CN102568646B - Fluorinated graphene oxide/polymer composite material and preparation method and application thereof - Google Patents
Fluorinated graphene oxide/polymer composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a fluorinated graphene oxide/polymer composite material and a preparation method and application thereof. The fluorinated graphene oxide/polymer composite material comprises fluorinated graphene oxide and polypyrrole which is deposited on the surface of the fluorinated graphene oxide and is prepared by performing in situ polymerization reaction on pyrrole monomers to generate the polypyrrole and depositing the polypyrrole on the surface of the fluorinated graphene oxide. The preparation method is simple in process, easy to operate and suitable for industrialized production; and the prepared fluorinated graphene oxide/polymer composite material has good properties and can be used for preparing electrodes of super capacitors and the like.
Description
Technical field
The present invention relates to electrode material, relate in particular to a kind of Fluorinated graphene oxide/polymer composite material and preparation method thereof, use.
Background technology
Since the strong K of the peace moral of Univ Manchester UK sea nurse (Andre K.Geim) etc. after 2004 prepare grapheme material, Graphene is because its unique structure and photoelectric property have been subject to people's extensive attention.Graphene is described as " nova " that is rising in material science and Condensed Matter Physics field, many novelties that it has and unique character and potential application are just attracting many scientific workers.
Single-layer graphene has large specific area, good conduction, heat conductivility and low thermal coefficient of expansion.As: 1. high strength, the Young mole, (1,100GPa), fracture strength: (125GPa); 2. high heat conductance, (5,000W/mK); 3. high conductivity, carrier transport rate, (200,000cm
2/ V*s); 4. high specific area, (calculated value: 2,630m
2/ g).Especially the structural property of the nanoscale of high conductivity matter, large specific surface character and monolayer two dimension, Graphene can be used as electrode material in ultracapacitor and lithium ion battery.
In addition, from Chinese patent CN101367516A as can be known, Yang Quanhong etc. are under vacuum degree 0.01Pa～10kPa, graphite oxide is warmed up to 150～600 ℃ with the heating rate of 5～50 ℃/min carries out high vacuum heat treatment, keep constant temperature 0.5～20h, the graphite oxide volume expands rapidly, obtains specific area 200～800m
2/ g, the graphene oxide material of electrochemical specific capacity 50～200F/g.Generally speaking, in the graphene oxide owing to contain-C-OH ,-C-O-C, even-groups such as COOH, thereby show stronger polarity.The dry aerial less stable of graphene oxide is easy to the moisture absorption and forms the aquation graphene oxide.
Summary of the invention
The technical problem to be solved in the present invention is, for the defective of Graphene in the prior art as electrode material, provides a kind of performance better Fluorinated graphene oxide/polymer composite material.
The technical problem that the present invention also will solve is, a kind of preparation method of Fluorinated graphene oxide/polymer composite material also is provided.
The technical problem that the present invention further will solve is, the application of above-mentioned Fluorinated graphene oxide/polymer composite material in the preparation electrode also is provided.
For reaching above-mentioned purpose, according to one aspect of the present invention, provide a kind of Fluorinated graphene oxide/polymer composite material, comprise Fluorinated graphene oxide and the polypyrrole that is deposited on described Fluorinated graphene oxide surface.
In the Fluorinated graphene oxide/polymer composite material of the present invention, preferably, described Fluorinated graphene oxide is made of the element of following mass percent:
C?50～70％
F?0～50％
O?0～40％
H?0～3％，
Wherein, the content of F, O and H all is not 0.
For reaching above-mentioned purpose, according to the present invention on the other hand, provide a kind of preparation method of Fluorinated graphene oxide/polymer composite material, may further comprise the steps:
1. Fluorinated graphene oxide is added dispersant for ultrasonic dispersion, forming concentration is the suspension of 0.2～2g/L;
2. in above-mentioned suspension, add pyrrole monomer, and ultrasonic dispersion, wherein, the mass ratio of Fluorinated graphene oxide and pyrrole monomer is 1: 2.9～1: 29;
3. add the aqueous solution of oxidant in step mixed liquor 2., and stir, wherein, the mass ratio of Fluorinated graphene oxide and oxidant is 1: 5～1: 50;
4. filtration step mixed liquor 3. obtains product, washing, and vacuumize namely gets Fluorinated graphene oxide/polymer composite material.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, the preparation method of described Fluorinated graphene oxide is: the graphite powder that with mass ratio is 2: 1: 1, in the concentrated sulfuric acid that potassium peroxydisulfate and phosphorus pentoxide adding are 70～90 ℃, stir, cooling, washing, dry, in the concentrated sulfuric acid with 0～20 ℃ of desciccate adding, and the potassium permanganate of 3 times of quality of adding graphite powder, keep mixture temperature below 20 ℃, 30～40 ℃ of oil bath 1.5～3h afterwards, add the deionized water that contains hydrogen peroxide, suction filtration, washing, ultrasonic dispersion, suction filtration again, dry, get graphene oxide, with fluorine gas reaction 0.5～24h under 20～200 ℃, namely get Fluorinated graphene oxide again.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, described dispersant is at least a in methyl alcohol, ethanol, ethylene glycol, the water.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, described oxidant is FeCl
36H
2O, (NH
4)
2S
2O
8, K
2S
2O
8, KMnO
4, K
2Cr
2O
7, H
2O
2In at least a.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, 1. described step is respectively 10～60min and 10～50min with the ultrasonic jitter time of step in 2..
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, 3. described step carries out under 0 ℃～25 ℃ temperature, and the mixing time of described step in 3. is 3～24h.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention, preferably, described step 4. in, with the washing of deionized water and acetone, and at 40 ℃～100 ℃ lower vacuumize 24～48h.
For reaching above-mentioned purpose, according to the present invention on the other hand, also provide the above-mentioned application of Fluorinated graphene oxide/polymer composite material in preparation electrode of super capacitor and lithium ion cell electrode.
Fluorinated graphene oxide/polymer composite material of the present invention, to generate polypyrrole by pyrrole monomer generation home position polymerization reaction, and be deposited on the Fluorinated graphene oxide surface and prepare, the Fluorinated graphene oxide/polymer composite material that obtains can be used for the preparation of electrode, for example for the preparation of high electrochemistry capacitance electrode of super capacitor and lithium ion cell electrode.
Fluorinated graphene oxide/polymer composite material of the present invention comprises Fluorinated graphene oxide and polypyrrole.Fluorinated graphite is than graphite oxide, and its stability and discharge capacity obviously improve.In addition, polypyrrole have higher room-temperature conductivity and completely reversibility electrochemical redox characteristic, stronger charge storage ability, be easy to synthesize, and in air, have preferably the advantage such as stability.Therefore, compound by the two, Fluorinated graphene oxide/polymer composite material of the present invention combines the advantage of Fluorinated graphene oxide and polypyrrole, and it has better performance as electrode material.
The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention is by the pyrrole monomer in-situ polymerization and be deposited on the Fluorinated graphene oxide surface forms, and has the advantages such as technique is simple, easy operating, suitable suitability for industrialized production.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the preparation method's of Fluorinated graphene oxide/polymer composite material of the present invention flow chart;
Fig. 2 is the SEM Electronic Speculum picture of Fluorinated graphene oxide/polymer composite material of the present invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples the present invention is further described in detail.
Fluorinated graphene oxide/polymer composite material of the present invention, comprise Fluorinated graphene oxide and the polypyrrole that is deposited on this Fluorinated graphene oxide surface, wherein, Fluorinated graphene oxide is respectively 50～70% C, 0～50% F, 0～40% O and 0～3% H by mass percent and forms, and the composition content of F, O and H element is all greater than 0.Fluorinated graphene oxide/polymer composite material of the present invention can be used for preparing electrode, for example the electrode of super capacitor of high electrochemistry capacitance and lithium ion cell electrode.
Below in conjunction with Fig. 1 the preparation method of Fluorinated graphene oxide/polymer composite material of the present invention is described.As shown in Figure 1, be the preparation method's of Fluorinated graphene oxide/polymer composite material of the present invention flow chart.The preparation method of Fluorinated graphene oxide/polymer composite material of the present invention may further comprise the steps:
1. Fluorinated graphene oxide is added dispersant for ultrasonic dispersion, forming concentration is the suspension of 0.2～2.0g/L.
Dispersant herein refers to alcohols dispersant or water, and the alcohols dispersant is such as being methyl alcohol, ethanol, ethylene glycol etc.Preferably, the time of ultrasonic dispersion is 10～60min.In addition, Fluorinated graphene oxide as the present invention's use, can be prepared by the known method of any appropriate, yet, preferably, the preparation method of the Fluorinated graphene oxide that the present invention uses is as follows: the graphite powder that with mass ratio is 2: 1: 1, in the concentrated sulfuric acid that potassium peroxydisulfate and phosphorus pentoxide adding are 70～90 ℃, stir, cooling, washing, dry, in the concentrated sulfuric acid with 0～20 ℃ of desciccate adding, and the potassium permanganate of 3 times of quality of adding graphite powder, keep mixture temperature below 20 ℃, 30～40 ℃ of oil bath 1.5～3h add the deionized water that contains hydrogen peroxide afterwards, suction filtration, washing, ultrasonic dispersion, suction filtration again, dry, get graphene oxide, with fluorine gas reaction 0.5～24h under 20～200 ℃, namely get Fluorinated graphene oxide again.
2. in the suspension of previous step, add pyrrole monomer, and ultrasonic dispersion, wherein, the mass ratio of Fluorinated graphene oxide and pyrrole monomer is 1: 2.9～1: 29.
In this step, the time of ultrasonic dispersion is preferably 10～50min.
3. add the aqueous solution of oxidant in the mixed liquor of previous step, and stir, wherein, the mass ratio of Fluorinated graphene oxide and oxidant is 1: 5～1: 50.
In this step, oxidant is preferably FeCl
36H
2O, (NH
4)
2S
2O
8, K
2S
2O
8, KMnO
4, K
2Cr
2O
7, H
2O
2In at least a.In addition, mixing time is preferably 3～24h.Although this step is not particularly limited, preferably, this step is carried out under 0 ℃～25 ℃ temperature.
4. the mixed liquor that filters previous step obtains product, washing, and vacuumize namely gets Fluorinated graphene oxide/polymer composite material.
In this step, preferably, washing adopts deionized water and acetone as washing lotion, and washs to filtrate colourless.In addition, vacuum drying condition is preferably: at 40 ℃～100 ℃ lower vacuumize 24～48h.
The preparation of embodiment 1 Fluorinated graphene oxide
The preparation of graphene oxide: 20g 50 order graphite powders (purity 99.5%), 10g potassium peroxydisulfate and 10g phosphorus pentoxide added in 80 ℃ the concentrated sulfuric acid, stir, more than the cooling 6h, washing is to neutral, drying.In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate, the temperature of mixture remains on below 20 ℃ again, then behind the maintenance 2h, slowly adds the 920mL deionized water in 35 ℃ oil bath.Behind the 15min, add 2.8L deionized water (wherein contain 50mL concentration be 30% hydrogen peroxide), the mixture color becomes glassy yellow afterwards again, and suction filtration while hot is that 10% hydrochloric acid washs with 5L concentration again.The brown color pastel of gained is joined ultrasonic dispersion 2-5h in the 5L distilled water, and suction filtration namely obtains graphene oxide at 50 ℃ of vacuumize 48h.
Fluoro-reaction prepares Fluorinated graphene oxide: the graphene oxide of drying is packed into passes into dry nitrogen 0.5-4h in the reactor, then passes into fluorine gas and graphene oxide at the 20-200 ℃ of lower 0.5-24h of reaction, namely can obtain Fluorinated graphene oxide.The gas that passes in the reactor is the fluorine nitrogen mixture, and fluorine gas accounts for the 5%-30% of mist, and nitrogen is as the diluent gas of fluorine.Its optimum reaction condition is to pass into fluorine gas to account for 10% fluorine nitrogen mixture gas react 1h about 100 ℃.
The Fluorinated graphene oxide of this step preparation is made of the element of following mass percent: 50～70% C, 0～50% F, 0～40% O and 0～3% H, wherein the content of F, O and H all is not 0.
The preparation of embodiment 2 Fluorinated graphene oxide/polymer composite materials
The 100mg Fluorinated graphene oxide is joined ultrasonic dispersion 10min in the 50mL methyl alcohol, so that it is uniformly dispersed.Then, add 0.3mL through the pyrrole monomer (analyzing pure) of heavily steaming and continue ultrasonic dispersion 10min formation mixed liquor.
Under 0 ℃, in above-mentioned mixed liquor, slowly be added dropwise to FeCl
36H
2O (content 0.5g) concentration is the aqueous solution of 0.5mol/L, and stirs 3h, makes the pyrrole monomer polymerization reaction take place.With reacting liquid filtering, the product that then filtration is obtained is used deionized water 200mL and acetone 200mL cyclic washing successively, until filtrate is colourless.At last, the black powder that washing is obtained through 40 ℃ of vacuumize 48h, namely gets Fluorinated graphene oxide/polymer composite material of the present invention in vacuum drying chamber.
Fig. 2 is the SEM Electronic Speculum picture of the Fluorinated graphene oxide/polymer composite material of this embodiment.As shown in Figure 2, in Fluorinated graphene oxide/polymer composite material of the present invention, the surface of Fluorinated graphene oxide lamella is coated by polypyrrole, has formed the composite material of sandwich structure.
The preparation of embodiment 3 Fluorinated graphene oxide/polymer composite materials
The 100mg Fluorinated graphene oxide is joined ultrasonic dispersion 60min in the 500mL water, so that it is uniformly dispersed.Then, add 3.0mL through the pyrrole monomer (analyzing pure) of heavily steaming and continue ultrasonic dispersion 50min formation mixed liquor.
Under 25 ℃, in above-mentioned mixed liquor, slowly be added dropwise to K
2S
2O
8The aqueous solution of (content 5.0g), and stir 24h, make the pyrrole monomer polymerization reaction take place.With reacting liquid filtering, the product that then filtration is obtained is used deionized water 200mL and acetone 200mL cyclic washing successively, until filtrate is colourless.At last, the black powder that washing is obtained through 100 ℃ of vacuumize 24h, namely gets Fluorinated graphene oxide/polymer composite material of the present invention in vacuum drying chamber.
The preparation of embodiment 4 Fluorinated graphene oxide/polymer composite materials
The 100mg Fluorinated graphene oxide is joined ultrasonic dispersion 30min in the 250mL ethanol, so that it is uniformly dispersed.Then, add 1.5mL through the pyrrole monomer (analyzing pure) of heavily steaming and continue ultrasonic dispersion 25min formation mixed liquor.
Under 15 ℃, in above-mentioned mixed liquor, slowly be added dropwise to (NH
4)
2S
2O
8(content 2.5g) concentration is the aqueous solution of 0.5mol/L, and stirs 15h, makes the pyrrole monomer polymerization reaction take place.With reacting liquid filtering, the product that then filtration is obtained is used deionized water 200mL and acetone 200mL cyclic washing successively, until filtrate is colourless.At last, the black powder that washing is obtained through 60 ℃ of vacuumize 36h, namely gets Fluorinated graphene oxide/polymer composite material of the present invention in vacuum drying chamber.
The above only is representative embodiment of the present invention, does not limit the present invention in any way, and all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces or improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a Fluorinated graphene oxide/polymer composite material is characterized in that, comprises Fluorinated graphene oxide and the polypyrrole that is deposited on described Fluorinated graphene oxide surface.
2. Fluorinated graphene oxide/polymer composite material according to claim 1 is characterized in that, described Fluorinated graphene oxide is made of the element of following mass percent:
C?50～70％
F?0～50％
O?0～40％
H?0～3％，
Wherein, the content of F, O and H all is not 0.
3. the preparation method of a Fluorinated graphene oxide/polymer composite material is characterized in that, may further comprise the steps:
1. Fluorinated graphene oxide is added dispersant for ultrasonic dispersion, forming concentration is the suspension of 0.2～2.0g/L;
2. in above-mentioned suspension, add pyrrole monomer, and ultrasonic dispersion, wherein, the mass ratio of Fluorinated graphene oxide and pyrrole monomer is 1: 2.9～1: 29;
3. add the aqueous solution of oxidant in step mixed liquor 2., and stir, wherein, the mass ratio of Fluorinated graphene oxide and oxidant is 1: 5～1: 50;
4. filtration step mixed liquor 3. obtains product, washing, and vacuumize namely gets Fluorinated graphene oxide/polymer composite material.
4. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3, it is characterized in that, the preparation method of described Fluorinated graphene oxide is: the graphite powder that with mass ratio is 2: 1: 1, in the concentrated sulfuric acid that potassium peroxydisulfate and phosphorus pentoxide adding are 70～90 ℃, stir, cooling, washing, dry, in the concentrated sulfuric acid with 0～20 ℃ of desciccate adding, and the potassium permanganate of 3 times of quality of adding graphite powder, keep mixture temperature below 20 ℃, 30～40 ℃ of oil bath 1.5～3h afterwards, add the deionized water that contains hydrogen peroxide, suction filtration, washing, ultrasonic dispersion, suction filtration again, dry, get graphene oxide, with fluorine gas reaction 0.5～24h under 20～200 ℃, namely get Fluorinated graphene oxide again.
5. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3 is characterized in that, described dispersant is at least a in methyl alcohol, ethanol, ethylene glycol, the water.
6. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3 is characterized in that, described oxidant is FeCl
36H
2O, (NH
4)
2S
2O
8, K
2S
2O
8, KMnO
4, K
2Cr
2O
7, H
2O
2In at least a.
7. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3 is characterized in that, 1. described step is respectively 10～60min and 10～50min with the ultrasonic jitter time of step in 2..
8. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3 is characterized in that, 3. described step carries out under 0 ℃～25 ℃ temperature, and the mixing time of described step in 3. is 3～24h.
9. the preparation method of Fluorinated graphene oxide/polymer composite material according to claim 3 is characterized in that, described step 4. in, with the washing of deionized water and acetone, and at 40 ℃～100 ℃ lower vacuumize 24～48h.
10. the application of Fluorinated graphene oxide/polymer composite material claimed in claim 1 in preparation electrode of super capacitor and lithium ion cell electrode.
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| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
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| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
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|---|
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| Preparation and characterization of graphite oxide/polypyrrole composites;Yongqin Han et al;《carbon》;20070721;第45卷;2394-2399 * |
| Rahul R.Nair el al.Fluorographene: a two-dimensional counterpart of teflon.《small》.2010,第6卷(第24期),2877-2884. |
| Reversible fluorination of graphene:towards a two-dimensional wide bandgap semiconductor;S.-H. Cheng et al;《arXiv》;20100501;1-7 * |
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