CN104319012B - A kind of flexible electrode preparation method based on graphene - Google Patents
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Abstract
The invention provides a kind of flexible electrode preparation method based on graphene, including the step of preparation graphene oxide solution, plated film, electronation, electrochemical reduction.In the step of electronation, reducing agent is acetic acid and hydroiodic acid, the fabulous removal graphite oxide of energy（Alkene）Functional group, improve redox graphene electric conductivity；In the step of electrochemical reduction, pressurizeed using linear sweep voltammetry, further reduce the presence of oxygen-containing functional group.The graphene oxide of heat treatment prepared by the preparation method of the fexible film electrode of the present invention can be widely used for the fields such as battery, touch-screen, OLED, electrochemical capacitance material and environmental protection automobile with the fexible film electrode of electrode active material hydridization.
Description
Technical field
The invention belongs to technical field of electronic materials, more particularly to a kind of flexible electrode preparation method based on graphene.
Background technology
Bidimensional (2D) cycle honeycomb lattice structure that graphene is made up of carbon hexatomic ring, theoretical specific surface area is up to
2600m2/ g, with prominent heat conductivility (3000W/ (mK)) and mechanical property (1060GPa), and at room temperature at a high speed
Electron mobility (15000cm2/(V·s)).The special two-dimensional structure of graphene, makes it have perfect quantum tunneling effect
Should, the electrical conductivity that never disappears, a series of properties such as flexible, cause the huge interest of scientific circles, graphene just starts one
The upsurge of stock research.
Graphene is most thin, the most hard nano material in known world, and it is almost fully transparent, only absorbs 2.3%
Light；Thermal conductivity factor is up to 5300 W/mK, higher than CNT and diamond, and its electron mobility is more than 15000 under normal temperature
cm2/ Vs, but it is higher than CNT or silicon crystal, and resistivity about 10-8Ω m, it is lower than copper or silver, it is world resistance
The minimum material of rate.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, therefore is expected to can be used to develop thinner, conduction
Speed faster electronic component or transistor of new generation.Because graphene is substantially a kind of transparent, good conductor, it also is adapted for
For manufacturing transparent touch screen, even tabula rasa, solar cell.
Graphene relies on its excellent electricity, mechanics and thermal property, is widely used in various fields, it is thereby achieved that its
On a large scale, inexpensive synthesis is significant.At present, the preparation method of graphene mainly includes micromechanics stripping method, changed
Vapour deposition process, epitaxial growth method and oxidation-reduction method are learned, and oxidation-reduction method is relatively low because of cost, is widely used in graphene
Large-scale production.The basic procedure of oxidation-reduction method is：First by graphite oxidation, pass through the carbon atom in graphite between layers
It is upper to introduce oxygen-containing functional group and increase spacing, and then weaken the interaction of interlayer；Then to graphite oxide（Alkene）Reduced.
With the progressively breakthrough of the problems such as mass production and large scale, the commercial application paces of graphene add
Hurry up, based on current existing achievement in research, the field that commercial applications are realized at first may be mobile device, Aero-Space,
New energy field of batteries.
Flexible screen gets most of the attention in consumer electronics show, the development trend as following mobile device display screen.It is flexible
Show that future market is wide, based on the graphene prospect of material be also expected.It data show the whole world in 2013 to mobile phone
The demand of touch-screen is probably at 9.65 hundred million.By 2015, panel computer was also up to 2.3 to the demand of large scale touch-screen
Hundred million, wide market is provided for the application of graphene.The researcher of Samsung of South Korea has also been produced by multilayer stone
The transparent flexible display screen of the materials such as black alkene composition, it is believed that extensive commercial within sight.
On the other hand, new energy battery is also a graphene big key areas commercial earliest.Masschusetts, U.S.A science and engineering before
Institute has successfully developed the flexible photovoltaic battery plate that surface has graphene nano figure layer, can greatly reduce manufacture transparent variable
The cost of shape solar cell, this battery is possible to apply in the small size digital equipment such as night vision goggles, camera.In addition, graphite
The successful research and development of alkene superbattery, the problem of also solving off-capacity and the long charging interval of new energy car battery, pole
The big development for accelerating new energy battery industry.This series of achievement in research is application of the graphene in new energy battery industry
Paving is with regard to road.
Due to characteristics such as high conductivity, high intensity, ultra-thins, graphene is also pole in the application advantage of space flight military industry field
To be prominent.Not long ago U.S. NASA developed the graphene sensor applied to space industry, just can be high to the earth well
Micro-, spaceborne structural defect of empty atmosphere etc. is detected.And graphene is in ultra light aircraft material etc.
Also prior effect will be played in potential application.
Ultracapacitor, also known as electrochemical capacitor, play the role of and its important in energy storage.Super capacitor utensil
The features such as having high power density, long service life, and have many potential applications in portable, it is suitable for
Mixed power electric car and implantable medical device etc..In recent years, increasing research concern ultracapacitor was used as storage
Can device, the application in different modern devices.One preferable flexible ultracapacitor, should be provided simultaneously with good
Pliability and excellent mechanical strength, and powerful electrochemistry ability；The flexible electrode prepared with graphene obviously can be very
Good meets its demand.Flexible electrode is the core component of ultracapacitor, and newest research shows that graphene is soft as preparing
Property electrode ideal material, be not only due to its structure, mechanical performance and electrical property, and it has very high access surface product.
Research shows that the flexible electrode prepared with graphene, its chemical property is more much lower than expected performance；That is, practice
The capacitance for the graphene flexible electrode produced, although can also substantially meet the use demand of ultracapacitor, still,
Its actual capacitance is more much smaller than the capacitance of theory expectation.
At present, the preparation on graphene, and the patent document of the flexible electrode based on graphene are many, still
There is problems with：
1st, oxidation-reduction method is applied to the production in enormous quantities of graphene.In oxidation-reduction process, conventional reducing agent has
Hydrazine hydrate, sodium borohydride etc., the use of hydrazine can cause the introducing of hetero atom nitrogen, and sodium borohydride is expensive and easily causes water
Solve the generation of accessory substance.In addition, simple electronation can not remove graphite oxide（Alkene）In whole oxygen-containing functional groups for containing.
2nd, in actual applications, graphene often tends to irreversible reunion or stacking due to its hydrophobicity, so as to lose
Original excellent properties.Although graphene can be by strengthening its stably dispersing in other molecules of its surface graft or polymer
Property, but can cause graphene that there is poor electric conductivity, while the dead volume of electrode material is also increased, therefore its electrochemistry
Performance is limited by very large among practical application.It is in the existing flexible electrode based on graphene, its preparation process
The dispersiveness and viscosity of solution are improved, portions additive can be added thereto, this undoubtedly reduces the electric conductivity of graphene,
And make it that technological process becomes complicated.
3rd, the graphene prepared using chemical gaseous phase depositing process is because graphene growth is in substrates such as metal substrates
Surface, therefore practical application is that graphene film must be transferred to required substrate surface.Conventional transfer method is in stone
Black alkene surface prepares a supporting layer, and metal substrate is dissolved afterwards, the supporting layer for carrying graphene then is transferred into target substrate
Surface, finally removes supporting layer.There are a large amount of shortcomings in the transfer method, such as：A large amount of wastes of metal substrate are caused, supporting layer is difficult
It is clean to remove, cause the pollution of graphene, it is difficult to a large amount of productions.
These above-mentioned shortcomings can influence the electric conductivity of graphene flexible electrode so that the electricity of graphene flexible electrode
Chemical property is more much lower than expected performance.
The content of the invention
It is an object of the invention to overcome drawbacks described above present in prior art, there is provided a kind of flexibility based on graphene
Electrode preparation method, to improve the electric conductivity of graphene flexible electrode.
To achieve the above object, the present invention uses following technical scheme：
A kind of flexible electrode preparation method based on graphene, comprises the following steps：
A, preparation graphene oxide solution：
By graphite, NaNO3With H2SO4After mixing, stirred under condition of ice bath；Add KMnO4, under water bath condition, stir
Mix to form film；Water is added to continue to stir；Stop stirring and add water, then add H2O2, cause solution colour to be changed into from dark brown
Yellow；Filtering solution, adds water washing, is dispersed in water filter residue again by mechanical agitation；Centrifugation is uneven to remove size
One graphene oxide sheet；Then again supernatant is centrifuged 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 for designing good pattern is adhered into flexible material substrate, substrate handled with oxygen plasma；Will step
The graphene oxide solution that rapid a is obtained is sprayed at above-mentioned substrate, is subsequently placed under infrared lamp and dries；
C, electronation：
By graphene oxide/flexible material film made from step b in the presence of reducing agent, electronation is carried out anti-
Should；Then film is rinsed successively using saturated sodium bicarbonate, distilled water and methanol, dry at room temperature；
D, electrochemical reduction：
Graphene/flexible material film that step c is obtained is as in na phosphates buffer solution, using linear sweep voltammetry
Pressurization.
Further, in step a, concretely comprising the following steps for graphene oxide solution is prepared：By graphite, NaNO3With H2SO4It is mixed
After conjunction, stirred under condition of ice bath；Add KMnO4, mixture is transferred to 30-40oUnder C water bath conditions, 1h is stirred, is formed
Film；Water is added, in 85-95o30min is stirred under the conditions of C；Stop stirring, and add water, it is 30% then to add mass concentration
H2O2, cause solution colour to be changed into yellow from dark brown；Filtering solution, adds water washing, is divided filter residue again by mechanical agitation
It is dispersed in water；Under rotating speed 1000rpm/min, 2min is centrifuged, repeats 3-5 times to remove the inhomogenous graphene oxide sheet of size；
Supernatant centrifuges 15min with rotating speed 8000rpm/min, repeats at least 2 times, with 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, spraying graphene oxide solution time be 1s, infrared lamp dry time be
20s。
Further, in step c, described reducing agent is hydroiodic acid and acetic acid.
Further, in the reducing agent, the volume ratio of hydroiodic acid and acetic acid is 2：5.
Further, the chemical reduction reaction reacts 24h in oil bath at 40 DEG C.
Further, in step d, na phosphates buffer solution（Na-PBS）PH value be 4.12.
Further, in step d, when being pressurizeed using linear sweep voltammetry, voltage transient is by -0.6V to -0.87V.
Further, the flexible material is polyethylene terephthalate（PET）Or dimethyl silicone polymer
（PDMS）.
The beneficial effects of the invention are as follows：
In chemical reduction reaction, reducing agent is acetic acid and hydroiodic acid, the fabulous removal graphite oxide of energy（Alkene）Functional group,
Improve the electric conductivity of redox graphene.Simple electronation can not remove graphite oxide（Alkene）In the whole that contains contain
Oxygen functional group, therefore, the present invention introduce subsequent step electrochemical reduction, further reduced oxygen-containing on the basis of electronation
The presence of functional group.Graphene oxide solution prepared by the present invention is because of some centrifugation steps in preparation process so that its
Dispersiveness is very excellent, and by introducing oxygen plasma so that solution is more easy to adhere to substrate, also improves the steady of flexible electrode
It is qualitative, therefore be not required to add other materials into solution again, the electric conductivity of flexible electrode is ensure that to a certain extent.In addition,
Substrate is handled using oxygen plasma, basal electrode can be patterned, the etching speed of graphene layer and substrate is improved
Degree, it is possible to increase product quality and yield.
The graphene oxide and electrode active material of heat treatment prepared by the preparation method of the fexible film electrode of the present invention
The fexible film electrode of hydridization can be widely used for the fields such as battery, touch-screen, OLED, electrochemical capacitance material and environmental protection automobile.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
Prepare flexible flexible graphene/PET flexible electrodes.Its step is：
（1）, prepare graphene oxide solution（GO solution）：
（1-2）Weigh 0.5g graphite, 0.5g NaNO3, with 23mL H2SO4After mixing, stirred under condition of ice bath；
（1-3）It is slowly added to 3g KMnO4, mixture is transferred to 30oUnder C water bath conditions, 1h is stirred, film is formed；
（1-4）Add 40mL water, 95o30min is stirred under the conditions of C；
（1-5）100mL water is added, the H that 3mL mass concentrations are 30% is then slowly added into2O2, solution colour is caused by depth
Palm fibre is changed into yellow；
（1-6）Filtering solution, adds 100 mL water washings, is dispersed in water filter residue again by mechanical agitation；
（1-7）Under rotating speed 1000rpm/min, 2min is centrifuged, is repeated 3 times to remove the inhomogenous graphene oxide of size
Piece；
（1-8）Supernatant centrifuges 15min with rotating speed 8000rpm/min, be repeated 2 times with remove reduced size GO fragments and
Hydrolysising by-product；
（1-9）Sediment is resuspended in water by mechanical agitation, final to obtain GO solution；
（2）, plated film：The mask for designing good pattern is adhered into polyethylene terephthalate（PET）Substrate, PET bases
The thickness at bottom is 50nm, and area is 5*5cm2Substrate is handled with oxygen plasma；By step（1）Obtained graphite oxide
Alkene solution spraying is in above-mentioned substrate, and the molten concentration of graphene oxide is 0.05mg/L, and quantity for spray is 80mL, is subsequently placed in infrared ray
Dried under lamp；The time for spraying graphene oxide solution is 1s, and the time that infrared lamp is dried is 20s；
（3）, electronation prepare graphene（RGO）
By step（2）Obtained graphene oxide/PET film is placed in 300ml wide-mouth bottle, the bottle hydroiodic acid containing 2ml and
5ml acetic acid, bottleneck is sealed with vacuum grease, is placed in oil bath pan and is reacted 24h at 40 DEG C；Then using saturated sodium bicarbonate,
Distilled water and methanol rinse film successively, dry at room temperature；
（4）, electrochemical reduction
Graphene/PET film that step c is obtained is as na phosphates buffer solution（Na-PBS）In, na phosphates buffer solution
PH value be 4.12, pressurizeed using linear sweep voltammetry, voltage transient is by -0.6V to -0.87V.
Polyethylene terephthalate, chemical formula is COC6H4COOCH2CH2O.（English：Polyethylene
Terephthalate, abbreviation PET）, have good mechanical property, impact strength is 3 ~ 5 times of other films, and folding resistance is good.
There is excellent physical and mechanical properties, long-term temperature in use is up to 120 DEG C, and electrical insulating property is excellent, very within the scope of wider temperature
To under high-temperature high-frequency, its electrical property is still preferable.
After testing, the light transmittance of graphene made from the present embodiment/PET flexible electrodes is 92.1%.
Voltage-curent change of obtained film is measured with comprehensive physical property measuring instrument, and calculates the graphene film
Conductance.The conductance of the graphene film prepared in the present embodiment is 780S/cm.
The graphene film prepared by the method is flexible very well, non-friable, foldable reduction, with excellent electric conductivity
With good pliability, and higher light transmittance.
Embodiment 2
Prepare stretchable flexible graphene/PDMS flexible electrodes.Its step is：
（1）, prepare graphene oxide solution（GO solution）：
（1-2）Weigh 0.3g graphite, 0.3g NaNO3, with 14mL H2SO4After mixing, stirred under condition of ice bath；
（1-3）It is slowly added to 1.8g KMnO4, mixture is transferred to 40oUnder C water bath conditions, 1h is stirred, film is formed；
（1-4）Add 24mL water, 85o30min is stirred under the conditions of C；
（1-5）60mL water is added, the H that 1.8mL mass concentrations are 30% is then slowly added into2O2, solution colour is caused by depth
Palm fibre is changed into yellow；
（1-6）Filtering solution, adds 60 mL water washings, is dispersed in water filter residue again by mechanical agitation；
（1-7）Under rotating speed 1000rpm/min, 2min is centrifuged, is repeated 5 times to remove the inhomogenous graphene oxide of size
Piece；
（1-8）Supernatant centrifuges 15min with rotating speed 8000rpm/min, be repeated 3 times with remove reduced size GO fragments and
Hydrolysising by-product；
（1-9）Sediment is resuspended in water by mechanical agitation, final to obtain GO solution；
（2）, plated film：The mask for designing good pattern is adhered into dimethyl silicone polymer（PDMS）Substrate, PDMS substrates
Thickness is 45nm, and area is 3*4cm2, substrate is handled with oxygen plasma；By step（1）Obtained graphene oxide
Solution spraying is in above-mentioned substrate, and the molten concentration of graphene oxide is 0.04mg/L, and quantity for spray is 40mL, is subsequently placed in infrared lamp
Lower drying；The time for spraying graphene oxide solution is 1s, and the time that infrared lamp is dried is 20s；
（3）, electronation prepare graphene（RGO）
By step（2）Obtained graphene oxide/PET film is placed in 150ml wide-mouth bottle, the bottle hydroiodic acid containing 1.2ml
With 3ml acetic acid, bottleneck is sealed with vacuum grease, is placed in oil bath pan and is reacted 24h at 40 DEG C；Then unsaturated carbonate hydrogen is used
Sodium, distilled water and methanol rinse film successively, dry at room temperature；
（4）, electrochemical reduction
By step（3）Obtained graphene/flexible material film is as na phosphates buffer solution（Na-PBS）In, na phosphates
Buffer solution（Na-PBS）Ph values be 4.12；Pressurizeed using linear sweep voltammetry, voltage transient by -0.6V to -0.87V,
Obtain graphene/PDMS flexible electrodes.
Dimethyl silicone polymer（PDMS）With physiological inertia, good chemical stability, electrical insulating property and weatherability, dredge
It is aqueous good, and with very high anti-shear ability, can for a long time be used at -50 DEG C~200 DEG C.
After testing, the light transmittance of graphene made from the present embodiment/PET flexible electrodes is 93.5%.
Voltage-curent change of obtained film is measured with comprehensive physical property measuring instrument, and calculates the graphene film
Conductance.The conductance of the graphene film prepared in the present embodiment is 840S/cm.
The graphene film prepared by the method is flexible very well, non-friable, foldable reduction, with excellent electric conductivity
With good pliability, and higher light transmittance.
Claims (7)
1. a kind of flexible electrode preparation method based on graphene, it is characterised in that：Comprise the following steps：
A, preparation graphene oxide solution：
By graphite, NaNO3With H2SO4After mixing, stirred under condition of ice bath；Add KMnO4, under water bath condition, stir shape
Into film；Water is added to continue to stir；Stop stirring and add water, then add H2O2, cause solution colour to be changed into yellow from dark brown
Color；Filtering solution, adds water washing, is dispersed in water filter residue again by mechanical agitation；Centrifuge to remove size heterogeneity
Graphene oxide sheet；Then again supernatant is centrifuged to remove reduced size graphene oxide fragment and hydrolysising by-product；It is heavy
Starch is resuspended in water by mechanical agitation, finally obtains graphene oxide solution；
B, plated film：
The mask for designing good pattern is adhered into flexible material substrate, substrate handled with oxygen plasma；Step a is obtained
To graphene oxide solution be sprayed at above-mentioned substrate, the time of spraying graphene oxide solution is 1s, is subsequently placed in infrared ray
20s is dried under lamp；
C, electronation：
By graphene oxide/flexible material film made from step b in the presence of reducing agent, chemical reduction reaction is carried out,
Wherein, described reducing agent is hydroiodic acid and acetic acid；Then rinse thin successively using saturated sodium bicarbonate, distilled water and methanol
Film, is dried at room temperature；
D, electrochemical reduction：
Graphene/flexible material film that step c is obtained as in na phosphates buffer solution, using linear sweep voltammetry plus
Pressure.
2. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：In step a, oxygen is prepared
Graphite alkene solution is concretely comprised the following steps：
By graphite, NaNO3With H2SO4After mixing, stirred under condition of ice bath；Add KMnO4, mixture is transferred to 30-40
Under DEG C water bath condition, 1h is stirred, film is formed；Water is added, 30min is stirred under the conditions of 85-95 DEG C；Stop stirring, and add
Water, then adds the H that mass concentration is 30%2O2, cause solution colour to be changed into yellow from dark brown；Filtering solution, adds washing
Wash, be dispersed in water filter residue again by mechanical agitation；Under rotating speed 1000rpm/min, 2min is centrifuged, repeats 3-5 times to go
Except the inhomogenous graphene oxide sheet of size；Supernatant centrifuges 15min with rotating speed 8000rpm/min, repeats at least 2 times, to go
Except reduced size graphene oxide fragment and hydrolysising by-product；Sediment is resuspended in water by mechanical agitation, finally obtains oxygen
Graphite alkene solution.
3. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：In the reducing agent,
The volume ratio of hydroiodic acid and acetic acid is 2：5.
4. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：The electronation is anti-
In oil bath 24h should be reacted at 40 DEG C.
5. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：In step d, sodium phosphoric acid
The pH value of salt buffer is 4.12.
6. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：In step d, using line
Property scanning voltammetry pressurization when, voltage transient is by -0.6V to -0.87V.
7. the flexible electrode preparation method as claimed in claim 1 based on graphene, it is characterised in that：The flexible material is
Polyethylene terephthalate or dimethyl silicone polymer.
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| CN105217605B (en) * | 2015-07-20 | 2018-01-02 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of patterned Graphene |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN105609217B (en) * | 2016-02-22 | 2017-06-23 | 京东方科技集团股份有限公司 | A kind of graphene transparent electrode, its preparation method and display device |
| CN105867018B (en) * | 2016-03-28 | 2019-08-02 | 深圳市华星光电技术有限公司 | Graphene liquid crystal display device, graphene light-emitting component and preparation method thereof |
| CN108337749A (en) * | 2018-01-23 | 2018-07-27 | 浙江大学 | A kind of oxidation resistant graphite alkene electric heating composite membrane and preparation method thereof |
| CN108517696B (en) * | 2018-05-14 | 2020-05-05 | 东南大学 | Preparation method of patterned flexible conductive graphene cloth |
| CN109183394A (en) * | 2018-08-30 | 2019-01-11 | 东华大学 | A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric |
| CN111816775A (en) * | 2019-04-11 | 2020-10-23 | 东泰高科装备科技有限公司 | Graphene transparent conductive electrode and preparation method and device thereof |
| CN114229836A (en) * | 2022-01-14 | 2022-03-25 | 曲靖华金雨林科技有限责任公司 | Method for electrochemically preparing graphene |
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| CH719596B1 (en) * | 2022-04-12 | 2024-02-29 | Graphenaton Tech Sa | Process for drying a layer of conductive ink on a polymeric layer of a flexible multilayer structure. |
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Effective date of registration: 20210312 Address after: 211111 No. 12, Mazhou East Road, Mau Ling Street, Jiangning District, Nanjing, Jiangsu Patentee after: JIANGSU ZHIJU INTELLECTUAL PROPERTY SERVICE Co.,Ltd. Address before: 210000 Building 2, No.1, Zidong Road, Maqun street, Qixia District, Nanjing City, Jiangsu Province Patentee before: NANJING HAOXUAN NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20211208 Address after: 257000 north of Gangcheng road and west of Gangxi Second Road, dongyinggang Economic Development Zone, Dongying City, Shandong Province Patentee after: Shandong Yiwei New Material Co.,Ltd. Address before: 211111 No. 12, Mazhou East Road, Mau Ling Street, Jiangning District, Nanjing, Jiangsu Patentee before: JIANGSU ZHIJU INTELLECTUAL PROPERTY SERVICE CO.,LTD. |
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