CN106479175A - A kind of preparation method of self-supporting Graphene polyaniline nano-line composite - Google Patents

A kind of preparation method of self-supporting Graphene polyaniline nano-line composite Download PDF

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CN106479175A
CN106479175A CN201611131643.5A CN201611131643A CN106479175A CN 106479175 A CN106479175 A CN 106479175A CN 201611131643 A CN201611131643 A CN 201611131643A CN 106479175 A CN106479175 A CN 106479175A
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graphene
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CN106479175B (en
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王宏志
李林鹏
侯成义
李耀刚
张青红
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National Dong Hwa University
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Abstract

The present invention relates to a kind of preparation method of self-supporting Graphene polyaniline nano-line composite, the film that graphite oxide is fully dispersed in water, sucking filtration becomes self-supporting after reduction, goes out the composite of Graphene polyaniline nano-line with the method growth in situ of three sections of electric currents in the electrolytic solution.The composite being formed has multi-level nano-structure.Drastically increase the specific surface area of material.The method simple and reliable process, effective reduces cost, it is with a wide range of applications.

Description

A kind of preparation method of self-supporting Graphene-polyaniline nano-line composite
Technical field
The invention belongs to the preparation field of graphene composite material, receive particularly to a kind of self-supporting Graphene-polyaniline The preparation method of rice noodle composite.
Background technology
Graphene is as a kind of new two-dimension nano materials, widely studied by scientific circles in recent years.As a kind of single former Sub-pieces layer material, it is not only construction zero dimension fullerene quantum dot, the basic structural unit of one-dimensional CNT, and can be with structure Make the graphite of three-dimensional.Due to the crystal structure of its uniqueness, Graphene has many excellent physicochemical properties, as high mechanics Performance, thermal conductivity, quantum hall effect of charge mobility, big specific surface area and uniqueness etc..Therefore, it is also applied to A lot of aspects, including polymer composite, field-effect transistor, liquid crystal display, energy stores etc..
(electrical conductivity is 10 to have metallic conductance from reported first doped polyacetylenes such as Shirakawa in 19773～105S/ Cm since), various conductive high sons as PPy, PTH, poly- to styrene (PPV) and polyaniline (Polyaniline, PANI) and he Derivant come out one after another.PANI, because preparing easy, good stability, is the most organic conjugate conducting polymer of practical application One of thing.By multiple synthetic technology such as template synthesis method, self-assembly method, interfacial polymerization can prepare nanometer rods, nanotube, The polyaniline nano material that nanofiber etc. comes in every shape.The method of wherein Electrochemical self-assembly is simple, controlled, can be in no template In the case of directly prepare polyaniline nano-line.With the development of nanosecond science and technology, a polyaniline nano structure especially wiener The successful preparation of rice structure (as nano wire, nanotube, nanometer rods etc.) makes people recognize nano polyaniline in electric transmission, light Learn and the size of uniqueness that the aspect such as mechanics manifests and dimensionality effect, imply that polyaniline nano structure nano-sensor, point The field such as sub-conductor and photoelectric nano device structure has wide potential application foreground.
Content of the invention
The technical problem to be solved is to provide a kind of self-supporting Graphene-polyaniline nano-line composite Preparation method, method is easy, mild condition, and the composite being formed has multi-level nano-structure.Drastically increase material Specific surface area.The method simple and reliable process, effective reduces cost, it is with a wide range of applications.
A kind of preparation method of the self-supporting Graphene-polyaniline nano-line composite of the present invention, including：
(1) graphite oxide is added to the water, ultrasonic disperse, obtains graphite oxide dispersion, is then reduced, vacuum is taken out Filter, obtains the graphene film of self-supporting；
(2) as working electrode after the graphene film of above-mentioned self-supporting being processed with sodium lauryl sulphate SDS solution, As to electrode, in the electrolytic solution with the method for three sections of electric currents, on Graphene, growth in situ goes out polyaniline nano-line to platinized platinum, that is, Obtain self-supporting Graphene-polyaniline nano-line composite.
In described step (1), the concentration of graphite oxide dispersion is 0.01～1mg/mL.
In described step (1), reduction is specially：Under the conditions of magnetic agitation, hydrazine hydrate and ammonia are added graphite oxide dispersion In liquid, it is heated to 70～100 DEG C, and keeps 0.5～2h.
Graphene dispersing solution, hydrazine hydrate, the volume ratio of ammonia are 1500～2500:0.5～5:3～7.
The mass percentage concentration of described hydrazine hydrate is 80～85%, the mass percentage concentration of ammonia is 20～30%.
In described step (1), vacuum filtration is：Pvdf membrane sucking filtration with 0.22 μm of aperture.
The graphene film obtaining self-supporting in step (1) is annealed reduction at high temperature, specially：Under an argon atmosphere, 0.5～3h, annealing is maintained at 200～500 DEG C of high temperature.
In described step (2), the mass percentage concentration of sodium lauryl sulphate SDS solution is 0.01～5%.
In described step (2), electrolyte is the mixed liquor of aniline and perchloric acid, and wherein in electrolyte, the concentration of aniline is 0.1 ～1M, the concentration of perchloric acid are 0.5～1.0M.
In described step (2), the method for three sections of electric currents is：First with 0.1～0.05mA/cm2Process 0.1～1h, then with 0.08 ～0.03mA/cm2Process 2～5h, finally with 0.03～0.01mA/cm2Process 2～5h.
Self-supporting Graphene-application in terms of gas sensing for the polyaniline nano-line composite.
Beneficial effect
(1) preparation method is simple of the present invention, raw material is easy to get, mild condition；
(2) present invention grows the nano wire of polyaniline, its structure-controllable, boundary on graphene-based bottom by in-situ method Face combines stable.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of the self-supporting Graphene-polyaniline nano-line composite material surface of embodiment 1 preparation；
Fig. 2 is the surface sweeping electron microscope in the self-supporting Graphene-polyaniline nano-line composite section of embodiment 1 preparation；
Fig. 3 is the surface sweeping electron microscope of the self-supporting Graphene-polyaniline nano-line composite material surface of embodiment 3 preparation.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, people in the art Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Scope.
Embodiment 1
Then plus deionized water 80mL is made at room temperature, weigh graphite oxide 20mg, be placed in 150mL beaker, Then beaker is placed on supersound process 6h in Ultrasound Instrument by the graphite oxide dispersion of 0.25mg/mL, obtains graphite oxide dispersion Liquid.
In the state of magnetic agitation, the hydrazine hydrate (80%) of 40 μ L and the ammonia (25%) of 280 μ L is taken to be added to oxidation Reduced in graphite dispersing solution, place into and in oil bath pan, be heated to 95 DEG C, be incubated 1h.By graphite oxide dispersion 0.22nm The pvdf membrane in aperture carries out vacuum filtration, then deionized water cleaning, peels off, obtains the graphene film of self-supporting.By graphite Alkene thin film, under argon state, calcines 1h under the conditions of 400 DEG C, strengthens reduction effect.
The graphene film of self-supporting mass fraction is that 1% SDS solution cleans, and makes SDS molecule on area load.With Stainless steel electrode chuck is clamped to be put in electrolyte and is served as working electrode.There are 0.5M aniline and 1M perchloric acid in electrolyte. With platinized platinum when work is to electrode.Use 0.08mA/cm2Electric current density process 0.5h, then use 0.04mA/cm2Process 3h, finally use 0.02mA/cm2Process the composite that 3h obtains Graphene-polyaniline nano-line.
Fig. 1 be preparation graphene/polyaniline nano wire scanning electron microscope (SEM) photograph it can be seen that：Diameter is had on Graphene 100nm about polyaniline nano-line generation.
Embodiment 2
Then plus deionized water 80mL is made at room temperature, weigh graphite oxide 20mg, be placed in 150mL beaker, Then beaker is placed on supersound process 6h in Ultrasound Instrument by the graphite oxide dispersion of 0.25mg/mL, obtains graphite oxide dispersion Liquid.
In the state of magnetic agitation, the hydrazine hydrate (80%) of 40 μ L and the ammonia (25%) of 280 μ L is taken to be added to oxidation Reduced in graphite dispersing solution, place into and in oil bath pan, be heated to 95 DEG C, be incubated 1h.By graphite oxide dispersion 0.22nm The pvdf membrane in aperture carries out vacuum filtration, then deionized water cleaning, peels off, obtains the graphene film of self-supporting.By graphite Alkene thin film, under argon state, calcines 1h under the conditions of 400 DEG C, strengthens reduction effect.
The graphene film of self-supporting mass fraction is that 1% SDS solution cleans, and makes SDS molecule on area load.With Stainless steel electrode chuck is clamped to be put in electrolyte and is served as working electrode.There are 0.5M aniline and 1M perchloric acid in electrolyte. With platinized platinum when work is to electrode.Use 0.04mA/cm2Electric current density process 6.5h, on result Graphene do not have polyaniline nano The generation of line.
Embodiment 3
Then plus deionized water 80mL is made at room temperature, weigh graphite oxide 20mg, be placed in 150mL beaker, Then beaker is placed on supersound process 6h in Ultrasound Instrument by the graphite oxide dispersion of 0.25mg/mL, obtains graphite oxide dispersion Liquid.
In the state of magnetic agitation, the hydrazine hydrate (80%) of 40 μ L and the ammonia (25%) of 280 μ L is taken to be added to oxidation Reduced in graphite dispersing solution, place into and in oil bath pan, be heated to 95 DEG C, be incubated 1h.By graphite oxide dispersion 0.22nm The pvdf membrane in aperture carries out vacuum filtration, then deionized water cleaning, peels off, obtains the graphene film of self-supporting.By graphite Alkene thin film, under argon state, calcines 1h under the conditions of 400 DEG C, strengthens reduction effect.
The graphene film of self-supporting mass fraction is that 1% SDS solution cleans, and makes SDS molecule on area load.With Stainless steel electrode chuck is clamped to be put in electrolyte and is served as working electrode.There are 0.5M aniline and 1M hydrochloric acid in electrolyte.With Platinized platinum is when work is to electrode.Use 0.08mA/cm2Electric current density process 0.5h, then use 0.04mA/cm2Process 3h, finally use 0.02mA/cm2Process the composite that 3h obtains Graphene-polyaniline nano-line.Fig. 3 is that the graphene/polyaniline of preparation is received The scanning electron microscope (SEM) photograph of rice noodle it can be seen that：Have on Graphene diameter 100nm about polyaniline nano-line generation.

Claims (10)

1. a kind of preparation method of self-supporting Graphene-polyaniline nano-line composite, including：
(1) graphite oxide is added to the water, ultrasonic disperse, obtains graphite oxide dispersion, is then reduced, and vacuum filtration obtains Graphene film to self-supporting；
(2) as working electrode, platinized platinum after the graphene film of above-mentioned self-supporting being processed with sodium lauryl sulphate SDS solution As to electrode, in the electrolytic solution with the method for three sections of electric currents, on Graphene, growth in situ goes out polyaniline nano-line, that is, derive from Support Graphene-polyaniline nano-line composite.
2. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (1), the concentration of graphite oxide dispersion is 0.01～1mg/mL.
3. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (1), reduction is specially：Under the conditions of magnetic agitation, hydrazine hydrate and ammonia are added graphite oxide dispersion In liquid, it is heated to 70～100 DEG C, and keeps 0.5～2h.
4. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 3, it is special Levy and be：Described graphene oxide dispersion, hydrazine hydrate, the volume ratio of ammonia are 1500～2500:0.5～5:3～7, hydration Hydrazine mass percentage concentration is 80～85%, and ammonia mass percentage concentration is 20～30%.
5. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (1), vacuum filtration is：Pvdf membrane sucking filtration with 0.22 μm of aperture.
6. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：The graphene film obtaining self-supporting in step (1) is annealed reduction at high temperature, specially：Under an argon atmosphere, high 0.5～3h, annealing is maintained at 200～500 DEG C of temperature.
7. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (2), the mass percentage concentration of sodium lauryl sulphate SDS solution is 0.01～5%.
8. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (2), electrolyte is the mixed liquor of aniline and perchloric acid, and wherein in electrolyte, the concentration of aniline is 0.1 ～1M, the concentration of perchloric acid are 0.5～1.0M.
9. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, it is special Levy and be：In described step (2), the method for three sections of electric currents is：First with 0.1～0.05mA/cm2Process 0.1～1h, then with 0.08 ～0.03mA/cm2Process 2～5h, finally with 0.03～0.01mA/cm2Process 2～5h.
10. the preparation method of a kind of self-supporting Graphene-polyaniline nano-line composite according to claim 1, its It is characterised by：Self-supporting Graphene-application in terms of gas sensing for the polyaniline nano-line composite.
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