CN101691280A - Method for preparing carbon nano tube film - Google Patents
Method for preparing carbon nano tube film Download PDFInfo
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- CN101691280A CN101691280A CN200910309105A CN200910309105A CN101691280A CN 101691280 A CN101691280 A CN 101691280A CN 200910309105 A CN200910309105 A CN 200910309105A CN 200910309105 A CN200910309105 A CN 200910309105A CN 101691280 A CN101691280 A CN 101691280A
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Abstract
The invention provides a method for preparing a carbon nano tube film in the technical field of nano materials. The method comprises the following steps: adding a carbon nano tube raw material into dispersion for dispersing by adopting ultrasonic processing, high-strength stirring processing or high pressure homogenization processing to prepare dispersion of the carbon nano tube; filtering the dispersion of the carbon nano tube by adopting a suction funnel for depositing process to acquire carbon nano tube deposit attached to the filter membrane; then, removing the dispersion through desorbing fluid; and finally, combining the carbon nano tube deposit and a substrate to remove the filter membrane so as to acquire the carbon nano tube film. The film prepared by the method has controllable thickness, has the minimum thickness of about 50nm, is nearly transparency, and has conductivity. The structure of the carbon nano tube does not have any chemical modification or destruction in a film preparing process, and can maintain excellent structure completeness.
Description
Technical field
What the present invention relates to is a kind of method of technical field of nano material, specifically is a kind of preparation method of carbon nano-tube film.
Background technology
Carbon nanotube (Carbon Nanotube, CNT) find first in 1991 by Japanese scientist Iijima, because its excellent properties at aspects such as mechanics, electricity, optics and Chu Qing causes people's extensive concern, the novel nano-material of representative that a large amount of with the carbon nanotube is continues to bring out.In recent years, along with deepening continuously of carbon nanotube and nano materials research, made that the use field of carbon nanotube was more wide.A large amount of applied researcies in fields such as field emitting electronic source, transmitter, novel optical material, soft ferromagnetic materials about carbon nanotube constantly are in the news.
Carbon nano-tube film is a kind of important use form of carbon nanotube.Various carbon nano-tube films is in area research and application such as field emission source, transparent conductive body, battery electrode, water purification material, luminescent material and biosensors.Therefore, the technology of preparing of carbon nano-tube film becomes the basis of above-mentioned research and application.The preparation method of existing carbon nano-tube film mainly is divided into direct growth method (as CN1349478A) and prepares carbon nano-tube film by carbon nanotube powder.It is the most convenient and swift wherein to prepare carbon nano-tube film with carbon nanotube powder, comprise that mainly point solvent drips desiccating method, L-B membrane process (CN1803594A, Sano M., et al., Langmuir 2001,17,5125-5128), print process (CN1670886A), electrophoretic method (CN1570220A) and filter membrane method etc.
Have the effect of intensive Van der Waals force between the carbon nanotube, many carbon nanotubes are easily assembled bunchy [Thess, A., etal., Science 1996,273:483], have a strong impact on performance [Yao.Z, the et al. of aspects such as its mechanics and electricity, J.Am.Chem.Soc., 2003,125:16015].In order to eliminate the influence of this congregation, ultrasonic, methods such as carbon nano tube surface chemical modification and physics coating often are used in the preparation carbon nano-tube film.In the congregation of eliminating between the carbon nanotube, these surface modifying methods also manifest the caused negative interaction of carbon nanotube chemical structural damage thereupon.The coating that uses is difficult to remove and equally also makes the electric property of carbon nanotube decrease in the physical method.
The preparation method of existing carbon nano-tube film can't fine dispersing Nano carbon tubes in preparation process, can produce the carbon nanotube heap of island on microcosmic, is difficult to form uniform carbon nano-tube film.Aforesaid method can't guarantee the integrity of carbon nanotube chemical structure for the processing of carbon nanotube in film-forming process simultaneously, can reduce the carbon nanotube performance.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method of carbon nano-tube film is provided, carbon nanotube in the carbon nano-tube film that this method is comparatively simple, efficient is higher and prepared can keep the integrity of its chemical structure well, and is evenly distributed.Simultaneously, its thickness also can be regulated and control as required.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
The first step, carbon nanometer tube material joined adopt ultrasonication, high-strength stir process or high-pressure homogeneous processing to disperse in the dispersion liquid, obtain the carbon nanotube dispersion liquid;
Described carbon nanometer tube material is a kind of or its modified product in Single Walled Carbon Nanotube, double-walled carbon nano-tube or the multi-walled carbon nano-tubes.
Described dispersion liquid is meant that mass percent concentration is the aqueous solution that 5% gum arabic or lid are carried the glue or derivatives thereof.
The concentration of carbon nanometer tube material is 0.1～5mg/mL in the described carbon nanotube dispersion liquid.
Second step, employing suction funnel suction filtration carbon nanotube dispersion liquid carry out the carbon nanotube settling that depositing treatment obtains to be attached to filter membrane, then by removing liquid or water is removed dispersion agent, at last the carbon nanotube settling is combined with substrate to remove filter membrane, obtain carbon nano-tube film.
Describedly remove dispersion agent and be meant by removing liquid or water: the carbon nanotube settling that will be attached to filter membrane places and removes liquid or water soaked more than 24 hours, and wherein every interval was changed and removed liquid or water once in 8 hours, and the dispersion agent in the filter membrane is removed the most at last.
The described liquid that removes is meant a kind of in 0.1M hydrochloric acid, 0.1M sodium hydroxide or the 1000IU proteolytic ferment buffered soln.
Described combining with substrate is meant to remove filter membrane: with desorption the sedimental filter membrane of carbon nanotube that is attached with of dispersion agent place on the base material, the carbon nanotube settling is combined with substrate material surface, after the compacting 90 ℃ of following vacuum-dryings 1 hour, in bathing, organic solvent steam removes filter membrane then, place 60 ℃ of following vacuum-dryings at last, obtain carbon nano-tube film.
Described base material is silicon chip or sheet glass.
Described organic solvent is an acetone.
Compared with prior art, the thickness that the present invention prepares the carbon nano-tube film of gained is controlled at more than 50 nanometers as required, its electroconductibility increases with the increase of film thickness, and can control by the control film thickness, this carbon nano-tube film can reach 97.5% in the transmitance of wavelength 550nm place visible light simultaneously, this method can thickness and the area density to carbon nano-tube film be controlled in preparation process, and operation is simple, is easy to practical application.
Description of drawings
Fig. 1 is an embodiment carbon nano-tube film synoptic diagram.
Fig. 2 is an embodiment carbon nano-tube film SEM photo.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Present embodiment may further comprise the steps:
1: use the gum arabic dispersion liquid that carbon nanotube powder is disperseed, the carbon nanotube dispersion liquid of preparation favorable dispersity.
In the present embodiment, the carbon nanotube dispersion liquid adopts physical method to disperse, and its concrete steps comprise: (a) 0.5g carbon nanotube powder and 5% gum arabic are disperseed liquid-phase mixing; (b) with about 5 ~ 8 hours of above-mentioned carbon nanotube dispersion liquid high-speed stirring; (c) the carbon nanotube dispersion liquid after stirring was carried out supersound process about 15～60 minutes.(d) after ultrasonic, continue to stir 2 hours.This dispersion liquid is good dispersion and stable carbon nanotube dispersion liquid.Carbon pipe in the dispersion liquid is many to be existed with single form, and this dispersion liquid can keep stablizing in 3 months, and sedimentation does not take place.
2: the preparation carbon nano-tube film.
Present embodiment is deposited on filter membrane by suction filtration with carbon nanotube with gained carbon nanotube dispersion liquid in the step 1, forms half wet carbon nano-tube film.The thickness of carbon nano-tube film is controlled by the controlling carbon nanotube deposition;
Remove the dispersion agent that is adsorbed in carbon nano tube surface, and remove filter membrane.
In the present embodiment, gained half wet carbon nano-tube film treatment step comprises in the step 2: (a) will be soaked in the filter membrane of carbon nano-tube film in the 0.1M hydrochloric acid more than 24 hours, and remove liquid once every replacing in 8 hours; (b) above-mentioned carbon nano-tube film is placed base material, compacting, 90oC vacuum-drying 1 hour; (c) dried carbon nano-tube film is placed acetone steam bathe and interiorly remove filter membrane more than 1 hour; (d) with the carbon nano-tube film that obtains 60oC vacuum-drying 12 hours, can obtain combining firm carbon nano-tube film with base material, its performance is as shown in table 1:
| Thickness (nm) | Transmitance (%, 550nm) |
| 53 | 97.5 |
| 96 | 88.3 |
| 127 | 65.5 |
| 142 | 55.2 |
Claims (7)
1. the preparation method of a carbon nano-tube film is characterized in that, may further comprise the steps:
The first step, carbon nanometer tube material joined adopt ultrasonication, high-strength stir process or high-pressure homogeneous processing to disperse in the dispersion liquid, obtain the carbon nanotube dispersion liquid;
Second step, employing suction funnel suction filtration carbon nanotube dispersion liquid carry out the carbon nanotube settling that depositing treatment obtains to be attached to filter membrane, then by removing liquid or water is removed dispersion agent, at last the carbon nanotube settling is combined with substrate to remove filter membrane, obtain carbon nano-tube film.
2. the preparation method of carbon nano-tube film according to claim 1 is characterized in that, described carbon nanometer tube material is a kind of or its modified product in Single Walled Carbon Nanotube, double-walled carbon nano-tube or the multi-walled carbon nano-tubes.
3. the preparation method of carbon nano-tube film according to claim 1 is characterized in that, described dispersion liquid is meant that mass percent concentration is the aqueous solution that 5% gum arabic or lid are carried the glue or derivatives thereof.
4. the preparation method of carbon nano-tube film according to claim 1 is characterized in that, the concentration of carbon nanometer tube material is 0.1～5mg/mL in the described carbon nanotube dispersion liquid.
5. the preparation method of carbon nano-tube film according to claim 1, it is characterized in that, describedly remove dispersion agent and be meant by removing liquid or water: the carbon nanotube settling that will be attached to filter membrane places and removes liquid or water soaks more than 24 hours, wherein every interval 8 hours is changed and is removed liquid or water once, and the dispersion agent in the filter membrane is removed the most at last.
6. the preparation method of carbon nano-tube film according to claim 1 is characterized in that, the described liquid that removes is meant 0.1M hydrochloric acid, 0.1M sodium hydroxide or 1000IU proteolysis enzyme aqueous solution.
7. the preparation method of carbon nano-tube film according to claim 1, it is characterized in that, described combining with substrate is meant to remove filter membrane: with desorption the sedimental filter membrane of carbon nanotube that is attached with of dispersion agent place on the base material, the carbon nanotube settling is combined with substrate material surface, after the compacting 90 ℃ of following vacuum-dryings 1 hour, in organic solvent steam is bathed, remove filter membrane then, place 60 ℃ of following vacuum-dryings at last, obtain carbon nano-tube film.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102110489A (en) * | 2010-12-24 | 2011-06-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Ultrathin film of transparent high-strength and high-conductivity electrical self-supporting carbon nano-tube and preparation method thereof |
| CN103316597A (en) * | 2013-07-01 | 2013-09-25 | 大连理工大学 | Carbon-nanotube hollow fiber membrane |
| CN103342471A (en) * | 2013-07-05 | 2013-10-09 | 西北师范大学 | Photoelectric nanometer composite membrane material and preparation method and application thereof |
| CN103395770A (en) * | 2013-08-01 | 2013-11-20 | 山东建筑大学 | Preparation method for stable carbon nanotube aqueous dispersion |
| CN103808247A (en) * | 2012-11-06 | 2014-05-21 | 沈阳航空航天大学 | Preparation method for strain sensor based on carbon nano tube three-dimensional network film |
| CN104174299A (en) * | 2014-07-30 | 2014-12-03 | 中国海洋大学 | High-flux positive osmosis membrane based on ultrathin support layer and preparation method thereof |
| CN104591125A (en) * | 2014-12-30 | 2015-05-06 | 广州聚能生物科技有限公司 | Method for dispersing one-dimensional or two-dimensional nanometer material |
| CN105551824A (en) * | 2015-12-17 | 2016-05-04 | 上海奥威科技开发有限公司 | Self-support supercapacitor free of metallic current collector |
| CN105565295A (en) * | 2015-12-31 | 2016-05-11 | 北京化工大学 | Preparation method of oriented carbon nanotube film |
| CN106413949A (en) * | 2014-05-22 | 2017-02-15 | 株式会社Lg化学 | Method for preparing carbon nanotube, and dispersion composition of carbon nanotube |
| CN107001046A (en) * | 2014-12-25 | 2017-08-01 | 日本瑞翁株式会社 | Carbon nano-tube film and its manufacture method |
| CN107570111A (en) * | 2016-07-04 | 2018-01-12 | 中国科学院金属研究所 | Height is adsorbed with the preparation method and application of engine dyeing material list wall carbon nano tube flexible membrane |
| CN110126384A (en) * | 2019-05-30 | 2019-08-16 | 哈尔滨工业大学 | Multi-wall carbon nano-tube film and galss fiber reinforced resin composite material and preparation method and application |
| CN110171815A (en) * | 2019-06-19 | 2019-08-27 | 昆明物理研究所 | A kind of preparation method of the high-purity carbon nano-tube film of low cost |
| CN110407164A (en) * | 2019-06-24 | 2019-11-05 | 东华大学 | A kind of preparation method and application of carbon nanotube polymer composite membrane |
| CN113651314A (en) * | 2021-09-08 | 2021-11-16 | 湖北中烟工业有限责任公司 | Preparation method of highly oriented carbon nanotube transparent film |
| CN115340085A (en) * | 2022-05-12 | 2022-11-15 | 中山大学 | Carbon nanotube film with controllable surface density and preparation method and application thereof |
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2009
- 2009-10-30 CN CN200910309105A patent/CN101691280A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102110489B (en) * | 2010-12-24 | 2012-08-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Ultrathin film of transparent high-strength and high-conductivity electrical self-supporting carbon nano-tube and preparation method thereof |
| CN102110489A (en) * | 2010-12-24 | 2011-06-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Ultrathin film of transparent high-strength and high-conductivity electrical self-supporting carbon nano-tube and preparation method thereof |
| CN103808247A (en) * | 2012-11-06 | 2014-05-21 | 沈阳航空航天大学 | Preparation method for strain sensor based on carbon nano tube three-dimensional network film |
| CN103808247B (en) * | 2012-11-06 | 2016-05-25 | 沈阳航空航天大学 | A kind of strain transducer preparation method based on CNT three-dimensional network film |
| CN103316597A (en) * | 2013-07-01 | 2013-09-25 | 大连理工大学 | Carbon-nanotube hollow fiber membrane |
| CN103342471B (en) * | 2013-07-05 | 2015-10-21 | 西北师范大学 | A kind of Photoelectric nanometer composite membrane material and its preparation method and application |
| CN103342471A (en) * | 2013-07-05 | 2013-10-09 | 西北师范大学 | Photoelectric nanometer composite membrane material and preparation method and application thereof |
| CN103395770A (en) * | 2013-08-01 | 2013-11-20 | 山东建筑大学 | Preparation method for stable carbon nanotube aqueous dispersion |
| CN106413949B (en) * | 2014-05-22 | 2019-04-26 | 株式会社Lg化学 | It is used to prepare the method and nanotube dispersion composition of carbon nanotube |
| US10435571B2 (en) | 2014-05-22 | 2019-10-08 | Lg Chem, Ltd. | Method for preparing carbon nanotube, and dispersion composition of carbon nanotube |
| CN106413949A (en) * | 2014-05-22 | 2017-02-15 | 株式会社Lg化学 | Method for preparing carbon nanotube, and dispersion composition of carbon nanotube |
| CN104174299B (en) * | 2014-07-30 | 2017-06-23 | 中国海洋大学 | High flux forward osmosis membrane based on ultra-thin supporting layer and preparation method thereof |
| CN104174299A (en) * | 2014-07-30 | 2014-12-03 | 中国海洋大学 | High-flux positive osmosis membrane based on ultrathin support layer and preparation method thereof |
| US10207929B2 (en) | 2014-12-25 | 2019-02-19 | Zeon Corporation | Carbon nanotube film and method for producing same |
| CN107001046A (en) * | 2014-12-25 | 2017-08-01 | 日本瑞翁株式会社 | Carbon nano-tube film and its manufacture method |
| CN107001046B (en) * | 2014-12-25 | 2019-05-03 | 日本瑞翁株式会社 | Carbon nano-tube film and its manufacturing method |
| CN104591125A (en) * | 2014-12-30 | 2015-05-06 | 广州聚能生物科技有限公司 | Method for dispersing one-dimensional or two-dimensional nanometer material |
| CN105551824A (en) * | 2015-12-17 | 2016-05-04 | 上海奥威科技开发有限公司 | Self-support supercapacitor free of metallic current collector |
| CN105565295B (en) * | 2015-12-31 | 2018-06-26 | 北京化工大学 | A kind of preparation method of orientation carbon nanotube film |
| CN105565295A (en) * | 2015-12-31 | 2016-05-11 | 北京化工大学 | Preparation method of oriented carbon nanotube film |
| CN107570111A (en) * | 2016-07-04 | 2018-01-12 | 中国科学院金属研究所 | Height is adsorbed with the preparation method and application of engine dyeing material list wall carbon nano tube flexible membrane |
| CN110126384A (en) * | 2019-05-30 | 2019-08-16 | 哈尔滨工业大学 | Multi-wall carbon nano-tube film and galss fiber reinforced resin composite material and preparation method and application |
| CN110171815A (en) * | 2019-06-19 | 2019-08-27 | 昆明物理研究所 | A kind of preparation method of the high-purity carbon nano-tube film of low cost |
| CN110407164A (en) * | 2019-06-24 | 2019-11-05 | 东华大学 | A kind of preparation method and application of carbon nanotube polymer composite membrane |
| CN113651314A (en) * | 2021-09-08 | 2021-11-16 | 湖北中烟工业有限责任公司 | Preparation method of highly oriented carbon nanotube transparent film |
| CN115340085A (en) * | 2022-05-12 | 2022-11-15 | 中山大学 | Carbon nanotube film with controllable surface density and preparation method and application thereof |
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