CN102723502B - Surface modification method for raising activity of electrode material of vanadium cell - Google Patents
Surface modification method for raising activity of electrode material of vanadium cell Download PDFInfo
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Abstract
The invention, relating to the field of cell manufacturing and energy storage, discloses a surface modification method for raising the activity of an electrode material of a vanadium cell, comprising the following steps: firstly cleaning the electrode material of the vanadium cell to remove surface impurities, then carrying out modification treatment of the electrode material by using plasma, reacting the gas which generates plasma with the electrode surface under ionization state to generate polar functional groups; and finally carrying out ultrasonic cleaning on the modified electrode material for 5-30 min and drying at 60-120 DEG C. According to the invention, by using the method of the invention to carry out surface modification on the electrode material of the vanadium cell, the hydrophilcity of the electrode surface is enhanced, partial polar functional groups has good catalytic influence on electrode reaction, and the energy storage efficiency of the cell is expected to increase. The method can be used for processing material surfaces with various morphologies and can keep mechanical properties and the like of material matrixes, the experiment condition are easy to control and the method has no pollution to environment. The method is efficient and environmentally friendly.
Description
Technical field
The present invention relates to battery manufacture and stored energy field, be specially a kind of surface modifying method that improves vanadium cell electrode material activity.
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, the electrode material that vanadium cell uses is mainly the graphite felt carbon felt of carbon element class, and this material has advantages of that resistivity is low, good stability, specific area are large.But vanadium cell electrode reaction is relatively low in the activity on its surface, so need to carry out activation processing to it, improve electro-chemical activity and battery performance.
At present the more activating treatment method of report comprises: noble metal decorated, acid activation processing, electrochemistry sun facture etc.Noble metal decorated, step complexity, needs high temperature sintering, is only confined to use in laboratory scope.Thermal activation treatment operating flexibility is little, and oxidation reaction is not easy to control, and over oxidation reduces stability and the useful life of electrode material.The effect of acid activation processing is not fairly obvious.And electrochemical treatments rule is simple and easy to do, successful.But use at present sulfuric acid for electrolyte, can cause fiber surface oxidation reaction more violent, the promotion effect of acid medium to oxidative degradation in addition, fiber surface etching phenomenon is serious, can reduce the useful life of material.
Summary of the invention
The heat treatment existing in prior art of the present invention and acid treatment easily cause the peroxidating of material and make that electrode material stability decreases, battery life reduce etc. weak point and the noble metal decorated problem such as numerous and diverse step and high temperature sintering impact, the object of the present invention is to provide that a kind of method technique is simple, treatment conditions relax, be easy to control the surface modifying method of the raising vanadium electricity electrode material activity of environmentally safe.
Technical scheme of the present invention is;
Improve a surface modifying method for vanadium cell electrode material activity, comprise the following steps and process:
1) preliminary treatment, removes material surface impurity;
2) form polar functional group in electrode material surface: using plasma carries out modification to electrode material, the gas that produces plasma reacts with electrode surface under ionized state, and generating polar functional group, plasma gas operating pressure is 10～200Pa;
The gas that wherein produces plasma is one or more mists in oxygen, nitrogen, fluorine gas, chlorine, ammonia or sulfurous gas;
3) entered step 2) electrode material of modification, adopt ultrasonic cleaning 5-30min, and dry at the temperature of 60～120 ℃.
Step 2) ionic medium body technology is microwave plasma, radio frequency plasma or direct-current plasma.
The processing time that adopts microwave plasma to form polar functional group in electrode material surface is 10～300S, and gas flow is 200mL/min～4L/min, and power is 200～2000W.
Adopting the parameter of radio frequency plasma is that power is 50～300W, and gas flow is 10～200mL/min, and the processing time is 10～300S.
Adopt the parameter at electrode material surface formation polar functional group of direct-current plasma to be, discharging distance is controlled at 3～5cm, and the processing time is 10～300S, and operating voltage is 10-200V.
Described electrode material is selected from graphite felt, charcoal felt, graphite cake or carbon paper.
Described graphite felt thickness is 2mm～6mm, is chosen as any one in polyacrylonitrile-radical graphite felt, viscose-based graphite felt, cellulose base graphite felt or asphaltic base graphite felt.
Carbon felt thickness is 1～20mm, is selected from any one in PAN based carbon felt, viscose glue base carbon felt, cellulose base carbon felt or pitch base carbon felt.
Graphite cake thickness is 1-10mm, analyzes pure graphite cake or spectroscopically pure graphite plate for being selected from.
Carbon paper thickness is 0.5-10mm.
Step 1) preliminary treatment is for passing through the ultrasonic soaking and washing 10～50min of deionized water, and then in 80～120 ℃ of oven dry, drying time is 1～8 hour.
The surface action degree of depth of the electrode material of modification is 5～200nm.
Polar functional group comprises one or more in the functional group of hydroxyl, carboxyl, nitrogenous, fluorine-containing and/or sulfur-bearing.
The gases used high-purity gas that is of the present invention.
The present invention has following advantage and technique effect:
1. the physicochemical properties of the change electrode material surface that the vanadium cell of the present invention's proposition can be pointed with the method for modifying of electrode material, improve the water-wet behavior of material surface by introducing polar functional group etc., the introducing of segment polarity group can also have certain catalytic action to electrode reaction, thereby electrode reaction area is increased, the invertibity of electrode reaction is improved, and improves the energy storage efficiency of battery;
2. the method for plasma processing that the present invention proposes, can process the sample surfaces of various patterns, the wet-chemical treatment technique more with respect to present use, plasma treatment process can save indispensable oven dry, the processes such as liquid waste processing, and also treatment process is simple, parameter is controlled well, can not use strong acid, highly basic etc. have corrosivity and are difficult to the raw material of processing, environmentally safe;
3. the apparatus for processing plasma structure that the present invention will use is comparatively simple, and can process continuously electrode material, and the efficiency of processing is higher, possesses the potentiality of industrial applications;
4. cheap, the easy operating of the inventive method, can realize controllable temperature and modification to vanadium cell electrode material surface, slows down the etching of fiber surface, the useful life of improving electrode material when increasing electrode active.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of vanadium cell electrode material in embodiment 2, and wherein Fig. 1 a is polyacrylonitrile-radical graphite felt before modification, and Fig. 1 b is the polyacrylonitrile-radical graphite felt after modification;
Fig. 2 is the schematic diagram of RF plasma processing electrode material;
Fig. 3 is the comparison diagram of embodiment 3 ammonia radio frequency plasma graphite felt after treatment and untreated graphite felt cyclic voltammetric.
embodiment
1) the PAN based carbon felt material that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 20min, puts into baking oven in 75 ℃ of oven dry 3 hours, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device.The structure of radio frequency plasma surface modification device as shown in Figure 2, wherein in reative cell d, sample stage is installed, sample stage below is circumscribed with the earth terminal of radio freqnency generator a by radio frequency electrode c, the other end of radio freqnency generator a is connected with the electrode of the sample stage top in reative cell d.During to electrode material modification, electrode material is placed on sample stage as sample b.Through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas oxygen, keep reative cell gas system pressure 100Pa, the processing time is 100S, and gas flow is 50mL/min, and instrument power is controlled at 100W.
3) will be through step 2) carbon felt material through ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Be with the difference of embodiment 1:
1) graphite felt of the polyacrylonitrile-radical that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 20min, puts into baking oven in 75 ℃ of oven dry 3 hours, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device.Through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 150Pa, the processing time is from 100S.Gas flow is 100mL/Min.Instrument power is controlled at 200W.
3) will be through step 2) graphite felt ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 3
Be with the difference of embodiment 1:
1) graphite felt of the polyacrylonitrile-radical that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 20min, puts into baking oven in 75 ℃ of oven dry 3 hours, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device, through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas ammonia, keep reative cell gas system pressure 100Pa, the processing time is from 300S.Gas flow is 100ml/min.Instrument power is controlled at 200w.
3) by step 2) in graphite felt material ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 4
1) graphite felt of the polyacrylonitrile-radical that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 20min, puts into baking oven in 75 ℃ of oven dry 3 hours, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device, through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas chlorine, keep reative cell gas system pressure 50Pa, the processing time is from 100S.Gas flow is 50ml/min.Instrument power is controlled at 100w.
3) by step 2) middle graphite felt ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 5
1) the graphite felt material of the polyacrylonitrile-radical that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 20min, puts into baking oven in 75 ℃ of oven dry 3 hours, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device.Through air feed and vacuum system, reative cell is vacuumized, then pass into the mist of reacting gas oxygen and nitrogen, gas ratio is 1: 1, passes into before gas, first gas is fully mixed in mixed gas tank.Keep reative cell gas system pressure 200Pa, the processing time is from 100S.Gas flow is 60ml/min.Instrument power is controlled at 100w.
3) by step 2) in graphite felt material ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 6
1) the carbon paper material of the polyacrylonitrile-radical that is 1mm by thickness is put into deionized water for ultrasonic and is cleaned 30min, puts into baking oven in 100 ℃ of oven dry 1 hour, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into radio frequency plasma surface modification device.Through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 100Pa, the processing time is from 200S.Gas flow is 100ml/min.Instrument power is controlled at 300w.
3) by step 2) in carbon paper material ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 7
1) the carbon paper material of the polyacrylonitrile-radical that is 1mm by thickness is put into deionized water for ultrasonic and is cleaned 30min, puts into baking oven in 100 ℃ of oven dry 1 hour, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into microwave plasma surface modification device, through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 150Pa, the processing time is from 50S.Gas flow is 200mL/min.Instrument power is controlled at 500w.
3) by step 2) in carbon paper material ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 8
1) the spectroscopically pure graphite plate material that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 30min, puts into baking oven in 100 ℃ of oven dry 1 hour, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into microwave plasma. surface modification device.Through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 100Pa, the processing time is from 200S.Gas flow is 400mL/min.Instrument power is controlled at 400w.
3) by step 2) in graphite cake material ultrasonic cleaning 2Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Embodiment 9
1) the spectroscopically pure graphite plate material that is 4mm by thickness is put into deionized water for ultrasonic and is cleaned 30min, puts into baking oven in 100 ℃ of oven dry 1 hour, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into direct-current plasma surface modification device, through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 30Pa, discharging distance is 5cm, operating voltage is 100 volts, and the processing time is from 100S.
3) by step 2) in graphite cake material ultrasonic cleaning 2Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
1) the polyacrylonitrile base carbon paper material that is 1mm by thickness is put into deionized water for ultrasonic and is cleaned 30min, puts into baking oven in 100 ℃ of oven dry 1 hour, is stored in drier for subsequent use.
2) by the step 1 of handling well) in electrode material put into direct-current plasma surface modification device.Through air feed and vacuum system, reative cell is vacuumized, then pass into reacting gas nitrogen, keep reative cell gas system pressure 160Pa, discharging distance is 4cm, and operating voltage is 200 volts, and the processing time is from 300S.
3) by step 2) in carbon paper material ultrasonic cleaning 5Min, take out in 100 ℃, baking oven and dry 3 hours, can be as the electrode material of vanadium cell, assembled battery.
Experimental example 1
Electronic scanner microscope observation will be carried out before and after electrode modification in embodiment 1-10, be the electromicroscopic photograph of vanadium cell electrode material in embodiment 2 as shown in Figure 1, Fig. 1 a is graphite felt material used, Fig. 1 b is the graphite felt material after plasma treatment, can find out that carbon fiber surface is after treatment more coarse, thereby its specific area is increased, for vanadium ion provides more reacting environment, be conducive to improve the electro-chemical activity of electrode.
Other embodiment all have the result same with embodiment 2, illustrate that the inventive method electrode material after treatment can increase its surface area, is conducive to improve the electro-chemical activity of electrode.
Experimental example 2
Cyclic voltammetry test, sweep speed: 5mv/s will be carried out before and after electrode modification in embodiment 1-10.
As shown in Figure 3, for the result of embodiment 3, wherein 1# represents untreated electrode, 2# represents ammonia plasmas electrode after treatment, as can be seen from Figure 3, graphite felt material after plasma modification, oxidation peak current is increased to 30.63 milliamperes from 28.62 milliamperes, and reduction peak current is increased to-27.53 milliamperes from-18.62 milliamperes.Peak electricity potential difference is less to 433 millivolts from 640 millivolts.The reduction peak of the electrode after 2# plasma treatment and the peak value of oxidation peak are substantially equal, and oxidation wave and reduction wave are symmetry status, there is this visible, the electro-chemical activity of treated graphite felt material improves greatly, there is good invertibity, be very beneficial for electrode active material and react in the above, will be expected to improve the energy storage efficiency of battery.
The peak value that the test result of other embodiment has reduction peak and oxidation peak is equally substantially equal, and oxidation wave and reduction wave are the result of symmetry status; The electro-chemical activity of treated graphite felt material improves greatly, has good invertibity, is very beneficial for electrode active material and reacts in the above.
Claims (9)
1. a surface modifying method that improves vanadium cell electrode material activity, is characterized in that: comprise the following steps and process:
1) preliminary treatment, removes material surface impurity;
2) form polar functional group in electrode material surface: using plasma carries out modification to electrode material, the gas that produces plasma reacts with electrode surface under ionized state, and generating polar functional group, plasma gas operating pressure is 10 ~ 200Pa;
The gas that wherein produces plasma is one or more mists in oxygen, nitrogen, fluorine gas, chlorine, ammonia;
3) through step 2) electrode material of modification, adopt ultrasonic cleaning 5-30min, and dry at the temperature of 60 ~ 120 ℃;
Step 2) ionic medium body technology is microwave plasma, radio frequency plasma or direct-current plasma;
The processing time that adopts microwave plasma to form polar functional group in electrode material surface is 10 ~ 300S, and gas flow is 200mL/min ~ 4L/min, and power is 200 ~ 2000W;
Adopting the parameter of radio frequency plasma is that power is 50 ~ 300W, and gas flow is 10 ~ 200mL/min, and the processing time is 10 ~ 300S;
Adopt the parameter at electrode material surface formation polar functional group of direct-current plasma to be, discharging distance is controlled at 3 ~ 5cm, and the processing time is 10 ~ 300S, and operating voltage is 10 ~ 200 volts.
2. the surface modifying method of raising vanadium cell electrode material activity according to claim 1, is characterized in that: described electrode material is selected from graphite felt, charcoal felt, graphite cake or carbon paper.
3. the surface modifying method of raising vanadium cell electrode material activity according to claim 2, it is characterized in that: described graphite felt thickness is 2mm ~ 6mm, be chosen as any one in polyacrylonitrile-radical graphite felt, viscose-based graphite felt, cellulose base graphite felt or asphaltic base graphite felt.
4. the surface modifying method of raising vanadium cell electrode material activity according to claim 2, is characterized in that: carbon felt thickness is 1 ~ 20mm, is selected from any one in PAN based carbon felt, viscose glue base carbon felt, cellulose base carbon felt or pitch base carbon felt.
5. the surface modifying method of raising vanadium cell electrode material activity according to claim 2, is characterized in that: graphite cake thickness is 1-10mm, analyzes pure graphite cake or spectroscopically pure graphite plate for being selected from.
6. the surface modifying method of raising vanadium cell electrode material activity according to claim 2, is characterized in that: carbon paper thickness is 0.5-10mm.
7. the surface modifying method of raising vanadium cell electrode material activity according to claim 1, is characterized in that: step 1) preliminary treatment is the ultrasonic soaking and washing 10 ~ 50min of process deionized water, and then in 80 ~ 120 ℃ of oven dry, drying time is 1 ~ 8 hour.
8. the surface modifying method of raising vanadium cell electrode material activity according to claim 1, is characterized in that: the surface action degree of depth of the electrode material of modification is 5 ~ 200nm.
9. the surface modifying method of raising vanadium cell electrode material activity according to claim 1, is characterized in that: polar functional group comprises a kind of or two or more in hydroxyl, carboxyl, nitrogenous, fluorine-containing functional group.
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