CN102180460A - Preparation method of highly-oriented carbon nanotube paper - Google Patents
Preparation method of highly-oriented carbon nanotube paper Download PDFInfo
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Abstract
The invention relates to a preparation method of a piece of highly-oriented carbon nanotube paper. The preparation method comprises the following steps: sticking and wrapping a carbon nanotube film onto a winding roller, then winding the carbon nanotube film, simultaneously, spraying a volatile solvent onto the winding roller, and then preparing the carbon nanotube paper with controllable orientation after the volatile solvent is fully volatilized. The preparation method is simple and efficient in process, avoids the damage of the structure and the morphology of a carbon nanotube and can achieve the carbon nanotube paper with controllable thickness, size and internal structure by changing equipment parameters; and the prepared carbon nanotube paper can be widely applied to batteries and filtering materials and further has a good application prospect.
Description
Technical field
The invention belongs to the preparation field of carbon nanotube paper, particularly a kind of preparation method of carbon nanotube paper of high-orientation.
Background technology
Carbon nanotube (CNT) is found in 1991 by Japanese Electronic Speculum expert Iijima, is the another newcomer who occurs in the carbon family after C60.Carbon nanotube has excellent physical chemistry because of it, emission on the scene, and battery and ultracapacitor, transmitter, fields such as high performance composite have good application prospects.Up to the present, by its macrostructure that assembles carbon nanotube silk ribbon, fiber, film and carbon nanotube paper (being also referred to as Buckypaper, Buckie paper) etc. are arranged.Carbon nanotube paper is by the carbon nanotube that tangles mutually, by the same carbon nanotube thin layer of sensitive paper of the formation of the Van der Waals force between the tube and tube.No matter as functional materials or strongthener, the excellent physical that carbon nanotube had, chemical property, carbon nanotube paper can both have.
The carbon nanotube paper of being made up of carbon nanotube not only has electroconductibility, also has excellent electric heating property and absorbing property, and its huge specific surface area makes it become good absorption filtering material.Though the Application Areas of relevant carbon nanotube paper is still in conceptual phase, its advantage with respect to carbon fiber paper has embodied its great using value.Another main application fields of carbon nanotube paper is a fuel cell, carbon nanotube paper can be used for making electrode, electric capacity and battery main body, and the battery of being made by carbon nanotube paper is nontoxic, and thermal diffusivity is good, lighter, more energy-conservation than the graphite battery that uses on the notebook computer.The reinforced composite of being made by carbon nanotube paper is realized in addition, has reported that the matrix material of being made by carbon nanotube paper has intensity 3GPa, and electroconductibility surpasses 5000S/cm, can match in excellence or beauty with carbon-fibre composite.In a word carbon nanotube paper as the purposes of functional materials and strongthener be far above above-mentioned some, its many performances are still waiting understanding, developing.For example, all exist extensive potential market in all conglomeraties such as environmental protection, aerospace, metallurgy, the energy and building materials.
The preparation method of carbon current nanotube paper has suction method, and spin-coating method, rolling process and direct growth go out the chemical Vapor deposition process of carbon nanotube paper.Suction method, spin-coating method and rolling process all are to prepare the carbon nanotube paper that carbon nanotube obtains by appropriate postprocessing more earlier.Wherein suction method is that the carbon nanotube that will prepare is dispersed in and forms suspension in the liquid solvent, obtains a kind of method of Buckie paper by suction filtration.The carbon nanotube paper of this traditional method preparation is tangled mutually by rambling carbon nanotube again and forms, and is difficult to realize the ordered arrangement of nanotube.Rolling process is directly vertical carbon nanotubes arranged array to be overwhelmed by certain orientation with the cylindrical surface to form carbon nanotube paper.The carbon pipe can only be height-oriented in one direction in the Buckie paper that this method forms, and can not bring significantly improving of mechanical property, and the size of Buckie paper limited by the carbon nano pipe array dimensions.Though chemical Vapor deposition process can obtain to have certain orientation degree carbon nanotube paper, the method complicated process of preparation is also higher to equipment requirements.In sum, traditional carbon nanotube Buckie paper mostly is rambling carbon nanotube mesh structures, and this structure has weakened mechanical property and electroconductibility in the Buckie paper greatly, has seriously limited the application of carbon nanotube paper.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of carbon nanotube paper of high-orientation, this method technology is simply efficient, structure and form to carbon nanotube do not cause damage, and can realize the carbon nanotube paper of controllable thickness, size and size by changing device parameter, the carbon nanotube paper of preparation can be widely used in having a good application prospect in battery and the filtering material.
The preparation method of the carbon nanotube paper that a kind of orientation degree of the present invention is controlled comprises:
Carbon nano-tube film is covered on wind up roll, and the coiling carbon nano-tube film sprays simultaneously the volatile solvent on wind up roll, treats that solvent fully volatilizees can make the controlled carbon nanotube paper of orientation degree.
Described wind up roll material is metal, superpolymer or glass, and wind up roll is done level with respect to film feeding direction and moved around, so that the narrower film of width covers whole coiling roll surface.As adopt metal or rubber as dielectric material, can coat one layer of polymeric or other metallic films thereon and get to make things convenient for taking off of carbon nanotube paper.As adopt glass as dielectric material, and can on the glass roller, spray releasing agent in advance, the carbon nanotube paper of Zhi Zuoing has more smooth even curface like this.
Described wind up roll links to each other with a motor with belt by a shaft coupling, and motor is by the rotating speed of regulated power supply control wind up roll.
Described carbon nanotube is a kind of or the two mixture in Single Walled Carbon Nanotube and the multi-walled carbon nano-tubes.
Described carbon nanotube is prepared by direct growth method or solid phase membrane method, and can further improve the wherein orientation degree of carbon nanotube by stretching to a certain degree.And,, be modified with at the enterprising one-step functional of the tube wall of various carbon nanotubes and include but not limited to carboxyl or amino etc. for mechanical property or the electric property that increases this carbon nanotube paper.
Described volatile solvent is one or more in ethanol, methyl alcohol, acetone, the water.As adopting ethanol as spraying solvent, film each other can tightr arrangement, can change the arrangement density between the carbon nanotube by the method that adds entry.Also can introduce the small part macromolecule group by the method for mixing other solvents.
The thickness of described carbon nanotube paper is by changing the control of winding speed and coiling time.
The width of described carbon nanotube paper and length are by changing the control of wind up roll diameter and coiling carbon nano-tube film area coverage.
The traffic direction of carbon nano-tube film of the present invention can be perpendicular with the coiling roll shaft, also can and the coiling roll shaft between have angle stable or that change, to obtain the carbon nano-tube film of multiple structure.Roll shaft also can be to comprise right cylinder, the multiple shape of cone or other curved-surface structure simultaneously.
Carbon nanotube is an orientation degree according to the degree of certain orientation ordered arrangement among the present invention, and high-orientation refers to that the carbon nanotube degree of alignment on a certain direction in the material is higher.
Above-mentioned high-strength high-orientation carbon nanotube paper of the present invention can make by the following method.As shown in Figure 1, continuous carbon nanometer tube film is sticked on skin be coated with on the wind up roll of film, with certain speed carbon nano-tube film is wound on the wind up roll by the driven by motor wind up roll.Meanwhile, have at volume to continue on the wind up roll of carbon nano-tube film to spray the volatile solvent,, the carbon nanotube paper of winding can be cut the high-orientation carbon nanotube paper that promptly becomes tiling by the coiling of certain hour.
Beneficial effect
Technology of the present invention is simply efficient, structure and form to carbon nanotube do not cause damage, and can realize the carbon nanotube paper of controllable thickness, size and size by changing device parameter, the carbon nanotube paper of preparation can be widely used in battery and the filtering material, also can develop into the strongthener of matrix material, establish material foundation for integrating functional matrix material exploitation, have a good application prospect with enhancing property.
Description of drawings
Fig. 1 is the simple and easy process schematic representation that the inventive method is made high-orientation carbon nanotube paper;
Fig. 2 is the tensile stress strain diagram of the high-orientation carbon nanotube paper of the inventive method making;
Fig. 3 is the sem photograph of the high-orientation carbon nanotube paper configuration of surface of the inventive method making;
Fig. 4 (a) is the simple and easy process schematic representation that the inventive method is made the different carbon nanotube paper of internal approach; (b) be the different carbon nanotube paper of the internal approach surface tissue synoptic diagram that the inventive method is made.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Prepare high-strength high-orientation carbon nanotube paper
(1) making of wind2: the chief component of winding apparatus is the wind up roll that stainless steel is made, and being with an external diameter on wind up roll has 3 centimetres Glass tubing.Wind up roll links to each other with a small machine with belt by a shaft coupling.Motor is by the rotating speed of regulated power supply control with the control wind up roll; (external diameter of the wind up roll in this step can require to regulate according to reality)
(2) after spraying releasing agent on the wind up roll outer layer glass tube, but carbon nano-tube film is extracted out from the spinning carbon nano pipe array and covered on Glass tubing, open the operation of motor by the rotation drive carbon nanotube of wind up roll, traffic direction is vertical with wireline reel; (experiment parameter in this step is aimed at and can requires to regulate according to reality)
(3) when carrying out step (2), volume there is the wind up roll surface sprinkling volatile solvent of carbon nano-tube film, solvent composition is the isometric(al) mixture of ethanol and deionized water;
(4) reel and spray operation after 1 hour, have the wind up roll of carbon nanotube paper to be positioned over volume and indoorly treated solvent evaporates 8 hours, with blade carbon nanotube paper is scratched afterwards and promptly obtained a height-oriented carbon nanotube paper.
Fig. 2 has shown by aforesaid method coiling solid phase membrane carbon nano-tube film (carbon nanotube parameter: diameter 8～10 nanometers, 300 microns of length), in oriented film speed be the tensile stress strain diagram of the high-orientation carbon nanotube paper that makes under the parameters such as 18 mm/second.Its maximum intensity has surpassed 400 MPas, can bear certain external influence power.Maximum tensile stress has embodied it above 5% and has had certain suppleness.
Fig. 3 is the surface sweeping sem image on this carbon nanotube paper surface, and wherein arrow place direction is the length direction of carbon nanometer paper.Can find out that wherein carbon nanotube paper is height-oriented on its length direction.This height-oriented orientation that depends primarily on carbon nanotube in the solid phase membrane carbon nano-tube film.
Prepare ultra-thin high-orientation carbon nanotube paper.
(1) making of wind2: the chief component of winding apparatus is the wind up roll that glass is made, and being with an external diameter on wind up roll has 3 centimetres Glass tubing.Wind up roll links to each other with a small machine with belt by a shaft coupling.Motor is by the rotating speed of regulated power supply control with the control wind up roll; (external diameter of the wind up roll in this step can require to regulate according to reality)
(2) with coating the one layer of polymeric film on the wind up roll, width is surpassed 1 centimetre solid phase membrane carbon nano-tube film, be wound on the wind up roll;
(3) when carrying out step (2), volume there is the wind up roll surface sprinkling volatile solvent of carbon nano-tube film, solvent composition is an ethanol, the film travelling speed is set to 5 millimeters per seconds;
(4) reel and polymeric film to be taken off behind two circles, promptly form height-orientedly on polymeric film, thickness is no more than 1 micron carbon nanotube paper.The width of ultra-thin high-orientation carbon nanotube paper and length dimension can require to be regulated by the area coverage of solid phase membrane carbon nano-tube film and the external diameter of wind up roll according to reality.(the travelling speed parameter in this example can require to regulate according to reality)
The different carbon nanotube paper of preparation internal approach.
(1) making of wind2: the chief component of winding apparatus is the wind up roll that stainless steel is made, and being with an external diameter on wind up roll has 3 centimetres Glass tubing.Wind up roll links to each other with a small machine with belt by a shaft coupling.Motor is by the rotating speed of regulated power supply control with the control wind up roll; (external diameter of the wind up roll in this step can require to regulate according to reality)
(2) shown in Fig. 4 (a), in winding process, carbon nano-tube film is wound on the wind up roll with 90 ° of winding angles, and makes film cover the whole surface of wind up roll by moving horizontally wind up roll.
(3) when carrying out step (2), volume there is the wind up roll surface sprinkling volatile solvent of carbon nano-tube film, solvent composition is an ethanol, the film travelling speed is set to 8 millimeters per seconds;
(4) coiling is after 2 hours, and changing winding angle is 45 °, and the film travelling speed is set to 10 millimeters per seconds, makes the different carbon nanotube paper of internal approach, and structural representation is shown in Fig. 4 (b).Simultaneously can be according to the carbon nanotube paper that angle is prepared approximate isotropic that is involved in of continuous change carbon nano-tube film.
Claims (6)
1. the preparation method of the carbon nanotube paper of a high-orientation comprises:
Carbon nano-tube film is covered on wind up roll, and the coiling carbon nano-tube film sprays simultaneously the volatile solvent on wind up roll, treats that solvent fully volatilizees can make the controlled carbon nanotube paper of orientation degree.
2. the preparation method of the carbon nanotube paper of a kind of high-orientation according to claim 1, it is characterized in that: described wind up roll material is metal, superpolymer or glass, wind up roll is done level with respect to film feeding direction and is moved around.
3. the preparation method of the carbon nanotube paper of a kind of high-orientation according to claim 2 is characterized in that: described wind up roll links to each other with a motor with belt by a shaft coupling, and motor is controlled the rotating speed of wind up roll by a regulated power supply.
4. the preparation method of the carbon nanotube paper of a kind of high-orientation according to claim 1, it is characterized in that: described carbon nanotube is a kind of or the two mixture in Single Walled Carbon Nanotube, the multi-walled carbon nano-tubes.
5. the preparation method of the carbon nanotube paper of a kind of high-orientation according to claim 4 is characterized in that: described carbon nanotube is by direct growth method or the preparation of solid phase membrane method.
6. the preparation method of the carbon nanotube paper of a kind of high-orientation according to claim 1, it is characterized in that: described volatile solvent is one or more in ethanol, methyl alcohol, acetone, the water.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102659092A (en) * | 2012-04-12 | 2012-09-12 | 东华大学 | Simple controllable carbon nanotube paper preparation device and method |
| CN102717536A (en) * | 2012-04-12 | 2012-10-10 | 东华大学 | Method for preparing carbon nano-tube electrical-conductive composite film |
| CN103031771A (en) * | 2011-09-29 | 2013-04-10 | 苏州捷迪纳米科技有限公司 | Carbon nanotube/active carbon core-shell structure carbon paper and preparation method |
| CN103317785A (en) * | 2012-03-20 | 2013-09-25 | 沈阳航空航天大学 | Method for preparing carbon nanometer paper flame resistant polymer matrix composite material |
| CN103342351A (en) * | 2013-07-10 | 2013-10-09 | 肖辉 | Method and device for preparing directionally arranged bucky paper in large scale |
| US8929076B2 (en) | 2011-12-21 | 2015-01-06 | Tsinghua University | Heat-dissipation structure and electronic device using the same |
| US9017503B2 (en) | 2011-12-21 | 2015-04-28 | Tsinghua University | Method for making carbon nanotube paper |
| CN104745856A (en) * | 2015-04-24 | 2015-07-01 | 云南大学 | Preparation method of wear-resisting carbon nano paper-metal composite material |
| US9576879B2 (en) | 2011-12-21 | 2017-02-21 | Tsinghua University | Heat-dissipation structure and electronic device using the same |
| CN107265439A (en) * | 2017-05-11 | 2017-10-20 | 江西理工大学 | A kind of method of the lossless separation of carbon nano-tube macroscopic film |
| CN108699734A (en) * | 2016-02-04 | 2018-10-23 | 日立造船株式会社 | The manufacturing method and carbon nanotube twisted yarn of carbon nanotube twisted yarn |
| CN109850872A (en) * | 2018-12-29 | 2019-06-07 | 北京旭江科技有限公司 | Carbon nano-tube macroscopic body film-forming machine |
| CN110777331A (en) * | 2019-11-07 | 2020-02-11 | 苏州第一元素纳米技术有限公司 | Preparation method of metal-coated carbon nano tube |
| CN114477146A (en) * | 2022-03-14 | 2022-05-13 | 中国航空制造技术研究院 | High-density orientation method for carbon nano tube in unit width |
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| CN1475437A (en) * | 2003-07-31 | 2004-02-18 | 清华大学 | Manufacturing method of carbon nano tube paper |
| CN1982209A (en) * | 2005-12-16 | 2007-06-20 | 清华大学 | Carbon nano-tube filament and its production |
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Patent Citations (2)
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| CN1475437A (en) * | 2003-07-31 | 2004-02-18 | 清华大学 | Manufacturing method of carbon nano tube paper |
| CN1982209A (en) * | 2005-12-16 | 2007-06-20 | 清华大学 | Carbon nano-tube filament and its production |
Cited By (21)
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| CN103031771B (en) * | 2011-09-29 | 2015-04-01 | 苏州捷迪纳米科技有限公司 | Carbon nanotube/active carbon core-shell structure carbon paper and preparation method |
| CN103031771A (en) * | 2011-09-29 | 2013-04-10 | 苏州捷迪纳米科技有限公司 | Carbon nanotube/active carbon core-shell structure carbon paper and preparation method |
| US9576879B2 (en) | 2011-12-21 | 2017-02-21 | Tsinghua University | Heat-dissipation structure and electronic device using the same |
| TWI491561B (en) * | 2011-12-21 | 2015-07-11 | Hon Hai Prec Ind Co Ltd | Preparation of carbon nanotube paper |
| US8929076B2 (en) | 2011-12-21 | 2015-01-06 | Tsinghua University | Heat-dissipation structure and electronic device using the same |
| US9017503B2 (en) | 2011-12-21 | 2015-04-28 | Tsinghua University | Method for making carbon nanotube paper |
| CN103317785A (en) * | 2012-03-20 | 2013-09-25 | 沈阳航空航天大学 | Method for preparing carbon nanometer paper flame resistant polymer matrix composite material |
| CN103317785B (en) * | 2012-03-20 | 2015-07-01 | 沈阳航空航天大学 | Method for preparing carbon nanometer paper flame resistant polymer matrix composite material |
| CN102717536B (en) * | 2012-04-12 | 2014-10-15 | 东华大学 | Method for preparing carbon nano-tube electrical-conductive composite film |
| CN102659092A (en) * | 2012-04-12 | 2012-09-12 | 东华大学 | Simple controllable carbon nanotube paper preparation device and method |
| CN102717536A (en) * | 2012-04-12 | 2012-10-10 | 东华大学 | Method for preparing carbon nano-tube electrical-conductive composite film |
| CN103342351B (en) * | 2013-07-10 | 2015-02-18 | 昆明纳太能源科技有限公司 | Method and device for preparing directionally arranged bucky paper in large scale |
| CN103342351A (en) * | 2013-07-10 | 2013-10-09 | 肖辉 | Method and device for preparing directionally arranged bucky paper in large scale |
| CN104745856A (en) * | 2015-04-24 | 2015-07-01 | 云南大学 | Preparation method of wear-resisting carbon nano paper-metal composite material |
| CN108699734A (en) * | 2016-02-04 | 2018-10-23 | 日立造船株式会社 | The manufacturing method and carbon nanotube twisted yarn of carbon nanotube twisted yarn |
| CN107265439A (en) * | 2017-05-11 | 2017-10-20 | 江西理工大学 | A kind of method of the lossless separation of carbon nano-tube macroscopic film |
| CN107265439B (en) * | 2017-05-11 | 2019-05-21 | 江西理工大学 | A kind of lossless isolated method of carbon nano-tube macroscopic film |
| CN109850872A (en) * | 2018-12-29 | 2019-06-07 | 北京旭江科技有限公司 | Carbon nano-tube macroscopic body film-forming machine |
| CN109850872B (en) * | 2018-12-29 | 2021-02-05 | 北京旭江科技有限公司 | Carbon nanotube macroscopic body film forming machine |
| CN110777331A (en) * | 2019-11-07 | 2020-02-11 | 苏州第一元素纳米技术有限公司 | Preparation method of metal-coated carbon nano tube |
| CN114477146A (en) * | 2022-03-14 | 2022-05-13 | 中国航空制造技术研究院 | High-density orientation method for carbon nano tube in unit width |
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Application publication date: 20110914 |