CN108440753A - Carbon nano-tube/poly aniline/graphene composite and flexible film and preparation method thereof - Google Patents
Carbon nano-tube/poly aniline/graphene composite and flexible film and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/02—Polyamines
Abstract
A kind of carbon nano-tube/poly aniline/graphene composite and flexible film of present invention offer and preparation method thereof.This method includes：The carbon nanotube that step 1. crosses acidification is added in the acid solution containing aniline, and oxidant is added after ultrasound, and 12~36h is reacted at 0~25 DEG C, obtains the carbon nanotube of polyaniline-coated, carbon nanotube, aniline, oxidant mass ratio be 0.01~1：0.1~1：0.5~2；Step 2. takes the carbon nanotube of polyaniline-coated to be added in graphene dispersing solution, in 5~20 DEG C of ultrasounds, is then filtered, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.This method preparation process is easy, obtained composite and flexible film has flexible and chemical property well, polyaniline can be effectively compound with nano-carbon material, reduce the aggregation of nano-carbon material, the multiplying power property and cyclical stability for improving material, have wide practical use in wearable electronic.
Description
Technical field
The invention belongs to composite materials and thin film materials art, and in particular to a kind of carbon nano-tube/poly aniline/graphene is multiple
Close fexible film and preparation method thereof.
Background technology
With popularizing for intelligent terminal, wearable electronic shows huge market prospects.It prepares a kind of flexible
Electronic device highlighted further to substitute the importance of traditional hard electronic device.How the energy storage of flexible electronic devices is solved
Problem is one of the important prerequisite for realizing these flexible device mass markets.
Carbon nanotube, due to its excellent mechanical property, electric property, has extensively with graphene in field of electronic devices
Application prospect.But carbon nanotube and graphene are all because the specific surface area of their superelevation, is easy to happen reunion, limits him
Application.Polyaniline draws as one of most common conducting polymer because it is readily synthesized, regulatable chemical property
The highest attention of domestic and international scientist is played.But individually polyaniline material volume during electrochemistry cycle charge-discharge becomes
Change greatly, the poor disadvantage of stability also counteracts its application in electrode material field.Therefore, by by polyaniline and carbon nanometer
Pipe or graphene these nano-carbon materials are combined with each other, and will effectively solve polyaniline and carbon nanotube or graphene are respective lacks
Point.And three kinds of carbon nanotube, graphene and polyaniline Material claddings are formed into new composite system, the boundary between three kinds
Face acts on the performance that synergistic effect will increase homogenous material.
In work before, patent CN106169379A and patent CN106183316A first prepares carbon nanotube/stone
Black alkene laminated film, then respectively by microwave radiation technology polymeric method and situ aggregation method, polyaniline is grown in carbon nanotube/stone
Black alkene laminated film surface, to obtain carbon nano tube/graphene/polyaniline laminated film.But there is no reduce for this method
The aggregation situation of carbon nanotube and graphene, and polyaniline is only compounded in film surface, there is no polyphenyl inside film
Amine is unfavorable for three and synergistic effect promotion chemical property occurs.Patent CN106571237A is by multi-walled carbon nanotube, polyphenyl
The oxidation stone that amine, the graphene oxide electrostatic spinning together with other auxiliary agents obtain laminated film, but contains in this laminated film
Black alkene and other auxiliary agents are non-conductive, reduce its chemical property.Patent CN103897183A is first by carbon nanotube and graphite
Alkene is dispersed in water, and adding aniline monomer makes its polymerization, and base is adsorbed on finally by the composite material that electrostatic interaction is three
Bottom surface forms laminated film, but this laminated film is simply possible to use in gas sensor, cannot obtain self-supporting fexible film, no
It can be used to build ultracapacitor.Xi'an University of Technology Di is sparkling et al. first to prepare carbon nanotube paper, then heavy with electrochemical polymerization
Aniline is gathered, graphene is then adsorbed, prepares carbon nano-tube/poly aniline/graphene composite film of sandwich structure.But this
Method operating procedure is complicated, and process is cumbersome, and this sandwich structure be three kinds of materials macroscopic view it is compound, it is difficult to control is multiple
Close the internal structure of film.
Invention content
The present invention be to solve the above-mentioned problems and carry out, and it is an object of the present invention to provide a kind of orderly controllable carbon nanotube/
Polyaniline/graphene composite and flexible film and preparation method thereof, preparation process is easy, and can obtain large specific surface area, electricity
Hold the thin-film electrode material of function admirable.
The present invention to achieve the goals above, uses following scheme：
<Preparation method>
The present invention provides a kind of preparation method of carbon nano-tube/poly aniline/graphene composite and flexible film, and feature exists
In including the following steps：The carbon nanotube that step 1. crosses acidification is added in the acid solution containing aniline, and ultrasound is certain
Oxidant is added after time, 12~36h is reacted at 0~25 DEG C, obtains the carbon nanotube of polyaniline-coated；Step 2. takes polyaniline
The carbon nanotube of cladding is added in graphene dispersing solution, in 5~20 DEG C of ultrasound a period of times, is then filtered, obtains carbon and receive
Mitron/polyaniline/graphene composite and flexible film, wherein in step 1, carbon nanotube that acidification is crossed, aniline, oxidation
The mass ratio of agent three is followed successively by 0.01~1：0.1~1：0.5~2, acid solution uses salt acid for adjusting pH value.
Preferably, in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
In, it can also have the feature that：In step 1, the pH value of acid solution is 1~3.
Preferably, in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
In, it can also have the feature that：In step 1, ultrasonic time is 1~2h.
In the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film, can also have
There is such feature：In step 1, carbon nanotube be single-walled carbon nanotube, double-walled carbon nano-tube, in multi-walled carbon nanotube at least
It is a kind of.
It, can be in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
It has the feature that：In step 1, the acid of acidification is the concentrated sulfuric acid or concentrated nitric acid.
It, can be in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
It has the feature that：In step 1, oxidant is ammonium persulfate, iron chloride or potassium peroxydisulfate.
Preferably, in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
In, it can also have the feature that：In step 2, the carbon nanotube of 0.1~0.5g polyaniline-coateds, graphene point are often taken
The dosage of dispersion liquid is 10~100mL, a concentration of 0.1~10mg/mL.
Preferably, in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
In, it can also have the feature that：In step 2, dispersant used in graphene dispersing solution is distilled water, alcohol, two
At least one of methylformamide, chloroform.
Preferably, in the preparation method of carbon nano-tube/poly aniline according to the present invention/graphene composite and flexible film
In, it can also have the feature that：In step 2, ultrasonic time is 1~3h.
<Film>
The present invention also provides a kind of carbon nano-tube/poly aniline/graphene composite and flexible films, it is characterised in that：Film is
Using above-mentioned<Preparation method>Described in method be prepared.
The effect of invention
Carbon nano-tube/poly aniline provided by the present invention/graphene composite and flexible film and preparation method thereof has following
Advantage：
1, the carbon nanotube being acidified participates in the polymerisation process of aniline so that polyaniline-coated in carbon nano tube surface,
And then with filtered together after graphene ultrasonic mixing, realize the effective compound of three；
2, the carbon nanotube of polyaniline-coated is dispersed in graphene nanometer sheet, effectively reduces the poly- of nano-carbon material
Collection, enhances the interface interaction and synergistic effect of three, and carbon nanotube also reduces polyaniline in electrochemical process with graphene
In volume change so that the multiplying power that the cyclical stability of composite material all 90% or more, improves composite material is special
Property and cyclical stability；
3, preparation process is simple, low for equipment requirements, and obtained composite and flexible film has flexible and electrochemistry well
Performance has wide practical use in wearable electronic；
4, preparation process more safety and environmental protection.
Description of the drawings
Fig. 1 is carbon nano-tube/poly aniline/graphene composite and flexible film of the preparation of embodiment one when being bent different angle
Cyclic voltammetry curve；
Fig. 2 is the charging and discharging curve of carbon nano-tube/poly aniline/graphene composite and flexible film prepared by embodiment one；
Fig. 3 is carbon nano-tube/poly aniline/graphene composite and flexible film of the preparation of embodiment one in 1000 cycle charge discharges
Capacitance when electric keeps figure.
Specific implementation mode
Referring to the drawings to carbon nano-tube/poly aniline/graphene composite and flexible film according to the present invention and its system
Preparation Method is elaborated.
<Embodiment one>
Preparation method：
It is 1 that the pH value containing 0.1g aniline, which is added, with the multi-walled carbon nanotube that dense sulfuric acid treatment is crossed in 0.05g by step 1.
In solution, the ammonium persulfate of 0.5g is added after ultrasonic 1h, reaction for 24 hours, obtains the carbon nanotube of polyaniline-coated at 10 DEG C；
Step 2. takes the carbon nanotube of 0.1g polyaniline-coateds that the volume containing a concentration of 4mg/mL graphenes is added
The distilled water of 20mL is filtered in 10v ultrasound 2h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, as shown in Figures 1 to 3, the cycle volt when being bent different angle
Peace curve essentially coincides, and time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, the specific capacitance under 1A/g current densities is
Up to 430F/g, capacity retention is 92.3% under 1000 cycle charge-discharges.
<Embodiment two>
Preparation method：
Step 1. by the processed single-walled carbon nanotube of 0.1g concentrated nitric acids be added the pH value containing 0.5g aniline be 2 it is molten
In liquid, the iron chloride of 0.6g is added after ultrasonic 2h, 18h is reacted at 0 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. takes the carbon nanotube of 0.2g polyaniline-coateds that the volume containing a concentration of 6mg/mL graphenes is added
The distilled water of 40mL is filtered in 20 DEG C of ultrasound 3h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 412F/g,
Capacity retention is 91.4% under 1000 cycle charge-discharges.
<Embodiment three>
Preparation method：
The double-walled carbon nano-tube that step 1. crosses 0.6g with dense sulfuric acid treatment be added the pH value containing 0.8g aniline be 3 it is molten
In liquid, the potassium peroxydisulfate of 1.8g is added after ultrasonic 1h, 30h is reacted at 20 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. takes the carbon nanotube of 0.3g polyaniline-coateds that the volume containing a concentration of 2mg/mL graphenes is added
The distilled water of 100mL is filtered in 15 DEG C of ultrasound 1h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 386F/g,
Capacity retention is 92.8% under 1000 cycle charge-discharges.
<Example IV>
Preparation method：
Step 1. by the processed multi-walled carbon nanotube of 0.2g concentrated nitric acids be added the pH value containing 0.4g aniline be 1 it is molten
In liquid, the ammonium persulfate of 0.6g is added after ultrasonic 1.5h, reaction for 24 hours, obtains the carbon nanotube of polyaniline-coated at 10 DEG C；
Step 2. takes the carbon nanotube of 0.15g polyaniline-coateds that the volume containing a concentration of 3mg/mL graphenes is added
The distilled water of 50mL is filtered in 20 DEG C of ultrasound 2h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 407F/g,
Capacity retention is 93.1% under 1000 cycle charge-discharges.
<Embodiment five>
Preparation method：
It is 2 that the pH value containing 0.25g aniline, which is added, with the single-walled carbon nanotube that dense sulfuric acid treatment is crossed in 0.3g by step 1.
In solution, the iron chloride of 0.5g is added after ultrasonic 1h, 20h is reacted at 20 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. takes the carbon nanotube of 0.25g polyaniline-coateds that the volume containing a concentration of 4mg/mL graphenes is added
The distilled water of 70mL is filtered in 10 DEG C of ultrasound 1.5h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 435F/g,
Capacity retention is 91.6% under 1000 cycle charge-discharges.
<Embodiment six>
Preparation method：
The solution that the pH value containing 0.1g aniline is 1 is added with the carbon nanotube that dense sulfuric acid treatment is crossed in 0.01g by step 1.
In, the ammonium persulfate of 0.5g is added after ultrasonic 1h, 12h is reacted at 4 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. takes the carbon nanotube of 0.1g polyaniline-coateds that the volume containing a concentration of 0.1mg/mL graphenes is added
The distilled water of 10mL is filtered in 5 DEG C of ultrasound 3h, obtains carbon nano-tube/poly aniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 392F/g,
Capacity retention is 90.1% under 1000 cycle charge-discharges.
<Embodiment seven>
Preparation method：
The solution that the pH value containing 1.0g aniline is 3 is added in the processed carbon nanotube of 1.0g concentrated nitric acids by step 1.
In, the iron chloride of 2.0g is added after ultrasonic 2h, 36h is reacted at 25 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. take 0.5g polyaniline-coateds carbon nanotube be added graphene dispersing solution in, the graphene dispersing solution be containing
The distilled water for having the volume of a concentration of 10mg/mL graphenes to be 90mL is filtered then in 20 DEG C of ultrasound 3h, obtains carbon and receive
Mitron/polyaniline/graphene composite and flexible film.
Performance test：
Electrochemical Detection is carried out to fexible film obtained, the cyclic voltammetry curve when being bent different angle weighs substantially
It closes, time-measuring electric potential curve symmetric, the charge and discharge time is close to 1:1, specific capacitance under 1A/g current densities be up to 418F/g,
Capacity retention is 91.7% under 1000 cycle charge-discharges.
Above example is only the illustration done to technical solution of the present invention.Carbon nanometer according to the present invention
Pipe/polyaniline/graphene composite and flexible film and preparation method thereof is not merely defined in described in the embodiment above
Structure, but it is subject to claim limited range.Those skilled in the art of the invention are on the basis of the embodiment
Any modify or supplement or equivalence replacement done, all in the claim range claimed of the present invention.
Claims (10)
1. a kind of preparation method of carbon nano-tube/poly aniline/graphene composite and flexible film, which is characterized in that including walking as follows
Suddenly：
The carbon nanotube that step 1. crosses acidification is added in the acid solution containing aniline, and oxygen is added in ultrasound after a certain period of time
Agent reacts 12~36h at 0~25 DEG C, obtains the carbon nanotube of polyaniline-coated；
Step 2. takes the carbon nanotube of polyaniline-coated to be added in graphene dispersing solution, in 5~20 DEG C of ultrasound a period of times, then
It is filtered, obtains carbon nano-tube/poly aniline/graphene composite and flexible film,
Wherein, in step 1, acidification is crossed carbon nanotube, aniline, oxidant three mass ratio be followed successively by 0.01~1：
0.1~1：0.5~2.
2. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 1, the pH value of acid solution is 1~3.
3. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 1, ultrasonic time is 1~2h.
4. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 1, carbon nanotube is at least one in single-walled carbon nanotube, double-walled carbon nano-tube, multi-walled carbon nanotube
Kind.
5. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 1, the acid of acidification is the concentrated sulfuric acid or concentrated nitric acid.
6. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 1, oxidant is ammonium persulfate, iron chloride or potassium peroxydisulfate.
7. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 2, the carbon nanotube of 0.1~0.5g polyaniline-coateds is often taken, the dosage of graphene dispersing solution is 10~
100mL, a concentration of 0.1~10mg/mL.
8. the preparation method of carbon nano-tube/poly aniline according to claim 1 or claim 7/graphene composite and flexible film, special
Sign is：
Wherein, in step 2, dispersant used in graphene dispersing solution is distilled water, alcohol, dimethylformamide, chloroform
At least one of.
9. the preparation method of carbon nano-tube/poly aniline according to claim 1/graphene composite and flexible film, feature
It is：
Wherein, in step 2, ultrasonic time is 1~3h.
10. a kind of carbon nano-tube/poly aniline/graphene composite and flexible film, it is characterised in that：
It is prepared using the preparation method described in any one of the claims 1 to 9.
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| CN111138661A (en) * | 2020-01-19 | 2020-05-12 | 上海应用技术大学 | Preparation method and application of graphene/carbon nanotube/polyaniline composite material |
| CN111729685A (en) * | 2020-07-17 | 2020-10-02 | 安徽大学 | Electrocatalytic material and preparation method and application thereof |
| CN113410063A (en) * | 2021-06-17 | 2021-09-17 | 北京佰耐特能源科技有限公司 | Carbon nano tube composite electrode material and preparation method thereof |
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| CN111138661A (en) * | 2020-01-19 | 2020-05-12 | 上海应用技术大学 | Preparation method and application of graphene/carbon nanotube/polyaniline composite material |
| CN111729685A (en) * | 2020-07-17 | 2020-10-02 | 安徽大学 | Electrocatalytic material and preparation method and application thereof |
| CN111729685B (en) * | 2020-07-17 | 2022-09-30 | 安徽大学 | Electrocatalytic material and preparation method and application thereof |
| CN113410063A (en) * | 2021-06-17 | 2021-09-17 | 北京佰耐特能源科技有限公司 | Carbon nano tube composite electrode material and preparation method thereof |
| CN116254036A (en) * | 2023-05-15 | 2023-06-13 | 牛墨石墨烯应用科技有限公司 | Preparation method of graphene carbon nanotube heat conduction slurry |
| CN116254036B (en) * | 2023-05-15 | 2023-09-15 | 牛墨石墨烯应用科技有限公司 | Preparation method of graphene carbon nanotube heat conduction slurry |
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