CN109468711A - Carbon nanotube-graphene composite fibre and its preparation method and application - Google Patents
Carbon nanotube-graphene composite fibre and its preparation method and application Download PDFInfo
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- CN109468711A CN109468711A CN201811139979.5A CN201811139979A CN109468711A CN 109468711 A CN109468711 A CN 109468711A CN 201811139979 A CN201811139979 A CN 201811139979A CN 109468711 A CN109468711 A CN 109468711A
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- graphene oxide
- carbon nanotube
- graphene
- composite fibre
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
Abstract
The invention discloses a kind of carbon nanotube-graphene composite fibres and its preparation method and application to obtain graphene oxide spinning solution this method comprises: (1) carries out ultrasonic disperse after mixing graphene oxide progress with solvent；(2) the graphene oxide spinning solution is subjected to wet spinning, obtains graphene oxide fiber；(3) the graphene oxide fiber is placed in thermal chemical vapor deposition furnace, is continually fed into hydrogen and precursors gas is reacted, obtains carbon nanotube-graphene composite fibre.Mechanical property and the excellent carbon nanotube-graphene composite fibre of electric conductivity can be prepared using this method, and the preparation process is not necessarily to catalyst, have it is easy to operate, can prepare with scale the characteristics of.
Description
Technical field
The invention belongs to carbon material preparation fields, specifically, the present invention relates to carbon nanotube-graphene composite fibre and
Preparation method and application.
Background technique
Graphene is since 2004 are found, since its excellent conductive, thermally conductive, mechanical, electron mobility etc. is many
Performance becomes most potential carbon material.An important problem in graphene research application is grapheme material macroscopic view knot
The design of structure and effectively assembling.Zhejiang University in 2011 is prepared by the wet spinning of graphene oxide, the method for electronation
Go out Flexible graphene fiber, expands the application of graphene.But due to graphene sheet layer interaction force is small etc., at present
Graphene fiber either intensity or electric conductivity it is not ideal enough.To solve this problem, researchers are by will be same
Sample has the carbon nanotube of excellent mechanical performance and electric conductivity compound with graphene, supports two kinds of materials mutually, to mention
While high interior porosity, its mechanics and electric conductivity are improved.However carbon nanotube-graphene that prior art preparation obtains
Composite fibre mechanical property and electric conductivity are undesirable.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of carbon nanotube-graphene composite fibres and preparation method thereof
And application, mechanical property and the excellent carbon nanotube-graphene composite fibre of electric conductivity can be prepared using this method,
And the preparation process be not necessarily to catalyst, have it is easy to operate, can prepare with scale the characteristics of.
In one aspect of the invention, carbon nanotube-graphene composite fibre method is prepared the invention proposes a kind of.
According to an embodiment of the invention, the described method includes: (1) by graphene oxide progress mixed with solvent after carry out ultrasonic disperse,
Obtain graphene oxide spinning solution；(2) the graphene oxide spinning solution is subjected to wet spinning, obtains graphene oxide fibre
Dimension；(3) the graphene oxide fiber is placed in thermal chemical vapor deposition furnace, is continually fed into hydrogen and precursors gas
It is reacted, obtains carbon nanotube-graphene composite fibre.
Optional, in step (1), based on the graphene oxide of 1 parts by weight, the dosage of the solvent is 50~300 weights
Measure part.
Optional, in step (1), the solvent is by least one of water, dimethyl sulfoxide and dimethylformamide
Composition.
Optional, step (2) is carried out according to the following steps: by the graphene oxide spinning solution with 0.1~3mL/min's
The spinneret that extruded velocity is 50~300 μm by aperture, 1-5min is then stopped in coagulating bath, is then obtained after drying
The graphene oxide fiber.
Optional, the coagulating bath is made of at least one of ethyl alcohol, methanol, ethyl acetate, acetone and butanone.
Optional, step (3) is carried out according to the following steps: the graphene oxide fiber is placed in heat chemistry gas by (3-1)
In phase cvd furnace, the argon gas of 100~1000mL/min is passed through after vacuumizing；(3-2) heats up the thermal chemical vapor deposition furnace
To 500~1000 DEG C, it is continually fed into the hydrogen of 50~200mL/min and the precursors gas of 50~200mL/min, constant temperature
10-60min stops heating, closes hydrogen and precursors gas；(3-3) continues the argon for being passed through 100~1000mL/min
Gas is down to room temperature to the thermal chemical vapor deposition furnace and closes argon gas after the meeting, obtains the compound fibre of carbon nanotube-graphene
Dimension.
It is optional, in step (3-2), the precursors gas by acetylene, methane, butane and acetone at least
One of composition.
In another aspect of the invention, the invention proposes a kind of carbon nanotube-graphene composite fibres.According to this hair
Bright embodiment, the carbon nanotube-graphene composite fibre are prepared using the above method.
In an additional aspect of the present invention, the invention proposes a kind of electrodes.According to an embodiment of the invention, the electrode
It is prepared using above-mentioned carbon nanotube-graphene composite fibre.
In an additional aspect of the present invention, the invention proposes a kind of electronic devices.According to an embodiment of the invention, described
Electronic device has above-mentioned electrode.
Compared with prior art, preparation carbon nanotube-graphene composite fibre method of the application is with graphene oxide
For raw material, graphene oxide fiber is prepared using wet spinning technology, wherein the primary raw materials of graphene oxide is graphite, is come
Source is extensive, low in cost, and prepares graphene oxide with spy easy to operate, easy to implement using wet spinning technology
Then obtained graphene oxide is placed in thermal chemical vapor deposition furnace by point, graphene oxide fiber surface oxygen-containing functional group
Active Growth point is generated when decomposition, so that carbon nanotube growth in situ is in graphene oxide fiber surface, simultaneous oxidation graphene
Fiber obtains carbon nanotube-graphene composite fibre by being heat reduced to for graphene fiber, which is not necessarily to catalyst, tool
Have it is easy to operate, can prepare with scale the characteristics of, while obtained carbon nanotube-graphene composite fibre have it is flexible, high-strength
Degree, high-specific surface area and high conductivity feature, the performances such as the conduction of electrode can be significantly improved by being used for preparing electrode material,
And the electrode can make electronic device have excellent conductive characteristic for electronic device.
Detailed description of the invention
Fig. 1 is 1 gained carbon nanotube of embodiment-graphene composite fibre electron microscope；
Fig. 2 is 1 gained carbon nanotube of embodiment-graphene composite fibre electron microscope.
Specific embodiment
Below by the invention will be further described in conjunction with the embodiments, it is not limit that following embodiment, which is descriptive,
Qualitatively, this does not limit the scope of protection of the present invention.
In one aspect of the invention, carbon nanotube-graphene composite fibre method is prepared the invention proposes a kind of.
According to an embodiment of the invention, this method comprises:
S1: ultrasonic disperse is carried out after graphene oxide progress is mixed with solvent
In the step, graphene oxide is mixed with solvent, ultrasonic disperse then is carried out to mixed liquor, is aoxidized
Graphene spinning solution.Specifically, the graphene oxide based on 1 parts by weight, the dosage of solvent is 50~300 parts by weight, and molten
Agent is to be made of at least one of water, dimethyl sulfoxide and dimethylformamide, such as solvent can be by water, dimethyl sulfoxide
With one of dimethylformamide or a variety of formed with arbitrary proportion mixing.
S2: graphene oxide spinning solution is subjected to wet spinning
In the step, oxidation is prepared through wet spinning technology in the graphene oxide spinning solution that above-mentioned steps obtain
Graphene fiber.Specifically, graphene oxide spinning solution is passed through aperture with the extruded velocity of 0.1~3mL/min as 50~300
μm spinneret, then in coagulating bath stop 1~5min, then obtain graphene oxide fiber after drying, wherein solidification
Bath be made of at least one of ethyl alcohol, methanol, ethyl acetate, acetone and butanone, such as solidification liquid can by ethyl alcohol, methanol,
One of substances such as ethyl acetate, acetone, butanone or a variety of mixed with arbitrary proportion form.
S3: graphene oxide fiber is placed in thermal chemical vapor deposition furnace, is continually fed into hydrogen and precursors gas
Body is reacted
In the step, graphene oxide obtained above is placed in thermal chemical vapor deposition furnace, is passed through 100 after vacuumizing
The argon gas of~1000mL/min；Then thermal chemical vapor deposition furnace is warming up to 500~1000 DEG C, is continually fed into 50~200mL/
The hydrogen of min and the precursors gas of 50~200mL/min, constant temperature 10-60min stop heating, close hydrogen and reaction
Precursor gas；Continue the argon gas for being passed through 100~1000mL/min, is down to room temperature to thermal chemical vapor deposition furnace and closes argon after the meeting
Gas obtains carbon nanotube-graphene composite fibre, wherein precursors gas is by acetylene, methane, butane and acetone
At least one composition, such as precursors gas can be by one of substances such as acetylene, methane, butane, acetone or a variety of
It is formed with arbitrary proportion mixing.Precursor gas cracks in high temperature inert atmosphere generates carbon source, and in graphene oxide sheet
Active site grows to form carbon nanotube.Specifically, carbon nanotube mass accounts for graphene matter in carbon nanotube-graphene composite fibre
The 1~5% of amount.
Preparation carbon nanotube-graphene composite fibre method of the application is using graphene oxide as raw material, using wet process
Spining technology prepares graphene oxide fiber, wherein and the primary raw materials of graphene oxide is graphite, from a wealth of sources, low in cost,
And preparing graphene oxide using wet spinning technology has the characteristics that oxygen easy to operate, easy to implement, then will to obtain
Graphite alkene is placed in thermal chemical vapor deposition furnace, and graphene oxide fiber surface oxygen-containing functional group generates Active Growth when decomposing
Point so that carbon nanotube growth in situ is in graphene oxide fiber surface, simultaneous oxidation graphene fiber by be heat reduced to for
Graphene fiber, obtains carbon nanotube-graphene composite fibre, which is not necessarily to catalyst, have it is easy to operate, can scale
The characteristics of preparation, while there is obtained carbon nanotube-graphene composite fibre flexible, high-intensitive, high-specific surface area and height to lead
Electrical feature.
In another aspect of the invention, the invention proposes a kind of carbon nanotube-graphene composite fibres.According to this hair
Bright embodiment, the carbon nanotube-graphene composite fibre are prepared using method described above.The carbon is received as a result,
Mitron-graphene composite fibre has the characteristics that flexible, high-intensitive, high-specific surface area and high conductivity.
In an additional aspect of the present invention, the invention proposes a kind of electrodes.According to an embodiment of the invention, the electrode
It is prepared using carbon nanotube described above-graphene composite fibre.As a result, by using above-mentioned carbon nanotube-graphite
For alkene composite fibre as the material for preparing electrode, obtained electrode has the performances such as excellent conduction.
In an additional aspect of the present invention, the invention proposes a kind of electronic devices.According to an embodiment of the invention, described
Electronic device has electrode described above.As a result, electronic device has excellent conductive characteristic.Specifically, electronics device
Part can be supercapacitor, wearable flexible electronic device etc..
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment 1
(1) 1g graphene oxide and 200g deionized water are mixed, 1h is ultrasonically treated with 50KHz at room temperature, obtains oxygen
Graphite alkene spinning solution；
(2) the resulting graphene oxide spinning solution of step (1) is taken, with the extruded velocity of 0.5mL/min by internal diameter for 100
μm spinneret, solidify 2min in ethanol, collect it is dry after obtain continuous oxidation graphene fiber；
(3) the graphene oxide fiber that step (2) obtains is placed in thermal chemical vapor deposition furnace, is passed through after vacuumizing
The argon gas of 500mL/min；Then gaseous phase deposition stove is warming up to 600 DEG C, is continually fed into the hydrogen and 100mL/ of 100mL/min
The acetylene gas of min, constant temperature 20min stop heating, close hydrogen and precursors gas；Continue to be passed through 500mL/min's
Argon gas is down to room temperature to thermal chemical vapor deposition furnace and closes argon gas after the meeting, obtains carbon nanotube-graphene composite fibre.
The carbon nanotube being made-graphene composite fibre, diameter are about 30 μm, and carbon nanotube mass is graphene quality
2%.20~40 μm of the length of carbon nanotube grown, 107 nanometers of diameter (as illustrated in fig. 1 and 2).Composite fibre intensity is
600-900MPa, conductivity are greater than 106S/m, specific surface area about 450m2/g。
Embodiment 2
(1) 1g graphene oxide and 100g dimethyl sulfoxide are mixed, 1h is ultrasonically treated with 50KHz at room temperature, is obtained
Graphene oxide spinning solution；
(2) the resulting graphene oxide spinning solution of step (1) is taken, with the extruded velocity of 2mL/min by internal diameter for 200 μm
Spinneret, solidify 3min in acetone, collect it is dry after obtain continuous oxidation graphene fiber；
(3) the graphene oxide fiber that step (2) obtains is placed in thermal chemical vapor deposition furnace, is passed through after vacuumizing
The argon gas of 500mL/min；Then gaseous phase deposition stove is warming up to 800 DEG C, is continually fed into the hydrogen and 200mL/ of 200mL/min
The acetylene gas of min, constant temperature 30min stop heating, close hydrogen and precursors gas；Continue to be passed through 500mL/min's
Argon gas is down to room temperature to thermal chemical vapor deposition furnace and closes argon gas after the meeting, obtains carbon nanotube-graphene composite fibre.
Obtained carbon nanotube-graphene composite fibre, diameter are about 50 μm, and carbon nanotube mass is graphene quality
5%.40-60 μm of the length of carbon nanotube grown, about 400 nanometers of diameter.Composite fibre intensity is 600-800MPa, conductivity
Greater than 106S/m, specific surface area are about 300m2/g。
Embodiment 3
(1) 1g graphene oxide and 150g deionized water are mixed, 1h is ultrasonically treated with 50KHz at room temperature, obtains oxygen
Graphite alkene spinning solution；
(2) the resulting graphene oxide spinning solution of step (1) is taken, with the extruded velocity of 2mL/min by internal diameter for 200 μm
Spinneret, solidify 3min in acetone, collect it is dry after obtain continuous oxidation graphene fiber；
(3) the graphene oxide fiber that step (2) obtains is placed in thermal chemical vapor deposition furnace, is passed through after vacuumizing
The argon gas of 300mL/min；Then gaseous phase deposition stove is warming up to 900 DEG C, is continually fed into the hydrogen and 100mL/ of 100mL/min
The acetylene gas of min, constant temperature 30min stop heating, close hydrogen and precursors gas；Continue to be passed through 300mL/min's
Argon gas is down to room temperature to thermal chemical vapor deposition furnace and closes argon gas after the meeting, obtains carbon nanotube-graphene composite fibre.
Obtained carbon nanotube-graphene composite fibre, diameter are about 50 μm, and carbon nanotube mass is graphene quality
3%.20-40 μm of the length of carbon nanotube grown, about 200 nanometers of diameter.Composite fibre intensity 600-800MPa, conductivity are big
In 106S/m, specific surface area are about 300m2/g。
Embodiment 4
(1) 1g graphene oxide and 150g dimethylformamide are mixed, 1h is ultrasonically treated with 50KHz at room temperature, is obtained
To graphene oxide spinning solution；
(2) the resulting graphene oxide spinning solution of step (1) is taken, with the extruded velocity of 0.5mL/min by internal diameter for 100
μm spinneret, solidify 3min in ethyl acetate, collect it is dry after obtain continuous oxidation graphene fiber；
(3) the graphene oxide fiber that step (2) obtains is placed in thermal chemical vapor deposition furnace, is passed through after vacuumizing
The argon gas of 600mL/min；Then gaseous phase deposition stove is warming up to 500 DEG C, is continually fed into the hydrogen and 150mL/ of 150mL/min
The butane gas of min, constant temperature 15min stop heating, close hydrogen and precursors gas；Continue to be passed through 600mL/min's
Argon gas is down to room temperature to thermal chemical vapor deposition furnace and closes argon gas after the meeting, obtains carbon nanotube-graphene composite fibre.
Obtained carbon nanotube-graphene composite fibre, diameter are about 25 μm, and carbon nanotube mass is graphene quality
3%.20-40 μm of the length of carbon nanotube grown, about 50 nanometers of diameter.Composite fibre intensity 600-800MPa, conductivity are big
In 106S/m, specific surface area are about 500m2/g。
The above is only preferred embodiments of the invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as the protection scope that do not invent.
Claims (10)
1. a kind of prepare carbon nanotube-graphene composite fibre method, wherein include:
(1) ultrasonic disperse is carried out after mixing graphene oxide progress with solvent, obtains graphene oxide spinning solution；
(2) the graphene oxide spinning solution is subjected to wet spinning, obtains graphene oxide fiber；
(3) the graphene oxide fiber is placed in thermal chemical vapor deposition furnace, is continually fed into hydrogen and precursors gas
Body is reacted, and carbon nanotube-graphene composite fibre is obtained.
2. the method for claim 1, wherein in step (1), based on the graphene oxide of 1 parts by weight, the solvent
Dosage be 50~300 parts by weight.
3. the solvent is by water, dimethyl sulfoxide and dimethyl the method for claim 1, wherein in step (1)
At least one of formamide composition.
4. the method for claim 1, wherein step (2) is carried out according to the following steps: by the graphene oxide spinning
Liquid with the extruded velocity of 0.1~3mL/min by aperture for 50~300 μm of spinneret, then stop 1 in coagulating bath~
Then 5min obtains the graphene oxide fiber after drying.
5. method as claimed in claim 4, wherein the coagulating bath is by ethyl alcohol, methanol, ethyl acetate, acetone and butanone
At least one of composition.
6. the method for claim 1, wherein step (3) is carried out according to the following steps:
The graphene oxide fiber is placed in thermal chemical vapor deposition furnace by (3-1), is passed through 100~1000mL/ after vacuumizing
The argon gas of min；
The thermal chemical vapor deposition furnace is warming up to 500~1000 DEG C by (3-2), is continually fed into the hydrogen of 50~200mL/min
With the precursors gas of 50~200mL/min, constant temperature 10-60min stops heating, closes hydrogen and precursors gas
Body；
(3-3) continues the argon gas for being passed through 100~1000mL/min, is down to room temperature to the thermal chemical vapor deposition furnace and closes after the meeting
Argon gas obtains the carbon nanotube-graphene composite fibre.
7. method as claimed in claim 6, wherein in step (3-2), the precursors gas by acetylene, methane,
At least one of butane and acetone composition.
8. a kind of carbon nanotube-graphene composite fibre, wherein the carbon nanotube-graphene composite fibre is wanted using right
Method described in any one of 1-7 is asked to be prepared.
9. a kind of electrode, wherein the electrode is prepared into using carbon nanotube according to any one of claims 8-graphene composite fibre
It arrives.
10. a kind of electronic device, wherein the electronic device has electrode as claimed in claim 9.
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