CN108455574A - A kind of preparation method of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nano generator - Google Patents
A kind of preparation method of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nano generator Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nano generator, including：Flexible 3 D porous graphene film is prepared using the method for ice template method assisted gravity self assembly, three-dimensional porous graphene/PDMS laminated films are prepared using the method for Joule heat auxiliary absorption, three-dimensional porous graphene/PDMS laminated films connection collector prepares friction nanometer power generator.Manufacture craft of the present invention is simple, the graphene synthesized using chemical method in the market, of low cost；Three-dimensional porous graphene/dimethyl silicone polymer compound friction the nano generator being prepared is simple in structure, it is soft, light and handy, it can be used under environment complicated and changeable, there is excellent mechanical property simultaneously, good cycling stability, due to the larger roughness of the good electric conductivity of graphene film and the surfaces PDMS so that generator has excellent electric property and working efficiency.
Description
Technical field
The invention belongs to the preparation field of engine, more particularly to a kind of flexible 3 D porous graphene/poly dimethyl silicon
The preparation method of oxygen alkane compound friction nano generator.
Background technology
With the continuous development of human society, global energy crisis problem getting worse, however in the utilization process of the energy
In, most of energy has been lost in mechanical friction.Therefore, effectively the energy of collecting mechanical frictional dissipation is particularly important.It is special
Not, developed rapidly in flexible electronic and wearable device current, research flexible mechanical energy collecting device has particularly significant
Practical value and realistic meaning.Traditional flexible generator is generally divided into two classes：(1) electromagnetic induction principle is utilized to generate electricity, this
Class generator needs conductive coil and magnet, generally heavier, it has not been convenient to carry；(2) piezoelectric principle is utilized to generate electricity, such hair
The general output power of motor is relatively low, it is difficult to effectively collecting mechanical energy.Friction nanometer power generator is a kind of utilization triboelectrification effect
The device of energy conversion should be carried out, it is to accumulate positive and negative charge using triboelectrification, then utilizes the positive and negative charge of movement and electricity
Electrostatic induction between pole externally exports electric energy.Friction nanometer power generator has output voltage height, green non-pollution, material source
Extensively, the advantages that of low cost, safe and reliable, light and handy convenient, thus its have in wearable device energy supply field it is wide
Application prospect.However, the multilevel hierarchy of friction nanometer power generator is complex, use occasion is restricted.
Graphene can be regarded as passing through SP by carbon atom2Hybrid form is constructed into the two dimension with monoatomic layer thickness
Planar structure.Pass through SP in plane between carbon atom2Hydridization, which is formed by σ keys, has the bond energy of superelevation so that graphene has super
High intensity；Delocalized electron network is formd perpendicular to the pi-electron of plane so that graphene has the electric conductivity of superelevation.Therefore,
There is mechanical stability outstanding and good electron-transport by the three-dimensional porous graphene film that graphene is presoma preparation
Property, there is huge application prospect in friction nanometer power generator field.However, current existing graphene-based friction nanometer generating
Machine structure is complex, it is difficult to give full play to the characteristic of graphene, and based on the flexible friction of three-dimensional porous graphene film
Nano generator is also not yet realized.
Invention content
Technical problem to be solved by the invention is to provide a kind of flexible 3 D porous graphene/dimethyl silicone polymer is multiple
The preparation method of friction nanometer power generator is closed, this method simple process and low cost is honest and clean, the friction nanometer power generator tool being prepared
There is excellent mechanical property, can be recycled for multiple times, the generator is ultralight, super soft, can be applied to various complex environments.
A kind of preparation of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nano generator of the present invention
Method, the specific steps are：
(1) flexible 3 D porous graphene film is prepared using the method for ice template method assisted gravity self assembly；
(2) it is powered to flexible 3 D porous graphene film in step (1), adsorbs prepolymerization polydimethylsiloxane
Solution is heating and curing, and obtains three-dimensional porous graphene/PDMS laminated films；
(3) one end connection collector of three-dimensional porous graphene/PDMS laminated films in step (2) is exported as signal
End, collector are connected with external circuit, obtain flexible 3 D porous graphene/PDMS compound friction nano generators.
It is specially using the method for ice template method assisted gravity self assembly in the step (1)：Graphene oxide is disperseed
Liquid pours into the sand core funnel of sealed bottom, freezing, the solution sealing of sand core funnel bottom, gravity self assembly, and freeze-drying is added also
Former agent reduction, obtains flexible 3 D porous graphene film, the wherein a concentration of 0.5-10mg/mL of graphene oxide dispersion,
The mass ratio of graphene oxide and reducing agent is 1:10~1:100.
The preparation method of the graphene oxide dispersion is：In deionized water by graphene oxide dispersion, 1- is stirred
5h, ultrasonic 2-10h, obtains graphene oxide dispersion.
The freezing is to use liquid nitrogen, cooling time 1-5min；The gravity self assembly time is 3-48h；Sublimation drying
For 12-24h.
Before the gravity self assembling process, the solution sealing of sand core funnel bottom.In gravity self assembling process, graphene oxide is slow
Slowly it dissolves and forms a film, self assembly time 3-48h.After gravity self assembling process, film freeze-drying, electronation are obtained porous
Graphene film.
The reducing agent is one or more of hydroiodic acid, vitamin C, hydrazine hydrate；Recovery time is 10-60min.
It is powered in the step (2) and generates Joule heat, so that the aperture of porous graphene film is further expanded, reduce simultaneously
The viscosity of prepolymerization PDMS.
The preparation method of prepolymerization polydimethylsiloxane solution is in the step (2)：PDMS presomas is pre-
Crosslinking, obtains prepolymerization PDMS, is dissolved in nonpolar solvent, obtains prepolymerization PDMS solution, wherein prepolymerization PDMS with it is non-
The mass ratio of polar solvent is 1:80-1:150.
The precrosslink temperature is 40-65 DEG C, and the precrosslink time is 30-50min；Nonpolar solvent is for dichloromethane or just
Hexane.
The voltage being powered in the step (2) is 1-10V, and the electric current of energization is 0.5-3A.
Adsorption time is 1-60min in the step (2)；The temperature that is heating and curing is 60-150 DEG C, and the time that is heating and curing is
1-6h。
Heating had both promoted the solidification of PDMS in the step (2), also promoted the volatilization of nonpolar solvent.
Collector is copper foil, conductive fiber or filamentary silver in the step (3).
The present invention utilize three-dimensional porous graphene film oleophylic absorption property, under conditions of energization PDMS adsorbed into
In the hole of graphene film, it is uniformly coated on hole wall surface, the groove and fold having due to hole wall itself so that cladding
There is certain roughness, obtained graphene/PDMS laminated films to have good electricity output performance on the surfaces PDMS later.
Advantageous effect
(1) manufacture craft of the present invention is simple, the graphene synthesized using chemical method in the market, of low cost；
(2) three-dimensional porous graphene/dimethyl silicone polymer compound friction nano generator knot that the present invention is prepared
Structure is simple, soft, light and handy, can be used under environment complicated and changeable, while having excellent mechanical property, cyclical stability
It is good；
(3) three-dimensional porous graphene/dimethyl silicone polymer compound friction nano generator that the present invention is prepared, by
In the roughness that the good electric conductivity of graphene film and the surfaces PDMS are larger so that generator has excellent electrical property
Energy and working efficiency.
Description of the drawings
Fig. 1 is the flow diagram that embodiment 1 prepares three-dimensional porous graphene/PDMS compound friction nano generators；
Fig. 2 is the section SEM figures that embodiment 1 prepares porous oxidation graphene film, and wherein a is low power figure, and b is high power
Figure；
Fig. 3 is the section SEM figures that embodiment 1 prepares porous graphene film, and wherein a is low power figure, and b is high power figure；
Fig. 4 is the schematic diagram of three-dimensional porous graphene film energization absorption prepolymerization PDMS in embodiment 1；
Fig. 5 is the section SEM figures that embodiment 1 prepares three-dimensional porous graphene/PDMS compound friction nano generators, wherein
A is low power figure, and b is high power figure；
Fig. 6 be embodiment 1 prepare three-dimensional porous graphene/PDMS compound frictions nano generator be bent 150 ° when
M- strain-stress curve；
Fig. 7 is output voltage-time that embodiment 1 prepares three-dimensional porous graphene/PDMS compound friction nano generators
Curve；
Fig. 8 is that embodiment 1 prepares three-dimensional porous graphene/PDMS compound frictions nano generator under different loads resistance
Efficiency curve.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) at room temperature, 80mg graphite oxides are dispersed in the dispersion that a concentration of 2mg/mL is made into the deionized water of 40mL
Liquid, mechanical agitation 3h, water bath sonicator 6h obtain finely dispersed graphene oxide solution.
(2) sand core funnel bottom is sealed with preservative film, sand core funnel is placed in foam mold, then by step (1)
Middle graphene oxide solution is poured into sand core funnel, with liquid nitrogen frozen 3min, obtains graphene oxide " ice cube "；Remove sand core leakage
The preservative film of bucket bottom, vacuum filtration for 24 hours, graphene oxide film are put into togerther to freeze in freeze drier together with filter membrane and is done
Dry 20h, then with the hydroiodic acid of mass fraction 55%, (mass ratio of graphene oxide and hydroiodic acid is 1:10) 1h is restored, is spent
After ionized water and alcohol alternately clean 3 times, it is put into freeze drier and is freeze-dried 12h, obtain flexible 3 D porous graphene
Film.
(3) PDMS presomas are put into heat cross-linking 35min in 60 DEG C of baking oven, obtain prepolymerization PDMS, then by pre-polymerization
Close PDMS and dichloromethane in mass ratio 1:80 ratio mixing, obtains PDMS solution.Flexible 3 D in step (2) is porous
The conductive silver paste of viscosity 300Pa.s is coated at the both ends of graphene film, and conductive silver paste cures in 80 DEG C of vacuum drying oven
Then two copper foils that width is 2mm are pasted at conductive silver paste, other end and the Keithley phase of copper foil by 10min respectively
Even；It is 5V in the power-on voltage of Keithley, graphene film is placed in above-mentioned PDMS solution by electric current under conditions of being 1A to be impregnated
1h then takes out film, is placed in 150 DEG C of vacuum drying chamber the 1h that is heating and curing, and it is compound to obtain three-dimensional porous graphene/PDMS
Film.
(4) film after solidification in step (3) is left into a wherein copper foil as collector, and by itself and external circuit phase
Even, you can obtain the three-dimensional porous graphene of single electrode formula/PDMS compound friction nano generators.
Fig. 2 shows：There is certain pore structure in graphene oxide film, but lamella totality or Close stack.
Fig. 3 shows：Film hole expands, and aperture reaches 5 μm.
Fig. 5 shows：PDMS is dispersed in pore interior, shows that graphene film effectively adsorbs PDMS.
Fig. 6 shows：Three-dimensional porous graphene/PDMS compound frictions nano generator is after 19 bend cycles, power
Performance is learned still to stablize.
Fig. 7 shows：The output voltage of friction nanometer power generator reaches 10V in the present embodiment, some can be driven small-sized
Wearable electronic equipment.
Fig. 8 shows：Friction nanometer power generator is when external loading (50M Ω) is matched with internal resistance in the present embodiment, work effect
Rate maximum can reach 52%, show that the generator has high energy conversion efficiency.
Embodiment 2
(1) at room temperature, 400mg graphite oxides are dispersed in point that a concentration of 10mg/mL is made into the deionized water of 40mL
Dispersion liquid, mechanical agitation 5h, water bath sonicator 10h obtain finely dispersed graphene oxide solution.
(2) sand core funnel bottom is sealed with preservative film, sand core funnel is placed in foam mold, then by step (1)
Middle graphene oxide solution is poured into sand core funnel, with liquid nitrogen frozen 5min, obtains graphene oxide " ice cube "；Remove sand core leakage
The preservative film of bucket bottom, is filtered by vacuum 48h, and graphene oxide film is put into togerther to freeze in freeze drier together with filter membrane and is done
It is dry for 24 hours, then use mass fraction 55% hydroiodic acid (mass ratio of graphene oxide and hydroiodic acid be 1:50) 1h is restored, is spent
After ionized water and alcohol alternately clean 3 times, it is put into freeze drier and is freeze-dried 12h, obtain flexible 3 D porous graphene
Film.
(3) PDMS presomas are put into heat cross-linking 30min in 65 DEG C of baking oven, obtain prepolymerization PDMS, then by pre-polymerization
Close PDMS and dichloromethane in mass ratio 1:150 ratio mixing, obtains PDMS solution.It is coated at the both ends of graphene film viscous
The conductive silver paste of 300Pa.s is spent, conductive silver paste cures 10min in 80 DEG C of vacuum drying oven, is then two of 2mm by width
Copper foil is pasted at conductive silver paste respectively, and the other end of copper foil is connected with Keithley；It is 10V in the power-on voltage of Keithley,
Graphene film is placed in above-mentioned PDMS solution by electric current under conditions of being 3A impregnates 1h, then takes out film, is placed in 90 DEG C
Be heating and curing 4h in vacuum drying chamber, obtains three-dimensional porous graphene/PDMS laminated films.
(4) film after solidification in step (3) is left into a wherein copper foil as collector, and by itself and external circuit phase
Even, you can obtain the three-dimensional porous graphene of single electrode formula/PDMS compound friction nano generators.
Embodiment 3
(1) at room temperature, 20mg graphite oxides are dispersed in point that a concentration of 0.5mg/mL is made into the deionized water of 40mL
Dispersion liquid, mechanical agitation 1h, water bath sonicator 2h obtain finely dispersed graphene oxide solution.
(2) sand core funnel bottom is sealed with preservative film, sand core funnel is placed in foam mold, then by step (1)
Middle graphene oxide solution is poured into sand core funnel, with liquid nitrogen frozen 1min, obtains graphene oxide " ice cube "；Remove sand core leakage
The preservative film of bucket bottom, is filtered by vacuum 3h, and graphene oxide film is put into togerther to freeze in freeze drier together with filter membrane and is done
Dry 12h, then with the hydroiodic acid of mass fraction 55%, (mass ratio of graphene oxide and hydroiodic acid is 1:100) 10min is restored,
After alternately being cleaned 3 times with deionized water and alcohol, it is put into freeze drier and is freeze-dried 12h, obtain flexible 3 D porous stone
Black alkene film.
(3) PDMS presomas are put into heat cross-linking 50min in 40 DEG C of baking oven, obtain prepolymerization PDMS, then by pre-polymerization
Close PDMS and dichloromethane in mass ratio 1:150 ratio mixing, obtains PDMS solution.It is coated at the both ends of graphene film viscous
The conductive silver paste of 300Pa.s is spent, conductive silver paste cures 10min in 80 DEG C of vacuum drying oven, is then two of 2mm by width
Copper foil is pasted at conductive silver paste respectively, and the other end of copper foil is connected with Keithley；It is 1V, electricity in the power-on voltage of Keithley
Graphene film is placed in PDMS solution under conditions of being 0.5A and impregnates 1min by stream, then takes out film, is placed in 60 DEG C true
Be heating and curing 6h in empty drying box, obtain three-dimensional porous graphene/PDMS laminated films.
(4) film after solidification in step (3) is left into a wherein copper foil as collector, and by itself and external circuit phase
Even, you can obtain the three-dimensional porous graphene of single electrode formula/PDMS compound friction nano generators.
Claims (9)
1. a kind of preparation method of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nano generator, specifically
Step is：
(1) flexible 3 D porous graphene film is prepared using the method for ice template method assisted gravity self assembly；
(2) it is powered to flexible 3 D porous graphene film in step (1), absorption prepolymerization polydimethylsiloxane is molten
Liquid is heating and curing, and obtains three-dimensional porous graphene/PDMS laminated films；
(3) one end of three-dimensional porous graphene/PDMS laminated films in step (2) is connected into collector, collector and external circuit
It is connected, obtains flexible 3 D porous graphene/PDMS compound friction nano generators.
2. a kind of flexible 3 D porous graphene described in accordance with the claim 1/dimethyl silicone polymer compound friction nanometer hair
The preparation method of motor, which is characterized in that specific using the method for ice template method assisted gravity self assembly in the step (1)
For：Graphene oxide dispersion is poured into the sand core funnel of sealed bottom, freezed, the solution sealing of sand core funnel bottom, gravity is certainly
Assembling, freeze-drying are added reducing agent reduction, obtain flexible 3 D porous graphene film, wherein graphene oxide dispersion
A concentration of 0.5-10mg/mL, the mass ratio of graphene oxide and reducing agent is 1:10~1:100.
3. a kind of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nanometer hair according to claim 2
The preparation method of motor, which is characterized in that the freezing is to use liquid nitrogen, cooling time 1-5min；The gravity self assembly time is
3-48h；Sublimation drying is 12-24h.
4. a kind of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nanometer hair according to claim 2
The preparation method of motor, which is characterized in that the reducing agent is one or more of hydroiodic acid, vitamin C, hydrazine hydrate；Also
The former time is 10-60min.
5. a kind of flexible 3 D porous graphene described in accordance with the claim 1/dimethyl silicone polymer compound friction nanometer hair
The preparation method of motor, which is characterized in that the preparation method of prepolymerization polydimethylsiloxane solution in the step (2)
For：By PDMS presoma precrosslink, prepolymerization PDMS is obtained, is dissolved in nonpolar solvent, obtains prepolymerization PDMS solution,
The mass ratio of middle prepolymerization PDMS and nonpolar solvent is 1:80-1:150.
6. a kind of flexible 3 D porous graphene/dimethyl silicone polymer compound friction nanometer hair according to claim 5
The preparation method of motor, which is characterized in that the precrosslink temperature is 40-65 DEG C, and the precrosslink time is 30-50min；Nonpolarity
Solvent is dichloromethane or n-hexane.
7. a kind of flexible 3 D porous graphene described in accordance with the claim 1/dimethyl silicone polymer compound friction nanometer hair
The preparation method of motor, which is characterized in that the voltage being powered in the step (2) is 1-10V, and the electric current of energization is 0.5-3A.
8. a kind of flexible 3 D porous graphene described in accordance with the claim 1/dimethyl silicone polymer compound friction nanometer hair
The preparation method of motor, which is characterized in that adsorption time is 1-60min in the step (2)；The temperature that is heating and curing is 60-150
DEG C, the time that is heating and curing is 1-6h.
9. a kind of flexible 3 D porous graphene described in accordance with the claim 1/dimethyl silicone polymer compound friction nanometer hair
The preparation method of motor, which is characterized in that collector is copper foil, conductive fiber or filamentary silver in the step (3).
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