silica tube two ends, charge into argon gas after vacuumizing, bleeding regulating amount and air input, it is stable that quartzy intraductal pressure is kept;
(5) open cooling circulating water, open the high-frequency induction device power supply (DPS), the temperature of mixture is risen to rapidly more than 1600 degrees centigrade;
(6) spray from the hollow carbon tube from the visible a large amount of smog of silica tube form, continue heating and disappear until smog;
(7) close the high-frequency induction device power supply (DPS), naturally cool to room temperature, on carbon fiber wire, can collect the light green material, be the nanometer silicon carbide pin.
3. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2 is characterized in that, the mol ratio of silicon monoxide powder described in the step (1) and coke powder is 1: 1.
4. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2 is characterized in that, the geometrical dimension of described silica tube is long 1.4 meters, 80 millimeters of external diameters, 72 millimeters of internal diameters; The first hollow graphite Guan Weiyi holds open, and end sealing is of a size of long 12 centimetres, 22 millimeters of internal diameters, 30 millimeters of external diameters; The second hollow graphite pipe is a both ends open, is of a size of long 12 centimetres, 32 millimeters of internal diameters, 40 millimeters of external diameters.
5. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2; It is characterized in that; Described carbon fiber wire is rubbed into puffy; This carbon fiber wire is a growth substrate, the gaseous substance that from the first hollow graphite pipe, sprays attachment reaction and grow into one-dimensional material on thomel.
6. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2 is characterized in that, the quartzy intraductal pressure described in the step (4) is 40-60 kPa.
7. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2 is characterized in that, the temperature of mixture was raised to more than 1600 degrees centigrade in 2 minutes in the step (5).
8. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 2 is characterized in that, the time of continuing heating in the step (6) look blowing what and decide, be no more than 5 minutes.
9. the method for a kind of catalyst-free synthetizing silicon carbide nano pin according to claim 1; It is characterized in that the required device of this method comprises 6 parts: recirculating cooling water system, vacuum system, high frequency induction power supply and can lead to the ruhmkorff coil of water coolant, high temperature resistant silica tube, two hollow graphite pipe, gas circuit and air-path control systems that size is different.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903971A (en) * | 2014-03-20 | 2014-07-02 | 上海华力微电子有限公司 | Method for improving quality of gate oxide |
| CN115259159A (en) * | 2022-07-05 | 2022-11-01 | 西北工业大学 | Inverted cone-shaped nitrogen-doped silicon carbide nanowire with high length-diameter ratio and preparation method thereof |
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| JPS57175718A (en) * | 1981-04-20 | 1982-10-28 | Hitachi Ltd | Preparation of silicon carbide fine powder |
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2011
- 2011-09-28 CN CN2011102985786A patent/CN102432012A/en active Pending
Patent Citations (5)
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| JPS57175718A (en) * | 1981-04-20 | 1982-10-28 | Hitachi Ltd | Preparation of silicon carbide fine powder |
| CN1834308A (en) * | 2006-03-02 | 2006-09-20 | 浙江大学 | Method of synthetizing silicon carbide nano rods |
| CN101327929A (en) * | 2008-07-31 | 2008-12-24 | 上海交通大学 | Method for rapidly preparing SiC nanowire |
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| WEI MIN ZHOU，ET AL.: "Large-scale synthesis and characterization of SiC nanowires by high-frequency induction heating", 《APPLIED SURFACE SCIENCE》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903971A (en) * | 2014-03-20 | 2014-07-02 | 上海华力微电子有限公司 | Method for improving quality of gate oxide |
| CN103903971B (en) * | 2014-03-20 | 2017-01-04 | 上海华力微电子有限公司 | A kind of method improving quality of gate oxide |
| CN115259159A (en) * | 2022-07-05 | 2022-11-01 | 西北工业大学 | Inverted cone-shaped nitrogen-doped silicon carbide nanowire with high length-diameter ratio and preparation method thereof |
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Application publication date: 20120502 |