CN107359056A - The preparation of a kind of graphene/poly- (1,3,6,8 4 thiophene pyrene) nanometer roll composite - Google Patents
The preparation of a kind of graphene/poly- (1,3,6,8 4 thiophene pyrene) nanometer roll composite Download PDFInfo
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- CN107359056A CN107359056A CN201710526088.4A CN201710526088A CN107359056A CN 107359056 A CN107359056 A CN 107359056A CN 201710526088 A CN201710526088 A CN 201710526088A CN 107359056 A CN107359056 A CN 107359056A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses the preparation method of a kind of graphene/poly- (1,3,6,8 4 thiophene pyrene) nanometer roll composite.Poly- (1,3,6,8 four thiophene pyrene) and graphene oxide are blended this method, by in-situ reducing, are prepared a nanometer volume structure, be may be used as the electrode materials such as ultracapacitor.The present invention relates to the preparation of graphene/poly- (1,3,6,8 four thiophene pyrene) nanometer roll composite, the electrode material as ultracapacitor can obtain higher specific capacitance value.This graphene roll preparation method is simple, stable working state is reliable, is worth being disclosed and protecting as the present invention.
Description
Technical field
The present invention relates to the preparation of graphene/poly- (1,3,6,8- tetra- thiophene pyrene) nanometer roll composite, belong to material skill
Art field.
Background technology
Graphene, the New Two Dimensional carbon nanomaterial of monoatomic thickness, possesses the advantages of numerous special, such as the ratio of superelevation
Surface area, quick electron transport ability, outstanding mechanical performance and mechanical property, significant heat conductivility and outstanding
Elastic performance, these performances cause graphene to turn into one kind and have very much potential material, and can be used in each work
In terms of industry, such as lithium ion battery, ultracapacitor, solar cell, transparency electrode, electron transistor, bio-sensing detection, gas
The super many-sides such as body storage.But simple grapheme material, during being prepared in technology, easily formed and stack and roll into a ball
It is poly-, so the introducing of graphene-based composite, both maximumlly make use of the performance of graphene, and there is incorporation compound
Intrinsic advantage.
Ultracapacitor is a kind of battery system of efficent electronic transmission and energy storage, because the capacity of itself is big, circulation makes
With long lifespan, security performance is high, stability is superior the advantages that, be a kind of one kind being most hopeful with potentiality substitution lithium ion battery
Electronic device, equally also it is widely used in various power supply equipments.Graphene, a kind of owner's superhigh specific surface area and
The new 2 dimension carbon material of super rapid electron transmission ability, since being announced to the world splendidly, has just obtained extensive concern, as application
Greatly hope and enthusiasm are had in arms by scientific research personnel in the electrode material of ultracapacitor.
Because the specific capacitance value of poly- (1,3,6,8- tetra- thiophene pyrene) this polymer is very high, but performance is unstable, and
This template of graphene can just play the structure for stablizing poly- (1,3,6,8- tetra- thiophene pyrene), and poly- (1,3,6,8- tetra- thiophene
Fen pyrene) lamella of graphene can also be allowed more open and flat, to obtain the specific capacitance value of more preferable electronics flow rate and Geng Gao.
Graphene by graphene oxide during being reduced, and due to the removal of surface oxygen functional group, surface is changed by hydrophily
For hydrophobicity, easily reunite and stack between layers, so as to have impact on the characteristics of specific surface area of graphene script is bigger
Play.And the insertion of polymer, the distance between graphene layer and layer can be effectively spaced, prevents graphene in reduction process
In stacking and reunion, can play a part of one well expand spacer support frame thing.In addition, simple graphene is used for making
If the electrode of standby ultracapacitor, because electron transport ability itself is very fast, when electronics from the positive pole of ultracapacitor to
During negative pole, electronics can not retain for a long time so that the power reservoir capacity of ultracapacitor is very low.And add conductive polymer
After polymer, in compound, have poly- (1,3,6,8- tetra- thiophene pyrene) that power reservoir capacity is very good, the addition of graphene is again right
Extraordinary stability is played in polymer.
The content of the invention
Goal of the invention:The present invention for graphene superelevation specific surface area and superpower electron transport ability, by with
The in-situ blending reduction reaction of poly- (1,3,6,8- tetra- thiophene pyrene) this conducting polymer, the graphene prepared/poly- (1,3,
6,8- tetra- thiophene pyrenes) nanometer roll composite be applied to ultracapacitor electrode material in, both utilize the superelevation of graphene
Specific capacitance value advantage, again using poly- (1,3,6,8- tetra- thiophene pyrene) inductive formation three-dimensional grapheme volume characteristic;It is prepared
Novel graphite alkene nanometer volume structure, it is a kind of very potential electrode material for super capacitor.The present invention prepares graphene/poly-
(1,3,6,8- tetra- thiophene pyrene) nanometer roll composite, the electrode material as ultracapacitor can obtain higher specific capacitance
Value.
Technical scheme:The preparation of a kind of graphene/poly- (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite of the present invention
Schematic diagram is as shown in Figure 5.
Poly- (1,3,6,8- tetra- thiophene pyrene) described in preparation principle figure of the present invention, has following structure:
Poly- (the thiophene pyrenes of 1,3,6,8- tetra-)
The preparation method of (the thiophene pyrenes of 1,3,6,8- tetra-) poly- described in preparation principle figure of the present invention is in chlorine by ferric trichloride
Benzene, o-dichlorohenzene or paracide, under the conditions of 40~60 degree, prepared by oxidative dehydrogenation polymerisation.Poly- (the thiophene of 1,3,6,8- tetra-
Pyrene) preparation method, it is characterized in that by three steps.Step 1,1,3,6,8- tetra- thiophene pyrene (1.0g, 1.5mmol) is slow
Slowly it is dissolved in 50mL solvents.Step 2, ferric trichloride (1.1g.6.5mmol) is dissolved in nitromethane (3~5 mL).Step
Rapid three, under nitrogen flowing, liquor ferri trichloridi is slowly added dropwise into 1,3,6,8- tetra- thiophene pyrene with syringe, waits to be added dropwise completely
Afterwards, continue reaction 24~48 hours under 40~60 degree, after having solid precipitation, the solid of precipitation is filtered, with chloroform or dichloromethane
The solid that alkane washing filters out, is finally obtained required poly- (1,3,6,8- tetra- thiophene pyrene).
The preparation of a kind of graphene described in principle of the invention formula/poly- (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite
Step includes:
A. by 30mg graphene oxide, it is put into 50mL microwave reaction pipe, and adds 10mL N, N- dimethyl methyls
Acid amides or DMA, it is put into ultrasound 0.5~1 hour in ultrasonic machine.
B. by 10~60mg poly- (1,3,6,8- tetra- thiophene pyrene), add in step a solution, continue ultrasound 1 hour.
D. after mixing ultrasound, brick-red or bronzing is presented in solution, and adds 2~4mL hydrazine hydrate solution thereto,
And the special magneton of microwave is added, with temperature-programmed mode, microwave is heated to 120~140 DEG C, reacts 30min.
E. question response system is cooled to room temperature, reaction solution is added in a large amount of 1mol/L watery hydrochloric acid, filtered, deionization
Water washing, obtain the graphene nano volume described in claim 1.
F. redox graphene (RGO) described in step a~e and poly- (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll compound
Pattern and performance can be regulated and controled by the weight ratio of used graphene oxide solid and poly- (the thiophene pyrenes of 1,3,6,8- tetra-).
Compared with prior art, the invention has the advantages that:
The present invention for graphene superelevation, superpower electron transport ability, by with poly- (1,3,6,8- tetra- thiophene pyrene) this
The In-situ reaction of kind conducting polymer, the graphene prepared/poly- (1,3,6,8- tetra- thiophene pyrene) nanometer roll composite can answer
Make the electrode material of ultracapacitor.Graphene oxide (GO) is to carry oxygen-containing functional group in itself, this makes in forming process
Between layers because Van der Waals force is apart from smaller, mixed with poly- (1,3,6,8- tetra- thiophene pyrene), add hydrazine hydrate, oxygen
By the induction of poly- (1,3,6,8- tetra- thiophene pyrene) while graphite alkene generation in-situ reducing, graphene nano clove hitch is formed
Structure, avoid stacking again in graphene oxide reduction process so that graphene keeps larger specific surface area, adds its knot again
Structure stability.Importantly, the composite of graphene and poly- (1,3,6,8- tetra- thiophene pyrene), power reservoir capacity and electric transmission
Ability is very high, is highly suitable to be applied in ultracapacitor.It is demonstrated experimentally that the maximum innovative point of this composite is stone
The pattern of black alkene lamella is influenceed by the macro adjustments and controls of poly- (1,3,6,8- tetra- thiophene pyrene) participation amount, poly- (1,3,6,8- tetra- thiophene
Pyrene) the proportion that accounts for of amount it is bigger, the pattern of graphene is adjusted and changes more, while the capacitance of composite is also more
It is stable, reduce slower.The present invention had both utilized the characteristic of graphene, make use of the ratio of poly- (1,3,6,8- tetra- thiophene pyrene) superelevation again
The advantages of capacitance, it is a kind of very potential electrode material for super capacitor.
Brief description of the drawings
The transmission electron microscope (TEM) of the compound of proportionings different from poly- (the thiophene pyrenes of 1,3,6,8- tetra-) GO made from Fig. 1
Figure.
Fig. 2 poly- (1,3,6,8- tetra- thiophene pyrene), the infrared spectrogram of the compound of GR, GO and 4 kinds of different ratios.
Cyclic voltammetry curve under the electrode system of composite two of tetra- kinds of different ratios of Fig. 3, it is 100mV/s to sweep speed.
The charge and discharge of poly- (the thiophene pyrenes of 1,3,6,8- tetra-) and different ratio composite under Fig. 4 .0.1A/g current density
Electric curve.
The preparation principle figure of Fig. 5 graphenes/poly- (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite
Embodiment
Following examples are the further explanations to the present invention, are not limitations of the present invention.
Embodiment 1:Poly- (the thiophene pyrenes of 1,3,6,8- tetra-) and corresponding graphene nano roll standby
1,3,6,8- tetra- thiophene pyrene (250mg, 0.375mmol) is slowly dissolved in 12mL chlorobenzenes, at room temperature by anhydrous three
Iron chloride (0.3g.1.6mmol) is dissolved in nitromethane (1.5mL), is maintained under nitrogen bubble and stirring, and ferric trichloride is molten
Liquid is added dropwise in 1,3,6,8- tetra- thiophene pyrene solution, and after being added dropwise completely, reaction system, which is placed in 45 degree of oil baths, to be continued to stir
Mix 24 hours, cool to room temperature, after there are a large amount of solids to separate out, filter the solid of precipitation, what the chloroform of 30mL × 3 filtered out consolidates
Body, it is poly- (1,3,6,8- tetra- thiophene pyrene) to finally obtain Chinese red sheet.Take 20mg, 10mg graphene oxide and 15mL therein
DMA is scattered in 50mL microwave reaction pipe, is put into ultrasound 1 hour in ultrasonic machine, is obtained brick-red suspended
Liquid, 1.5mL hydrazine hydrate is added thereto, with temperature-programmed mode, microwave is heated to 130~135 DEG C, reacts 30min.Heating
After completion of the reaction, question response system is cooled to room temperature, in the watery hydrochloric acid for the 1mol/L that reaction solution is added to 150 milliliters, through centrifuging,
Filtering, deionized water washing, obtain the graphene nano volume 17mg described in claim 1.
Embodiment 2:Poly- (the thiophene pyrenes of 1,3,6,8- tetra-) and corresponding graphene nano roll standby
1,3,6,8- tetra- thiophene pyrene (500mg, 0.75mmol) is slowly dissolved in 20mL o-dichlorohenzenes, at room temperature will be anhydrous
Ferric trichloride (0.7g.3.4mmol) is dissolved in nitromethane (4mL), is maintained under nitrogen bubble and stirring, and ferric trichloride is molten
Liquid is added dropwise in 1,3,6,8- tetra- thiophene pyrene solution, and after being added dropwise completely, reaction system, which is placed in 60 degree of oil baths, to be continued to stir
Mix 36 hours, cool to room temperature, after there are a large amount of solids to separate out, filter the solid of precipitation, what the chloroform of 30mL × 3 filtered out consolidates
Body, finally obtain poly- (1,3,6, the 8- tetra- thiophene pyrene) powder of bronzing.Take 30mg, 30mg graphene oxide and 25mL therein
DMA is scattered in 50mL microwave reaction pipe, is put into ultrasound 1 hour in ultrasonic machine, it is suspended to obtain brownish red
Liquid, add 3.0mL hydrazine hydrate thereto, with temperature-programmed mode, microwave is heated to 130~135 DEG C, reacts 30min.Heating is anti-
After answering, question response system is cooled to room temperature, in the watery hydrochloric acid for the 1mol/L that reaction solution is added to 150 milliliters, through centrifugation, mistake
Filter, deionized water washing, obtain the graphene nano volume 52mg described in claim 1.
Embodiment 3:Performance of the supercapacitor test CV tests
In electrode production process, rule are cut into from collector of the nickel foam as electrode slice, and by foam nickel electrode piece
Whole circle, then the electrode slice sheared is placed in tablet press machine to the thin slice for being pressed into original thickness 1/3rd, then by thin slice
Around carry out cutting out somewhat.Finally, circular shaped foam nickel disk is placed on 100 DEG C of 12 h of drying in vacuum drying oven.Dry it
Afterwards, weigh nickel foam disk quality and be designated as m0.Stannic oxide/graphene nano prepared by example 1 rolls up grind into powder, according to 75:
20:5 graphene nano volume:Acetylene black:The proportioning of polytetrafluoroethylene (PTFE) (PTFE), is put into mortar, adds fraction of anhydrous second
Alcohol, grinding clockwise, after to pasty state, medication spoon is equably applied in the one side of nickel foam, until not seeing nickel foam sheet
The color of body.The thickness of sample of foam nickel surface after smearing uniformly is moderate, the partially silver-colored black of color, foam nickel sheet is positioned over
100 DEG C of baking oven 10h, you can obtain the electrode of super capacitor of graphene-containing nanometer roll.
Using the electrochemical package of two electrode systems, electrochemical workstation is CHI660C types work station (Shanghai China occasion instrument
Company), electrolyte is 1mol/L Li2SO4.CV (cyclic voltammetry) potential window is set to the V of -0.5V~0.5, charge and discharge electrical measurement
The potential window of examination is set to -0.5V~0.5V, and it is 100mV/s to sweep speed.Constant current charge-discharge test is in the case where current density is 0.1A/g
Carry out.Ac impedance measurement is to be carried out under the OCP under 100kHz~0.01Hz in frequency range.
It is c=Ac+Ad/ (ν * Δ V*m) according to the specific capacitance calculation formula of two electrode test systems
Wherein, Ac+Ad is expressed as the area of the CV curves formed in charging process and discharge process, and ν is represented and swept
Speed, and Δ V represents potential window, what m was represented is the average value of active material quality on two electrode slices.
It is CV curve map of the graphene nano circle as electrode of four kinds of different proportionings in Fig. 4.
Embodiment 4:
In order to confirm whether graphene and poly- (1,3,6,8- tetra- thiophene pyrene) are completely compound, and we enter to various composites
The shooting of microcosmic transmission electron microscope is gone, in Fig. 1, what (a) was represented is that Hummer ' s methods generate to obtain by graphite oxide
The transmission electron microscope picture of graphene oxide (GO), from figure (a) it can be seen that graphene is that sheet is scattered in the solution, their face
Color presentation is translucent, illustrates that the GO lamellas after oxidation are not very thick, comparatively, the number of plies is more relatively thin.Scheme the band in (b)
The transmission electron microscope picture of shape thing poly- (the thiophene pyrenes of 1,3,6,8- tetra-).Polythiophene presentation strip in figure, and it is apparent that
The width of bar is highly uniform.Figure (c) compound is GO and the weight proportion of poly- (the thiophene pyrenes of 1,3,6,8- tetra-) is 1:1 is former
Position reduction preparation is drawn.From TEM pictures it can be clearly seen that the pattern of the graphene after reduction does not occur significantly to change
Become, graphene is still to exist with sheet.But the color of graphene here is more transparent than the GO in figure (a), institute
Can illustrate here, the graphene number of plies table after reduction is few, and lamella is thinning.Figure (d) compound is GO and poly- (1,3,6,8- tetra-
Thiophene pyrene) proportioning be 1:2, in-situ reducing is prepared and drawn.It can be seen that the lamella pattern of the graphene after reduction has
There is bend somewhat and fold in some changes, the edge of graphene, and this shows poly- (1,3,6,8- tetra- thiophene pyrene) this
In the case of proportioning, play the role of on the pattern of graphene and influence.This influence equally can from (e) and (f)
Go out.Figure (e) compound is GO and the proportioning of poly- (the thiophene pyrenes of 1,3,6,8- tetra-) is 1:4 in-situ reducings are prepared and drawn.Match somebody with somebody this
Than under, with amount the dramatically increasing relative to GO of poly- (1,3,6,8- tetra- thiophene pyrene), the graphene of generation is reduced.Pattern hair
Give birth to and obviously changed, graphene major part lamellar structure disappears, and the substitute is poly- (1,3,6,8- tetra- thiophene pyrene)
Regulate and control pattern of the graphene in reduction process, be not lamella tiling simply, but for proportioning before, compared with
Significantly it is wrapped the profile parcel of poly- (the thiophene pyrenes of 1,3,6,8- tetra-) bar.But it is overall to show bulked state, be not
Snugly unusual consolidation.A figure below (f) is further studied, in the compound for scheming (f), GO and poly- (1,3,6,8- tetra- thiophene
Pyrene) proportioning be 1:8, for first three matches, the amount of poly- (1,3,6,8- tetra- thiophene pyrene) is even more increase at double,
Here for graphene in reduction process, the dynamics that pattern is regulated and controled by poly- (1,3,6,8- tetra- thiophene pyrene) is even more increase at double,
So that graphene tightly wraps poly- (the thiophene pyrenes of 1,3,6,8- tetra-) bar.
Claims (4)
- The preparation method of a kind of graphene/poly- 1. (1,3,6,8- tetra- thiophene pyrene) nanometer roll composite, it is characterised in that have Following structure:
- The preparation of a kind of graphene according to claim 1/poly- 2. (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite Method, poly- (1,3,6,8- tetra- thiophene that graphene/poly- (1,3,6,8- tetra- thiophene pyrene) nanometer roll composite of preparation is related to Pyrene) preparation method is that oxidative dehydrogenation gathers by ferric trichloride under the conditions of chlorobenzene, o-dichlorohenzene or paracide, 40~60 degree Close reaction to prepare, the preparation method of poly- (1,3,6,8- tetra- thiophene pyrene), it is characterised in that by three steps:Step 1, by 1, The thiophene pyrenes (1.0g, 1.5mmol) of 3,6,8- tetra- are slowly dissolved in 50mL solvents;Step 2, by ferric trichloride (1.1g.6.5mmol) is dissolved in nitromethane (3~5mL);Step 3, under nitrogen flowing, trichlorine is slowly added dropwise with syringe Change ferrous solution into 1,3,6,8- tetra- thiophene pyrene, after being added dropwise completely, continue reaction under 40~60 degree 24~48 hours, have solid After body separates out, filter the solid of precipitation, the solid filtered out with chloroform or dichloromethane washing, finally obtain needed for it is poly- (1,3,6, The thiophene pyrenes of 8- tetra-).
- The preparation of a kind of graphene according to claim 1/poly- 3. (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite Method, it is characterised in that methods described includes following synthesis step:A. by 30mg graphene oxide, it is put into 50mL microwave reaction pipe, and adds 10mL DMF Or DMA, it is put into ultrasound 0.5~1 hour in ultrasonic machine;B. by 10~60mg poly- (1,3,6,8- tetra- thiophene pyrene), add in step a solution, continue ultrasound 1 hour;D. after mixing ultrasound, brick-red or bronzing is presented in solution, and adds 2~4mL hydrazine hydrate solution thereto, and adds Enter microwave dedicated magnetic, with temperature-programmed mode, microwave is heated to 120~140 DEG C, reacts 30min;E. question response system is cooled to room temperature, reaction solution is added in a large amount of 1mol/L watery hydrochloric acid, filtered, deionization washing Wash, obtain the graphene nano volume described in claim 1.
- The preparation of a kind of graphene according to claim 3/poly- 4. (the thiophene pyrenes of 1,3,6,8- tetra-) nanometer roll composite Method, it is characterised in that described to prepare redox graphene (RGO) and poly- (1,3,6,8- tetra- thiophene pyrene) nanometer roll is compound Thing, matched according to graphene oxide solid and poly- (1,3,6,8- tetra- thiophene pyrene) different weight ratio, realize different-shape and The graphene nano volume of performance.
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