CN102877367A - 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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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 the nano-carbon material preparing technical field.
Background technology
The nanometer carbon paper is the nonwoven fabric form that is made of the disordered carbon nanotube, it is the simplest macroscopic material form of CNT, characteristics with lightweight, flexibility, conduction, heat conduction and huge specific area, combine simultaneously the functional characteristic of CNT self excellence, 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 the CNT size is at nanoscale, conventional carbon paper conversion technology of preparing all can't be suitable for the preparation of nanometer carbon paper, in the urgent need to development of new nano-sized carbon standby technology made of paper.
The preparation method of nanometer carbon paper is mainly three classes at present, that is:
1) CVD deposition technique direct growth goes out the 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 such 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 takes off to a direction, but or use special spinning array, also successively be stacked from the ordered carbon nanotube film of wherein pulling out meter level length, infiltrate with alcohol, can get large-area nanometer carbon paper;
3) wet-chemical filter method, the method is disperseed and suction filtration based on the wet method water of carbon nanotube dust, selects suitable pumping and filtering device can make the nanometer carbon paper of required form.
Wherein, front two kinds of methods are subject to device-restrictive; preparation efficiency can't improve always; seriously limit its large-scale production; and for the third method; although it can realize that lower cost prepares the nanometer carbon paper; but because CNT is seriously cut off in dispersion process; it is large to cause filtering acquisition nanometer carbon paper fragility; be difficult to preparation large scale product, simultaneously, the CNT of nanoscale makes its efficient in filter process very low; solve the preparation of serialization and high efficiency, therefore also be very difficult to realize.How to develop a kind of efficient technology of preparing and become a key core difficult problem that solves the preparation of nano-sized carbon lateral modelling.
Summary of the invention
The purpose 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 of CNT and staple fibre, strengthen as strengthening toughness reinforcing skeleton with staple fibre, and keeping CNT self functional characteristic, formation has good flexible composite nanometer carbon paper.And adopt the vacuum aided casting film-forming to realize the 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 mainly by disordered carbon nanotube and staple fibre and forms, and is the macroscopic form of nonwoven fabric construct,
And the thickness of described composite nanometer carbon paper is 0.5 μ m-5 mm, and 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 the Single Walled Carbon Nanotube,
And the caliber of described CNT is 0.4 nm-150 nm, and 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 the artificial fiber, and described natural fabric comprises string, animal fiber and mineral fibres, and described chemical fibre comprises artificial fibre, synthetic fiber and inorfil.
The continuous production method of a kind of CNT/staple fibre composite nanometer carbon paper comprises:
At first, CNT is dispersed under dispersant is auxiliary forms dispersion liquid in the solvent;
, 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 form initial composite nanometer carbon paper, the dispersant in post processing removal initial composite nanometer carbon paper obtains target product again.
As one of better embodiment, described CNT is dispersed under dispersant is auxiliary and forms dispersion liquid in the solvent, and described dispersant is selected from any one among polyvinyl alcohol, polyvinylpyrrolidone, cellulose, lauryl sodium sulfate, neopelex, softex kw, Tween-80, the Qu Latong-100 at least.
Further, the technique that in the method carbon nanotube dispersed is formed dispersion liquid in solvent is selected from any one or the two or more combinations in high speed shear dispersions, ultrasonic dispersion, grinding distribution and the ball milling dispersion,
And described solvent is selected from water, ethanol, isopropyl alcohol, N at least, any one in dinethylformamide, 1-METHYLPYRROLIDONE, ethyl acetate and the chloroform.
As one of better specific embodiments, the concentration of institute's carbon nanotubes is 0.001-10wt% in the described dispersion liquid, and wherein the weight ratio of CNT and dispersant is 1:10-1:0.1.
As one of better specific embodiments, 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 that passes through from porous filter plate continuously, accompany by simultaneously and utilize the operation that vacuum equipment vacuumizes aforementioned closed cavity and utilize scraper plate that the slurry that is distributed on the filter membrane is carried out the operation of knifing, make solid content uniform deposition in the slurry on filter membrane, and form continuous initial composite nanometer carbon paper.
As one of better specific embodiments, be to select any method in eluent solvent and the 300-400 ℃ of calcining to remove dispersant in initial composite nanometer carbon paper in the method.
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, and is toughness reinforcing as strengthening with staple fibre, forms to have 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 remove polymer in the process such as follow-up drip washing, obtains the high quality nano carbon paper;
The advantageous feature such as (3) to have technique simple in whole technological process, and efficient is high, and equipment requirement is low have greatly reduced the preparation processing cost of nanometer carbon paper, have boundless Commercial Prospect.
Description of 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 embodiment of the invention 1 prepared nanometer carbon paper;
Fig. 3 a-3c is respectively the electron scanning micrograph of the embodiment of the invention 2 prepared nanometer carbon papers;
Fig. 4 a-4c is respectively the electron scanning micrograph of the embodiment of the invention 3 prepared nanometer carbon papers;
Fig. 5 a-5c is respectively the electron scanning micrograph of the embodiment of the invention 4 prepared nanometer carbon papers.
The specific embodiment
An aspect as technical solution of the present invention, this CNT/staple fibre composite nanometer carbon paper has and mainly is comprised of disordered carbon nanotube and staple fibre, the macroscopic form that is 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 the 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 may further comprise the steps:
At first, CNT is dispersed under dispersant is auxiliary forms dispersion liquid in the solvent;
Subsequently, in stirring at low speed, staple fibre is slowly sneaked in the dispersion liquid, and high speed shear makes staple fibre by fine dispersion, obtain slurry;
Then, aforementioned slurry is formed initial composite nanometer carbon paper by the vacuum aided casting film-forming, through post processing dispersant is removed and namely 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 the 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 the chloroform or multiple, but be not limited to this.
As one of optional embodiment, also contain dispersant in the described dispersion liquid, 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, the content of CNT is preferably 0.001-10wt% in the described dispersion liquid, 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 the assisted vacuum suction filtration, forms negative pressure partial solvent is separated.
Further, the method for described removal polymer can be to pass through eluent solvent in vacuum aided casting film-forming subsequent technique, and polymer is removed in washing; Perhaps directly adopt 300-400 ℃ of calcining with 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 by weighing 30 gram multi-walled carbon nano-tubes, be dissolved in 1 liter of concentration and be in 1% Qu Latong-100 aqueous solution, adopt subsequently the grinder grinding distribution, rotating speed 3000 rpm dispersed with stirring 1 hour obtain uniform carbon nano tube dispersion liquid (being called for short " dispersion liquid ") after 200 mesh filter screens sieve; Adding 5 gram length in slowly stirring 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 the high speed shear dispersion machine, disperse to form stable slurry in 20 minutes, 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 the polymer eccysis through follow-up drip washing, namely be obtained the CNT that full material with carbon element consists of/carbon fiber composite nanometer carbon paper.Fig. 2 a-Fig. 2 c is depicted as the electron scanning micrograph of the obtained nanometer carbon paper of present embodiment.
The structure of aforementioned vacuum aided casting film-forming device sees also 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: provide continuously filter membrane 9 by continuous filter membrane feed unit 1 and conveyer belt on the porous filter plate 3 that is placed on the enclosed cavity, and in enclosed cavity, form negative pressure by vacuum equipment 8, simultaneously, on the filter membrane that is laid on porous filter plate 3, be continuously applied aforementioned dispersion liquid by charging bucket 4, and utilize scraper 5 to carry out knifing and process, thereby form composite nanometer carbon paper at filter membrane, to by barrier film 10 that continuous barrier film feed unit 6 provide be covered in composite nanometer carbon paper on, and collect with nanometer carbon paper collector unit 7 thereafter.
Embodiment 2Present embodiment is substantially the same manner as Example 1, and its difference is that 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 present embodiment.
Embodiment 3Present embodiment is substantially the same manner as Example 1, and its difference is that 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 present embodiment.
Embodiment 4Present embodiment is substantially the same manner as Example 1, and its difference is that 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 present embodiment.
Embodiment shown in more than explanation reaches on drawing can not resolve the design philosophy surely of the present invention that is limited.Holding the identical the knowledgeable of knowing in technical field of the present invention can be with technical thought of the present invention with various form improvement change, and such improvement and change are interpreted as belonging in protection scope of the present invention.
Claims (10)
1. CNT/staple fibre composite nanometer carbon paper is characterized in that, it has mainly by disordered carbon nanotube and staple fibre and forms, and is the macroscopic form of nonwoven fabric construct,
And the thickness of described composite nanometer carbon paper is 0.5 μ m-5 mm, and wherein the weight ratio of CNT and staple fibre is 100:1-1:1.
2. CNT according to claim 1/staple fibre composite nanometer carbon paper is characterized in that, 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 the Single Walled Carbon Nanotube,
And the caliber of described CNT is 0.4 nm-150 nm, and length is 200 nm-1 cm.
3. CNT according to claim 1/staple fibre composite nanometer carbon paper is characterized in that, 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 the chemical fibre, and described natural fabric comprises string, animal fiber and mineral fibres, and described chemical fibre comprises artificial fibre, synthetic fiber and inorfil.
4. the continuous production method of CNT/staple fibre composite nanometer carbon paper is characterized in that it comprises:
At first, CNT is dispersed under dispersant is auxiliary forms dispersion liquid in the solvent;
, 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 form initial composite nanometer carbon paper, the dispersant in post processing removal initial composite nanometer carbon paper obtains target product again.
5. the continuous production method of CNT according to claim 4/staple fibre composite nanometer carbon paper, it is characterized in that, described CNT is dispersed under dispersant is auxiliary and forms dispersion liquid in the solvent, and described dispersant is selected from any one among polyvinyl alcohol, polyvinylpyrrolidone, cellulose, lauryl sodium sulfate, neopelex, softex kw, Tween-80, the Qu Latong-100 at least.
6. according to claim 4 or the continuous production method of 5 described CNT/staple fibre composite nanometer carbon papers, it is characterized in that, the technique that in the method carbon nanotube dispersed is formed dispersion liquid in solvent is selected from any one or the two or more combinations in high speed shear dispersions, ultrasonic dispersion, grinding distribution and the ball milling dispersion
And described solvent is selected from water, ethanol, isopropyl alcohol, N at least, any one in dinethylformamide, 1-METHYLPYRROLIDONE, ethyl acetate and the chloroform.
7. the continuous production method of CNT according to claim 5/staple fibre composite nanometer carbon paper, it is characterized in that, the concentration of institute's carbon nanotubes is 0.001-10wt% in the described dispersion liquid, and wherein the weight ratio of CNT and dispersant is 1:10-1:0.1.
8. the continuous production method of CNT according to claim 4/staple fibre composite nanometer carbon paper is characterized in that, the method high speed is sheared and disperseed the process conditions of staple fibre to comprise: mixing speed 1000-5000 rpm, jitter time 1-120 min.
9. the continuous production method of CNT according to claim 4/staple fibre composite nanometer carbon paper is characterized in that, 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 that passes through from porous filter plate continuously, accompany by simultaneously and utilize the operation that vacuum equipment vacuumizes aforementioned closed cavity and utilize scraper plate that the slurry that is distributed on the filter membrane is carried out the operation of knifing, make solid content uniform deposition in the slurry on filter membrane, and form continuous initial composite nanometer carbon paper.
10. the continuous production method of CNT according to claim 4/staple fibre composite nanometer carbon paper is characterized in that, in the method is to select any technique in eluent solvent and the 300-400 ℃ of calcining to remove dispersant in initial composite nanometer carbon paper.
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