CN105489392B - A kind of graphene pole piece and preparation method thereof - Google Patents
A kind of graphene pole piece and preparation method thereof Download PDFInfo
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- CN105489392B CN105489392B CN201510838223.XA CN201510838223A CN105489392B CN 105489392 B CN105489392 B CN 105489392B CN 201510838223 A CN201510838223 A CN 201510838223A CN 105489392 B CN105489392 B CN 105489392B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of graphene pole piece and preparation method thereof, including current collector layers, graphene conductive layer, porous graphene layer, the surface of current collector layers is graphene conductive layer, and graphene conductive layer surface is porous graphene layer;Porous graphene layer is gathered into laminar film by porous graphene particle by carbon based fibers and binding agent, and laminar film passes through roll-in, obtains the connected thin slice of bulk, and thin slice passes through roll-in, obtains porous graphene layer.The graphene pole piece of the present invention, preparation technology are simple, it is easy to accomplish, a variety of chemically or physically power supply systems can be applied.
Description
Technical field
The present invention relates to pole piece, and in particular to a kind of graphene pole piece and preparation method thereof.
Background technology
At present, common power accumulator has Ni-MH battery, lithium ion battery, ultracapacitor etc..Ultracapacitor is
A kind of energy storage device between battery and conventional capacitive, by adsorption and diffusion of the ion on bigger serface active material
Carry out energy storage, have specific power high, have extended cycle life, high current charge-discharge is environment-friendly, it is safe and non-maintaining the advantages of.Lithium
Ion battery relies primarily on lithium ion and realizes energy storage in the insertion and abjection of positive and negative pole material, and lithium ion is in diffusion process is transmitted
Similar to " whirlwind chair ".Lithium ion battery have it is higher than energy, operating voltage is high, self-discharge rate is small, advantages of environment protection.Cause
The development prospect of this ultracapacitor and lithium ion battery in high-power, high-energy electrokinetic cell is even more to allow people to expect.
Ultracapacitor and lithium ion battery as electrokinetic cell need high current, high-power charge and discharge in use
Electricity, therefore the chemical property to both, security and hot property propose new requirement.In order to obtain having big multiplying power charge and discharge special
The battery of property, the internal resistance of cell should be as small as possible.The internal resistance of cell includes ohmic internal resistance and activation polarization and concentration polarization causes
Polarization resistance.Battery ohmic internal resistance is by the contact resistance group of electrode material, electrolyte, membrane electrical resistance and each several part part
Into relevant with the size, structure, assembling of battery etc..Polarization resistance is the electrochemical reaction of anode, negative pole, and ion
The impedance caused by concentration polarization caused by diffusion.Improve battery high rate charge-discharge ability, it is necessary to reduce as much as possible
Internal resistance caused by terms of above-mentioned three.Battery pole piece must also have the high capacity of heat transmission simultaneously, during by high current charge-discharge
Caused heat exports as early as possible from inside battery, prevents inside battery hot-spot and causes electrolyte decomposition or diaphragm breakup.
Graphene is that one kind has individual layer or a small number of several layers of sp2The lonsdaleite material of hydridization, with pi bond between sandwich construction middle level
Form combines, because the electron-like in Fermi can be nearby diracelectron, effective mass zero, therefore electrical conductivity reaches
106S/cm, it is the electric conductivity highest material that the current mankind have found.Simultaneously graphene be most thin, intensity known today most
Big material, there is extremely excellent heat conductivility, and the hardness of superelevation and good ductility.Grapheme material is due to tool
Have a series of above-mentioned excellent performances so that its have in nano-device, heat conduction, conduction and energy storage field it is huge it is potential should
With value, turn into the focus of recent research.Porous graphene is by method system physically or chemically in the lamella of graphene
Making some has the hole of nano-scale, and this structure causes porous graphene when as the energy, catalysis or sorbing material, no
Only there is higher specific surface area, while also good mass transfer effect, given full play to the advantage of two-dimensional nano sheet layer material.
While the distinctive structure of graphene makes it have excellent performance, also come to the process bands in its application process new
Influence.The water-based binder important as clean manufacturing, during electrode slurry is prepared with graphene, phase point can be produced
From, the pole piece shedding of preparation, scaling-off, many adverse effects are brought to its application.In order to improve this situation, can add
Surfactant, graphenic surface energy is reduced, improves its dispersive property in water, but these auxiliary agents may influence pole piece
Energy.
The content of the invention
It is an object of the invention to provide a kind of graphene pole piece and preparation method thereof, including current collector layers, graphene to lead
Electric layer, porous graphene layer, the porous graphene layer prepared using low solvent or solvent-free method, it is possible to achieve porous graphite
Alkene and carbon based fibers are be combined with each other by binding agent, improve pole piece performance.
As lithium ion battery or the pole piece of ultracapacitor and metal-air battery, metal afflux is generally comprised
Body layer, active coating, in order to reduce pole piece internal resistance, also have and adhere to conductive layer on a current collector, then apply active layer and pole is made
Piece.Active coating as lithium ion battery is made generally by positive electrode or negative material with conductive agent and binding agent
Slurry, obtained coated in collection liquid surface or conductive layer surface;Super-capacitor pole piece can also be obtained using similar process
To active coating, can also by active material and conductive agent and binding agent in the case of low no solvent by mechanical or super
Acoustic wave energy is well mixed, binding agent, typically forms fiber using polytetrafluoroethylene (PTFE), with active material and conductive agent complexing one
Rise, carbon film is formed by roll-in, as active layer;Metal-air battery electrode can use second similar to ultracapacitor
Mode, in the presence of a small amount of solvent, film is made as electrode layer.
The technical proposal of the invention is realized in this way:A kind of graphene pole piece, including current collector layers, graphene conductive
Layer, porous graphene layer, the surface of current collector layers is graphene conductive layer, and graphene conductive layer surface is porous graphene layer;
It is characterized in that:Porous graphene layer is gathered into laminar film, sheet by porous graphene particle by carbon based fibers and binding agent
Film passes through roll-in, obtains the connected thin slice of bulk, and thin slice pass through roll-in, obtains porous graphene layer, described carbon based fibers with
The mass percent that binding agent accounts for porous graphene layer is 0.5 ~ 10%;Described porous graphene accounts for the matter of porous graphene layer
It is 90 ~ 97% to measure percentage.
Preparing porous graphene layer step includes(As shown in Fig. 1~8):
(1)Carbon based fibers and porous graphene obtain the composition of carbon based fibers and porous graphene by mixing;It is carbon-based
Fiber and porous graphite ene compositions obtain dispersion of the carbon based fibers in porous graphene by disperseing;
(2)Binding agent be added to carbon based fibers with by mix, obtained in the dispersion of porous graphene binding agent with
The composition of carbon based fibers and porous graphene;The composition of binding agent and carbon based fibers and porous graphene obtains by disperseing
The laminar film being bound to each other to form to porous graphene and carbon based fibers by binding agent.
(3)Laminar film passes through initial roll-in, obtains the connected thin slice of bulk;Thin slice passes through roll-in again, obtains porous stone
Black alkene layer.
Heretofore described " mixing " and " scattered " is not offered as the limitation to mixing and process for dispersing, but represents to deposit
In at least one method that can realize invention being mentioned to.Mixing of the described carbon based fibers in porous graphene and point
Dissipate, can be carried out by mixer, bidirectional mixer, airslide disintegrating mill and ball mill, mix and exported with equipment low-power, low turn
Speed stirring, low sheraing are carried out;It is scattered to be carried out with equipment high-power output, high-speed stirred, high impact forces, high shear.
In mixing and dispersion process, solvent can be added, can be deionized water, ethanol, isopropanol, kerosene, castor oil, N-
Methyl pyrrolidone, the use of solvent can improve the degree that is uniformly dispersed of composition, can be according to final porous graphene layer
Hole between porous graphene particle and carbon based fibers particle and binding agent, be advantageous to the diffusion transport of electrolyte ion, fill
Sub-dip moistens porous graphene, improves effective energy storage of material, and the moulding process of porous graphene layer, and porous graphene
The interaction of pore structure and specific surface area and auxiliary agent selects auxiliary agent and dosage.Therefore, in the embodiment of the present invention, with go from
Sub- water is solvent, and loose dampness is presented after scattered, give external force gently pressure can form bulk, carbon based fibers and binding agent with
Porous graphene is gathered into laminar film.Laminar film roll-in flakiness, thin slice roll-in, drying go to remove water, and form hole.
In mixing and dispersion process, solvent can be added without, is distributed using the granular gradient of porous graphene, forms electrolysis
The diffusion transport passage of matter ion, abundant impregnating porous graphene, improve effective energy storage of material.Small particle(2~10um)It is more
Hole graphene content is not higher than 10%.On the one hand particle small particle can increase the dispersed difficulty of composition, on the other hand can drop
The compacted density of low pole piece.
Binding agent can be that powdered granule material adds or emulsion adds.Added in the embodiment of the present invention 1 with powder-material
Enter.The composition of binding agent and carbon based fibers and porous graphene is mixed, disperseed, can by mixer, airslide disintegrating mill,
Ball mill and banbury are carried out, and stirring at low speed mixing is exported with equipment low-power, and slow-speed of revolution stirring, low sheraing is carried out;High-speed stirring
Mix scattered with equipment high-power output, high-speed stirred, high impact forces, high shear progress.
Heretofore described " initial roll-in " and " roll-in again " are not offered as to by " lamellar membrane " to " porous graphene
The limitation of layer " former and method, but represent at least one method that can realize invention being mentioned to be present.Described
Roll-in can be carried out by twin rollers, spreader bar, sheet extruder, can be heated in nipping process, and heating-up temperature is 40 ~ 320
DEG C, preferably 100 ~ 250 DEG C.Porous graphene thickness degree is 20 ~ 200um.
Described carbon based fibers include CNT, carbon fiber, carbon nano-fiber;Described porous graphene can be by oxygen
After graphite reduction, obtain, can also be passed through by biomass through the activation pore-creating such as chemical reagent or vapor, carbon dioxide
After crossing metallic compound catalyzing and carbonizing, obtained through the activation pore-creating such as chemical reagent or vapor, carbon dioxide, its specific surface area
For 800 ~ 3500m2/ g, 2 ~ 30um of particle diameter;Described binding agent is the polymer that homopolymerization/copolymerization monomer is tetrafluoroethene, including
Polytetrafluoroethylene (PTFE).
Glue is made by graphene particles and binding agent in described graphene conductive layer, and coating or printing are on a current collector
Formed.Described graphene can be reduced to obtain by graphite oxide, can pass through transistion metal compound catalytic carbon by biomass
Change, it is purified to obtain, it can be vapor-deposited and obtained under catalyst action use by organic gas molecule, can also be by the machine of graphite
Tool is peeled off to obtain.Described current collector layers include metal foil, wire netting, foam metal.
Described current collector layers include metal foil, wire netting, foam metal, and described graphene pole piece can be used for super electricity
Container, lithium ion battery, metal-air battery, including lithium-air battery, magnesium air cell, zinc-air battery, aluminium-air cell,
Fuel cell.
The positive effect of the present invention is the diffusion transport for the storage and ion that electric charge is realized with porous graphene layer;Carbon-based fibre
Dimension also improves pole piece intensity, fibrous leads in addition to transmission electronically forms conductive path with together with the fiber that binding agent is formed
Electric agent and binding agent are advantageous to the diffusion transport of electrolyte ion, the abundant infiltration to porous graphene.The graphene of the present invention
Pole piece is simple using low solvent or solvent-free method, preparation technology, it is easy to accomplish, a variety of chemically or physically power supplys can be applied
System, include lithium-air battery, magnesium air cell, zinc sky for preparing ultracapacitor, lithium ion battery, metal-air battery
Pneumoelectric pond, aluminium-air cell and fuel cell.
Brief description of the drawings
Fig. 1 is the structural representation of the graphene pole piece of the present invention.
Fig. 2 is the preparation flow schematic diagram of the graphene pole piece of the present invention.
Fig. 3 is the porous graphene and the mixed photo of CNT of embodiments of the invention 1.
Fig. 4 is light pressure caking photo of the porous graphene of embodiments of the invention 1 with CNT after scattered.
Fig. 5 is the mixed photo of porous graphene, CNT and polytetrafluorethylepowder powder of embodiments of the invention 1
(White point is polytetrafluorethylepowder powder in figure).
Fig. 6 is the photograph that the polytetrafluorethylepowder powder of embodiments of the invention 1 disperses in porous graphene and CNT
Piece(White point disappears in figure).
Fig. 7 is that laminar film is made in the porous graphene, CNT and polytetrafluorethylepowder powder of embodiments of the invention 1
Photo.
Fig. 8 is porous stone made of the porous graphene, CNT and polytetrafluorethylepowder powder of embodiments of the invention 1
The photo of black alkene layer.
Fig. 9 is the SEM figures of the porous graphene layer of embodiments of the invention 1.
Figure 10 is that the graphene pole piece of embodiments of the invention 1 is used for the charging and discharging curve of ultracapacitor.
Embodiment
The graphene pole piece of the present invention is illustrated with reference to embodiment, described embodiment is simply to the present invention
The specific descriptions of claim, claim include but is not limited to described embodiment content.
Embodiment 1
(1)Weigh 3.6g porous graphenes(The hexa-atomic element in Changzhou, SE4532, specific surface area 2202m2/ g, particle diameter D90 are
10.8um)With 1.2g CNTs, stirring at low speed mixing 10min, the composition of CNT and porous graphene is obtained;Add
5g deionized waters, high-speed stirred 1h, obtain the dispersion of CNT and porous graphene.
(2)2.8g polytetrafluoroethylene (PTFE) powders are weighed, are added to(1)Dispersion in, stirring at low speed mixing 5min, white
Polytetrafluoroethylene (PTFE) powder disappear, obtain the composition of binding agent and CNT and porous graphene;High-speed stirred 2h, is obtained
The laminar film that porous graphene and CNT are bound to each other to form by polytetrafluoroethylene (PTFE).
(3)Laminar film passes through 5 initial roll-ins, obtains the connected thin slice of bulk;Thin slice passes through 5 roll-ins repeatedly, obtains
Porous graphene layer.
(4)According to 0.5:0.5:1:8 ratios weigh sodium carboxymethylcellulose, butadiene-styrene rubber, graphene and deionized water system
Into glue, coated on corrosive aluminum foil, 5min is stood, porous graphene layer is adhered to, 120 DEG C of dry 5h.
(5)Will(4)Roll-in, graphene pole piece is obtained, for ultracapacitor.
Embodiment 2
(1)Weigh 4.65g porous graphenes(The hexa-atomic element in Changzhou, SE4532, specific surface area 2202m2/ g, particle diameter D90 are
10.8um)With 0.15g carbon nano-fibers, stirring at low speed mixing 10min, the combination of porous graphene and carbon nano-fiber is obtained
Thing;5g deionized waters are added, high-speed stirred 1h, obtain the dispersion of carbon nano-fiber and porous graphene.
(2)Weigh 0.33g ptfe emulsions(60% solid content), it is added to(1)Dispersion in, stirring at low speed
2min is mixed, obtains the composition of binding agent and carbon nano-fiber and porous graphene;High-speed stirred 2h, obtains porous graphene
The laminar film being bound to each other to form with carbon nano-fiber by polytetrafluoroethylene (PTFE).
(3)Laminar film passes through 3 roll-ins, obtains the connected thin slice of bulk;Thin slice passes through 5 roll-ins repeatedly, obtains porous
Graphene layer.
(4)According to 1:1:8 ratios weigh Kynoar, graphene and 1-METHYLPYRROLIDONE and glue are made, and are coated in
On aluminium foil, 5min is stood, porous graphene layer is adhered to, 180 DEG C of dry 10h.
(5)Will(4)Roll-in, graphene pole piece is obtained, for lithium ion battery.
Embodiment 3
(1)Weigh 4g porous graphenes(The hexa-atomic element in Changzhou, SE4532, specific surface area 2202m2/ g, particle diameter D90 are
10.8um)With 0.5g carbon fibers, stirring at low speed mixing 10min, the composition of porous graphene and carbon fiber is obtained;High-speed stirred
1h, obtain the dispersion of carbon fiber and porous graphene.
(2)0.5g polytetrafluoroethylene (PTFE) powders are weighed, are added to(1)Dispersion in, stirring at low speed mixing 5min, white
Polytetrafluoroethylene (PTFE) powder disappear, obtain the composition of binding agent and carbon fiber and porous graphene;High-speed stirred 2h, obtain more
The laminar film that hole graphene and carbon fiber are bound to each other to form by polytetrafluoroethylene (PTFE).
(3)Laminar film passes through 10 initial roll-ins, obtains the connected thin slice of bulk;Thin slice passes through 5 roll-ins repeatedly, obtains
Porous graphene layer.
(4)According to 0.5:0.5:1:8 ratios weigh sodium carboxymethylcellulose, butadiene-styrene rubber, graphene and deionized water system
Into glue, coated in nickel foam, 5min is stood, 100 DEG C of dry 3h, obtains foamed nickel current collector.
(5)Porous graphene layer, into pole piece, is dried with catalyst layer and foamed nickel current collector roll pressing, cut-parts, zinc is made
Air cell electrode.
Claims (5)
1. a kind of graphene pole piece, including current collector layers, graphene conductive layer, porous graphene layer, the surface of current collector layers are
Graphene conductive layer, graphene conductive layer surface are porous graphene layer, it is characterised in that porous graphene layer is by porous graphite
Alkene particle is gathered into laminar film by carbon based fibers and binding agent, and laminar film passes through roll-in, obtains the connected thin slice of bulk, thin slice
By roll-in, porous graphene layer is obtained;The mass percent that described carbon based fibers and binding agent account for porous graphene layer is
0.5 ~ 10%;Porous graphene in described porous graphene layer account for the mass percent of porous graphene layer for 90 ~
97%。
A kind of 2. graphene pole piece according to claim 1, it is characterised in that described carbon based fibers include CNT,
Carbon fiber, carbon nano-fiber.
3. a kind of graphene pole piece according to claim 1, it is characterised in that porous in described porous graphene layer
Graphene specific surface area is 800 ~ 3500m, 2/g, 2 ~ 30um of particle diameter.
4. a kind of graphene pole piece according to claim 1, it is characterised in that described binding agent is homopolymerization/copolymerization monomer
For the polymer of tetrafluoroethene.
5. a kind of graphene pole piece according to claim 1, it is characterised in that described graphene conductive layer is by graphene
Glue is made with binding agent in particle, and coating or printing are formed on a current collector.
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CN105788879B (en) * | 2016-04-27 | 2019-05-03 | 东华大学 | A kind of graphene film and its continuous preparation method |
CN107565086B (en) * | 2016-06-30 | 2022-12-13 | 卢云峰 | Preparation method of battery plate |
CN106158429A (en) * | 2016-08-24 | 2016-11-23 | 刘爽 | The method manufacturing graphene-based ultracapacitor |
CN109935785A (en) * | 2017-12-15 | 2019-06-25 | 东莞市凯金新能源科技股份有限公司 | A kind of production method of fast charge graphite cathode piece |
CN108470635A (en) * | 2018-02-07 | 2018-08-31 | 宁波中车新能源科技有限公司 | A kind of low internal resistance, high power graphene super capacitor electrode slice and preparation method thereof |
CN108365224B (en) * | 2018-02-13 | 2021-03-19 | 青海百能汇通新能源科技有限公司 | Polar plate and preparation method thereof |
CN108963188B (en) * | 2018-09-17 | 2020-09-04 | 江苏瑞濏新能源有限公司 | Lithium battery cathode, preparation method thereof and lithium battery |
CN111525114A (en) * | 2020-05-09 | 2020-08-11 | 四川聚创石墨烯科技有限公司 | Method for continuously preparing current collector-free silicon-carbon negative electrode paper |
CN112863900B (en) * | 2021-01-04 | 2021-12-28 | 西安交通大学 | Porous graphene electrode for supercapacitor and preparation method thereof |
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