CN102877367B - Carbon nanotube/short-fiber composited nano-carbon paper and continuous preparation method thereof - Google Patents
Carbon nanotube/short-fiber composited nano-carbon paper and continuous preparation method thereof Download PDFInfo
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- CN102877367B CN102877367B CN201210418509.9A CN201210418509A CN102877367B CN 102877367 B CN102877367 B CN 102877367B CN 201210418509 A CN201210418509 A CN 201210418509A CN 102877367 B CN102877367 B CN 102877367B
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Abstract
The invention provides a kind of carbon nanotube/short-fiber composited nano-carbon paper and a continuous preparation method thereof. The nano-carbon paper mainly comprises disordered carbon nanotubes and short fibers, and is in a non-woven form. The preparation method of the nano-carbon paper comprises the following steps that: the disordered carbon nanotubes are dispersed in a solvent so as to form a dispersion liquid; then, mixing and dispersing the short fibers so as to form a size; preparing an initial film through vacuum assisted flow-casting film-forming; and then, removing polymers in the initial film through subsequent processing so as to obtain a target product. The composited nano-carbon paper disclosed by the invention integrates the huge specific surface areas, superior conductivity and functional characteristics of the carbon nanotubes and the enhancement effect of the short fibers on the strength and flexibility of the carbon paper, therefore, the composited nano-carbon paper is good in self-supporting property and flexibility; meanwhile, through the direct film-forming implemented by using a flow-casting method, the continuous film-forming of the nano-carbon paper is realized, therefore, the nano-carbon paper has the advantages of high efficiency, rapidness and easy large-scale preparation. The composited nano-carbon paper disclosed by the invention has a wide application prospect in the fields of energy electrodes, catalytic carriers, environmental management, static resistance, electromagnetic shielding, wave-absorbing camouflage, and the like.
Description
Technical field
The present invention be more particularly directed to a kind of CNT/staple fibre composite nanometer carbon paper and continuous production method thereof, belong to nano-carbon material preparing technical field.
Background technology
Nanometer carbon paper is the nonwoven fabric form being made up of disordered carbon nanotube, it is the simplest macroscopic material form of CNT, there is the feature of lightweight, flexibility, conduction, heat conduction and huge specific area, combine the functional characteristic of CNT self excellence simultaneously, having important application prospect in fields such as electrode material, environmentally conscious materials, filtering material, catalytic carrier, electronic materials, is New Type of Carbon paper product after traditional carbon fibres paper, graphite paper.Because CNT size is at nanoscale, conventional carbon paper conversion technology of preparing all cannot be suitable for the preparation of nanometer carbon paper, in the urgent need to development of new nano-sized carbon paper technology of preparing.
The preparation method of nanometer carbon paper is mainly three classes at present, that is:
1) CVD deposition technique direct growth goes out nanometer carbon paper, by ceaselessly adding catalyst (ferrocene) and carbon source (alcohol, ester, ether etc.), can obtain carbon nano-tube film at the tube furnace other end continuously, can obtain the nanometer carbon paper of different-thickness by adjusting growth conditions as temperature, carbon source kind and concentration etc.;
2) the direct dry method press mold of carbon nano pipe array or membrane technology, it is mainly based on highly large or the special vertical carbon nanotube array of structure, the carbon nano pipe array of micron order height is directly overwhelmed in flakes and taken off to a direction, or use special can spinning array, from wherein pulling out the ordered carbon nanotube film of meter level length and being successively stacked, infiltrate with alcohol, can obtain large-area nanometer carbon paper;
3) wet-chemical filter method, the wet method water of the method based on carbon nanotube dust disperses and suction filtration, selects suitable pumping and filtering device can make the nanometer carbon paper of required form.
Wherein, first two method is subject to device-restrictive; preparation efficiency cannot improve always; seriously limit its large-scale production; and for the third method; although can realizing lower cost, it prepares nanometer carbon paper; but because CNT is seriously cut off in dispersion process; cause filtering acquisition nanometer carbon paper fragility large; be difficult to preparation large scale product, meanwhile, the CNT of nanoscale makes its efficiency in filter process very low; solve serialization and high efficiency preparation, be therefore also very difficult to realize.How to develop a kind of efficient technology of preparing and become a key core difficult problem prepared by solution nano-sized carbon lateral modelling.
Summary of the invention
The object of this invention is to provide a kind of CNT/staple fibre composite nanometer carbon paper and continuous production method thereof, the nonwoven fabric form that this composite nanometer carbon paper is made up of CNT and staple fibre, strengthen as strengthening toughness reinforcing skeleton using staple fibre, and keep CNT self functional characteristic, form and there is good flexible composite nanometer carbon paper.And adopt vacuum aided casting film-forming to realize serialization preparation, thereby overcome deficiency of the prior art.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of CNT/staple fibre composite nanometer carbon paper, it has and is mainly made up of disordered carbon nanotube and staple fibre, is the macroscopic form of nonwoven fabric construct,
And the thickness of described composite nanometer carbon paper is 0.5 μ m-5 mm, wherein the weight ratio of CNT and staple fibre is 100:1-1:1.
As one of comparatively preferred embodiment, described CNT is selected from any one or the two or more combinations in multi-walled carbon nano-tubes, double-walled carbon nano-tube and Single Walled Carbon Nanotube,
And the caliber of described CNT is 0.4 nm-150 nm, length is 200 nm-1 cm.
As one of comparatively preferred embodiment, the length of described staple fibre is 0.5 mm-10 mm, and diameter is 500 nm-50 μ m;
And described staple fibre is selected from any one or more combination in natural fabric and artificial fiber, described natural fabric comprises string, animal fiber and mineral fibres, and described chemical fibre comprises artificial fibre, synthetic fiber and inorfil.
A continuous production method for CNT/staple fibre composite nanometer carbon paper, comprising:
First, during being dispersed in to solvent under dispersant is auxiliary, CNT forms dispersion liquid;
, staple fibre slowly sneaked in dispersion liquid, and make staple fibre by fine dispersion through high speed shear, obtain slurry thereafter;
Then, utilize vacuum aided casting film-forming technique that slurry is processed and formed initial composite nanometer carbon paper, then remove the dispersant in initial composite nanometer carbon paper through post processing, obtain target product.
As one of embodiment preferably, described CNT forms dispersion liquid be dispersed in solvent under dispersant is auxiliary in, and described dispersant is at least selected from any one in polyvinyl alcohol, polyvinylpyrrolidone, cellulose, lauryl sodium sulfate, neopelex, softex kw, Tween-80, Qu Latong-100.
Further, in the method, carbon nanotube dispersed is formed to the technique of dispersion liquid in solvent and is selected from any one or the two or more combinations in high speed shear dispersions, ultrasonic dispersion, grinding distribution and ball milling dispersion,
And described solvent is at least selected from water, ethanol, isopropyl alcohol, N, any one in dinethylformamide, 1-METHYLPYRROLIDONE, ethyl acetate and chloroform.
As one of specific embodiments preferably, in described dispersion liquid, the concentration of institute's carbon nanotubes is 0.001-10wt%, and wherein the weight ratio of CNT and dispersant is 1:10-1:0.1.
As one of specific embodiments preferably, the method high speed is sheared and is disperseed the process conditions of staple fibre to comprise: mixing speed 1000-5000 rpm, jitter time 1-120 min.
Further, described vacuum aided casting film-forming technique comprises:
Porous filter plate is covered on the peristome of closed cavity, and slurry is continuously applied to the filter membrane passing through from porous filter plate continuously, accompany by simultaneously and utilize the operation that vacuum equipment vacuumizes aforementioned closed cavity and utilize scraper plate to carry out the operation of knifing to the slurry being distributed on filter membrane, make solid content uniform deposition in slurry on filter membrane, and form continuous initial composite nanometer carbon paper.
As one of specific embodiments preferably, in the method, be to select any method in eluent solvent and 300-400 DEG C of calcining to remove the dispersant in initial composite nanometer carbon paper.
Compared with prior art, advantage of the present invention is at least:
(1) CNT/staple fibre composite nanometer carbon paper has overcome the large deficiency of pure nanometer carbon paper fragility, toughness reinforcing as strengthening using staple fibre, forms and has good self-supporting and flexible full carbon nanometer carbon paper, and kept the functional characteristic of CNT;
(2) technique of employing vacuum aided casting film-forming, can realize the continuous film forming of nanometer carbon paper, and in the processes such as follow-up drip washing, remove polymer, obtains high quality nano carbon paper;
(3) to have technique simple in whole technological process, and the advantageous feature such as efficiency is high, and equipment requirement is low has greatly reduced the preparation processing cost of nanometer carbon paper, has boundless Commercial Prospect.
Brief description of the drawings
The structural representation of Fig. 1 vacuum aided casting film-forming device;
Fig. 2 a-2c is respectively the electron scanning micrograph of the prepared nanometer carbon paper of the embodiment of the present invention 1;
Fig. 3 a-3c is respectively the electron scanning micrograph of the prepared nanometer carbon paper of the embodiment of the present invention 2;
Fig. 4 a-4c is respectively the electron scanning micrograph of the prepared nanometer carbon paper of the embodiment of the present invention 3;
Fig. 5 a-5c is respectively the electron scanning micrograph of the prepared nanometer carbon paper of the embodiment of the present invention 4.
Detailed description of the invention
As an aspect of technical solution of the present invention, this CNT/staple fibre composite nanometer carbon paper has and is mainly made up of disordered carbon nanotube and staple fibre, be the macroscopic form of nonwoven fabric construct, its thickness is generally 0.5 μ m-5 mm, and wherein the weight ratio of CNT and staple fibre is 100:1-1:1.
Further, the caliber of aforementioned CNT is preferably 0.4 nm-150 nm, and length is preferably 200 nm-1 cm, can be any one or multiple combination in multi-walled carbon nano-tubes, double-walled carbon nano-tube and Single Walled Carbon Nanotube.
Further, the length of described staple fibre is preferably 0.5 mm-10 mm, diameter is preferably 500 nm-50 μ m, can be any one or any combination of the chemical fibres such as the natural fabrics such as string, animal fiber and mineral fibres and artificial fibre, synthetic fiber, inorfil.
As another aspect of technical solution of the present invention, the continuous production method of this CNT/staple fibre composite nanometer carbon paper comprises the following steps:
First, during being dispersed in to solvent under dispersant is auxiliary, CNT forms dispersion liquid;
Subsequently, in stirring at low speed, staple fibre is slowly sneaked in dispersion liquid, and high speed shear makes staple fibre by fine dispersion, obtain slurry;
Then, aforementioned slurry is formed to initial composite nanometer carbon paper by vacuum aided casting film-forming, through post processing, dispersant is removed and obtained composite nanometer carbon paper.
Further, the dispersing technology of aforementioned CNT can adopt any one in high speed shear dispersion, ultrasonic dispersion, grinding distribution and ball milling dispersion, but is not limited to this.
Aforementioned solvents can be water, ethanol, isopropyl alcohol, N, any one in dinethylformamide, 1-METHYLPYRROLIDONE, ethyl acetate and chloroform or multiple, but be not limited to this.
As one of optional embodiment, in described dispersion liquid, also contain dispersant, described dispersant optional in polyvinyl alcohol, polyvinylpyrrolidone, cellulose, lauryl sodium sulfate, neopelex, softex kw, Tween-80, Qu Latong-100 any one or multiple, but be not limited to this.
Further, in described dispersion liquid, the content of CNT is preferably 0.001-10wt%, and the weight ratio of CNT and dispersant is preferably 1:10-1:0.1.
Further, described high speed shear disperses the mixing speed of staple fibre to be preferably 1000-5000 rpm, and jitter time is preferably 1-120 min.
Further, described vacuum aided casting film-forming technology is a kind of continuous filtration film technique, on the basis of traditional casting machine, fine and close base plate is changed into porous filter plate, and assisted vacuum suction filtration, forms negative pressure partial solvent is separated.
Further, the method for described removal polymer can be in vacuum aided casting film-forming subsequent technique, to pass through eluent solvent, and polymer is removed in washing; Or directly adopt 300-400 DEG C of calcining by the method for organic matter burn off for CNT/inorganic staple fibre nanometer carbon paper.
Below in conjunction with accompanying drawing and some exemplary embodiments, technical scheme of the present invention is further described.
embodiment 1take 30 grams of multi-walled carbon nano-tubes, be dissolved in Qu Latong-100 aqueous solution that 1 liter of concentration is 1%, adopt subsequently grinder grinding distribution, rotating speed 3000 rpm dispersed with stirring 1 hour, obtains uniform carbon nano tube dispersion liquid (being called for short " dispersion liquid ") after 200 mesh filter screens sieve; In slowly stirring, adding 5 grams of length is the chopped carbon fiber of 3 mm, the weight ratio of CNT and carbon fiber is 6:1, disperses rotating speed 3000 rpm after mixing in high speed shear dispersion machine, disperse within 20 minutes, to form stable slurry, leave standstill de-bubble in 20 minutes and can carry out film forming processing afterwards.Thereafter, prepare the initial composite nanometer carbon paper of 70 microns of thickness by vacuum aided casting film-forming device,, carbon paper directly can be opened from filter membrane polymer eccysis through follow-up drip washing, be obtained CNT/carbon fiber composite nanometer carbon paper that full material with carbon element forms.Fig. 2 a-Fig. 2 c is depicted as the electron scanning micrograph of the obtained nanometer carbon paper of the present embodiment.
The structure of aforementioned vacuum aided casting film-forming device refers to Fig. 1, and it comprises continuous filter membrane feed unit 1, conveyer belt 2, porous filter plate 3, charging bucket 4, scraper 5, continuous barrier film feed unit 6, nanometer carbon paper collector unit 7, vacuum equipment 8 etc.Its operation principle is roughly: on the porous filter plate 3 being placed on an enclosed cavity, provide continuously filter membrane 9 by continuous filter membrane feed unit 1 and conveyer belt, and in enclosed cavity, form negative pressure by vacuum equipment 8, simultaneously, be continuously applied aforementioned dispersion liquid by charging bucket 4 to being laid on the filter membrane of porous filter plate 3, and utilize scraper 5 to carry out knifing processing, thereby on filter membrane, form composite nanometer carbon paper, the barrier film 10 that by continuous barrier film feed unit 6 provided be covered in composite nanometer carbon paper on, and collect with nanometer carbon paper collector unit 7 thereafter.
embodiment 2the present embodiment is substantially the same manner as Example 1, and its difference is, the weight ratio of CNT and carbon fiber is 8:1, and Fig. 3 a-Fig. 3 c is depicted as the electron scanning micrograph of the obtained nanometer carbon paper of the present embodiment.
embodiment 3the present embodiment is substantially the same manner as Example 1, and its difference is, the weight ratio of CNT and carbon fiber is 10:1, and Fig. 4 a-Fig. 4 c is depicted as the electron scanning micrograph of the obtained nanometer carbon paper of the present embodiment.
embodiment 4the present embodiment is substantially the same manner as Example 1, and its difference is, the weight ratio of CNT and carbon fiber is 15:1, and Fig. 5 a-Fig. 5 c is depicted as the electron scanning micrograph of the obtained nanometer carbon paper of the present embodiment.
More than explanation and on drawing shown in embodiment, can not resolve the design philosophy surely of the present invention that is limited.In technical field of the present invention, holding the identical the knowledgeable of knowing can change technical thought of the present invention with various form improvement, such improvement and change are interpreted as belonging in protection scope of the present invention.
Claims (6)
1. a continuous production method for CNT/staple fibre composite nanometer carbon paper, is characterized in that, it comprises:
First be, to form dispersion liquid during 0.4nm-150nm, the length CNT that is 200nm-1cm is dispersed in solvent under dispersant is auxiliary by caliber;
Thereafter, be that 0.5mm-10mm, diameter are that the short carbon fiber of 500nm-50 μ m is slowly sneaked in dispersion liquid by length, and make short carbon fiber by fine dispersion through high speed shear, and obtain slurry, in slurry, the weight ratio of CNT and short carbon fiber is 100:1-1:1;
Then, utilize vacuum aided casting film-forming technique that slurry is processed and formed initial composite nanometer carbon paper, then remove the dispersant in initial composite nanometer carbon paper through post processing, to obtain thickness be 0.5 μ m-5mm, be the macromorphologic target product of nonwoven fabric construct;
Wherein, described vacuum aided casting film-forming technique comprises: porous filter plate is covered on the peristome of closed cavity, and slurry is continuously applied to the filter membrane passing through from porous filter plate continuously, accompany by simultaneously and utilize the operation that vacuum equipment vacuumizes aforementioned closed cavity and utilize scraper plate to carry out the operation of knifing to the slurry being distributed on filter membrane, make solid content uniform deposition in slurry on filter membrane, and form continuous initial composite nanometer carbon paper.
2. the continuous production method of CNT/staple fibre composite nanometer carbon paper according to claim 1, it is characterized in that, described CNT forms dispersion liquid be dispersed in solvent under dispersant is auxiliary in, and described dispersant is selected from any one in polyvinyl alcohol, polyvinylpyrrolidone, cellulose, lauryl sodium sulfate, neopelex, softex kw, Tween-80, Qu Latong-100.
3. the continuous production method of CNT/staple fibre composite nanometer carbon paper according to claim 1 and 2, it is characterized in that, in the method, carbon nanotube dispersed is formed to the technique of dispersion liquid in solvent and be selected from any one or the two or more combinations in high speed shear dispersions, ultrasonic dispersion, grinding distribution and ball milling dispersion, and, described solvent is selected from any one in water, ethanol, isopropyl alcohol, DMF, 1-METHYLPYRROLIDONE, ethyl acetate and chloroform.
4. the continuous production method of CNT/staple fibre composite nanometer carbon paper according to claim 1, it is characterized in that, in described dispersion liquid, the concentration of institute's carbon nanotubes is 0.001-10wt%, and wherein the weight ratio of CNT and dispersant is 1:10-1:0.1.
5. the continuous production method of CNT/staple fibre composite nanometer carbon paper according to claim 1, is characterized in that, the method high speed is sheared and disperseed the process conditions of short carbon fiber to comprise: mixing speed 1000-5000rpm, jitter time 1-120min.
6. the continuous production method of CNT/staple fibre composite nanometer carbon paper according to claim 1, is characterized in that, is to select any technique in eluent solvent and 300-400 DEG C of calcining to remove the dispersant in initial composite nanometer carbon paper in the method.
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| CN101440208B (en) * | 2008-12-09 | 2011-01-12 | 东华大学 | Preparation of functionalized carbon nano-tube modification polyurethane elastomer |
| CN102351165A (en) * | 2011-06-23 | 2012-02-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Large-area freestanding carbon nanotube paper and preparation method thereof |
| CN102500255A (en) * | 2011-10-31 | 2012-06-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nano tube dispersing method |
| CN102516569B (en) * | 2011-11-18 | 2014-05-14 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for carbon nanotube non-woven fabric interlayer modified fiber reinforced composite materials |
| CN102561109A (en) * | 2011-12-20 | 2012-07-11 | 南昌大学 | Method for preparing carbon nano tube conductive paper |
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