CN103030130A - Method for self-assembling carbon nano tubes in water by regulating temperature to guide polymer to modify carbon nano tubes - Google Patents
Method for self-assembling carbon nano tubes in water by regulating temperature to guide polymer to modify carbon nano tubes Download PDFInfo
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Abstract
The invention relates to a method for self-assembling carbon nano tubes in water by regulating the temperature to guide polymer to modify the carbon nano tubes. The method comprises the following steps: adsorbing the polymer onto the surfaces of the carbon nano tubes; then dispersing the carbon nano tubes to which the polymer is adsorbed into the water; changing the temperature to enable the carbon nano tubes to be self-assembled in a solvent; and standing or centrifuging to separate a carbon nano tube self-assembling body. The self-assembling body is a carbon nano tube beam with a regular appearance and is formed by tightly arranging tens of to thousands of highly oriented carbon nano tubes in parallel. Self-assembly can centralize and enlarge excellent performance of the carbon nano tubes in the axial direction and enables the carbon nano tubes to have a wider application prospect. The method has simple steps and is easy to realize; the self-assembling operation is carried out in the water; a toxic organic solvent is not used; and the method is more environmental-friendly.
Description
Technical field
The present invention relates to a kind ofly by the method for the carbon nano-tube modified self-assembly in water of temperature adjustment directs polymer, the polymkeric substance of utilize selecting carries out finishing to carbon nanotube, makes carbon nanotube have the ability of self-assembly in water.The method can obtain, and carbon nanotube height-oriented, that be arranged in parallel is restrained, and self-assembly neat appearance, size reach micron order.
Background technology
Japan Iijima has found carbon nanotube in 1991, this monodimension nanometer material is reeled and formed by single or multiple lift graphite, has hollow column type structure.Carbon nanotube has excellent machinery, optics, electricity and thermal property, can not only be as microelectronic components such as the probe of detecting instrument and sensor, nm-class conducting wires, and can also be used for preparing strongthener, electro-conductive material, thermally conductive material, photoelectric material and thermoelectric material.
Study at present morely to be how to improve the dispersed of carbon nanotube and with the consistency of body material, but finely dispersed carbon nanotube is all random arrangement, the mixed and disorderly carbon nanotube of arranging shows as isotropy, can not embody the characteristic of one-dimensional material.Carbon nanotube has great length-to-diameter ratio, shows anisotropy, the same performance that mechanics, conduction and the heat conductivility on it is axial makes progress higher than footpath far away.The tube bank of regular arrangement can the excellent properties on axially be concentrated single-root carbon nano-tube and amplified, and as microelectronic component, self-assembly has the application prospect more long-range than single-root carbon nano-tube.Self-assembly is added to body material, can make the special type function material of conduction, heat conduction, anisotropy of mechanical properties, can be widely used in aerospace, communications and transportation, field of wind power generation.
For realizing aligning and regular arrangement of carbon nanotube, carried out a large amount of work both at home and abroad, mainly contain " dry method " and " wet method " two kinds of approach.Wherein " dry method " by catalyzer " plantation " in default, regular masterplate or utilize extra electric field to guide carbon nano-tube oriented growth, thereby realize carbon nano-tube oriented arrangement and be arranged in parallel.With respect to " dry method ", " wet method " instigates carbon nanotube to realize aligning or regular arrangement in liquid.Have the researchist by carbon nanotube dispersed in the liquid of directed flow, realized aligning of carbon nanotube by field of flow.Also have the investigator by etch the micron-sized groove of a lot of on body material, make the carbon nanotube natural subsidence in groove, thus realize carbon nanotube orientation, be arranged in parallel.
Summary of the invention
The object of the present invention is to provide a kind of by the method for the carbon nano-tube modified self-assembly in water of temperature adjustment directs polymer
.
The method of passing through the carbon nano-tube modified self-assembly in solvent of temperature adjustment directs polymer that the present invention proposes, to carbon nano tube surface by Polymer adsorption, then absorption is had to the carbon nanotube dispersed of polymkeric substance in water, make carbon nanotube Rapid self assembly in water by changing temperature, can obtain the self-assembly of carbon nanotube by settled process or centrifuging.
Concrete steps are as follows:
(1): by carbon nanotube 0.1~10g and acid with strong oxidizing property 1~1 * 10
3mL mixes, and ultrasonication 0.5~12 hour, in 25~120 ℃ of oxidations 0.5~24 hour.Reaction finishes by deionized water dilution washing, filtering separation then, it is neutral that repetitive scrubbing to filtrate is, after drying the acidifying carbon nanotube;
(2): acidifying carbon nanotube 0.1~10g and 0.1~50g polymkeric substance that step (1) is obtained join 25~1 * 10
3in ml water, ultrasonic wave is disperseed 0.1~24 hour, in 35~45 ℃ of stirrings 1~72 hour, obtains polymer-modified carbon nanotube, and the adsorption rate of polymkeric substance is 30 ~ 80%(polymer quality/polymer quality and carbon nanotube quality sum);
(3): absorption is increased to 50~80 ℃ by temperature, with 10 after finishing
2r/min ~ 10
6centrifugal 0.1~8 hour of r/min speed, obtain the carbon nanotube self-assembly at container bottom; Carbon nanotube self-assembly tube bank length is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
In the present invention, carbon nanotube described in step (1) is any multi-walled carbon nano-tubes prepared in arc-over, chemical gaseous phase deposition, template, sun power method or laser evaporation method or the mixture that mixes with its arbitrary proportion.The length of carbon nanotube is 5 ~ 100 μ m, and diameter is 5 ~ 25nm.
In the present invention, acid with strong oxidizing property described in step (2) is any or its multiple combination in 1~90% weight acid concentration nitric acid, 1~98% weight acid concentration sulfuric acid, 1 ∕ 100~100 ∕ 1 mol ratio nitric acid and sulfuric acid mixed solution.
In the present invention, the described polymkeric substance of step (2) comprises: in hydroxypropylcellulose, Natvosol, Vltra tears or polyvinyl alcohol any.The molecular weight of polymkeric substance is 1 * 10
3~ 1 * 10
5.
The method of passing through the carbon nano-tube modified self-assembly in water of temperature adjustment directs polymer that the present invention proposes, concrete steps are as follows:
(1): carbon nanotube 0.1~10g and 0.1~50g polymkeric substance are joined to 25~2.5 * 10
3in the ml dispersion agent, ultrasonic wave is disperseed 0.1~24 hour, in 35~45 ℃, stirs 1~72 hour.After absorption finishes with 10
2r/min ~ 10
6centrifugal 0.1~8 hour of r/min speed, bottom settlings is after the deionized water dilution disperseing by ultrasonic wave, and recentrifuge separates, and 5~20 times repeatedly, make polymer-modified carbon nanotube, the adsorption rate of polymkeric substance is 5 ~ 60%;
(2): by the polymer-modified carbon nanotube dispersed that obtains in step (1), in dispersion agent, the concentration of dispersion system is 0.01mg/ml ~ 1mg/ml.Temperature is reduced to 15~40 ℃, standing 1~48 hour, at container bottom, collects the carbon nanotube self-assembly.The length of self-assembly is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
Perhaps: by the polymer-modified carbon nanotube dispersed that obtains in step (1), in dispersion agent, the concentration of dispersion system is 0.01mg/ml ~ 1mg/ml.Temperature is reduced to 15~40 ℃, and 10
2r/min ~ 10
4centrifugal 0.1~4 hour of r/min speed, collect the carbon nanotube self-assembly at container bottom.The length of self-assembly is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
In the present invention, carbon nanotube described in step (1) is any multi-walled carbon nano-tubes prepared in arc-over, chemical gaseous phase deposition, template, sun power method or laser evaporation method or the mixture that mixes with its arbitrary proportion.The length of carbon nanotube is 5 ~ 100 μ m, and diameter is 5 ~ 25nm.
In the present invention, the described polymkeric substance of step (1) comprises: in hydroxypropylcellulose, Natvosol, Vltra tears or polyvinyl alcohol any.The molecular weight of polymkeric substance is 1 * 10
3~ 1 * 10
5.
In the present invention, dispersion agent described in step (1) and step (2) is a kind of or its multiple combination in methyl alcohol, ethanol, propyl alcohol, Virahol, formic acid, acetic acid, acetone, tetrahydrofuran (THF) or dimethyl formamide.
Step of the present invention is simple, easily realization, can in water, realize the self-assembly of carbon nanotube.The self-assembly shape of micron level is regular, and in assembly, carbon nanotube is height-oriented, closely be arranged in parallel.For carbon nanotube has been opened up new Application Areas.
The accompanying drawing explanation
Fig. 1: embodiment 1 carbon nanotube self-assembly opticmicroscope transmission photo;
Fig. 2: embodiment 2 carbon nanotube self-assembly opticmicroscope transmission photos;
Fig. 3: embodiment 3 carbon nanotube self-assembly stereoscan photographs.
Embodiment
The following examples are to further illustrate of the present invention, rather than limit the scope of the invention.
Embodiment 1: multi-walled carbon nano-tubes prepared with arc discharge method by 500mg (pipe external diameter ≈ 15nm) adds in 150ml concentrated nitric acid (65%), and ultrasonic wave is disperseed 10 minutes, 60 ℃ of oxidations 12 hours.Reaction finishes by deionized water dilution washing, and filtering separation, until filtrate is neutral.50 ℃ of vacuum-dryings obtain the acidifying carbon nanotube in 24 hours; Acidifying carbon nanotube and each 200mg of methylcellulose gum are added in 50ml water, and ultrasonic wave is disperseed 10 minutes, and 40 ℃ adsorb 48 hours, obtain the carbon nanotube of high methylcellulose gum adsorptive capacity.After absorption finishes, temperature is increased to 80 ℃, with the speed of 10000r/min centrifugal 30 minutes, at container bottom, obtains the carbon nanotube self-assembly.Carbon nanotube self-assembly tube bank length is that 25 ~ 40 μ m, diameter are 3 ~ 6 μ m.
Embodiment 2: multi-walled carbon nano-tubes prepared with chemical Vapor deposition process by 500mg (pipe external diameter ≈ 15nm) adds in 150ml concentrated nitric acid (65%), and ultrasonic wave is disperseed 10 minutes, 60 ℃ of oxidations 12 hours.Reaction finishes by deionized water dilution washing, and filtering separation, until filtrate is neutral.50 ℃ of vacuum-dryings obtain the acidifying carbon nanotube in 24 hours; Acidifying carbon nanotube and each 200mg of hydroxypropylcellulose are added in 50ml ethanol, ultrasonic wave is disperseed 10 minutes, 40 ℃ adsorb 48 hours, centrifugation after finishing, bottom settlings is after deionized water dilution washing disperseing by ultrasonic wave, recentrifuge separates, and 2 times repeatedly, makes the carbon nanotube of high hydroxypropylcellulose adsorptive capacity.It is dispersed in water, and temperature is increased to 60 ℃, standing 24 hours, can collect the carbon nanotube self-assembly at container bottom.The length of self-assembly is that 25 ~ 40 μ m, diameter are 3 ~ 6 μ m.
Embodiment 3: multi-walled carbon nano-tubes that will be standby with the laser evaporation legal system (pipe external diameter ≈ 15nm) and each 200mg of Natvosol add in 50ml methyl alcohol, and ultrasonic wave is disperseed 10 minutes, and 55 ℃ adsorb 48 hours.Centrifugation after end, bottom settlings is after deionized water dilution washing disperseing by ultrasonic wave, and recentrifuge separates, and 10 times repeatedly, makes the carbon nanotube that hangs down the Natvosol adsorptive capacity.It is dispersed in water, and temperature is reduced to 20 ℃, standing 48 hours, can collect the carbon nanotube self-assembly at container bottom.The length of self-assembly is that 25 ~ 40 μ m, diameter are 3 ~ 6 μ m.
Embodiment 4: multi-walled carbon nano-tubes prepared with arc discharge method by 500mg (pipe external diameter ≈ 15nm) adds in 90ml concentrated nitric acid (65%) and the 30ml vitriol oil (98%), ultrasonic wave dispersion 10 minutes, 120 ℃ of oxidations 8 hours.Reaction finishes by deionized water dilution washing, and filtering separation, until filtrate is neutral.50 ℃ of vacuum-dryings obtain the acidifying carbon nanotube in 24 hours; Acidifying carbon nanotube and each 200mg of Vltra tears are added in 50ml water, and ultrasonic wave is disperseed 10 minutes, and 60 ℃ adsorb 48 hours, obtain the carbon nanotube of high Vltra tears adsorptive capacity.After absorption finishes, temperature is increased to 80 ℃, with the speed of 10000r/min centrifugal 30 minutes, at container bottom, obtains the carbon nanotube self-assembly.Carbon nanotube self-assembly tube bank length is that 25 ~ 40 μ m, diameter are 3 ~ 6 μ m.
Embodiment 5: the multi-walled carbon nano-tubes that will prepare with chemical Vapor deposition process (pipe external diameter ≈ 15nm) and polyvinyl alcohol 1799 each 200mg add in 50ml acetone, then ultrasonic wave disperses 10 minutes, and 65 ℃ adsorb 48 hours.Centrifugation after finishing, bottom settlings is after deionized water dilution washing disperseing by ultrasonic wave, and recentrifuge separates, and 10 times repeatedly, makes the carbon nanotube of pure 1799 adsorptive capacitys of oligomerisation of ethylene.It is dispersed in water, and temperature is reduced to 15~40 ℃, with 4000 r/min speed centrifugal 15 minutes, at container bottom, collects the carbon nanotube self-assembly.The length of self-assembly is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
The above-mentioned description to embodiment is to understand and apply the invention for the ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and the improvement that the present invention is made and modification all should be within protection scope of the present invention.
Claims (7)
1. one kind by the method for the carbon nano-tube modified self-assembly in water of temperature adjustment directs polymer, it is characterized in that concrete steps are as follows:
(1): by carbon nanotube 0.1~10g and acid with strong oxidizing property 1~1 * 10
3mL mixes, and ultrasonication 0.5~12 hour, in 25~120 ℃ of oxidations 0.5~24 hour; Reaction finishes by deionized water dilution washing, filtering separation then, it is neutral that repetitive scrubbing to filtrate is, after drying the acidifying carbon nanotube;
(2): acidifying carbon nanotube 0.1~10g and 0.1~50g polymkeric substance that step (1) is obtained join 25~1 * 10
3in ml water, ultrasonic wave is disperseed 0.1~24 hour, in 35~45 ℃ of absorption 1~72 hour, obtains polymer-modified carbon nanotube, and the adsorption rate of polymkeric substance is that polymer quality/polymer quality and carbon nanotube quality sum are 30 ~ 80%;
(3): absorption is increased to 50~80 ℃ by temperature, with 10 after finishing
2r/min ~ 10
6centrifugal 0.1~8 hour of r/min speed, obtain the carbon nanotube self-assembly at container bottom; Carbon nanotube self-assembly tube bank length is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
2. one kind by the method for the carbon nano-tube modified self-assembly in water of temperature adjustment directs polymer, it is characterized in that concrete steps are as follows:
(1): carbon nanotube and each 0.1~10g of polymkeric substance are joined to 25~2.5 * 10
3in the ml dispersion agent, ultrasonic wave was disperseed 0.1~24 hour, in 35~45 ℃ of absorption 1~72 hour; After end with 10
2r/min ~ 10
6centrifugal 0.1~8 hour of r/min speed, bottom settlings is after the deionized water dilution disperseing by ultrasonic wave, and recentrifuge separates, and 5~20 times repeatedly, make polymer-modified carbon nanotube, the adsorption rate of polymkeric substance is 5 ~ 60%;
(2): by the polymer-modified carbon nanotube dispersed that obtains in step (1), in dispersion agent, the concentration of dispersion system is 0.01mg/ml ~ 1mg/ml.
3. temperature is reduced to 15~40 ℃, standing 1~48 hour, at container bottom, collects the carbon nanotube self-assembly; The length of self-assembly is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m;
Perhaps: by the polymer-modified carbon nanotube dispersed that obtains in step (1), in water, the concentration of dispersion system is 0.01mg/ml ~ 1mg/ml; Temperature is reduced to 15~40 ℃, and 10
2r/min ~ 10
4centrifugal 0.1~4 hour of r/min speed, collect the carbon nanotube self-assembly at container bottom; The length of self-assembly is 25 ~ 40 μ m, and diameter is 3 ~ 6 μ m.
4. method according to claim 1 and 2, is characterized in that carbon nanotube described in step (1) is any multi-walled carbon nano-tubes prepared in arc-over, chemical gaseous phase deposition, template, sun power method or laser evaporation method or the mixture that mixes with its arbitrary proportion; The length of carbon nanotube is 5 ~ 100 μ m, and diameter is 5 ~ 25nm.
5. method according to claim 1, is characterized in that acid with strong oxidizing property described in step (1) is any or its multiple combination in 1~90% weight acid concentration nitric acid, 1~98% weight acid concentration sulfuric acid, 1 ∕ 100~100 ∕ 1 mol ratio nitric acid and sulfuric acid mixed solution.
6. method according to claim 2, is characterized in that dispersion agent described in step (1) and step (2) is a kind of or its multiple combination in methyl alcohol, ethanol, propyl alcohol, Virahol, formic acid, acetic acid, acetone, tetrahydrofuran (THF) or dimethyl formamide.
7. method according to claim 1 and 2, is characterized in that described polymkeric substance is any or its multiple combination in methylcellulose gum, hydroxypropylcellulose, Natvosol, Vltra tears, polyvinyl alcohol, and the molecular weight of polymkeric substance is 1 * 10
3~ 1 * 10
5.
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CN104045056A (en) * | 2014-07-04 | 2014-09-17 | 中国科学院微电子研究所 | Manufacturing method for nanowire films/bodies accumulated in order |
CN110915008A (en) * | 2017-07-25 | 2020-03-24 | 国立大学法人奈良先端科学技术大学院大学 | Carbon nanotube composite and method for producing same |
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