CN103993475B - A kind of preparation method at carbon fiber surface coated Si/C nano wire - Google Patents
A kind of preparation method at carbon fiber surface coated Si/C nano wire Download PDFInfo
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- CN103993475B CN103993475B CN201410228144.2A CN201410228144A CN103993475B CN 103993475 B CN103993475 B CN 103993475B CN 201410228144 A CN201410228144 A CN 201410228144A CN 103993475 B CN103993475 B CN 103993475B
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Abstract
A kind of preparation method at carbon fiber surface coated Si/C nano wire, the preparation method that the present invention relates to SiC nanowire.The invention solves the problems that the preparation method of existing SiC nanowire exists the problem that cost is high and purity is low, and prior art does not adopt the preparation method at carbon fiber surface coated Si/C nano wire.Method: one, mixing；Two, ball milling；Three, pickling；Four, washing；Five, the process of ultrasonic disperse and carbon fiber；Six, dry and vacuum drying oven processes, and namely obtains being coated on the SiC nanowire of carbon fiber surface.The SiC nanowire diameter of prepared by the present invention be coated on carbon fiber surface is between 10nm～50nm, and length can reach less than 100 microns, technique is simple, in course of reaction without catalyst, cost is low, conversion ratio is high, purity is high.The present invention is used for a kind of preparation at carbon fiber surface coated Si/C nano wire.
Description
Technical field
The preparation method that the present invention relates to SiC nanowire.
Background technology
Metal or ceramic nano cause the great interest of people in the preparation of carbon fiber surface clad structure, and carborundum has the resistance to elevated temperatures of excellence, and what the elasticity of silicon carbide nanometer line and intensity will be higher than silicon carbide fibre or carborundum is many；Carborundum is also a kind of semi-conducting material simultaneously, and silicon carbide nanometer line or nanotube have huge potential using value in nano structural material, functional material and photoelectric device, field-transmitting cathode electron source and High Density Integration electronic device etc..
The preparation method of existing SiC nanowire has: masterplate method, chemical vapour deposition technique, arc discharge method, sol-gal process and carbothermic method etc..
In above-mentioned preparation method, masterplate method to use CNT as masterplate, reacts preparation SiC nanowire by SiO or Si, owing to CNT is expensive, thus makes the preparation of SiC nanowire be restricted.The VLS mechanism that chemical vapour deposition technique all uses mostly, namely the participation of catalyst is wherein had, catalyst is in liquid, the predecessor of siliceous and carbon constantly by entering catalyst after dissociating or reacting generation target product on catalyst droplets surface, precipitates out after supersaturation in the catalyst, grows into SiC nanowire.Owing to catalyst is in liquid, so the temperature of preparation is by a definite limitation of catalyst, the SiC nanowire of preparation all contains catalyst residue.Arc discharge method is to be anode by the SiC rod containing Fe, and graphite is negative electrode, carries out arc discharge at low pressure, forms SiC nanowire on the quartz ampoule inwall of reative cell, and also there is Fe nano-particle on nano wire top prepared by this method, and SiO is contained on surface2Affect its purity and quality.It is raw material that sol-gal process is generally adopted the Organic substance containing Si and C, forms collosol and gel, obtains SiC nanowire under reducing atmosphere through high-temperature heat treatment.The method shortcoming is that easily to form reunion, dispersibility and crystallization degree poor.In carbothermic method, multiplex containing SiO2Raw material mix with the C of activation, under 1600 DEG C of high temperature above and inertia or reducibility gas obtain SiC nanowire, the method preparation temperature is higher, and adopts Si and CCl4Gas is the carbothermic method of raw material, although can generate SiC nanowire under the low temperature of 700 DEG C, but it is generally required to 10h～48h, and need to carry out in autoclave.But the preparation method how obtaining the SiC nanowire being coated on carbon fiber surface have not been reported.
In sum, the preparation method of existing SiC nanowire makes cost high because of cost of material height, preparation condition harshness etc., most methods needs to use catalyst to cause containing impurity such as Fe, Ni in product, and prior art does not adopt the preparation method at carbon fiber surface coated Si/C nano wire.
Summary of the invention
The invention solves the problems that the preparation method of existing SiC nanowire exists the problem that cost is high and purity is low, and prior art does not adopt the preparation method at carbon fiber surface coated Si/C nano wire, and a kind of preparation method at carbon fiber surface coated Si/C nano wire is provided.
A kind of preparation method at carbon fiber surface coated Si/C nano wire, specifically carries out according to following steps:
One, mixing: Si powder is mixed homogeneously with graphite powder, obtains mixture；
The amount of substance of described Si powder and graphite powder is than for (0.8～1.2): 1；
Two, ball milling: be placed in by mixture in vacuum sphere grinding jar, is (15～20) in ball material mass ratio: the ratio of 1 puts into abrading-ball, and by vacuum sphere grinding jar evacuation, is then filled with 0.01 × 10 in vacuum sphere grinding jar5Pa～0.2 × 105The argon of Pa, when argon shield, with the speed ball milling 24h～48h of 430r/min～480r/min, obtains the powder body that particle diameter is 5nm～30nm；
Described purity of argon is more than 99.99%；
Three, pickling: be immersed in hydrochloric acid solution A by the powder body that particle diameter is 5nm～30nm, impregnates 24h～36h, obtains the powder body after preliminary pickling, be immersed in hydrochloric acid solution B by the powder body after preliminary pickling, impregnates 24h～36h, obtains the powder body after pickling；
Described hydrochloric acid solution A is volume ratio is (0.8～1.2): the hydrochloric acid of the mass fraction 30%～40% of 1 and the mixture of water；Described hydrochloric acid solution B is volume ratio is (0.8～1.2): the hydrochloric acid of the mass fraction 10%～15% of 1 and the mixture of water；
Four, washing: the distilled water of the powder body after pickling is washed, the powder body after being washed；
Five, the process of ultrasonic disperse and carbon fiber: the powder body after washing is joined in organic solvent, it is under 200W～300W at power, ultrasonic disperse 10min～20min, obtain the suspension after ultrasonic disperse, the suspension after ultrasonic disperse is stood 0.5h～1h, takes upper strata slurry, carbon fiber is added in the slurry of upper strata, it is under 200W～300W at power, ultrasonic disperse 10min～15min, the carbon fiber after being processed；
The quality of the described powder body after washing and the volume ratio of organic solvent are 1g:(80～100) mL；The mass ratio of described carbon fiber and upper strata slurry is 1:(4～6)；
Six, dry and vacuum drying oven processes: be placed in graphite crucible by the carbon fiber after processing, in the vacuum drying oven that temperature is 40 DEG C～60 DEG C, dry 20min～30min, obtain dried carbon fiber, will be equipped with the graphite crucible of dried carbon fiber again and be placed in vacuum drying oven, vacuum drying oven is evacuated to 10-2Pa～10-1Pa or be filled with 0.1 × 10 in vacuum drying oven by after vacuum drying oven evacuation5Pa～0.9 × 105The argon of Pa, then with programming rate for 10 DEG C/min～15 DEG C/min, by vacuum drying oven by room temperature to 1000 DEG C～1200 DEG C, and is insulation 1h～2h at 1000 DEG C～1200 DEG C in temperature, namely obtains being coated on the SiC nanowire of carbon fiber surface.
The invention has the beneficial effects as follows: observed with SEM, the present invention prepares the diameter of the SiC nanowire being coated on carbon fiber surface between 10nm～50nm, and length can reach less than 100 microns.The inventive method is simple and practical, and efficiency is high, and low for equipment requirements, raw material and preparation cost are low.Conversion ratio of the present invention is high, conversion ratio more than 80%, after reaction raw material almost without residual, the SiC nanowire obtained is pure, is coated on carbon fiber surface, does not contain the pollution of catalyst residue.
The present invention is used for a kind of preparation at carbon fiber surface coated Si/C nano wire.
Accompanying drawing explanation
Fig. 1 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that embodiment one prepares, and amplification is 10000；
Fig. 2 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that embodiment one prepares, and amplification is 100000；
Fig. 3 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that embodiment two prepares, and amplification is 10000；
Fig. 4 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that embodiment two prepares, and amplification is 100000.
Detailed description of the invention
Technical solution of the present invention is not limited to the detailed description of the invention of act set forth below, also includes the combination in any between each detailed description of the invention.
Detailed description of the invention one: a kind of preparation method at carbon fiber surface coated Si/C nano wire described in present embodiment, specifically carries out according to following steps:
One, mixing: Si powder is mixed homogeneously with graphite powder, obtains mixture；
The amount of substance of described Si powder and graphite powder is than for (0.8～1.2): 1；
Two, ball milling: be placed in by mixture in vacuum sphere grinding jar, is (15～20) in ball material mass ratio: the ratio of 1 puts into abrading-ball, and by vacuum sphere grinding jar evacuation, is then filled with 0.01 × 10 in vacuum sphere grinding jar5Pa～0.2 × 105The argon of Pa, when argon shield, with the speed ball milling 24h～48h of 430r/min～480r/min, obtains the powder body that particle diameter is 5nm～30nm；
Described purity of argon is more than 99.99%；
Three, pickling: be immersed in hydrochloric acid solution A by the powder body that particle diameter is 5nm～30nm, impregnates 24h～36h, obtains the powder body after preliminary pickling, be immersed in hydrochloric acid solution B by the powder body after preliminary pickling, impregnates 24h～36h, obtains the powder body after pickling；
Described hydrochloric acid solution A is volume ratio is (0.8～1.2): the hydrochloric acid of the mass fraction 30%～40% of 1 and the mixture of water；Described hydrochloric acid solution B is volume ratio is (0.8～1.2): the hydrochloric acid of the mass fraction 10%～15% of 1 and the mixture of water；
Four, washing: the distilled water of the powder body after pickling is washed, the powder body after being washed；
Five, the process of ultrasonic disperse and carbon fiber: the powder body after washing is joined in organic solvent, it is under 200W～300W at power, ultrasonic disperse 10min～20min, obtain the suspension after ultrasonic disperse, the suspension after ultrasonic disperse is stood 0.5h～1h, takes upper strata slurry, carbon fiber is added in the slurry of upper strata, it is under 200W～300W at power, ultrasonic disperse 10min～15min, the carbon fiber after being processed；
The quality of the described powder body after washing and the volume ratio of organic solvent are 1g:(80～100) mL；The mass ratio of described carbon fiber and upper strata slurry is 1:(4～6)；
Six, dry and vacuum drying oven processes: be placed in graphite crucible by the carbon fiber after processing, in the vacuum drying oven that temperature is 40 DEG C～60 DEG C, dry 20min～30min, obtain dried carbon fiber, will be equipped with the graphite crucible of dried carbon fiber again and be placed in vacuum drying oven, vacuum drying oven is evacuated to 10-2Pa～10-1Pa or be filled with 0.1 × 10 in vacuum drying oven by after vacuum drying oven evacuation5Pa～0.9 × 105The argon of Pa, then with programming rate for 10 DEG C/min～15 DEG C/min, by vacuum drying oven by room temperature to 1000 DEG C～1200 DEG C, and is insulation 1h～2h at 1000 DEG C～1200 DEG C in temperature, namely obtains being coated on the SiC nanowire of carbon fiber surface.
The ratio that ball material mass ratio is the mill ball quality gross mass with Si powder and graphite powder described in present embodiment step 2.
Present embodiment provides the benefit that: observed with SEM, and present embodiment prepares the diameter of the SiC nanowire being coated on carbon fiber surface between 10nm～50nm, and length can reach less than 100 microns.Present embodiment method simple practical, efficiency is high, and low for equipment requirements, raw material and preparation cost are low.Conversion ratio of the present invention is high, conversion ratio more than 80%, after reaction raw material almost without residual, the SiC nanowire obtained is pure, is coated on carbon fiber surface, does not contain the pollution of catalyst residue.
Detailed description of the invention two: present embodiment and detailed description of the invention one are the difference is that the amount of substance ratio of: the Si powder described in step one and graphite powder is for 1:1.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two the difference is that: the Si powder purity described in step one is 99.99%.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three the difference is that: the hydrochloric acid solution A described in step 3 is volume ratio is the mixture of the hydrochloric acid of mass fraction 30%～40% of 1:1 and water；Hydrochloric acid solution B described in step 3 is volume ratio is the mixture of the hydrochloric acid of mass fraction 10%～15% of 1:1 and water.Other is identical with detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four the difference is that: the powder body that particle diameter is 5nm～30nm is immersed in hydrochloric acid solution A by step 3, dipping 24h, obtain the powder body after preliminary pickling, powder body after preliminary pickling is immersed in hydrochloric acid solution B, dipping 24h, obtains the powder body after pickling.Other is identical with detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five the difference is that: the organic solvent described in step 5 is ethanol, acetone or isopropanol.Other is identical with detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are 1:5 the difference is that the mass ratio of: the carbon fiber described in step 5 with upper strata slurry.Other is identical with detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven the difference is that: with programming rate for 10 DEG C/min in step 6, by vacuum drying oven by room temperature to 1000 DEG C.Other is identical with detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight the difference is that: with programming rate for 15 DEG C/min in step 6, by vacuum drying oven by room temperature to 1200 DEG C.Other is identical with detailed description of the invention one to eight.
Adopt following example checking beneficial effects of the present invention:
Embodiment one:
A kind of preparation method at carbon fiber surface coated Si/C nano wire described in the present embodiment, specifically carries out according to following steps:
One, mixing: Si powder is mixed homogeneously with graphite powder, obtains mixture；
The amount of substance of described Si powder and graphite powder is than for 1:1；
Two, ball milling: be placed in by mixture in vacuum sphere grinding jar, puts into abrading-ball in the ratio that ball material mass ratio is 20:1, and by vacuum sphere grinding jar evacuation, is then filled with 0.5 × 10 in vacuum sphere grinding jar5The argon of Pa, when argon shield, with the speed ball milling 36h of 480r/min, obtains the powder body that particle diameter is 5nm～30nm；
Described purity of argon is more than 99.99%；
Three, pickling: be immersed in hydrochloric acid solution A by the powder body that particle diameter is 5nm～30nm, impregnates 24h, obtains the powder body after preliminary pickling, be immersed in hydrochloric acid solution B by the powder body after preliminary pickling, impregnates 24h, obtains the powder body after pickling；
Described hydrochloric acid solution A is volume ratio is the mixture of the hydrochloric acid of mass fraction 37% of 1:1 and water；Described hydrochloric acid solution B is volume ratio is the mixture of the hydrochloric acid of mass fraction 10% of 1:1 and water；
Four, washing: the distilled water of the powder body after pickling is washed, the powder body after being washed；
Five, the process of ultrasonic disperse and carbon fiber: the powder body after washing is joined in ethanol, it is under 200W at power, ultrasonic disperse 10min, obtain the suspension after ultrasonic disperse, the suspension after ultrasonic disperse is stood 1h, takes upper strata slurry, carbon fiber is added in the slurry of upper strata, it is under 200W at power, ultrasonic disperse 10min, the carbon fiber after being processed；
The quality of the described powder body after washing and the volume ratio of organic solvent are 1g:100mL；The mass ratio of described carbon fiber and upper strata slurry is 1:6；
Six, dry and vacuum drying oven processes: be placed in graphite crucible by the carbon fiber after processing, in the vacuum drying oven that temperature is 60 DEG C, dry 30min, obtain dried carbon fiber, will be equipped with the graphite crucible of dried carbon fiber again and be placed in vacuum drying oven, in vacuum drying oven, be filled with 0.9 × 10 by after vacuum drying oven evacuation5The argon of Pa, then with programming rate for 15 DEG C/min, by vacuum drying oven by room temperature to 1200 DEG C, and temperature be at 1200 DEG C under be incubated 1h, namely obtain being coated on the SiC nanowire of carbon fiber surface.
Fig. 1 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that the present embodiment prepares, and amplification is 10000；Fig. 2 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that the present embodiment prepares, and amplification is 100000；As seen from the figure, nano wire uniform fold is at carbon fiber surface, and diameter is comparatively uniform, for 30nm～45nm.
By calculating, it is known that the present embodiment conversion ratio is 85%.
By sem energy spectrum analysis, sample is without impurity such as Fe, Ni, it is known that prepared by the present embodiment is coated on the SiC nanowire purity height of carbon fiber surface.
Embodiment two: the present embodiment and embodiment one the difference is that: the suspension after ultrasonic disperse is stood 0.5h by step 5.Other is identical with detailed description of the invention one.
Fig. 3 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that the present embodiment prepares, and amplification is 10000；Fig. 4 is the SEM photograph of the SiC nanowire being coated on carbon fiber surface that the present embodiment prepares, and amplification is 100000；As seen from the figure, more nano wire covers carbon fiber surface, but carbon fiber surface has a small amount of granule, and the nanowire diameter uniformity is not as embodiment one.
By calculating, it is known that the present embodiment conversion ratio 80%.
By sem energy spectrum analysis, sample is without impurity such as Fe, Ni, it is known that prepared by the present embodiment is coated on the SiC nanowire purity height of carbon fiber surface.
Claims (1)
1. the preparation method at carbon fiber surface coated Si/C nano wire, it is characterised in that a kind of preparation method at carbon fiber surface coated Si/C nano wire carries out according to following steps:
One, mixing: Si powder is mixed homogeneously with graphite powder, obtains mixture；
The amount of substance of described Si powder and graphite powder is than for 1:1；
Two, ball milling: be placed in by mixture in vacuum sphere grinding jar, puts into abrading-ball in the ratio that ball material mass ratio is 20:1, and by vacuum sphere grinding jar evacuation, is then filled with 0.5 × 10 in vacuum sphere grinding jar5The argon of Pa, when argon shield, with the speed ball milling 36h of 480r/min, obtains the powder body that particle diameter is 5nm～30nm；
Described purity of argon is more than 99.99%；
Three, pickling: be immersed in hydrochloric acid solution A by the powder body that particle diameter is 5nm～30nm, impregnates 24h, obtains the powder body after preliminary pickling, be immersed in hydrochloric acid solution B by the powder body after preliminary pickling, impregnates 24h, obtains the powder body after pickling；
Described hydrochloric acid solution A is volume ratio is the mixture of the hydrochloric acid of mass fraction 37% of 1:1 and water；Described hydrochloric acid solution B is volume ratio is the mixture of the hydrochloric acid of mass fraction 10% of 1:1 and water；
Four, washing: the distilled water of the powder body after pickling is washed, the powder body after being washed；
Five, the process of ultrasonic disperse and carbon fiber: the powder body after washing is joined in ethanol, it is under 200W at power, ultrasonic disperse 10min, obtain the suspension after ultrasonic disperse, the suspension after ultrasonic disperse is stood 1h, takes upper strata slurry, carbon fiber is added in the slurry of upper strata, it is under 200W at power, ultrasonic disperse 10min, the carbon fiber after being processed；
The quality of the described powder body after washing and the volume ratio of organic solvent are 1g:100mL；The mass ratio of described carbon fiber and upper strata slurry is 1:6；
Six, dry and vacuum drying oven processes: be placed in graphite crucible by the carbon fiber after processing, in the vacuum drying oven that temperature is 60 DEG C, dry 30min, obtain dried carbon fiber, will be equipped with the graphite crucible of dried carbon fiber again and be placed in vacuum drying oven, in vacuum drying oven, be filled with 0.9 × 10 by after vacuum drying oven evacuation5The argon of Pa, then with programming rate for 15 DEG C/min, by vacuum drying oven by room temperature to 1200 DEG C, and temperature be at 1200 DEG C under be incubated 1h, namely obtain being coated on the SiC nanowire of carbon fiber surface.
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| CN112028075B (en) * | 2020-09-03 | 2021-12-21 | 天能帅福得能源股份有限公司 | Preparation method of nano SiC used as lithium ion battery cathode material and lithium ion battery prepared by using cathode material |
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| CN100497804C (en) * | 2006-12-29 | 2009-06-10 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| CN100488873C (en) * | 2007-04-05 | 2009-05-20 | 哈尔滨工业大学 | Method for preparing one dimension SiC Nano fiber |
| CN101104515B (en) * | 2007-08-24 | 2012-02-15 | 哈尔滨工业大学 | Preparing method of SiC nano-wire |
| CN101560728A (en) * | 2009-05-07 | 2009-10-21 | 浙江理工大学 | Method for generating silicon carbide coating on surface of carbon fiber |
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