CN103993475A - Preparation method for coating carbon fiber surface with SiC nanowire - Google Patents
Preparation method for coating carbon fiber surface with SiC nanowire Download PDFInfo
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- CN103993475A CN103993475A CN201410228144.2A CN201410228144A CN103993475A CN 103993475 A CN103993475 A CN 103993475A CN 201410228144 A CN201410228144 A CN 201410228144A CN 103993475 A CN103993475 A CN 103993475A
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Abstract
The invention discloses a preparation method for coating a carbon fiber surface with an SiC nanowire, relates to a method for preparing a SiC nanowire and aims at solving the problems that a conventional method for preparing a SiC nanowire is high in cost while the SiC nanowire is low in purity, and a preparation method for coating a carbon fiber surface with a SiC nanowire does not exist in the prior art. The method comprises the following steps: 1, mixing; 2, performing ball-milling; 3, performing acid pickling; 4, washing; 5, performing ultrasonic dispersion and carbon fiber treatment; and 6, drying and performing vacuum furnace treatment, thereby obtaining the SiC nanowire coating the carbon fiber surface. The prepared SiC nanowire coating the carbon fiber surface has the diameter of 10nm-50nm and can reach the length of 100 microns or below, the process is simple, a catalyst is not added in the reaction process, the method is low in cost, and the SiC nanowire is high in conversion rate and high in purity. The method is used for preparing the SiC nanowire coating the carbon fiber surface.
Description
Technical field
The present invention relates to the preparation method of SiC nano wire.
Background technology
Metal or ceramic nano cause people's very big interest in the preparation of carbon fiber surface clad structure, carborundum has excellent resistance to elevated temperatures, and the elasticity of silicon carbide nanometer line and intensity are all much higher than silicon carbide fibre or carborundum; Carborundum is also a kind of semi-conducting material simultaneously, and silicon carbide nanometer line or nanotube have huge potential using value at aspects such as nano structural material, functional material and photoelectric device, field-transmitting cathode electron source and High Density Integration electronic devices.
The preparation method of existing SiC nano wire has: masterplate method, chemical vapour deposition technique, arc discharge method, sol-gal process and carbothermic method etc.
In above-mentioned preparation method, masterplate method will be used CNT as masterplate, by SiO or Si, reacts with it preparation SiC nano wire, because CNT is expensive, thereby the preparation of SiC nano wire is restricted.The VLS mechanism that chemical vapour deposition technique is all used mostly, wherein have the participation of catalyst, catalyst is in liquid state, the predecessor of siliceous and carbon constantly enters catalyst by dissociating or reacting after generating target product on catalyst drop surface, separates out, grows into SiC nano wire in catalyst after supersaturation.Because catalyst is in liquid state, so the temperature of preparation is subject to the certain limitation of catalyst, the SiC nano wire of preparation all contains catalyst residue.Arc discharge method is to be anode by the SiC rod that contains Fe, and graphite is negative electrode, carries out arc discharge under low pressure, forms SiC nano wire 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 surface
2affect its purity and quality.The organic matter that the general employing of sol-gal process contains Si and C is raw material, forms collosol and gel, under reducing atmosphere, through high-temperature heat treatment, obtains SiC nano wire.The method shortcoming is easily to form and reunite, and dispersiveness and crystallization degree are poor.In carbothermic method, multiplex containing SiO
2raw material mix with the C of activation, under more than 1600 ℃ high temperature and inertia or reducibility gas, obtain SiC nano wire, the method preparation temperature is higher, and adopts Si and CCl
4gas is the carbothermic method of raw material, although can generate SiC nano wire under the low temperature of 700 ℃, generally needs 10h～48h, and need in autoclave, carry out.But the preparation method who how to obtain the SiC nano wire that is coated on carbon fiber surface have not been reported.
In sum, the preparation method of existing SiC nano wire makes cost high because cost of material is high, preparation condition is harsh etc., most methods need to be used catalyst to cause containing in product the impurity such as Fe, Ni, and prior art does not have the preparation method who adopts at carbon fiber surface coated Si/C nano wire.
Summary of the invention
There is the problem that cost is high and purity is low in the preparation method that the present invention will solve existing SiC nano wire, and prior art does not have the preparation method who adopts 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.
In a preparation method for carbon fiber surface coated Si/C nano wire, specifically according to following steps, carry out:
One, mix: Si powder is mixed with graphite powder, obtain mixture;
Described Si powder is (0.8～1.2) with the amount of substance of graphite powder ratio: 1;
Two, ball milling: mixture is placed in to vacuum sphere grinding jar, is (15～20) in ball material mass ratio: 1 ratio is put into abrading-ball, and vacuum sphere grinding jar is vacuumized, be then filled with 0.01 * 10 in vacuum sphere grinding jar
5pa～0.2 * 10
5the argon gas of Pa, under the condition of argon shield, the speed ball milling 24h～48h with 430r/min～480r/min, obtains the powder that particle diameter is 5nm～30nm;
Described purity of argon is more than 99.99%;
Three, pickling: the powder that is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h～36h, obtains the powder after preliminary pickling, and the powder after preliminary pickling is immersed in hydrochloric acid solution B, and dipping 24h～36h, obtains the powder after pickling;
Described hydrochloric acid solution A is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 30%～40% and the mixture of water; Described hydrochloric acid solution B is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 10%～15% and the mixture of water;
Four, washing: the powder after pickling is washed to the powder after being washed with distilled water;
Five, the processing of ultrasonic dispersion and carbon fiber: the powder after washing is joined in organic solvent, at power, be under 200W～300W, ultrasonic dispersion 10min～20min, obtain the turbid liquid after ultrasonic dispersion, by the standing 0.5h～1h of the turbid liquid after ultrasonic dispersion, get upper strata slurry, carbon fiber is added in the slurry of upper strata, at power, be under 200W～300W, ultrasonic dispersion 10min～15min, the carbon fiber after being processed;
The quality of the powder after described 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 is processed: the carbon fiber after processing is placed in to graphite crucible, in temperature is the vacuum drying chamber of 40 ℃～60 ℃, dry 20min～30min, obtain dried carbon fiber, again the graphite crucible that dried carbon fiber is housed is placed in to vacuum drying oven, vacuum drying oven is evacuated to 10
-2pa～10
-1pa or vacuum drying oven is vacuumized in backward vacuum drying oven and is filled with 0.1 * 10
5pa～0.9 * 10
5the argon gas of Pa, then take programming rate as 10 ℃/min～15 ℃/min, vacuum drying oven is warming up to 1000 ℃～1200 ℃ by room temperature, and is to be incubated 1h～2h at 1000 ℃～1200 ℃ in temperature, obtains being coated on the SiC nano wire of carbon fiber surface.
The invention has the beneficial effects as follows: with SEM, observe, the present invention makes the diameter of the SiC nano wire that is coated on carbon fiber surface between 10nm～50nm, and length can reach below 100 microns.The inventive method is simple and practical, and efficiency is high, low for equipment requirements, and raw material and preparation cost are low.Conversion ratio of the present invention is high, and conversion ratio is greater than 80%, the almost noresidue of raw material after reaction, and the SiC nano wire obtaining is pure, is coated on carbon fiber surface, does not contain the pollution of catalyst residue.
The present invention is for a kind of preparation at carbon fiber surface coated Si/C nano wire.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of embodiment mono-, and multiplication factor is 10000;
Fig. 2 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of embodiment mono-, and multiplication factor is 100000;
Fig. 3 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of embodiment bis-, and multiplication factor is 10000;
Fig. 4 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of embodiment bis-, and multiplication factor is 100000.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment 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, mix: Si powder is mixed with graphite powder, obtain mixture;
Described Si powder is (0.8～1.2) with the amount of substance of graphite powder ratio: 1;
Two, ball milling: mixture is placed in to vacuum sphere grinding jar, is (15～20) in ball material mass ratio: 1 ratio is put into abrading-ball, and vacuum sphere grinding jar is vacuumized, be then filled with 0.01 * 10 in vacuum sphere grinding jar
5pa～0.2 * 10
5the argon gas of Pa, under the condition of argon shield, the speed ball milling 24h～48h with 430r/min～480r/min, obtains the powder that particle diameter is 5nm～30nm;
Described purity of argon is more than 99.99%;
Three, pickling: the powder that is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h～36h, obtains the powder after preliminary pickling, and the powder after preliminary pickling is immersed in hydrochloric acid solution B, and dipping 24h～36h, obtains the powder after pickling;
Described hydrochloric acid solution A is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 30%～40% and the mixture of water; Described hydrochloric acid solution B is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 10%～15% and the mixture of water;
Four, washing: the powder after pickling is washed to the powder after being washed with distilled water;
Five, the processing of ultrasonic dispersion and carbon fiber: the powder after washing is joined in organic solvent, at power, be under 200W～300W, ultrasonic dispersion 10min～20min, obtain the turbid liquid after ultrasonic dispersion, by the standing 0.5h～1h of the turbid liquid after ultrasonic dispersion, get upper strata slurry, carbon fiber is added in the slurry of upper strata, at power, be under 200W～300W, ultrasonic dispersion 10min～15min, the carbon fiber after being processed;
The quality of the powder after described 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 is processed: the carbon fiber after processing is placed in to graphite crucible, in temperature is the vacuum drying chamber of 40 ℃～60 ℃, dry 20min～30min, obtain dried carbon fiber, again the graphite crucible that dried carbon fiber is housed is placed in to vacuum drying oven, vacuum drying oven is evacuated to 10
-2pa～10
-1pa or vacuum drying oven is vacuumized in backward vacuum drying oven and is filled with 0.1 * 10
5pa～0.9 * 10
5the argon gas of Pa, then take programming rate as 10 ℃/min～15 ℃/min, vacuum drying oven is warming up to 1000 ℃～1200 ℃ by room temperature, and is to be incubated 1h～2h at 1000 ℃～1200 ℃ in temperature, obtains being coated on the SiC nano wire of carbon fiber surface.
Ball material mass ratio described in present embodiment step 2 is mill ball quality and the ratio of the gross mass of Si powder and graphite powder.
The beneficial effect of present embodiment is: with SEM, observe, present embodiment makes the diameter of the SiC nano wire that is coated on carbon fiber surface between 10nm～50nm, and length can reach below 100 microns.Present embodiment method simple practical, efficiency is high, low for equipment requirements, and raw material and preparation cost are low.Conversion ratio of the present invention is high, and conversion ratio is greater than 80%, the almost noresidue of raw material after reaction, and the SiC nano wire obtaining is pure, is coated on carbon fiber surface, does not contain the pollution of catalyst residue.
The specific embodiment two: present embodiment is different from the specific embodiment one: the Si powder described in step 1 is 1:1 with the amount of substance ratio of graphite powder.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from one of the specific embodiment one or two: the Si powder purity described in step 1 is 99.99%.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three: the hydrochloric acid solution A described in step 3 is that volume ratio is the hydrochloric acid of mass fraction 30%～40% and the mixture of water of 1:1; Hydrochloric acid solution B described in step 3 is that volume ratio is the hydrochloric acid of mass fraction 10%～15% and the mixture of water of 1:1.Other is identical with the specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four: the powder that step 3 is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h, obtain the powder after preliminary pickling, powder after preliminary pickling is immersed in hydrochloric acid solution B, dipping 24h, obtains the powder after pickling.Other is identical with the specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five: the organic solvent described in step 5 is ethanol, acetone or isopropyl alcohol.Other is identical with the specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six: the mass ratio of the carbon fiber described in step 5 and upper strata slurry is 1:5.Other is identical with the specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven: take programming rate in step 6 as 10 ℃/min, vacuum drying oven is warming up to 1000 ℃ by room temperature.Other is identical with the specific embodiment one to seven.
The specific embodiment nine: present embodiment is different from one of specific embodiment one to eight: take programming rate in step 6 as 15 ℃/min, vacuum drying oven is warming up to 1200 ℃ by room temperature.Other is identical with the specific embodiment one to eight.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
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, mix: Si powder is mixed with graphite powder, obtain mixture;
Described Si powder is 1:1 with the amount of substance of graphite powder ratio;
Two, ball milling: mixture is placed in to vacuum sphere grinding jar, and the ratio that is 20:1 in ball material mass ratio is put into abrading-ball, and vacuum sphere grinding jar is vacuumized, and is then filled with 0.5 * 10 in vacuum sphere grinding jar
5the argon gas of Pa, under the condition of argon shield, the speed ball milling 36h with 480r/min, obtains the powder that particle diameter is 5nm～30nm;
Described purity of argon is more than 99.99%;
Three, pickling: the powder that is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h, obtains the powder after preliminary pickling, and the powder after preliminary pickling is immersed in hydrochloric acid solution B, and dipping 24h, obtains the powder after pickling;
Described hydrochloric acid solution A is that volume ratio is the hydrochloric acid of mass fraction 37% and the mixture of water of 1:1; Described hydrochloric acid solution B is that volume ratio is the hydrochloric acid of mass fraction 10% and the mixture of water of 1:1;
Four, washing: the powder after pickling is washed to the powder after being washed with distilled water;
Five, the processing of ultrasonic dispersion and carbon fiber: the powder after washing is joined in ethanol, at power, be under 200W, ultrasonic dispersion 10min, obtain the turbid liquid after ultrasonic dispersion, by the standing 1h of the turbid liquid after ultrasonic dispersion, get upper strata slurry, carbon fiber is added in the slurry of upper strata, at power, be under 200W, ultrasonic dispersion 10min, the carbon fiber after being processed;
The quality of the powder after described 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 is processed: the carbon fiber after processing is placed in to graphite crucible, in temperature is the vacuum drying chamber of 60 ℃, dry 30min, obtain dried carbon fiber, again the graphite crucible that dried carbon fiber is housed is placed in to vacuum drying oven, vacuum drying oven is vacuumized in backward vacuum drying oven and is filled with 0.9 * 10
5the argon gas of Pa, then take programming rate as 15 ℃/min, and vacuum drying oven is warming up to 1200 ℃ by room temperature, and is lower insulation 1h at 1200 ℃ in temperature, obtains being coated on the SiC nano wire of carbon fiber surface.
Fig. 1 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of the present embodiment, and multiplication factor is 10000; Fig. 2 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of the present embodiment, and multiplication factor is 100000; As seen from the figure, nano wire uniform fold is at carbon fiber surface, and diameter is comparatively even, is 30nm～45nm.
By calculating, known the present embodiment conversion ratio is 85%.
By sem energy spectrum analysis, sample is not containing impurity such as Fe, Ni, and the SiC nano wire purity that is coated on carbon fiber surface prepared by known the present embodiment is high.
Embodiment bis-: the present embodiment is different from embodiment mono-: in step 5 by the standing 0.5h of the turbid liquid after ultrasonic dispersion.Other is identical with the specific embodiment one.
Fig. 3 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of the present embodiment, and multiplication factor is 10000; Fig. 4 is the SEM photo of the SiC nano wire that is coated on carbon fiber surface that makes of the present embodiment, and multiplication factor is 100000; As seen from the figure, more nano wire covers carbon fiber surface, but carbon fiber surface has a small amount of particle, and the nanowire diameter uniformity is not as embodiment mono-.
By calculating, known the present embodiment conversion ratio 80%.
By sem energy spectrum analysis, sample is not containing impurity such as Fe, Ni, and the SiC nano wire purity that is coated on carbon fiber surface prepared by known the present embodiment is high.
Claims (9)
1. in a preparation method for carbon fiber surface coated Si/C nano wire, it is characterized in that a kind of preparation method at carbon fiber surface coated Si/C nano wire carries out according to following steps:
One, mix: Si powder is mixed with graphite powder, obtain mixture;
Described Si powder is (0.8～1.2) with the amount of substance of graphite powder ratio: 1;
Two, ball milling: mixture is placed in to vacuum sphere grinding jar, is (15～20) in ball material mass ratio: 1 ratio is put into abrading-ball, and vacuum sphere grinding jar is vacuumized, be then filled with 0.01 * 10 in vacuum sphere grinding jar
5pa～0.2 * 10
5the argon gas of Pa, under the condition of argon shield, the speed ball milling 24h～48h with 430r/min～480r/min, obtains the powder that particle diameter is 5nm～30nm;
Described purity of argon is more than 99.99%;
Three, pickling: the powder that is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h～36h, obtains the powder after preliminary pickling, and the powder after preliminary pickling is immersed in hydrochloric acid solution B, and dipping 24h～36h, obtains the powder after pickling;
Described hydrochloric acid solution A is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 30%～40% and the mixture of water; Described hydrochloric acid solution B is that volume ratio is (0.8～1.2): 1 the hydrochloric acid of mass fraction 10%～15% and the mixture of water;
Four, washing: the powder after pickling is washed to the powder after being washed with distilled water;
Five, the processing of ultrasonic dispersion and carbon fiber: the powder after washing is joined in organic solvent, at power, be under 200W～300W, ultrasonic dispersion 10min～20min, obtain the turbid liquid after ultrasonic dispersion, by the standing 0.5h～1h of the turbid liquid after ultrasonic dispersion, get upper strata slurry, carbon fiber is added in the slurry of upper strata, at power, be under 200W～300W, ultrasonic dispersion 10min～15min, the carbon fiber after being processed;
The quality of the powder after described 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 is processed: the carbon fiber after processing is placed in to graphite crucible, in temperature is the vacuum drying chamber of 40 ℃～60 ℃, dry 20min～30min, obtain dried carbon fiber, again the graphite crucible that dried carbon fiber is housed is placed in to vacuum drying oven, vacuum drying oven is evacuated to 10
-2pa～10
-1pa or vacuum drying oven is vacuumized in backward vacuum drying oven and is filled with 0.1 * 10
5pa～0.9 * 10
5the argon gas of Pa, then take programming rate as 10 ℃/min～15 ℃/min, vacuum drying oven is warming up to 1000 ℃～1200 ℃ by room temperature, and is to be incubated 1h～2h at 1000 ℃～1200 ℃ in temperature, obtains being coated on the SiC nano wire of carbon fiber surface.
2. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that the Si powder described in step 1 and the amount of substance ratio of graphite powder are 1:1.
3. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that the Si powder purity described in step 1 is 99.99%.
4. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that the hydrochloric acid solution A described in step 3 is that volume ratio is the hydrochloric acid of mass fraction 30%～40% and the mixture of water of 1:1; Hydrochloric acid solution B described in step 3 is that volume ratio is the hydrochloric acid of mass fraction 10%～15% and the mixture of water of 1:1.
5. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, it is characterized in that the powder that step 3 is 5nm～30nm by particle diameter is immersed in hydrochloric acid solution A, dipping 24h, obtain the powder after preliminary pickling, powder after preliminary pickling is immersed in hydrochloric acid solution B, dipping 24h, obtains the powder after pickling.
6. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that the organic solvent described in step 5 is ethanol, acetone or isopropyl alcohol.
7. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, the mass ratio that it is characterized in that the carbon fiber described in step 5 and upper strata slurry is 1:5.
8. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that take programming rate as 10 ℃/min in step 6, and vacuum drying oven is warming up to 1000 ℃ by room temperature.
9. a kind of preparation method at carbon fiber surface coated Si/C nano wire according to claim 1, is characterized in that take programming rate as 15 ℃/min in step 6, and vacuum drying oven is warming up to 1200 ℃ by room temperature.
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| CN112028075A (en) * | 2020-09-03 | 2020-12-04 | 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 |
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
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| CN112028075A (en) * | 2020-09-03 | 2020-12-04 | 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 |
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN112608156B (en) * | 2020-12-29 | 2021-12-03 | 内蒙古海特华材科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
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