CN109473685A - A kind of preparation method of the compound carbon felt of graphene - Google Patents
A kind of preparation method of the compound carbon felt of graphene Download PDFInfo
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The present invention relates to vanadium redox battery (VRB electrode Material Fields, specifically, it is a kind of preparation method of compound carbon felt of the High-performance graphene suitable for vanadium redox battery, it is intended to solve at this stage the problems such as vanadium cell is low with commercialization carbon felt electrode electro-chemical activity, conductivity is low, vanadium ion is electric low to catalytic performance difference and monocell working efficiency.For the present invention to be commercialized carbon felt as raw material, the method bonded using binder prepares the compound carbon felt of graphene.Compound carbon felt prepared by the present invention has many advantages, such as good electrochemical catalysis performance, conductivity, chemical stability and good single VRB battery performance.Preparation method of the invention have operation is simple, low cost product is easy to industrialization production and advantages of environment protection, can be widely used in vanadium redox battery field.
Description
Technical field:
The present invention relates to a kind of vanadium redox battery (VRB electrode Material Fields, specifically, being be applicable in
In the preparation method of the compound carbon felt of the High-performance graphene of vanadium redox battery.
Figure viewed from behind technology:
21 century is the critical period of new energy technology and new energy materials development, and new energy is environmental-friendly with its, cost
Low advantage, attracts extensive attention.However, wherein the renewable energy power generations process such as wind energy, solar energy is with discontinuously and not
In order to solve this problem stable disadvantage must develop high efficiency, low cost, low pollution and highly-safe extensive energy storage
Technology.Vanadium redox battery (VRB) because its power and energy Independent adjustable, have extended cycle life, energy efficiency is high, dimension
Protect it is at low cost, can fast deep charge and discharge the advantages that, and be widely used in wind energy, the power station energy storage of solar power generation, electricity
Net peak regulation etc..Electrode material is one of the critical material for restricting vanadium cell development.A kind of good vanadium cell electrode material is answered
Have good chemical stability, good mechanical performance, superior electro-chemical activity, high physical electrical conductivity and at low cost etc.
Advantage.Traditional metal material electrochemical reversibility difference is easily passivated, although and the noble metals such as platinum, iridium have electrochemistry
Active high, good reversibility and good chemical stability, but the high cost of this metalloid restricts its large-scale application.
Carbon materials (such as: graphite felt, graphite, carbon cloth and carbon fiber) are at this stage with its good stability and cheap
Cost causes widely to study, and is at present using most electrode materials.But this kind of direct application process electrochemistry of material is lived
Property is low, and battery performance is poor.Therefore it is necessary to processing is modified to this kind of material, to improve the electro-chemical activity of this kind of material.But
So far it can really solve the problems, such as that this kind of material is existing without a kind of suitable method of modifying.
Summary of the invention:
In order to overcome the shortcomings of existing electrode material, the purpose of the present invention is to provide a kind of graphite suitable for vanadium cell
The preparation method of the compound carbon felt of alkene, solve carbon felt stability existing in the prior art is poor, conductivity is low, electro-chemical activity it is low with
And the problems such as single VRB working efficiency low difference.Low cost and high performance compound carbon felt can get using this method, there is electricity
The advantages that conductance is high, stability is good and VRB monocell is functional.
Technical scheme is as follows:
A kind of preparation method of the compound carbon felt of graphene, includes the following steps and process conditions:
(1) the binder diaphragm of 50~150mg is shredded, and is put into the n,N-Dimethylformamide of 100~300mL,
After stirring 2~5h under the conditions of 120~150 DEG C of temperature, diaphragm is completely dissolved in n,N-Dimethylformamide, forms mixing
Liquid；
Wherein, binder diaphragm is Nafion diaphragm, N-Methyl pyrrolidone NMP diaphragm, polythene PE diaphragm, polytetrafluoro
Ethylene PTFE particle gathers inclined fluorine vinyl chloride PVDF powder, binder diaphragm with a thickness of 40~60 μm；
(2) 100~300mg graphene is put into the mixed liquor that step (1) obtains；
(3) organic solvent of 400~500mL is mixed into step (2) resulting mixed liquor, and stirs 8~20h, revolving speed 500
~700rpm/s；
(4) by carbon felt slice, label, and original weight is weighed；
(5) mixed liquor 5~25 times for obtaining carbon felt immersion step (3) of step (4), deposit graphene after immersing every time
Time be 2~5s；
(6) carbon felt that step (5) obtains is put into baking oven, and 100~150 DEG C at a temperature of drying time 8~
20h obtains the compound carbon felt of graphene, and the graphene thicknesses of layers in carbon felt is 1~10 μm；
(7) carbon felt of corresponding label is taken out after drying, and weighs weight record, after weighing, seals carbon felt up for safekeeping, for use.
The preparation method of the compound carbon felt of the graphene, in step (2), graphene is universal graphene, highly conductive
The compound material of type graphene or all kinds of graphenes.
The preparation method of the compound carbon felt of the graphene, in step (3), organic solvent is 1-Methyl-2-Pyrrolidone
NMP。
The preparation method of the compound carbon felt of the graphene, in step (4), the size of carbon felt according to specific battery size and
Depending on test request, 1 × 2cm2For cyclic voltammetry, 3 × 5cm2It is tested for circulating battery.
The preparation method of the compound carbon felt of the graphene, in step (5), the frequency of depositing of graphene is preferably 10~20
It is secondary.
The preparation method of the compound carbon felt of the graphene, in step (6), drying temperature ranges preferably from 110~130
℃。
The technical indicator of the preparation method of the compound carbon felt of the graphene, the compound carbon felt of graphene is as follows: in carbon felt
Graphene thicknesses of layers is 1~10 μm, and the mass ratio of binder is 5%~20% in graphene layer.
Compared with prior art, the present invention have the advantages that it is following significant and the utility model has the advantages that
1, technical process: the present invention is using all kinds of graphenes as raw material, and with Nafion, NMP, PE, PTFE etc. is used as binder,
Successfully prepare the compound carbon felt electrode material of graphene.
2, the present invention method used for preparing compound carbon felt, raw material is easy to get, is low in cost, operation is simple, is suitble to big
Scale development.
3, there are the works such as equipment price is cheap, raw material is easy to get, process is simple, operation is convenient in whole preparation process of the present invention
Industry functionization feature, technological parameter is reliable and easily controllable, facilitates the production of the commercialization electrode material of VRB.
4, the modified carbon felt of graphene of the present invention not only has higher conductivity, and specific surface area is also improved,
It is more preferable to the catalytic effect of tetravalence, pentavalent vanadium ion.
In short, the present invention passes through to be commercialized graphene as raw material, with Nafion, NMP, PE, the binders such as PTFE, preparation
The modified carbon felt combination electrode of graphene, improves conductivity, effective active area, the electrochemical catalysis performance of carbon felt, therefore with
The single VRB battery comparison equipped with commercialization carbon felt, the single VRB battery equipped with compound carbon felt have charge-discharge energy efficiency,
The advantages that voltage efficiency is high, has extended cycle life is (see Fig. 2).Using the graphene of high conductivity, Nafion, NMP are utilized with this,
The binders such as PE, PTFE are combined on carbon felt material, and high performance combination electrode is prepared.Such methods are raw materials used easily
, low in cost and suitable extensive industrialized development is expected to prepare a kind of vanadium cell commercialization of low-cost and high-performance
Carbon felt.
Detailed description of the invention:
Fig. 1 is equipped with the cyclic voltammetry figure of compound carbon felt and original carbon felt.Wherein, (a) voltage efficiency and circulation time
Several relationships, (b) relationship of energy efficiency and cycle-index.
Fig. 2 is equipped with the single vanadium cell efficiency and cycle-index figure of compound carbon felt.
Specific embodiment:
In the specific implementation process, the present invention is raw material using graphene, on Nafion bonding graphene to carbon felt, is made
Standby compound carbon felt electrode.The electrode material has high conductivity, electro-chemical activity height and single vanadium cell charge-discharge performance good
The advantages that.
The present invention is described further below with reference to embodiment.
Embodiment 1
In the present embodiment, the compound carbon felt of graphene the preparation method is as follows:
1, the configuration of mixed liquor is bonded:
(1) the Nafion212 diaphragm of 100mg (with a thickness of 50 μm) is shredded, and is put into the N of 200mL, N- dimethyl formyl
In amine (DMF), 3h is stirred under conditions of 140 DEG C, diaphragm is completely dissolved into and forms mixed liquor；
(2) the highly conductive graphene of 225mg is weighed to be put into aforesaid liquid；Wherein, highly conductive graphene (TNHRGO
TNERGO technical indicator) is as follows: the number of plies < 3, and 1~5 μm of piece diameter, 50~80m of specific surface area2/ g, volume resistivity 600~800
μΩ·m。
(3) 1-Methyl-2-Pyrrolidone of 450mL (NMP) is mixed into step (2) resulting mixed liquor, and stirs 12h,
Revolving speed 600rpm/s；
2, the preparation of modified carbon felt:
(4) by certain specification (1 × 2cm2For cyclic voltammetry, 3 × 5cm2For circulating battery test) carbon felt cut
Piece, label simultaneously weigh original weight；
(5) carbon felt in step (4) is immersed obtained in step (3) mixed liquor 15 times, deposits graphite after immersing every time
The time of alkene is 2~5s；
(6) carbon felt in step (5) is put into baking oven, and 120 DEG C at a temperature of dry 12h, it is compound to obtain graphene
Carbon felt, the graphene thicknesses of layers in carbon felt are 5 μm.
In the present embodiment, the phenomenon that each raw material associativity is good in the compound carbon felt of acquisition, and no graphene falls off.
The correlated performance data of the present embodiment is as follows:
The internal resistance for measuring vanadium redox battery at room temperature is 80m Ω, and the battery performance in VRB is much higher than former carbon
Felt adapts to the application requirement of VRB, can promote the industrialization development of vanadium redox battery.
As shown in Figure 1, can be seen that compound carbon felt from the cyclic voltammetry figure equipped with compound carbon felt and original carbon felt
Potential difference corresponding to redox peak current is 0.10~0.12V, lower than the test result (0.14V) of original carbon felt, graphite
The compound carbon felt of alkene improves anode electricity to the invertibity of (tetravalence, pentavalent vanadium ion)；The ratio between best peak current of compound carbon feltAbsolute value be 1.04, the ratio of original carbon felt is 1.78, and the compound carbon felt of graphene is to positive electricity to excellent
Catalytic activity.
As shown in Fig. 2, having equipped with the single VRB battery for being modified carbon felt combination electrode material, in charge and discharge process very high
Coulombic efficiency, energy efficiency.By repeatedly recycling, battery efficiency does not decay.Modified carbon felt is in VRB battery pentavalent vanadium
It can be stabilized in concentrated sulfuric acid solution, there is good chemical stability.So the compound carbon felt can be good at adapting to vanadium electricity
Pond body system, cheap price, good battery performance can promote the industrialization production of vanadium cell.
Embodiment 2:
Difference from Example 1 is:
1, the highly conductive graphene in step (2) is changed to universal graphene；Wherein, the technical indicator of universal graphene
It is as follows: 0.55~3.74nm of thickness, 0.5~3 μm of diameter, the number of plies < 10 layer, 500~1000m of specific surface area2/g。
2, compound carbon felt is prepared using step same after embodiment 1.
The correlated performance data of the present embodiment is as follows:
The internal resistance for measuring vanadium redox battery at room temperature is 85m Ω, and the battery performance in VRB is still better than original
Carbon felt adapts to the application requirement of VRB.
Embodiment 3
In the present embodiment, the compound carbon felt of graphene the preparation method is as follows:
1, the configuration of mixed liquor is bonded:
(1) poly- inclined fluorine vinyl chloride (PVDF) powder of 80mg is put into the n,N-Dimethylformamide (DMF) of 100mL,
4h is stirred under conditions of 130 DEG C, diaphragm is completely dissolved into and forms mixed liquor；
(2) the highly conductive graphene of 120mg is weighed to be put into aforesaid liquid；Wherein, highly conductive graphene (TNHRGO
TNERGO technical indicator) is as follows: the number of plies < 3, and 1~5 μm of piece diameter, 50~80m of specific surface area2/ g, volume resistivity 600~800
μΩ·m。
(3) 1-Methyl-2-Pyrrolidone of 400mL (NMP) is mixed into step (2) resulting mixed liquor, and stirs 10h,
Revolving speed 550rpm/s；
2, the preparation of modified carbon felt:
(4) by certain specification (1 × 2cm2For cyclic voltammetry, 3 × 5cm2For circulating battery test) carbon felt cut
Piece, label simultaneously weigh original weight；
(5) carbon felt in step (4) is immersed obtained in step (3) mixed liquor 10 times, deposits graphite after immersing every time
The time of alkene is 2~5s；
(6) carbon felt in step (5) is put into baking oven, and 130 DEG C at a temperature of dry 10h, it is compound to obtain graphene
Carbon felt, the graphene thicknesses of layers in carbon felt are 1~5 μm.
In the present embodiment, the phenomenon that each raw material associativity is good in the compound carbon felt of acquisition, and no graphene falls off.
The correlated performance data of the present embodiment is as follows:
The internal resistance for measuring vanadium redox battery at room temperature is 87m Ω, and the battery performance in VRB is much higher than former carbon
Felt adapts to the application requirement of VRB, can promote the industrialization development of vanadium redox battery.
Embodiment 4
In the present embodiment, the compound carbon felt of graphene the preparation method is as follows:
1, the configuration of mixed liquor is bonded:
(1) by the polytetrafluoroethylene (PTFE) of 120mg (PTFE) particle, and it is put into the n,N-Dimethylformamide (DMF) of 300mL
In, 2h is stirred under conditions of 150 DEG C, diaphragm is completely dissolved into and forms mixed liquor；
(2) the universal graphene of 150mg is weighed to be put into aforesaid liquid；Wherein, the technical indicator of universal graphene is such as
Under: 0.55~3.74nm of thickness, 0.5~3 μm of diameter, the number of plies < 10 layer, 500~1000m of specific surface area2/g。
(3) 1-Methyl-2-Pyrrolidone of 500mL (NMP) is mixed into step (2) resulting mixed liquor, and stirs 15h,
Revolving speed 650rpm/s；
2, the preparation of modified carbon felt:
(4) by certain specification (1 × 2cm2For cyclic voltammetry, 3 × 5cm2For circulating battery test) carbon felt cut
Piece, label simultaneously weigh original weight；
(5) carbon felt in step (4) is immersed obtained in step (3) mixed liquor 15 times, deposits graphite after immersing every time
The time of alkene is 2~5s；
(6) carbon felt in step (5) is put into baking oven, and 140 DEG C at a temperature of dry 8h, obtain graphene composite carbon
Felt, the graphene thicknesses of layers in carbon felt are 1~10 μm.
In the present embodiment, the phenomenon that each raw material associativity is good in the compound carbon felt of acquisition, and no graphene falls off.
The correlated performance data of the present embodiment is as follows:
The internal resistance for measuring vanadium redox battery at room temperature is 88m Ω, and the battery performance in VRB is much higher than former carbon
Felt adapts to the application requirement of VRB, can promote the industrialization development of vanadium redox battery.
Embodiment the result shows that, for the present invention to be commercialized carbon felt as raw material, the method bonded using binder prepares graphite
The compound carbon felt of alkene solves vanadium cell at this stage and is commercialized that carbon felt electrode electro-chemical activity is low, conductivity is low, vanadium ion is electric to urging
The problems such as changing performance difference and low monocell working efficiency.Compound carbon felt prepared by the present invention has good electrochemical catalysis
The advantages that energy, conductivity, chemical stability and good single VRB battery performance.Preparation method of the invention has operation letter
Single easy, low cost product is easy to industrialization production and advantages of environment protection, can be widely used in whole vanadium oxide reduction
Flow battery field.
Claims (7)
1. a kind of preparation method of the compound carbon felt of graphene, characterized in that include the following steps and process conditions:
(1) the binder diaphragm of 50~150mg is shredded, and be put into the n,N-Dimethylformamide of 100~300mL, 120
After stirring 2~5h under the conditions of~150 DEG C of temperature, diaphragm is completely dissolved in n,N-Dimethylformamide, forms mixed liquor；
Wherein, binder diaphragm is Nafion diaphragm, N-Methyl pyrrolidone NMP diaphragm, polythene PE diaphragm, polytetrafluoroethylene (PTFE)
PTFE particle gathers inclined fluorine vinyl chloride PVDF powder, binder diaphragm with a thickness of 40~60 μm；
(2) 100~300mg graphene is put into the mixed liquor that step (1) obtains；
(3) organic solvent of 400~500mL is mixed into step (2) resulting mixed liquor, and stirs 8~20h, revolving speed 500~
700rpm/s；
(4) by carbon felt slice, label, and original weight is weighed；
(5) mixed liquor 5~25 times that the carbon felt of step (4) is immersed that step (3) obtain, deposited after immersing every time graphene when
Between be 2~5s；
(6) carbon felt that step (5) obtains is put into baking oven, and in 100~150 DEG C of at a temperature of 8~20h of drying time, obtained
The compound carbon felt of graphene is obtained, the graphene thicknesses of layers in carbon felt is 1~10 μm；
(7) carbon felt of corresponding label is taken out after drying, and weighs weight record, after weighing, seals carbon felt up for safekeeping, for use.
2. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that in step (2), graphene is
The compound material of universal graphene, highly conductive type graphene or all kinds of graphenes.
3. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that in step (3), organic solvent
For 1-Methyl-2-Pyrrolidone NMP.
4. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that in step (4), the ruler of carbon felt
It is very little depending on specific battery size and test request, 1 × 2cm2For cyclic voltammetry, 3 × 5cm2It is surveyed for circulating battery
Examination.
5. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that in step (5), graphene
Frequency of depositing is preferably 10~20 times.
6. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that in step (6), drying temperature
Range preferably from 110~130 DEG C.
7. the preparation method of the compound carbon felt of graphene according to claim 1, characterized in that the skill of the compound carbon felt of graphene
Art index is as follows: graphene thicknesses of layers in carbon felt is 1~10 μm, in graphene layer the mass ratio of binder be 5%~
20%.
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| CN110456118A (en) * | 2019-08-13 | 2019-11-15 | 大同新成新材料股份有限公司 | A kind of preparation method for adsorbing fused salt mixt carbon felt electrode |
| CN110523376A (en) * | 2019-08-21 | 2019-12-03 | 大同新成新材料股份有限公司 | A kind of preparation method of the compound carbon felt of graphene |
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| CN111509238A (en) * | 2020-03-20 | 2020-08-07 | 长沙理工大学 | Preparation method of macroscopic quantity graphene modified electrode material |
| CN113047035A (en) * | 2021-04-16 | 2021-06-29 | 重庆信合启越科技有限公司 | High-temperature preparation method of graphene composite carbon felt |
| CN113809338A (en) * | 2021-09-22 | 2021-12-17 | 广州市上万科技有限公司 | Preparation method of electrode material for all-vanadium redox flow battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110456118A (en) * | 2019-08-13 | 2019-11-15 | 大同新成新材料股份有限公司 | A kind of preparation method for adsorbing fused salt mixt carbon felt electrode |
| CN110523376A (en) * | 2019-08-21 | 2019-12-03 | 大同新成新材料股份有限公司 | A kind of preparation method of the compound carbon felt of graphene |
| CN110552196A (en) * | 2019-08-28 | 2019-12-10 | 大同新成新材料股份有限公司 | Preparation method of graphene composite carbon felt |
| CN111509238A (en) * | 2020-03-20 | 2020-08-07 | 长沙理工大学 | Preparation method of macroscopic quantity graphene modified electrode material |
| CN113047035A (en) * | 2021-04-16 | 2021-06-29 | 重庆信合启越科技有限公司 | High-temperature preparation method of graphene composite carbon felt |
| CN113809338A (en) * | 2021-09-22 | 2021-12-17 | 广州市上万科技有限公司 | Preparation method of electrode material for all-vanadium redox flow battery |
| CN113809338B (en) * | 2021-09-22 | 2023-09-08 | 贵州志喜科技有限公司 | Preparation method of electrode material for all-vanadium redox flow battery |
| CN115020720A (en) * | 2022-07-07 | 2022-09-06 | 北京普能世纪科技有限公司 | Vanadium redox flow battery integrated electrode and preparation method thereof |
| CN115020720B (en) * | 2022-07-07 | 2024-05-28 | 北京普能世纪科技有限公司 | Vanadium redox flow battery integrated electrode and preparation method thereof |
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Application publication date: 20190315 |