CN103088648A - Preparation method for carbon fiber material with composite nano structure - Google Patents
Preparation method for carbon fiber material with composite nano structure Download PDFInfo
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Abstract
The invention relates to a preparation method for a carbon fiber material with a composite nano structure. The preparation method comprises the following steps of: pretreating carbon fiber cloth, adhering a layer of thin iron film catalyst on the carbon fiber cloth by a liquid-phase method or a physical deposition method, in a chemical gas-phase reaction chamber, carrying out in-situ growth of carbon nanotubes on the carbon fiber cloth by using argon or nitrogen as a carrier gas, ethylene or acetylene gas as a carbon source gas, and hydrogen as a reducing gas, then carrying a gas containing titanium organism into the chemical gas-phase deposition reaction chamber through the carrier gas, growing titanium dioxide at the peripheries of the carbon nanotubes to form titanium dioxide nanoshells which wrap the carbon nanotubes, thus obtaining the carbon fiber material with the composite nano structure. The carbon fiber material obtained by the preparation method has the advantages of high mechanical strength, high thermal stability, good chemical inertness and high adsorption property, supernormal strength of carbon nanotubes, large length-diameter ratio, high thermal conductivity, good catalytic activity, high chemical stability, non-toxicity and super-hydrophilicity. The carbon fiber material with the composite nano structure can have important applications in photocatalysis, electrocatalysis and other aspects.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of composite nanostructure carbon fibre material.
Background technology
Carbon fiber is through carbonization and graphitization processing and the micro crystal graphite material that obtains by organic fiber.Carbon fiber has excellent mechanical property, and its proportion is less than 1/4 of steel, and carbon fiber resin composite material tensile strength is 7-9 times of steel, and tensile modulus of elasticity is also higher than steel.Carbon fiber also has unique chemical property, and it is phosphorus content higher than 90% inorganic polymer fiber, and its fatigue durability is good, specific heat and electric conductivity are between nonmetal and metal, and thermal coefficient of expansion is little, good corrosion resistance, the density of fiber is low, and the X ray permeability is good, and chemical stability is strong.So carbon fibre material as protective materials, radiation resistance material, aviation and wide and electrode material, is widely used at present.
CNT is as monodimension nanometer material, and is lightweight, has many abnormal mechanics, calorifics, electricity and chemical property.CNT is because have huge specific surface, and its surperficial rejected region is with numerous active groups, so CNT is also in order to make the composite of a lot of excellent performances.
Titanium dioxide nano material is the best catalysis material of present performance, has high catalytic activity, high stability.Simultaneously the nano titania material is also showing great application prospect aspect fuel cell and photochemistry decomposition water, provides engineering feasibility for the green energy resource in future solves.
But the nano combined mode of carbon current fibrous material and carbon all divided for two steps completed, and namely first grew CNT, then carbon nanotube dispersed was obtained the dispersion liquid of CNT in the solution, utilized the carbon nano tube dispersion liquid after disperseing compound with carbon fiber again.This preparation carbon fiber/carbon nano tube compound material preparation method's shortcoming is: (1) carbon nanotube dispersed is undesirable, is difficult to form single the dispersion, so the excellent properties of compound rear CNT itself is not reflected; (2) CNT is first to grow rear compoundly, is not that growth in situ is on carbon fiber, so combination both is more weak, so the CNT after compound is easy to break away from carbon fiber.
Prepare the shortcoming of carbon fiber/carbon nano tube compound material in order to overcome existing two step method, the invention provides a kind of method that in situ synthesis prepares the composite nanostructure carbon fibre material.
Summary of the invention
the object of the invention is, a kind of preparation method of composite nanostructure carbon fibre material is provided, the method realizes by in-situ growing carbon nano tube on carbon cloth and nano titanium oxide, carbon cloth is first passed through preliminary treatment, then adhere to one deck iron thin film catalyst by liquid phase method or physical deposition method on carbon cloth, with load the carbon cloth of catalyst put the chemical gas phase reaction chamber into, do carrier gas with argon gas or nitrogen, make carbon-source gas with ethene or acetylene gas, hydrogen is made reducing gas, in-situ growing carbon nano tube on carbon cloth, to contain the organic gas of titanium is brought in chemical vapor deposition reaction chamber by carrier gas again, at the peripheral growth of CNT titanium dioxide, formation is coated on the nano titania shell on CNT, obtain the composite nanostructure carbon fibre material, the high mechanical properties that possesses carbon fiber by the material of method acquisition of the present invention, the high heat stability performance, good chemical inertness and high absorption property, possesses simultaneously the extraordinary intensity of CNT, huge draw ratio, high thermal conductivity, good catalytic activity, possesses again the high chemical stability of nano titanium oxide, avirulence, Superhydrophilic, excellent photocatalysis performance.Therefore this composite nanostructure carbon fibre material can obtain important application at aspects such as photocatalysis, electro-catalysis.
The preparation method of a kind of composite nanostructure carbon fibre material of the present invention follows these steps to carry out:
A, carbon cloth carry out preliminary treatment: carbon cloth is put in the sodium carbonate liquor that concentration is 20-40g/L, temperature is 60 ℃, ultrasonic wave is auxiliary to be cleaned 30 minutes, use washed with de-ionized water, to put into carbon cloth in acetone soln again, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere, with 400 ℃ of heat treatments of carbon cloth temperature 30 minutes;
B, by liquid phase method, pretreated carbon cloth is put into the FeCl that concentration is 0.05-1.00mol/L
3Flood in solution, obtain adhering on carbon cloth one deck Fe catalyst, then at the indoor cleaned air that passes into of vapour deposition, the Fe catalyst heat treatment of adhering on to carbon cloth 450 ℃ of temperature 15 minutes, then temperature is warming up to 650-700 ℃, and the hydrogen that passes into flow and be 30-100sccm carries out reductase 12-8 minute;
Or pass through physical vaporous deposition, Fe take purity as 99.99% is as target, carbon cloth is passed through magnetron sputtering or hot vapor deposition, the thickness of the Fe film that adheres on carbon cloth is 0.5-8nm, to adhere to the carbon cloth of Fe catalyst and directly send into CVD chamber, heating rate with temperature 50 C/min is warming up to 600-700 ℃, and the hydrogen that then passes into flow and be 10-80sccm carries out reductase 12-8 minute;
C, the carbon cloth that liquid phase method or physical vaporous deposition obtain that passes through in step b is passed through chemical gas-phase method, do carrier gas with argon gas or nitrogen, make carbon-source gas with ethene or acetylene gas, hydrogen is made reducing gas, reaction temperature is 600-700 ℃, and the time is 1-30 minute in-situ growing carbon nano tube on carbon cloth;
D, pass through chemical gas-phase method, first doing carrier gas with argon gas or nitrogen rinses phase depositing reaction chamber, gas flow is 300-600sccm, washing time is 5-8 minute, do carrier gas with argon gas or nitrogen again, make titanium source gas with tetraisopropoxy titanium steam, reaction temperature is 300-720 ℃, time is 5-30 minute growth nano titania shell outside CNT, can obtain the composite nanostructure carbon fibre material.
In step c, to make the flow of carrier gas be 50-500sccm for argon gas or nitrogen, and the flow that ethene or acetylene gas are made carbon-source gas is 20-200sccm, and the flow that hydrogen is made reducing gas is 5-50 sccm.
In steps d, to make the flow of carrier gas be 50-300sccm for argon gas or nitrogen, and the flow that tetraisopropoxy titanium steam is made titanium source gas is 10-250sccm.
the preparation method of a kind of composite nanostructure carbon fibre material of the present invention, the advantage of the method is, CNT and nano titanium oxide are all realized compound by growth in situ, do not connect by physical absorption, large common surface between CNT and carbon fiber, in conjunction with tight, nano titania shell in CNT outside growth, titanium dioxide wherein from the ratio of institutional framework single crystal titanium dioxide point greater than 95%, only having a little is unbodied and titanium dioxide polycrystalline, in single crystal titanium dioxide, the shared ratio of anatase structured titanium dioxide is greater than 90%, so farthest kept the advantage of material itself separately, allow the composite nanostructure carbon fibre material that finally obtains be the best performance.
The specific embodiment
Below in conjunction with the specific embodiment, the method that the present invention prepares the composite nanostructure carbon fibre material is described in further detail, but the present invention is not only limited to the embodiment that provides.
Embodiment 1
A, carbon cloth is carried out preliminary treatment: the twin shaft of 100 * 100mm is put in the sodium carbonate liquor that concentration is 30g/L to carbon cloth, be 60 ℃ by heating by electric cooker to solution temperature, ultrasonic wave is auxiliary to be cleaned 30 minutes, with washed with de-ionized water 2 times, carbon cloth is put in acetone soln, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere again, carbon cloth is put in the tube furnace of both ends open 400 ℃ of heat treatments of temperature 30 minutes;
B, by liquid phase method, pretreated carbon cloth is put into the FeCl that concentration is 0.4 mol/L
3Flood in solution, obtain adhering on carbon cloth one deck Fe catalyst, then pass into cleaned air in CVD chamber, the Fe catalyst heat treatment of adhering on to carbon cloth 450 ℃ of temperature 15 minutes, then temperature is warming up to 650 ℃, and the hydrogen that passes into flow and be 60sccm reduced 5 minutes;
C, the carbon cloth that obtains by liquid phase method in step b is passed through chemical gas-phase method, flow with argon gas is that 100sccm does carrier gas, flow with acetylene is that 50sccm gas is made carbon-source gas, the flow of hydrogen is that 25sccm makes reducing gas, reaction temperature is 600 ℃, and the time is 12 minutes in-situ growing carbon nano tubes on carbon cloth;
d, pass through chemical gas-phase method, first doing carrier gas with argon gas rinses phase depositing reaction chamber, gas flow is 600sccm, washing time is 5 minutes, purpose is other gas of getting rid of in reative cell, for growth of nano titanium dioxide provides clean environment, flow with argon gas is that 120sccm does carrier gas again, be that 18sccm makes titanium source gas with the flow of tetraisopropoxy titanium steam, reaction temperature is 480 ℃, time is 16 minutes, at CNT outside growth nano titania shell, can obtain the composite nanostructure carbon fibre material, the length average out to 750 μ m of CNT wherein, the thickness average out to 8nm of the nano titanium oxide shell of CNT periphery, anatase structured for monocrystalline.
Embodiment 2
A, carbon cloth is carried out preliminary treatment: the three axial carbon fibres cloth of 120 * 120mm are put in the sodium carbonate liquor that concentration is 20g/L, are 60 ℃ by heating by electric cooker to solution temperature, and ultrasonic wave is auxiliary to be cleaned 30 minutes, with washed with de-ionized water 2 times; Carbon cloth is put in acetone soln, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere, carbon cloth was put in the tube furnace of both ends open 400 ℃ of heat treatments of temperature 30 minutes again;
B, pass through physical vaporous deposition, Fe take purity as 99.99% is as target, with carbon cloth by hot vapor deposition, the thickness of the Fe film that adheres on carbon cloth is 5nm, to adhere to the carbon cloth of Fe catalyst and directly send into CVD chamber, heating rate with temperature 50 C/min is warming up to 680 ℃, and the hydrogen that then passes into flow and be 80sccm carries out reductase 12 minute;
C, the carbon cloth that obtains by physical vaporous deposition in step b is passed through chemical gas-phase method, flow with nitrogen is that 200sccm does carrier gas, flow with ethylene gas is that 120sccm makes carbon-source gas, the flow of hydrogen is that 50sccm makes reducing gas, reaction temperature is 700 ℃, time is 15 minutes, in-situ growing carbon nano tube on carbon cloth;
d, pass through chemical gas-phase method, first doing carrier gas with nitrogen rinses phase depositing reaction chamber, gas flow is 300sccm, washing time is 8 minutes, purpose is other gas of getting rid of in reative cell, for growth of nano titanium dioxide provides clean environment, flow with nitrogen is that 200sccm does carrier gas again, be that 50sccm makes titanium source gas with the flow of tetraisopropoxy titanium steam, reaction temperature is 430 ℃, time is 12 minutes growth nano titania shells outside CNT, can obtain the composite nanostructure carbon fibre material, the length average out to 720 μ m of CNT wherein, the thickness average out to 5nm of the nano titanium oxide shell of CNT periphery, anatase structured for monocrystalline.
Embodiment 3
A, carbon cloth is carried out preliminary treatment: the twin shaft of 100 * 100 mm is put in the sodium carbonate liquor that concentration is 40g/L to carbon cloth, solution temperature is 60 ℃, ultrasonic wave is auxiliary to be cleaned 30 minutes, with washed with de-ionized water 2 times, carbon cloth is put in acetone soln, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere again, carbon cloth is put in the tube furnace of both ends open 400 ℃ of heat treatments of temperature 30 minutes;
B, pass through physical vaporous deposition, Fe take purity as 99.99% is as target, carbon cloth is passed through magnetron sputtering deposition, the thickness of the Fe film that adheres on carbon cloth is 0.5 nm, to adhere to the carbon cloth of Fe catalyst and directly send into CVD chamber, heating rate with temperature 50 C/min is warming up to 600 ℃, and the hydrogen that then passes into flow and be 10 sccm carries out reductase 12 minute;
C, the carbon cloth that obtains by physical vaporous deposition in step b is passed through chemical gas-phase method, flow with nitrogen is that 50sccm does carrier gas, flow with ethylene gas is that 20sccm makes carbon-source gas, the flow of hydrogen is that 5sccm makes reducing gas, reaction temperature is 600 ℃, and the time is 1 minute in-situ growing carbon nano tube on carbon cloth;
d, pass through chemical gas-phase method, first doing carrier gas with argon gas rinses phase depositing reaction chamber, gas flow is 600sccm, washing time is 6 minutes, purpose is other gas of getting rid of in reative cell, for growth of nano titanium dioxide provides clean environment, flow with nitrogen is that 50sccm does carrier gas, be that 10 sccm make titanium source gas with the flow of tetraisopropoxy titanium steam, reaction temperature is 300 ℃, time is 5 minutes growth nano titania shells outside CNT, can obtain the composite nanostructure carbon fibre material, the length average out to 50 μ m of CNT wherein, the thickness average out to 6nm of the nano titanium oxide shell of CNT periphery, anatase structured for monocrystalline.
Embodiment 4
A, carbon cloth is carried out preliminary treatment: the three axial carbon fibres cloth of 120 * 120 mm are put into carbon cloth in the sodium carbonate liquor that concentration is 35g/L, solution temperature is 60 ℃, ultrasonic wave is auxiliary to be cleaned 30 minutes, use washed with de-ionized water, to put into carbon cloth in acetone soln, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere again, carbon cloth is put in the tube furnace of both ends open 400 ℃ of heat treatments of temperature 30 minutes;
B, by liquid phase method, pretreated carbon cloth is put into the FeCl that concentration is 1.00 mol/L
3Flood in solution, obtain adhering on carbon cloth one deck Fe catalyst, then at the indoor cleaned air that passes into of vapour deposition, the Fe catalyst heat treatment of adhering on to carbon cloth 450 ℃ of temperature 15 minutes, then temperature is warming up to 700 ℃, and the hydrogen that passes into flow and be 100sccm reduced 8 minutes;
C, the carbon cloth that obtains by liquid phase method in step b is passed through chemical gas-phase method, flow with argon gas is that 500sccm does carrier gas, flow with ethylene gas is that 200 sccm make carbon-source gas, the flow of hydrogen is that 50sccm makes reducing gas, reaction temperature is 700 ℃, and the time is 30 minutes in-situ growing carbon nano tubes on carbon cloth;
d, pass through chemical gas-phase method, first doing carrier gas with argon gas rinses phase depositing reaction chamber, gas flow is 600 sccm, washing time is 7 minutes, purpose is other gas of getting rid of in reative cell, for growth of nano titanium dioxide provides clean environment, flow with argon gas is that 300 sccm do carrier gas, make titanium source gas with flow 250 sccm of tetraisopropoxy titanium steam, reaction temperature is 720 ℃, time is 30 minutes growth nano titania shells outside CNT, can obtain the composite nanostructure carbon fibre material, the length average out to 920 μ m of CNT wherein, the thickness average out to 25nm of the nano titanium oxide shell of CNT periphery, anatase structured for monocrystalline.
Claims (3)
1. the preparation method of a composite nanostructure carbon fibre material is characterized in that following these steps to carrying out:
A, carbon cloth carry out preliminary treatment: carbon cloth is put in the sodium carbonate liquor that concentration is 20-40g/L, temperature is 60 ℃, ultrasonic wave is auxiliary to be cleaned 30 minutes, use washed with de-ionized water, to put into carbon cloth in acetone soln again, ultrasonic wave is auxiliary to be cleaned 20 minutes, then in air atmosphere, with 400 ℃ of heat treatments of carbon cloth temperature 30 minutes;
B, by liquid phase method, pretreated carbon cloth is put into the FeCl that concentration is 0.05-1.00mol/L
3Flood in solution, obtain adhering on carbon cloth one deck Fe catalyst, then at the indoor cleaned air that passes into of vapour deposition, the Fe catalyst heat treatment of adhering on to carbon cloth 450 ℃ of temperature 15 minutes, then temperature is warming up to 650-700 ℃, and the hydrogen that passes into flow and be 30-100sccm carries out reductase 12-8 minute;
Or pass through physical vaporous deposition, Fe take purity as 99.99% is as target, carbon cloth is passed through magnetron sputtering or hot vapor deposition, the thickness of the Fe film that adheres on carbon cloth is 0.5-8nm, to adhere to the carbon cloth of Fe catalyst and directly send into CVD chamber, heating rate with temperature 50 C/min is warming up to 600-700 ℃, and the hydrogen that then passes into flow and be 10-80sccm carries out reductase 12-8 minute;
C, the carbon cloth that liquid phase method or physical vaporous deposition obtain that passes through in step b is passed through chemical gas-phase method, do carrier gas with argon gas or nitrogen, make carbon-source gas with ethene or acetylene gas, hydrogen is made reducing gas, reaction temperature is 600-700 ℃, and the time is 1-30 minute in-situ growing carbon nano tube on carbon cloth;
D, pass through chemical gas-phase method, first doing carrier gas with argon gas or nitrogen rinses phase depositing reaction chamber, gas flow is 300-600sccm, washing time is 5-8 minute, do carrier gas with argon gas or nitrogen again, make titanium source gas with tetraisopropoxy titanium steam, reaction temperature is 300-720 ℃, time is 5-30 minute growth nano titania shell outside CNT, can obtain the composite nanostructure carbon fibre material.
2. method according to claim 1 is characterized in that it is 50-500sccm that argon gas in step c or nitrogen are made the flow of carrier gas, and the flow that ethene or acetylene gas are made carbon-source gas is 20-200 sccm, and the flow that hydrogen is made reducing gas is 5-50sccm.
3. method according to claim 1 is characterized in that it is 50-300sccm that argon gas in steps d or nitrogen are made the flow of carrier gas, and the flow that tetraisopropoxy titanium steam is made titanium source gas is 10-250 sccm.
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| CN104862948A (en) * | 2015-04-28 | 2015-08-26 | 武汉纺织大学 | Production method of color carbon fibers |
| CN105107509A (en) * | 2015-09-08 | 2015-12-02 | 徐金富 | Flexible loading type carbon fiber loaded CoB catalyst and preparation method thereof |
| CN108360250A (en) * | 2018-02-05 | 2018-08-03 | 天津大学 | A kind of preparation method of carbon nano-tube in situ modified carbon fiber reinforced resin based structures-damp composite material |
| CN108625159A (en) * | 2017-03-24 | 2018-10-09 | 山东大学 | Device and method for carbon cloth surface homoepitaxial carbon nanotube |
| CN109092245A (en) * | 2018-08-24 | 2018-12-28 | 华南理工大学 | A kind of tripolite loading carbon nanotube adsorption agent and preparation method thereof |
| CN111389365A (en) * | 2020-04-16 | 2020-07-10 | 郑州大学 | Carbon nanotube/titanium dioxide composite film and preparation method and application thereof |
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| CN109092245B (en) * | 2018-08-24 | 2020-12-22 | 华南理工大学 | Diatomite-loaded carbon nanotube adsorbent and preparation method thereof |
| CN111389365A (en) * | 2020-04-16 | 2020-07-10 | 郑州大学 | Carbon nanotube/titanium dioxide composite film and preparation method and application thereof |
| CN111900423A (en) * | 2020-06-29 | 2020-11-06 | 华南理工大学 | Flexible air electrode, flexible metal-air battery and wearable electronic equipment |
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| CN103088648B (en) | 2015-01-07 |
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