CN104319012A - Preparation method of flexible electrode based on graphene - Google Patents
Preparation method of flexible electrode based on graphene Download PDFInfo
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Abstract
The invention provides a preparation method of a flexible electrode based on graphene. The preparation method comprises the steps of graphene oxide solution preparation, coating, chemical reduction and electrochemical reduction. In the chemical reduction step, acetic acid and hydroiodic acid are adopted as reducing agents so that the functional groups of the graphite (graphene) oxide can be well removed and the electrical conductivity of the graphene oxide can be improved; in the electrochemical reduction, pressurization is realized by virtue of linear sweep voltammetry to further reducing the oxygen-containing functional groups. The flexible thin-film electrode which is prepared by use of the preparation method of the flexible thin-film electrode and hybridized with the heat-treated graphene oxide and an electrode active material can be widely applied to the fields of batteries, touch screens, OLEDs, super capacitance materials, green and environment-friendly automobiles and the like.
Description
Technical field
The invention belongs to technical field of electronic materials, particularly a kind of flexible electrode preparation method based on Graphene.
Background technology
Bidimensional (2D) the cycle honeycomb lattice structure that Graphene is made up of carbon hexatomic ring, theoretical specific surface area is up to 2600m
2/ g, has outstanding heat conductivility (3000W/ (mK)) and mechanical property (1060GPa), and electron mobility (15000cm at a high speed under room temperature
2/ (Vs)).The two-dimensional structure that Graphene is special, make it have perfect quantum tunneling effect, the conductivity never disappeared, the series of properties such as flexible, cause the huge interest of scientific circles, Graphene is just starting the upsurge of one research.
Graphene is thin, the hardest nano material in known world, and it is almost completely transparent, only absorbs the light of 2.3%; Conductive coefficient is up to 5300 W/mK, and higher than carbon nano-tube and diamond, under normal temperature, its electron mobility is more than 15000 cm
2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height, and resistivity only about 10
-8Ω m, than copper or silver lower, be the material that world resistivity is minimum.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, and is therefore expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster.Because Graphene is in fact a kind of transparent, good conductor, be also applicable to for manufacturing transparent touch screen, tabula rasa or even solar cell.
Graphene relies on the electricity of its excellence, mechanics and thermal property, is widely used in various field, thus, realizes that it is extensive, the synthesis of low cost is significant.At present, the preparation method of Graphene mainly comprises micromechanics stripping method, chemical vapour deposition technique, epitaxial growth method and oxidation-reduction method, and oxidation-reduction method is lower because of cost, is widely used in the large-scale production of Graphene.The basic procedure of oxidation-reduction method is: first by graphite oxidation, increases spacing by introducing oxygen-containing functional group on graphite carbon atom between layers, and then weakens the interaction of interlayer; Then graphite oxide (alkene) is reduced.
Along with the progressively breakthrough of the difficult problem such as mass production and large scale, the commercial application paces of Graphene are accelerated, based on current existing achievement in research, the field realizing commercial applications at first may be mobile device, Aero-Space, new forms of energy field of batteries.
In consumer electronics show, flexible screen gets most of the attention, and becomes the development trend of following mobile device display screen.Flexible Displays future market is wide, based on the Graphene prospect of material be also expected.Data show that the global demand to handset touch panel in 2013 is probably at 9.65 hundred million.By 2015, panel computer also will reach 2.3 hundred million to the demand of large scale touch-screen, and the application for Graphene provides wide market.The researcher of Samsung of Korea S has also produced the transparent flexible display screen be made up of materials such as multi-layer graphenes, believes extensive commercial within sight.
On the other hand, new forms of energy battery is also a large key areas of Graphene commercialization the earliest.Massachusetts Institute Technology successfully develops the flexible photovoltaic battery plate of surface with graphene nano layer before, greatly can reduce the cost manufacturing transparent deformability solar cell, this battery is likely applied in the small size digital such as night vision goggles, camera equipment.In addition, the successful research and development of Graphene superbattery, also solve the off-capacity of new energy car battery and the problem of charging interval length, greatly accelerate the development of new forms of energy battery industry.This series of achievement in research is that the application paving of Graphene at new forms of energy battery industry is with regard to road.
Due to characteristics such as high conductivity, high strength, ultra-thins, Graphene is also very given prominence at the application advantage of space flight military industry field.Not long ago U.S. NASA developed the graphene sensor being applied to space industry, just can well detect the trace element of earth upper atmosphere, spaceborne structural defect etc.And Graphene also will play prior effect in the potential application such as ultra light aircraft material.
Ultracapacitor, also known as electrochemical capacitor, energy storage has and important effect.The features such as ultracapacitor has high power density, long service life, and have many potential application in portable, be suitable for mixed power electric car and implantable medical device etc.In recent years, increasing research paid close attention to ultracapacitor as energy storage device, the application in different modern devices.A desirable ultracapacitor flexibly, should possess good pliability and excellent mechanical strength simultaneously, and powerful electrochemistry ability; The flexible electrode prepared with Graphene obviously can be good at meeting its demand.Flexible electrode is the core component of ultracapacitor, and up-to-date research display, Graphene is as the ideal material preparing flexible electrode, and not only due to its structure, mechanical performance and electrical property, and it has very high access list area.Research shows, the flexible electrode prepared with Graphene, and its chemical property is more much lower than the performance of expection; That is, put into practice the capacitance of the Graphene flexible electrode produced, although the user demand of ultracapacitor also substantially can be met, its actual capacitance is more much smaller than the capacitance of theory expectation.
At present, about the preparation of Graphene, and existing many based on the patent documentation of the flexible electrode of Graphene, but there is following problem:
1, oxidation-reduction method is applicable to the production in enormous quantities of Graphene.In oxidation-reduction process, conventional reducing agent has hydrazine hydrate, sodium borohydride etc., and the use of hydrazine can cause the introducing of hetero-atom nitrogen, and sodium borohydride is expensive and easily cause the generation of hydrolysising by-product.In addition, simple electronation cannot remove the whole oxygen-containing functional groups contained in graphite oxide (alkene).
2, in actual applications, Graphene usually tends to irreversible reunion or stacking due to its hydrophobicity, thus loses original excellent properties.Although Graphene can by strengthening its dispersion stabilization at other molecules of its surface graft or polymer, but Graphene can be caused to have poor conductivity, too increase the dead volume of electrode material, therefore its chemical property is limited by very large in the middle of practical application simultaneously.The existing flexible electrode based on Graphene, in order to improve dispersiveness and the viscosity of solution in its preparation process, can add portions additive wherein, this reduces the electric conductivity of Graphene undoubtedly, and makes technological process become complicated.
3, the Graphene adopting chemical gaseous phase depositing process to prepare is because graphene growth is at substrate surfaces such as such as metal substrates, and therefore practical application graphene film must be transferred to required substrate surface.Conventional transfer method prepares a supporting layer at graphenic surface, and rear dissolution of metals substrate, then transfers to target substrate surface by the supporting layer carrying Graphene, finally remove supporting layer.There is a large amount of shortcoming in this transfer method, as: a large amount of wastes causing metal substrate, supporting layer is difficult to remove totally, causes the pollution of Graphene, is difficult to a large amount of production.
These above-mentioned shortcomings all can affect the electric conductivity of Graphene flexible electrode, make the chemical property of Graphene flexible electrode more much lower than the performance of expection.
Summary of the invention
The object of the invention is to overcome the above-mentioned defect existed in prior art, a kind of flexible electrode preparation method based on Graphene is provided, to improve the electric conductivity of Graphene flexible electrode.
For achieving the above object, the present invention is by the following technical solutions:
Based on a flexible electrode preparation method for Graphene, comprise the following steps:
A, preparation graphene oxide solution:
By graphite, NaNO
3with H
2sO
4after mixing, stir under condition of ice bath; Add KMnO
4, under water bath condition, stir and form film; Add water to continue to stir; Stop stirring and adding water, then add H
2o
2, cause solution colour to become yellow from dark brown; Filtering solution, adds water washing, is again dispersed in water by filter residue by mechanical agitation; Centrifugal to remove the inhomogenous graphene oxide sheet of size; And then by centrifugal for supernatant to remove reduced size graphene oxide fragment and hydrolysising by-product; Sediment is resuspended in water by mechanical agitation, finally obtains graphene oxide solution;
B, plated film:
The mask designing pattern is adhered to flexible material substrate, with oxygen plasma, substrate is processed; The graphene oxide solution obtained by step a is sprayed at above-mentioned substrate, dry under being then placed in infrared lamp;
C, electronation:
Graphene oxide/flexible material film that step b is obtained is deposited in case at reducing agent, carries out chemical reduction reaction; Then saturated sodium bicarbonate, distilled water and methyl alcohol is used to rinse film successively, dry under room temperature;
D, electrochemical reduction:
Graphene/the flexible material film obtained by step c, as in na phosphates buffer solution, adopts linear sweep voltammetry pressurization.
Further, in step a, the concrete steps of preparation graphene oxide solution are: by graphite, NaNO
3with H
2sO
4after mixing, stir under condition of ice bath; Add KMnO
4, mixture is proceeded to 30-40
ounder C water bath condition, stir 1h, form film; Add water, at 85-95
o30min is stirred under C condition; Stop stirring, and add water, then add the H that mass concentration is 30%
2o
2, cause solution colour to become yellow from dark brown; Filtering solution, adds water washing, is again dispersed in water by filter residue by mechanical agitation; Under rotating speed 1000rpm/min, centrifugal 2min, repeats 3-5 time to remove the inhomogenous graphene oxide sheet of size; Supernatant is with rotating speed 8000rpm/min, and centrifugal 15min, repeats at least 2 times, to remove reduced size graphene oxide fragment and hydrolysising by-product; Sediment is resuspended in water by mechanical agitation, finally obtains graphene oxide solution.
Further, in step b, the time of spraying graphene oxide solution is 1s, and the time of infrared lamp drying is 20s.
Further, in step c, described reducing agent is hydroiodic acid and acetic acid.
Further, in described reducing agent, the volume ratio of hydroiodic acid and acetic acid is 2:5.
Further, described chemical reduction reaction, in oil bath, reacts 24h at 40 DEG C.
Further, in steps d, the pH value of na phosphates buffer solution (Na-PBS) is 4.12.
Further, in steps d, when adopting linear sweep voltammetry pressurization, voltage transient is by-0.6V to-0.87V.
Further, described flexible material is PETG (PET) or dimethyl silicone polymer (PDMS).
The invention has the beneficial effects as follows:
In chemical reduction reaction, reducing agent is acetic acid and hydroiodic acid, the functional group of removal graphite oxide (alkene) that can be fabulous, improves the electric conductivity of redox graphene.Simple electronation cannot remove the whole oxygen-containing functional groups contained in graphite oxide (alkene), and therefore, the present invention, on the basis of electronation, introduces subsequent step electrochemical reduction, reduces the existence of oxygen-containing functional group further.Graphene oxide solution prepared by the present invention is because some centrifugation step in preparation process, make its dispersiveness very excellent, and make solution more easily adhere to substrate by introducing oxygen plasma, also improve the stability of flexible electrode, therefore do not need in solution, to add other materials again, ensure that the electric conductivity of flexible electrode to a certain extent.In addition, adopt oxygen plasma to process substrate, to basal electrode patterning, the etching speed of graphene layer and substrate can be improve, can improve the quality of products and yield.
The fexible film electrode of heat treated graphene oxide prepared by the preparation method of fexible film electrode of the present invention and electrode active material hydridization can be widely used in the fields such as battery, touch-screen, OLED, electrochemical capacitance material and environmental protection automobile.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
embodiment 1
Prepare the Graphene/PET flexible electrode of flexible flexibility.The steps include:
(1), graphene oxide solution (GO solution) is prepared:
(1-2) 0.5g graphite, 0.5g NaNO is taken
3, with 23mL H
2sO
4after mixing, stir under condition of ice bath;
(1-3) 3g KMnO is slowly added
4, mixture proceeds to 30
ounder C water bath condition, stir 1h, form film;
(1-4) 40mL water is added, 95
o30min is stirred under C condition;
(1-5) add 100mL water, then slowly add the H that 3mL mass concentration is 30%
2o
2, cause solution colour to become yellow from dark brown;
(1-6) filtering solution, is added 100 mL water washings, is again dispersed in water by filter residue by mechanical agitation;
(1-7) under rotating speed 1000rpm/min, centrifugal 2min, repeats 3 times to remove the inhomogenous graphene oxide sheet of size;
(1-8) supernatant is with rotating speed 8000rpm/min, centrifugal 15min, repeats 2 times to remove reduced size GO fragment and hydrolysising by-product;
(1-9) sediment is resuspended in water by mechanical agitation, final acquisition GO solution;
(2), plated film: the mask designing pattern is adhered to PETG (PET) substrate, the thickness of PET base is 50nm, and area is 5*5cm
2with oxygen plasma, substrate is processed; The graphene oxide solution that step (1) obtains is sprayed at above-mentioned substrate, and the molten concentration of graphene oxide is 0.05mg/L, and quantity for spray is 80mL, dry under being then placed in infrared lamp; The time of spraying graphene oxide solution is 1s, and the time of infrared lamp drying is 20s;
(3), Graphene (RGO) is prepared in electronation
Graphene oxide/PET film that step (2) is obtained is placed in the wide-mouth bottle of 300ml, this bottle is containing 2ml hydroiodic acid and 5ml acetic acid, and bottleneck vacuum grease seals, and reacts 24h at being placed in oil bath pan 40 DEG C; Then saturated sodium bicarbonate, distilled water and methyl alcohol is used to rinse film successively, dry under room temperature;
(4), electrochemical reduction
Graphene/the PET film obtained by step c is as in na phosphates buffer solution (Na-PBS), and the pH value of na phosphates buffer solution is 4.12, and adopt linear sweep voltammetry pressurization, voltage transient is by-0.6V to-0.87V.
PETG, chemical formula is COC
6h
4cOOCH
2cH
2o.
(english: Polyethylene terephthalate, be called for short PET), have good mechanical property, impact strength is 3 ~ 5 times of other films, and folding resistance is good.In wider temperature range, have excellent physical and mechanical properties, Long-Time Service temperature can reach 120 DEG C, and electrical insulating property is excellent, and even under high-temperature high-frequency, its electrical property is still better.
After testing, the light transmittance of Graphene/PET flexible electrode that the present embodiment is obtained is 92.1%.
Measure the voltage-curent change of the film obtained with comprehensive physical property measuring instrument, and calculate the conductance of this graphene film.The conductance of the graphene film prepared in the present embodiment is 780S/cm.
The graphene film prepared by the method is very well flexible, non-friable, collapsible reduction, has excellent conductivity and good pliability, and higher light transmittance.
embodiment 2
Preparation can stretch flexible Graphene/PDMS flexible electrode.The steps include:
(1), graphene oxide solution (GO solution) is prepared:
(1-2) 0.3g graphite, 0.3g NaNO is taken
3, with 14mL H
2sO
4after mixing, stir under condition of ice bath;
(1-3) 1.8g KMnO is slowly added
4, mixture proceeds to 40
ounder C water bath condition, stir 1h, form film;
(1-4) 24mL water is added, 85
o30min is stirred under C condition;
(1-5) add 60mL water, then slowly add the H that 1.8mL mass concentration is 30%
2o
2, cause solution colour to become yellow from dark brown;
(1-6) filtering solution, is added 60 mL water washings, is again dispersed in water by filter residue by mechanical agitation;
(1-7) under rotating speed 1000rpm/min, centrifugal 2min, repeats 5 times to remove the inhomogenous graphene oxide sheet of size;
(1-8) supernatant is with rotating speed 8000rpm/min, centrifugal 15min, repeats 3 times to remove reduced size GO fragment and hydrolysising by-product;
(1-9) sediment is resuspended in water by mechanical agitation, final acquisition GO solution;
(2), plated film: the mask designing pattern is adhered to dimethyl silicone polymer (PDMS) substrate, the thickness of PDMS substrate is 45nm, and area is 3*4cm
2, with oxygen plasma, substrate is processed; The graphene oxide solution that step (1) obtains is sprayed at above-mentioned substrate, and the molten concentration of graphene oxide is 0.04mg/L, and quantity for spray is 40mL, dry under being then placed in infrared lamp; The time of spraying graphene oxide solution is 1s, and the time of infrared lamp drying is 20s;
(3), Graphene (RGO) is prepared in electronation
Graphene oxide/PET film that step (2) is obtained is placed in the wide-mouth bottle of 150ml, this bottle is containing 1.2ml hydroiodic acid and 3ml acetic acid, and bottleneck vacuum grease seals, and reacts 24h at being placed in oil bath pan 40 DEG C; Then saturated sodium bicarbonate, distilled water and methyl alcohol is used to rinse film successively, dry under room temperature;
(4), electrochemical reduction
Graphene/flexible material film step (3) obtained is as in na phosphates buffer solution (Na-PBS), and the ph value of na phosphates buffer solution (Na-PBS) is 4.12; Employing linear sweep voltammetry is pressurizeed, and voltage transient, by-0.6V to-0.87V, obtains Graphene/PDMS flexible electrode.
Dimethyl silicone polymer (PDMS) has physiological inertia, good chemical stability, electrical insulating property and weatherability, hydrophobicity is good, and has very high anti-shear ability, can at-50 DEG C ~ 200 DEG C Long-Time Service.
After testing, the light transmittance of Graphene/PET flexible electrode that the present embodiment is obtained is 93.5%.
Measure the voltage-curent change of the film obtained with comprehensive physical property measuring instrument, and calculate the conductance of this graphene film.The conductance of the graphene film prepared in the present embodiment is 840S/cm.
The graphene film prepared by the method is very well flexible, non-friable, collapsible reduction, has excellent conductivity and good pliability, and higher light transmittance.
Claims (9)
1., based on a flexible electrode preparation method for Graphene, it is characterized in that: comprise the following steps:
A, preparation graphene oxide solution:
By graphite, NaNO
3with H
2sO
4after mixing, stir under condition of ice bath; Add KMnO
4, under water bath condition, stir and form film; Add water to continue to stir; Stop stirring and adding water, then add H
2o
2, cause solution colour to become yellow from dark brown; Filtering solution, adds water washing, is again dispersed in water by filter residue by mechanical agitation; Centrifugal to remove the inhomogenous graphene oxide sheet of size; And then by centrifugal for supernatant to remove reduced size graphene oxide fragment and hydrolysising by-product; Sediment is resuspended in water by mechanical agitation, finally obtains graphene oxide solution;
B, plated film:
The mask designing pattern is adhered to flexible material substrate, with oxygen plasma, substrate is processed; The graphene oxide solution obtained by step a is sprayed at above-mentioned substrate, dry under being then placed in infrared lamp;
C, electronation:
Graphene oxide/flexible material film that step b is obtained is deposited in case at reducing agent, carries out chemical reduction reaction; Then saturated sodium bicarbonate, distilled water and methyl alcohol is used to rinse film successively, dry under room temperature;
D, electrochemical reduction:
Graphene/the flexible material film obtained by step c, as in na phosphates buffer solution, adopts linear sweep voltammetry pressurization.
2. as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: in step a, the concrete steps of preparation graphene oxide solution are:
By graphite, NaNO
3with H
2sO
4after mixing, stir under condition of ice bath; Add KMnO
4, mixture is proceeded to 30-40
ounder C water bath condition, stir 1h, form film; Add water, at 85-95
o30min is stirred under C condition; Stop stirring, and add water, then add the H that mass concentration is 30%
2o
2, cause solution colour to become yellow from dark brown; Filtering solution, adds water washing, is again dispersed in water by filter residue by mechanical agitation; Under rotating speed 1000rpm/min, centrifugal 2min, repeats 3-5 time to remove the inhomogenous graphene oxide sheet of size; Supernatant is with rotating speed 8000rpm/min, and centrifugal 15min, repeats at least 2 times, to remove reduced size graphene oxide fragment and hydrolysising by-product; Sediment is resuspended in water by mechanical agitation, finally obtains graphene oxide solution.
3. as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: in step b, the time of spraying graphene oxide solution is 1s, and the time of infrared lamp drying is 20s.
4., as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: in step c, described reducing agent is hydroiodic acid and acetic acid.
5., as claimed in claim 4 based on the flexible electrode preparation method of Graphene, it is characterized in that: in described reducing agent, the volume ratio of hydroiodic acid and acetic acid is 2:5.
6., as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: described chemical reduction reaction, in oil bath, reacts 24h at 40 DEG C.
7., as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: in steps d, the pH value of na phosphates buffer solution is 4.12.
8. as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: in steps d, when adopting linear sweep voltammetry pressurization, voltage transient is by-0.6V to-0.87V.
9., as claimed in claim 1 based on the flexible electrode preparation method of Graphene, it is characterized in that: described flexible material is PETG or dimethyl silicone polymer.
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