CN110350201A - A kind of highly conductive graphene collector of water system battery lightweight and preparation method thereof - Google Patents
A kind of highly conductive graphene collector of water system battery lightweight and preparation method thereof Download PDFInfo
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- CN110350201A CN110350201A CN201910581466.8A CN201910581466A CN110350201A CN 110350201 A CN110350201 A CN 110350201A CN 201910581466 A CN201910581466 A CN 201910581466A CN 110350201 A CN110350201 A CN 110350201A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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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
Abstract
The invention discloses highly conductive graphene collectors of a kind of water system battery lightweight and preparation method thereof.This method comprises: graphite is mixed with the concentrated sulfuric acid, stir, pre-oxidation sequentially adds hydrogen peroxide and foaming agent thereto, is stored at room temperature after being uniformly mixed, both obtained a large amount of graphene；Made graphene is passed through after different pressure roll-ins under roll squeezer later, obtains the highly conductive graphene collector of the water system battery lightweight.Path is simply realized with a low cost the present invention provides a kind of highly conductive Flexible graphene paper of magnanimity preparation lightweight, whole process need to only be handled by a simple physical mixed and dry-pressing, without being related to the complex process such as any high temperature or heating, without using any complex instrument equipment.The preparation process is reduced compared with the sour dosage of conventional graphite alkene preparation method, therefore this method is a kind of green preparation method being simple and efficient, and the industrialization production of graphene collector is advantageous.
Description
Technical field
The present invention relates to the graphene-based conductive current collector fields of low temperature energy storage, and in particular to a kind of water system battery lightweight
Highly conductive graphene collector and preparation method thereof.
Background technique
Lithium ion battery is the highest chemical energy storage battery of current energy density.However, inflammable organic electrolyte makes
It obtains lithium ion battery safety accident to take place frequently, the accidents such as the kindling of tesla's electric car, the explosion of Samsung mobile phone are come clearly into view.Therefore,
Safe and clean water system battery is considered to be the following optimal selection for replacing organic system battery.
Current battery device is mainly by positive and negative pole material, diaphragm, electrolyte, collector and battery case composition.And show
Some is mainly based on the research of collector and electrolyte about the research article of battery system, and collector is scientific research personnel
Pay close attention to relatively small number of research direction.In principle, a kind of battery can real industrialization, conduct electricity very well, it is cheap, add
Work is simple and the collector that has holding stable in battery system is to first have to consider the problems of.Once these problems are solved
Certainly, can substantially accomplish to put things right once and for all.
Current collector mainly includes Metal Substrate collector and two kinds of carbon-based collector, and wherein Metal Substrate collector is main
Be with the aluminium of the copper and plus plate current-collecting body that do negative current collector, it is and highly developed in organic system, but due to aqueous electrolyte
A high reaction activity, the presence that almost all of Metal Substrate collector all cannot be stable.And these metals again can be to water system
The liberation of hydrogen oxygen evolution reaction of electrolyte plays catalysis and facilitation, so that the voltage window for causing entire battery stable becomes smaller, into
And influence the energy density of final battery.And the mainly commercial carbon paper and carbon cloth of carbon-based collector at present, both collection
The hydrophily of fluid is poor, it is necessary to which improving hydrophily by pre-treatment could normal use.Simultaneously most importantly at present these
The quality of collector is all bigger, higher than the quality for the active material being coated on, and present research calculate capacity when
The amount for often all only calculating independent active material is waited, the capacity of entire battery will give a discount greatly if collector etc. is counted in
Button.Therefore, it is badly in need of a kind of lightweight, it is highly conductive and keep stable collector in water system battery system.
Graphene, this novel two-dimentional carbon material, while being also the particular semiconductor material without band gap, have excellent
Electric conductivity, excellent flexibility and unit mass is lighter.This series of advantages just can satisfy above-mentioned ideal water system battery
The use demand of collector.Also it is based on this, has had pertinent literature report to be applied to flexible device for graphene as substrate
In part, chemical property outstanding is shown.But these preparation methods are all very complicated, and higher cost, are only applicable in
In research, and it can not accomplish real large-scale production.
Summary of the invention
It is an object of the invention to the deficiencies above-mentioned for the prior art, provide a kind of highly conductive stone of water system battery lightweight
Black alkene collector and preparation method thereof.
The problem to be solved by the present invention is that providing a kind of lightweight height that can stablize under water system battery system and use
Conductive Flexible graphene paper, and the preparation method of the graphene is compared with the preparation method of traditional graphene, more
It is simple and efficient, cost is lower, and it is suitable for industrialization productions.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of preparation method of the highly conductive graphene collector of water system battery lightweight provided by the invention, including walk as follows
It is rapid:
(1) graphite is mixed with concentrated sulfuric acid solution, is stirred evenly, carry out pre-oxidation treatment, form mixture；
(2) hydrogenperoxide steam generator and foaming agent are sequentially added into the mixture that step (1) obtains, stirred evenly, room temperature condition
Under, extruding obtains graphene powder after standing；
(3) step (2) graphene powder is subjected to roller process (1-50Mpa) by roll squeezer, the water system electricity is made
The highly conductive graphene collector of pond lightweight.
Further, step (1) graphite is natural flake graphite, and the granularity of the graphite is 50-5000 mesh；Purity
It is 99.99%.
Further, step (1) concentrated sulfuric acid solution is the sulfuric acid solution that mass fraction is greater than or equal to 70%.
Further, the mass volume ratio of step (1) graphite and concentrated sulfuric acid solution is 1-20:5-300 g/mL；Institute
The time for stating pre-oxidation treatment is 1-30min.
Preferably, the time of step (1) described stirring is 1-60 min, and the rate of stirring is 50-300 r/min.
Further, the mass percent concentration of step (2) described hydrogenperoxide steam generator is 30%wt.
Further, the mass volume ratio of step (1) graphite and step (2) described hydrogenperoxide steam generator is 1-20:
2-200g/mL。
Further, step (2) foaming agent is azodicarbonamide, polyurethane, dinitrosopentamethylene tetramine
And one or more of unifor；The mass ratio of step (1) graphite and step (2) described foaming agent is 1-20:
1-40。
Preferably, step (2) mixing time is 1-60min, stirring rate 50-300r/min；
Further, the time of step (2) described standing is 1-24h, and the temperature of the standing is room temperature.
Further, the pressure of step (3) described roller process is 1-50 Mpa.
A kind of highly conductive graphene collector of water system battery lightweight as made from above-mentioned method, lightweight is highly conductive, should
The conductivity of graphene collector is 0.8-6.3 x104 S m-1。
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) method of the preparation highly conductive graphene collector of water system battery lightweight provided by the invention, it is only necessary at normal temperature
By simple physical mixed and being stored at room temperature processing, can either extruding go out a large amount of graphene, be not necessarily to high temperature or heating etc. its
His complex process is a kind of simple and has cost-benefit method；
(2) method of the preparation highly conductive graphene collector of water system battery lightweight provided by the invention, the acid amount of introducing is less,
The only 10%-20% of conventional oxidation reduction method reduces the emission treatment pressure of later period waste liquid spent acid, the graphene prepared
Sample quality compared to conventional method synthesis is higher, is a kind of method of high-efficiency cleaning；
(3) method of the preparation highly conductive graphene collector of water system battery lightweight provided by the invention, can roller under dry-pressing
Highly conductive light flexible graphene paper is extruded, without using the instrument of complex precise, to realization graphene paper as collector
Industrialization production have certain meaning.
Detailed description of the invention
Fig. 1 is the microcosmic SEM figure for the highly conductive graphene collector of water system battery lightweight that embodiment 1 obtains；
Fig. 2 is the hydrophily test chart for the highly conductive graphene collector of water system battery lightweight that embodiment 1 obtains；
Fig. 3 is the hydrophily test chart of commercial carbon cloth；
Fig. 4 is the hydrophily test chart of commercial carbon paper.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with attached drawing and example, but implementation and protection of the invention
It is without being limited thereto.If it is existing to be that those skilled in the art can refer to it is noted that there is the not special process of detailed description below
Technology realize or understand.Reagents or instruments used without specified manufacturer, be considered as can by it is commercially available be commercially available it is normal
Advise product.
Embodiment 1
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The natural flake graphite of 50 mesh of 1 g and the concentrated sulfuric acid solution of 15mL are stirred 10 min, stirring rate 100
R/min is stirred evenly, pre-oxidation treatment 15min, then sequentially adds the mistake that 6 ml mass percent concentrations are 30% thereto
Then hydrogen peroxide solution and 2 g azodicarbonamides stir 3 min with 50 r/min speed, are stored at room temperature 10 after mixing
H, that is, extruding obtains graphene powder；Obtained graphene powder is rolled into soft graphite under the pressure of 25 Mpa later
Alkene paper, i.e., the described highly conductive graphene collector of water system battery lightweight.
Fig. 1 is the microcosmic SEM figure for the highly conductive graphene collector of water system battery lightweight that embodiment 1 obtains；Such as Fig. 1 institute
Show, it will thus be seen that for crystalline flake graphite after decomposing the dual extruding for generating gas by foaming agent and hydrogen peroxide, interlayer is complete
It is peeled away entirely to extruding, expansion effect is significantly, can be more intuitive to see graphene film from scanning electron microscope (SEM) photograph on piece
Layer is more transparent, and the graphene number of plies for showing that this method is removed is less.The effect that other embodiments are observed under scanning electron microscope
Fruit is similar to Example 1, can refer to Fig. 1.
One that the obtained highly conductive graphene collector of water system battery lightweight is formed on roll squeezer by dry-pressing
The graphene paper slip of a 5*20cm, 360 ° of graphene paper folding is still intact, shows good flexibility, is applicable in
In flexible device.
Fig. 2, Fig. 3 and it is shown in Fig. 4 be the one of above-mentioned graphene paper slip (5*20cm) and commercial carbon cloth, commercial carbon paper respectively
A hydrophily contrast test, the results showed that, the hydrophily of the graphene paper slip is better than commercial carbon cloth and commercial carbon paper, wetting
Angle only has 85 °, better than commercial carbon cloth and commercial carbon paper (142.8 ° and 123.7 °) this for its actual use as collector
It is advantageously.Simultaneously resulting graphene paper slip passed through into four probe methods at room temperature and measure its square resistance rate and is
0.319 Ω/cm, being converted into conductivity is 6.3x104 S m-1, this is suitable with commercial carbon cloth, the commercial conductivity of carbon paper, shows
The graphene paper slip has higher electric conductivity, can be used as collector use.Other embodiments effect and 1 phase of embodiment
Seemingly, Fig. 2, Fig. 3 and Fig. 4 be can refer to.
Embodiment 2
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The natural flake graphite of 300 mesh of 0.2g and the concentrated sulfuric acid solution of 1mL are stirred 3min, stirring rate is 50 r/
Min is stirred evenly, pre-oxidation treatment 5min, then sequentially adds the peroxidating that 2ml mass percent concentration is 30% thereto
Hydrogen solution and 0.3g polyurethane stir 1min with 50 r/min speed, are stored at room temperature 2h i.e. extruding after mixing and obtain graphite
Alkene powder；Obtained graphene powder is rolled into Flexible graphene paper under the pressure of 10Mpa later, i.e., the described water system electricity
The highly conductive graphene collector of pond lightweight, passes through potentiostatic method for resulting graphene collector at room temperature and measures conductivity
For 2.2x104 S m-1.Water system battery made from embodiment 2 is observed under scanning electron microscope with the highly conductive graphene collector of lightweight
Effect it is similar to Example 1, can refer to Fig. 1.The highly conductive graphene collector of water system battery lightweight made from embodiment 2
Hydrophily is similar to Example 1, can refer to Fig. 2.
Embodiment 3
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The concentrated sulfuric acid solution of the natural flake graphite of 500 mesh of 0.8g and 12 mL is stirred 8min, stirring rate 80
R/min is stirred evenly, pre-oxidation treatment 10min, then sequentially adds the mistake that the mass percent concentration of 6ml is 30% thereto
The dinitrosopentamethylene tetramine of hydrogen peroxide solution and 1.5g stirs 3 min with 50 r/min speed, after mixing room temperature
It stands 6h, that is, extruding and obtains graphene powder；Obtained graphene powder is rolled into flexibility under the pressure of 20Mpa later
Graphene paper, i.e., the highly conductive graphene collector of water system battery lightweight of the described preparation, resulting graphene collector is existed
Measuring conductivity by potentiostatic method at room temperature is 1.6x104 S m-1.Water system battery lightweight made from embodiment 3 is highly conductive
The effect that graphene collector is observed under scanning electron microscope is similar to Example 1, can refer to Fig. 1.The electricity of water system made from embodiment 3
The hydrophily of the highly conductive graphene collector of pond lightweight is similar to Example 1, can refer to Fig. 2.
Embodiment 4
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The natural flake graphite of 1000 mesh of 1.5g and the concentrated sulfuric acid solution of 20mL are stirred 15 min, stirring rate is
150 r/min, stir evenly, pre-oxidation treatment 20min, and then sequentially adding 12 ml mass percent concentrations thereto is 30%
Hydrogenperoxide steam generator and 3 g unifor, with 150 r/min speed stir 5 min be stored at room temperature after mixing
16 h, that is, extruding obtains graphene powder；Obtained graphene powder is rolled into flexible stone under the pressure of 35 Mpa later
Black alkene paper, i.e., the highly conductive graphene collector of water system battery lightweight of the described preparation, by resulting graphene collector in room
Temperature is lower to measure conductivity by potentiostatic method as 8.0x104 S m-1.The highly conductive stone of water system battery lightweight made from embodiment 4
The effect that black alkene collector is observed under scanning electron microscope is similar to Example 1, can refer to Fig. 1.Water system battery made from embodiment 4
Hydrophily with the highly conductive graphene collector of lightweight is similar to Example 1, can refer to Fig. 2.
Embodiment 5
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The concentrated sulfuric acid solution of the natural flake graphite of 3000 mesh of 2 g and 30 mL is stirred 20 min, stirring rate is
200 r/min, stir evenly, and after 30 min of pre-oxidation treatment, sequentially adding 12ml mass percent concentration thereto is 30%
The unifor of hydrogenperoxide steam generator and 4g stirs 7 min with 200 r/min speed and is stored at room temperature 24 h after mixing
I.e. extruding obtains graphene powder.Obtained graphene powder is rolled into Flexible graphene under the pressure of 50 Mpa later
Paper, i.e., the highly conductive graphene collector of water system battery lightweight of the described preparation, at room temperature by resulting graphene collector
Measuring conductivity by potentiostatic method is 4.5x104 S m-1.The highly conductive graphene of water system battery lightweight made from embodiment 5
The effect that collector is observed under scanning electron microscope is similar to Example 1, can refer to Fig. 1.Water system battery made from embodiment 5 is with gently
The hydrophily of the highly conductive graphene collector of matter is similar to Example 1, can refer to Fig. 2.
Embodiment 6
A method of the highly conductive graphene collector of water system battery lightweight is prepared, is included the following steps:
The natural flake graphite of 5000 mesh of 0.5g and the concentrated sulfuric acid solution of 10mL are stirred 10 min, stirring rate is
100 r/min, stir evenly, pre-oxidation treatment 6min, and the mass percent concentration for then sequentially adding 12mL thereto is 30%
Hydrogenperoxide steam generator, the unifor of 0.5g and the dinitrosopentamethylene tetramine of 0.6g, with 100 r/min speed
2 min of degree stirring are stored at room temperature 4h i.e. extruding after mixing and obtain graphene powder；Later by obtained graphene powder
Flexible graphene paper is rolled under the pressure of 12 Mpa, i.e., the described highly conductive graphene collector of water system battery lightweight will
It is 2.4x10 that resulting graphene collector passes through potentiostatic method to measure conductivity at room temperature4 S m-1.Made from embodiment 6
The effect that water system battery is observed under scanning electron microscope with the highly conductive graphene collector of lightweight is similar to Example 1, can refer to figure
1.The hydrophily of the highly conductive graphene collector of water system battery lightweight made from embodiment 6 is similar to Example 1, can refer to figure
2。
Embodiment 7
A kind of method of the highly conductive graphene collector of water system battery lightweight, includes the following steps:
The natural flake graphite of 80 mesh of 1.7g and the concentrated sulfuric acid solution of 25mL are stirred 30min, stirring rate 300
R/min is stirred evenly, pre-oxidation treatment 25min, then sequentially adds the mistake that 18mL mass percent concentration is 30% thereto
The polyurethane of hydrogen peroxide solution, the azodicarbonamide of 1.5g and 1.8g, after stirring 4min with 300 r/min speed, mixing is equal
Be stored at room temperature after even 18h can extruding obtain graphene powder.Later by obtained graphene powder under the pressure of 40Mpa
It is rolled into Flexible graphene paper, i.e., the described highly conductive graphene collector of water system battery lightweight, by resulting graphene afflux
It is 5.6x10 that body passes through potentiostatic method to measure conductivity at room temperature4 S m-1.Water system battery lightweight height made from embodiment 7
The effect that conductive graphene collector is observed under scanning electron microscope is similar to Example 1, can refer to Fig. 1.Water made from embodiment 7
Be the highly conductive graphene collector of battery lightweight hydrophily it is similar to Example 1, can refer to Fig. 2.
Embodiment 8
A kind of method of the highly conductive graphene collector of water system battery lightweight, includes the following steps:
The natural flake graphite of 50 mesh of 1.2g and the concentrated sulfuric acid solution of 16ml are stirred 12min, stirring rate 120
R/min is stirred evenly, pre-oxidation treatment 20min, then sequentially adds the mistake that the mass percent concentration of 8mL is 30% thereto
The unifor of hydrogen peroxide solution, the azodicarbonamide of 1g and 1.5g, after stirring 3.5min with 120 r/min speed,
Be stored at room temperature after mixing 14h can extruding obtain graphene powder.Later by obtained graphene powder 30Mpa's
Flexible graphene paper is rolled under pressure, i.e., the described highly conductive graphene collector of water system battery lightweight, by resulting graphite
It is 9.6x10 that alkene collector passes through potentiostatic method to measure conductivity at room temperature3 S m-1.Water system battery made from embodiment 8 is used
The effect that the highly conductive graphene collector of lightweight is observed under scanning electron microscope is similar to Example 1, can refer to Fig. 1.Embodiment 8 is made
The hydrophily of the highly conductive graphene collector of water system battery lightweight obtained is similar to Example 1, can refer to Fig. 2.
In conclusion a kind of preparation method of the highly conductive graphene collector of water system battery lightweight provided by the invention,
The graphene conductive rate prepared is up to 6.3 x103 S m-1.This will be high than general metallic conductivity, while the graphite
The angle of wetting of alkene paper is shown to be hydrophilic less than 90 °, and wetability is better than commercial carbon cloth and commercial carbon paper.Preparation simultaneously
The highly conductive graphene collector of water system battery lightweight has flexibility well, even if its structure is when folding 360 ° to have saved
It is good.
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (10)
1. a kind of preparation method of the highly conductive graphene collector of water system battery lightweight, which comprises the steps of:
(1) graphite is mixed with concentrated sulfuric acid solution, is stirred evenly, carry out pre-oxidation treatment, form mixture；
(2) hydrogenperoxide steam generator and foaming agent are sequentially added into step (1) described mixture, stirs evenly, is obtained after standing
Graphene powder；
(3) step (2) graphene powder is subjected to roller process, the highly conductive graphene of water system battery lightweight is made
Collector.
2. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
Step (1) graphite is natural flake graphite, and the granularity of the graphite is 50-5000 mesh.
3. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
Step (1) concentrated sulfuric acid solution is the sulfuric acid solution that mass fraction is greater than or equal to 70%.
4. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
The mass volume ratio of step (1) graphite and concentrated sulfuric acid solution is 1-20:5-300 g/mL；The time of the pre-oxidation treatment
For 1-30min.
5. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
The mass percent concentration of step (2) described hydrogenperoxide steam generator is 30%wt.
6. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
The mass volume ratio of step (1) graphite and step (2) described hydrogenperoxide steam generator is 1-20:2-200g/mL.
7. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
Step (2) foaming agent is in azodicarbonamide, polyurethane, dinitrosopentamethylene tetramine and unifor
More than one；The mass ratio of step (1) graphite and step (2) described foaming agent is 1-20:1-40.
8. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
The time of step (2) described standing is 1-24h.
9. the preparation method of the highly conductive graphene collector of water system battery lightweight according to claim 1, which is characterized in that
The pressure of step (3) described roller process is 1-50 Mpa.
10. a kind of highly conductive graphene of water system battery lightweight as made from claim 1-9 described in any item preparation methods
Collector.
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| CN113555229A (en) * | 2020-04-26 | 2021-10-26 | 中天超容科技有限公司 | Graphene paper current collector, preparation method and supercapacitor |
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