CN102468493B - Preparation method of high-activity vanadium battery electrode material - Google Patents
Preparation method of high-activity vanadium battery electrode material Download PDFInfo
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- CN102468493B CN102468493B CN201010536225.0A CN201010536225A CN102468493B CN 102468493 B CN102468493 B CN 102468493B CN 201010536225 A CN201010536225 A CN 201010536225A CN 102468493 B CN102468493 B CN 102468493B
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Abstract
Relating to the fields of battery manufacturing and energy storage, the invention specifically provides a preparation method of a high-activity vanadium battery electrode material, and solves the problem that in prior art, low electrode reaction activity of carbon materials can influence vanadium battery performances. With natural flaky graphite powder as a base material, graphite oxide powder as an active additive, and a polytetrafluoroethylene emulsion as a dispersion medium, the method mixes the natural flaky graphite powder, the graphite oxide powder and the polytetrafluoroethylene emulsion fully under stirring so as to obtain a paste, which is then applied on a stainless steel sheet and dried for molding in a drying oven, so that a vanadium battery electrode material can be obtained. The method of the invention effectively utilizes the catalytic activity of graphite oxide powder in electrode reaction and prepares a high-activity vanadium battery electrode material, and has the advantages of simple process and low cost. With the high-activity vanadium battery electrode material prepared in the invention, the peak current value of electrode reaction activity can be doubled.
Description
Technical field
The present invention relates to battery manufacture and stored energy field, be specially a kind of high-activity vanadium battery electrode material preparation method.
Background technology
Vanadium redox battery (vanadium cell) is the secondary power system that utilizes the redox reaction between the vanadium ion of different valence state to carry out energy storage and conversion.Be characterized in: without exhaust emission, capacity is adjustable, have extended cycle life, can degree of depth high current density discharge, charging rapidly, energy transformation ratio is high.Vanadium cell is mainly used in the accumulation power supply of peak-load regulation, extensive opto-electronic conversion, wind power generation as accumulation power supply and as outlying district energy-storage system, uninterrupted power supply or emergency power system.
At present, carbon element class material is that vanadium cell is used maximum electrode materials, but the electrode reaction activity of such material is lower, has had a strong impact on the battery performance of vanadium cell.
Summary of the invention
The present invention is directed to above problem, propose a kind of high-activity vanadium battery electrode material preparation method, in solution prior art, carbon element class material electrode reaction activity is lower, has affected the problems such as battery performance of vanadium cell.
Technical scheme of the present invention is:
A kind of high-activity vanadium battery electrode material preparation method, the natural flaky graphite powder of take is base-material, graphite oxide powder is active additive, ptfe emulsion is decentralized medium, under agitation make natural flaky graphite powder, graphite oxide powder and ptfe emulsion fully mix, be prepared into paste, then paste be applied on corrosion resistant plate, drying forming in baking oven.
The weight percentage of each component that the present invention adopts is:
Graphite oxide powder 2～15;
Natural flaky graphite powder 75～88;
Ptfe emulsion 10 (solid weight percentage composition is 5～50);
Each composition weight sum meets 100 above.
In the present invention, natural flaky graphite powder is commercially available, and particle diameter is 10 μ m-500 μ m.
In the present invention, graphite oxide powder adopts the preparation of conventional H ummers method, and the atomic ratio scope of the C/O in graphite oxide that obtains is 5～2, and wherein optimum range is 4～2.5.
In the present invention, the polytetrafluoroethylene solid weight percentage composition in polytetrafluoroethylene (PTFE, Poly tetra fluoro ethylene) emulsion is 5～50, and wherein optimum range is 10～40.
In the present invention, mixing speed is at the uniform velocity, and velocity interval is 100～2000 revs/min, and optimum range is 500～1800 revs/min.Mixing time is 0.5-10 hour, and Best Times is 1～8 hour.
In the present invention, the material of corrosion resistant plate is 316 stainless steels, and the thickness that is coated with cream on corrosion resistant plate is 0.5～10mm, and optimum thickness is 1-8mm.
In the present invention, the bake out temperature in baking oven is 20～100 ℃, and optimum temperature is 30～90 ℃, dries to weight constant.
Preparation method of the present invention is as follows:
1, according to the above ratio graphite oxide powder, natural flaky graphite powder and ptfe emulsion are together joined in container, with dispersion machine, fully at the uniform velocity stir, make paste.
2, paste is evenly applied to 316 corrosion resistant plate both sides, is prepared into electrode.
3, the electrode coating is put in baking oven to drying forming.
Advantage of the present invention:
1, the electrode material that prepared by the present invention, has good electro-chemical activity, especially, for the anodal reaction of vanadium cell, can improve 1.5～2 times of peak currents.
2, electrode material preparation technology of the present invention, technique is simple, can carry out through engineering approaches application, has opened up the new way that vanadium cell is prepared with electrode.
Accompanying drawing explanation
Fig. 1 is the SEM figure of graphite oxide powder used in the present invention (C/O atomic ratio=3).
Fig. 2 is the cyclic voltammogram of the electrode material of embodiment 1～embodiment 4, and wherein peak point current is larger, shows that electrode activity is higher.
Embodiment
Embodiment 1
The weight of each component of the present embodiment is:
Graphite oxide powder 5g (C/O atomic ratio=3);
Natural flaky graphite powder 85g (particle diameter is 50 μ m);
Ptfe emulsion 10g (polytetrafluoroethylene solid weight percentage composition is 30);
By three's total weight, be 100g, at the uniform velocity mixing speed is 800 revs/min, stirs 1h and makes paste.Paste is applied on 316 corrosion resistant plates, and it is 3mm that both sides are coated with cream thickness, in baking oven, dries to weight constantly for 50 ℃, carries out cyclic voltammetry experiment, draws the peak point current of the anodal reaction of vanadium cell.
As shown in Figure 1, graphite oxide powder adopts the preparation of conventional H ummers method, referring to document (W.Hummers, R.Offman, J.Am.Chem.Soc.80 (1958) 1339.), in the present embodiment, the atomic ratio of C/O is that the advantage that 3, Hummers method is prepared graphite oxide powder is to utilize the method for wet-chemical by graphite oxidation, and can obtain higher oxygenation efficiency.
Embodiment 2
The weight of each component of the present embodiment is:
Graphite oxide powder 10g (C/O atomic ratio=2.6);
Natural flaky graphite powder 80g (particle diameter is 100 μ m);
Ptfe emulsion 10g (polytetrafluoroethylene solid weight percentage composition is 40);
By three's total weight, be 100g, at the uniform velocity mixing speed is 1000 revs/min, stirs 2h and makes paste.Paste is applied on 316 corrosion resistant plates, and it is 5mm that both sides are coated with cream thickness, in baking oven, dries to weight constantly for 60 ℃, carries out cyclic voltammetry experiment, draws the peak point current of the anodal reaction of vanadium cell.
Embodiment 3
The weight of each component of the present embodiment is:
Graphite oxide powder 15g (C/O atomic ratio=3.5);
Natural flaky graphite powder 75g (particle diameter is 300 μ m);
Ptfe emulsion 10g (polytetrafluoroethylene solid weight percentage composition is 45);
By three's total weight, be 100g, at the uniform velocity mixing speed is 1200 revs/min, stirs 3h and makes paste.Paste is applied on 316 corrosion resistant plates, and it is 8mm that both sides are coated with cream thickness, in baking oven, dries to weight constantly for 70 ℃, carries out cyclic voltammetry experiment, draws the peak point current of the anodal reaction of vanadium cell.
Embodiment 4
The weight of each component of the present embodiment is:
Graphite oxide powder 8g (C/O atomic ratio=3.1);
Natural flaky graphite powder 82g (particle diameter is 300 μ m);
Ptfe emulsion 10g (polytetrafluoroethylene solid weight percentage composition is 25);
By three's total weight, be 100g, at the uniform velocity mixing speed is 1800 revs/min, stirs 1h and makes paste.Paste is applied on 316 corrosion resistant plates, and it is 2mm that both sides are coated with cream thickness, in baking oven, dries to weight constantly for 80 ℃, carries out cyclic voltammetry experiment, draws the peak point current of the anodal reaction of vanadium cell.
The cyclic voltammogram of embodiment 1～embodiment 4 is listed in accompanying drawing 2, and the anodal reaction of gained peak point current is listed in table 1, can find out 2 times of left and right of all improving, and has good electro-chemical activity.
Table 1: the peak point current of the positive pole reaction of cyclic voltammetry gained
Embodiment result shows, the inventive method is cheap, easy operating, can prepare highly active vanadium cell electrode material.
Claims (5)
1. a high-activity vanadium battery electrode material preparation method, it is characterized in that: the natural flaky graphite powder of take is base-material, graphite oxide powder is active additive, ptfe emulsion is decentralized medium, under agitation make natural flaky graphite powder, graphite oxide powder and ptfe emulsion fully mix, be prepared into paste, then paste is applied on corrosion resistant plate, drying forming in baking oven, prepares vanadium cell electrode material;
The weight percentage of each component is:
Graphite oxide powder 2～15%;
Natural flaky graphite powder 75～88%;
Ptfe emulsion 10%;
Each composition weight percentage composition sum meets 100% above;
Take graphite oxide powder as active additive, and graphite oxide powder adopts the preparation of Hummers method, and the atomic ratio scope of the C/O in graphite oxide is (5～2): 1.
2. high-activity vanadium battery electrode material preparation method according to claim 1, is characterized in that: the polytetrafluoroethylene solid weight percentage composition in ptfe emulsion is 5～50%.
3. high-activity vanadium battery electrode material preparation method according to claim 1, is characterized in that: mixing speed is at the uniform velocity, and velocity interval is 100～2000 revs/min, and mixing time is 0.5-10 hour.
4. high-activity vanadium battery electrode material preparation method according to claim 1, is characterized in that: the material of corrosion resistant plate is 316 stainless steels, and the thickness that is coated with cream on corrosion resistant plate is 0.5～10mm.
5. high-activity vanadium battery electrode material preparation method according to claim 1, is characterized in that: the bake out temperature in baking oven is 20～100 ℃, dries to weight constant.
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| CN102468493B true CN102468493B (en) | 2014-03-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887950A (en) * | 2006-07-28 | 2007-01-03 | 北京科技大学 | Process of preparing graphite-base current collector |
| CN101150192A (en) * | 2007-08-29 | 2008-03-26 | 中国工程物理研究院电子工程研究所 | A making method for liquid battery compound conductive plastic current collector body |
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| JPS6046514B2 (en) * | 1978-12-27 | 1985-10-16 | 古河電池株式会社 | Manufacturing method of battery air electrode |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887950A (en) * | 2006-07-28 | 2007-01-03 | 北京科技大学 | Process of preparing graphite-base current collector |
| CN101150192A (en) * | 2007-08-29 | 2008-03-26 | 中国工程物理研究院电子工程研究所 | A making method for liquid battery compound conductive plastic current collector body |
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| JP昭55-88273A 1980.07.03 |
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