CN1475437A - Manufacturing method of carbon nano tube paper - Google Patents
Manufacturing method of carbon nano tube paper Download PDFInfo
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- CN1475437A CN1475437A CNA031500528A CN03150052A CN1475437A CN 1475437 A CN1475437 A CN 1475437A CN A031500528 A CNA031500528 A CN A031500528A CN 03150052 A CN03150052 A CN 03150052A CN 1475437 A CN1475437 A CN 1475437A
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Abstract
A carbon nanotube paper is prepared from carbon nanotubes through adding them to acid, heating or thermal reflux, and/or ultrasonic stirring, removing impurity, diluting in water, filtering, washing the filtered cake, dispersing the carbon nanotubes in water by ultrasonic stirring, spreading on carrier, and drying. It has regular structure, high uniformity, purity and electric conductivity, and enough mechanical strength.
Description
Technical field
The present invention relates to the forming technique of carbon nanotube, relate in particular to a kind of preparation method of carbon nanotube paper.
Background technology
Nanotechnology is the commanding elevation of 21 century development in science and technology, is the dominant technology of the new Industrial Revolution.In November, 1991, the Electronic Speculum expert Iijima of Japanese NEC has at first found carbon nanotube under high resolution transmission electron microscopy (HRTEM), caused people's extensive concern.The one dimension carbon material that carbon nanotube is made up of the hexagonal mesh of similar graphite, pipe is to be made of single or multiple lift, and between tens nanometers, length can reach several microns to diameter in several nanometers, its lamellar spacing is 0.34nm, and is bigger slightly than the lamellar spacing (0.335nm) of graphite.Carbon nanotube is concentrated the nano-grade size that distributes, high effective ratio area, good electrical conductivity and excellent chemical stability owing to having, thereby has application very widely.
Though the carbon nanotube excellent performance has widely and uses, carbon nanotube is a particulate state or Powdered generally speaking, and this application for people has caused a lot of inconvenience.In order to make flaky material, often need to adopt the high temperature compacting or add binding agent.As Ma Renzhi, Wei Bingqing, (E collects Xu Cailu etc., 2000 on " Chinese science " magazine, the 30th the 2nd phase of volume, the 112-116 page or leaf) " based on the ultracapacitor of carbon nanotube " delivered is before carbon nanotube uses, through the peroxy-nitric acid purification process, promptly remove metal catalyst through 20% nitric acid dousing 24h, with two kinds of methods carbon nanotube is made flaky material then, a kind of is under argon shield, and the pressure that adopts 25MPa is in the moulding of 2000 ℃ of hot pressing pure nano-carbon tubes; Another kind is that carbon nanotube and 20% resol are mixed, at low temperature (100 ℃) and certain pressure compacted under, then in nitrogen atmosphere in 800 ℃ of charings, the charing rear electrode carries out chemical after-treatment in concentrated nitric acid solution manages.Though the first method preparation is pure nano-carbon tube, manufacture craft is cumbersome.Though second method does not need high temperature, but can not get pure carbon nanometer.Wang Xiaofeng etc. on " Chinese Journal of Inorganic Chemistry " magazine (2003, the 19th the 2nd phase of volume, the 137-141 page or leaf) " development of nickel oxide/carbon nanotube hybrid supercapacitor " delivered, take by weighing an amount of carbon nanotube, it is wetting with it to add small quantity of deionized water, add an amount of ptfe emulsion and fully stirring subsequently, carbon nanotube and tetrafluoroethylene mass ratio are 95/5.With slurry 60 ℃ of bakings to the half-dried attitude shape in that to be pressed into thickness on the twin rollers be the film about 0.2mm and cut thereon that to obtain diameter be the 2cm electrode slice.Electrode slice is rolled on the nickel foam collector, and pressure-controlling is at 12-15MPa.This method is made binding agent with an amount of tetrafluoroethylene, is pressed into carbon nano-tube film, can not get pure carbon nanotube.Wear dawn, the Chinese patent " multilayer carbon nanotube films " of Huang Shaoming application (open day: 2002.05.15, publication number: 1349478), the method of the nano-tube film that a kind of arrangement for preparing no matrix that proposes is good, this method comprises: (a) in the presence of the catalyzer that is fit to nanotube formation, by the pyrolysis carbon nanotube that synthetic one deck is arranged on silica glass matrix of carbonaceous material; And (b) in nanotube/matrix interface etching silica glass matrix, so that peel off the good nanotube layer of described arrangement from matrix.This method needs catalyzer and silica glass matrix, need be in nanotube/matrix interface etching silica glass matrix, so that peel off the good nanotube layer of described arrangement from matrix.The Chinese patent of applications such as Wei Fei " a kind of method of utilizing external force to crush, wash and purify slender carbon nanotube " (open day 2002.10.16 publication number 1374250), be a kind of method of utilizing external force to crush, wash and purify slender carbon nanotube, do not form carbon nanotube paper.Chunming Niu, Deng at " Appl.Phys.Lett. " (Vol.70, No.11, " the Highpower electrochemical capacitors based on carbon nanotube electrodes " that delivers on 1840-1842), use the nitric acid treatment carbon nanotube, filtration and washing after the drying, adds the carbon nanotube after the 0.2g processing in the 200mL water, refilter, after the drying, heat cross-linking has formed uniform inflexible thin electrode.But this method adopts filtering method to form carbon nano-tube sheets, and in the reality, the diameter of carbon nanotube is nano level, this requires the aperture of filter membrane very little (such filter membrane cost is also than higher), and when filtering, can lose a part of carbon nanotube, especially when the carbon nanotube sheet material that forms as thin as a wafer, the quality of carbon nanotube is difficult to control on its thickness and the unit surface.Since be subjected to the restriction of filtration unit, the size and dimension of thin electrode, and shape also is restricted.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of carbon nanotube paper, this method is simple to operate, need not binding agent, and the thickness of carbon nanotube paper, shape and size can control, and can make the various carbon nanotube paper that meet people's needs.This carbon nanotube paper have compound with regular structure, highly evenly, high purity, high conductivity and enough physical strengths.
Technical scheme of the present invention is as follows: a kind of preparation method of carbon nanotube paper, this method comprises the steps:
A. purifying carbon nanometre tube: carbon nanotube is poured in the acid, and heating or reflux continuously or/and ultrasonic concussion, or/and stir, are fully disperseed and are removed impurity up to carbon nanotube, and dilute with water filters then, and it is standby to wash the gained filter cake with water clean back;
B. dispersing Nano carbon tubes: the clean filter cake of gained among the step a is put into water, and ultrasonic concussion or stirring form homodisperse carbon nano-tube solution;
C. form carbon nanotube paper: homodisperse carbon nano-tube solution is poured on carries out drying on the carrier, form carbon nanotube paper.
Sulfuric acid, nitric acid, hydrochloric acid or their mixture are adopted in acid described in the present invention.
Carrier described in the present invention adopts plastics, stone, stainless steel, aluminium foil or glass material.
The present invention forms carbon nanotube paper with carbon nanotube, is convenient to people and uses carbon nanotube, has expanded the range of application of carbon nanotube; This method not only technology is simple, need not binding agent, also need not pressurization and high temperature, can obtain under normal pressure and lower temperature; And the carbon nanotube paper of making has compound with regular structure, and quality is even, purity height, the high and enough physical strengths of specific conductivity.Because it can form uniform nano aperture, can be used as nanofiltration membrane, also can in ultracapacitor, lithium cell, electrochemical synthesis or electrolytic process, be used as electrode materials.Can make ultra-capacitor have higher specific storage, specific energy, specific power, good environmental stability, and increase the service life greatly.The thickness of this film, shape and size can be controlled, and can make the carbon nanotube paper of the needs that meet people.
Description of drawings
Fig. 1 is the structure of primary carbon nanotube.
Fig. 2 is the structure of the carbon nanotube paper that forms on plastic carrier.
Fig. 3 is the infrared spectrum of primary carbon nanotube.
Fig. 4 is the infrared spectrum of carbon nanotube paper.
Fig. 5 is the structure of the carbon nanotube paper that forms on stainless steel carrier.
Fig. 6 is the structure of the carbon nanotube paper that forms on the stone matter carrier.
Fig. 7 is the structure of the carbon nanotube paper that forms on glass carrier.
Fig. 8 is the structure of the carbon nanotube paper that forms on aluminium carrier.
Embodiment
The invention will be described further below by embodiment.
The used carbon nanotube of the present invention can be to use any method, as laser bombardment method, chemical vapor deposition method, electric glow discharge method, direct current arc electric discharge, gaseous combustion method, catalyzer high temperature pyrolytic cracking (HTP) etc., the carbon nanotube of preparation.Because the carbon nanotube of different methods preparation, the kind of impurity such as its structure, composition and catalyzer is also different with content, in order to remove impurity, and even carbon nanotube is disperseed, the composition of the consumption of its required acid and acid also will be done suitable adjustment, till the abundant dispersion that reaches carbon nanotube.If, can repeatedly handle, till carbon nanotube is fully disperseed and removing impurity for the first time carbon nanotube fully being disperseed in afterwards to the carbon nanotube purifying treatment with acid.
Take by weighing the 1g carbon nanotube, pour in the mixed solution (volume ratio of the vitriol oil and concentrated nitric acid 3: 1) of the 1000ml vitriol oil and concentrated nitric acid, under 70 ℃, ultrasonic concussion, and stir, react after 24 hours, with deionized water dilution, filter, with filter cake with deionized water wash clean after, ultrasonic filter cake is dispersed in the deionized water, forms carbon nano-tube solution; Carbon nano-tube solution is poured in the smooth plastic containers in bottom, at room temperature dry, form carbon nanotube paper.Gained carbon nanotube paper, its thickness are 50 μ m, have higher specific conductivity, and its square resistance is 13 Ω/1cm, and far above the specific conductivity of carbon fiber paper (its thickness is 500 μ m), the square resistance of carbon fiber paper is 35 Ω/1cm.Fig. 1 is the structure of primary carbon nanotube, and Fig. 2 is the structure of the carbon nanotube paper that forms on plastic carrier.Compare with primary carbon nanotube, carbon nanotube paper has compound with regular structure, highly even, and has enough mechanical strengths, owing to do not add any binding agent, so gained carbon nanotube paper has high purity, the infrared spectrum of carbon nanotube paper has also confirmed this point.Fig. 3 is the infrared spectrum of primary carbon nanotube, and Fig. 4 is the infrared spectrum of carbon nanotube paper, and therefrom carbon nanotube paper has high purity as can be seen.
Owing to form carbon nanotube paper,, can make the carbon nanotube paper of the needs that meet people so the thickness of carbon nanotube paper, shape and size can be controlled by dry.
Embodiment 2
Take by weighing the 1g carbon nanotube, pour in the mixed solution (volume ratio of the vitriol oil and concentrated nitric acid 3: 1) of the 1000ml vitriol oil and concentrated nitric acid, under 70 ℃, ultrasonic concussion, and stir, react after 24 hours, dilute with deionized water then, filter, with filter cake with deionized water wash clean after, ultrasonic filter cake is disperseed in the deionized water, form carbon nano-tube solution, carbon nano-tube solution is poured in the smooth stainless steel vessel in bottom, at room temperature dry, form carbon nanotube paper.Gained carbon nanotube paper, its thickness are 70 μ m, have higher specific conductivity, and its square resistance is 10 Ω/1cm, and far above the specific conductivity of carbon fiber paper (its thickness is 500 μ m), the square resistance of carbon fiber paper is 35 Ω/1cm.Fig. 5 is the structure of the carbon nanotube paper that forms on stainless steel carrier.Compare with primary carbon nanotube, carbon nanotube paper has compound with regular structure, height advantage of uniform.
Embodiment 4. takes by weighing the 1g carbon nanotube, pour in the mixed solution (volume ratio of the vitriol oil and concentrated nitric acid 3: 1) of the 100ml vitriol oil and concentrated nitric acid, and stir, reaction is diluted with deionized water after 48 hours then under the room temperature, filter, with filter cake with deionized water wash clean after, ultrasonic filter cake is disperseed in the deionized water, form carbon nano-tube solution, pour carbon nano-tube solution in the smooth Glass Containers in bottom drying, under 100 degree, form carbon nanotube paper.Gained carbon nanotube paper, its thickness are 430 μ m, have higher specific conductivity, and its square resistance is 13 Ω/1cm, and far above the specific conductivity of carbon fiber paper (its thickness is 500 μ m), the square resistance of carbon fiber paper is 35 Ω/1cm.Fig. 7 is the structure of the carbon nanotube paper that forms on glass carrier.Compare with primary carbon nanotube, carbon nanotube paper has compound with regular structure, height advantage of uniform.
Embodiment 5. takes by weighing the 1g carbon nanotube, pours the 100ml vitriol oil into, ultrasonic concussion 2 hours, constant temperature is about 200 ℃, continuous backflow heating 13 hours, filter with the deionized water dilution cooling back, with filter cake with deionized water wash clean after, ultrasonic filter cake is disperseed in the deionized water, form carbon nano-tube solution, carbon nano-tube solution is poured in the smooth aluminum container in bottom, at room temperature dry, form carbon nanotube paper.Gained carbon nanotube paper, its thickness are 100 μ m, have higher specific conductivity, and its square resistance is 19 Ω/1cm, and far above the specific conductivity of carbon fiber paper (its thickness is 500 μ m), the square resistance of carbon fiber paper is 35 Ω/1cm.Fig. 8 is the structure of the carbon nanotube paper that forms on aluminium carrier.Compare with primary carbon nanotube, carbon nanotube paper has compound with regular structure, height advantage of uniform.
Claims (3)
1. the preparation method of a carbon nanotube paper is characterized in that this method comprises the steps:
A. purifying carbon nanometre tube: carbon nanotube is poured in the acid, and heating or reflux continuously or/and ultrasonic concussion, or/and stir, are fully disperseed and are removed impurity up to carbon nanotube, and dilute with water filters then, and it is standby to wash the gained filter cake with water clean back;
B. dispersing Nano carbon tubes: the clean filter cake of gained among the step a is put into water, and ultrasonic concussion or stirring form homodisperse carbon nano-tube solution;
C. form carbon nanotube paper: homodisperse carbon nano-tube solution is poured on carries out drying on the carrier, form carbon nanotube paper.
2. according to claim 1 or 2 described preparation methods, it is characterized in that: sulfuric acid, nitric acid, hydrochloric acid or their mixture are adopted in described acid.
3. according to the described preparation method of claim 1, it is characterized in that: described carrier adopts plastics, stone material, stainless steel, aluminium or glass material.
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| CN1309104C (en) * | 2005-04-06 | 2007-04-04 | 清华大学 | Method for increasing electrochemical lithium storage content of nano-carbon tube |
| WO2007093081A1 (en) * | 2006-02-16 | 2007-08-23 | Dalian Institute Of Chemical Physics Chinese Academy Of Sciences | Catalyst and process for syngas conversion |
| CN100427388C (en) * | 2005-11-25 | 2008-10-22 | 清华大学 | Large-area ultra-thin carbon nanotube film and its preparation process |
| CN100469691C (en) * | 2006-07-17 | 2009-03-18 | 中国科学院过程工程研究所 | Method of improving chemical activity of carbon nano-tube |
| CN100555611C (en) * | 2005-07-22 | 2009-10-28 | 鸿富锦精密工业（深圳）有限公司 | The manufacture method of radiator |
| CN101845750A (en) * | 2010-04-30 | 2010-09-29 | 冯静 | Manufacturing method of carbon nano tube modified fiber line and manufacturing device thereof |
| CN101284662B (en) * | 2007-04-13 | 2011-01-05 | 清华大学 | Preparing process for carbon nano-tube membrane |
| CN101947417A (en) * | 2010-08-25 | 2011-01-19 | 上海理工大学 | Carbon nano tube-based nanofiltration membrane device and preparation method thereof |
| CN101284661B (en) * | 2007-04-13 | 2011-03-23 | 鸿富锦精密工业（深圳）有限公司 | Preparing process for carbon nano-tube sheets |
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