CN101859903B - Carbon electrode material treating agent and method for treating electrode materials by using same - Google Patents
Carbon electrode material treating agent and method for treating electrode materials by using same Download PDFInfo
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- CN101859903B CN101859903B CN2010101978244A CN201010197824A CN101859903B CN 101859903 B CN101859903 B CN 101859903B CN 2010101978244 A CN2010101978244 A CN 2010101978244A CN 201010197824 A CN201010197824 A CN 201010197824A CN 101859903 B CN101859903 B CN 101859903B
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Abstract
The invention provides a carbon electrode material treating agent, which is prepared by the following materials: rare earth compounds, ethylene diamine tetraacetic acid and a proper amount of solvent. The use of the carbon treating fluid to treat electrode materials can improve the electrochemical activity of the electrode materials, improve the reversibility of cathode electricity pairs, reduce hydrogen evolution electric potential of negative electrodes, and can obviously improve charge-discharge performance of a battery using the treated electrode; and meanwhile, the invention also provides a method for treating the electrode materials, which is simple and is easy to be popularized.
Description
Technical field
The present invention relates to the flow battery field, more specifically, relate to carbon electrode material treating agent and handle the method for electrode material with this inorganic agent.
Background technology
The graphite felt of carbon element class or carbon felt are during as electrode material; It has, and resistivity is low, specific area big, good stability in the system of the electrolyte of vanadium redox battery with highly acid and strong oxidizing property; And cheap advantage, but the hydrophily of such electrode and electro-chemical activity are relatively poor.At present kind electrode there is a lot of surface modifying methods, like methods such as metal ion modification, electrochemical oxidation process, acid treatment, heat treatments.
Electrochemical oxidation process, acid treatment, heat treatment all are a kind of oxidizing processs to the graphite felt electrode surface; Can improve electrode surface C-OH, CO ,-quantity of oxygen-containing functional groups such as COOH; Improve the wetting capacity of electrode surface to cell active materials; Improve the adsorption capacity of electrode surface, strengthen electrochemical reaction active material.But all there are some shortcomings in these methods: acid treatment improves DeGrain to electro-chemical activity; Heat treatment operation elasticity is little, and oxidation reaction is wayward, and can increase the weight of the evolving hydrogen reaction of negative pole; Electrochemical oxidation process uses sulfuric acid to be electrolyte at present, can cause the fiber surface oxidation reaction more violent, and acid medium is to the promotion effect of oxidative degradation in addition, and the carbon fiber surface corrosion phenomenon is serious, reduces mechanical strength of electrodes, and can produce acid mist.And for the metal ion method of modifying, the complicated steps that a lot of metal ions are modified, and can improve hydrogen-evolution overpotential, like Mn
2+, Co
2+, the Ir modified electrode also makes the negative pole evolving hydrogen reaction serious when improving chemical property, adopts Pd
2+, Au
4+, Pt
4+The graphite felt surface is modified, and electrode reaction is unstable, has hydrogen to separate out, and iridium, palladium and platinum all is noble metal, costs an arm and a leg, and is unfavorable for the large-scale commercial applications application.
The electro-chemical activity of carbon element class electrode (graphite felt/carbon felt etc.) is not high, and existing surface modifying method can improve the electro-chemical activity of electrode, but has improved the negative pole hydrogen-evolution overpotential simultaneously yet, and the liberation of hydrogen side reaction is increased.How improve carbon element class electrode electro Chemical active in, but do not improve the hydrogen-evolution overpotential of negative pole, become scientific research personnel's problem demanding prompt solution in the field of batteries.
Summary of the invention
The object of the present invention is to provide a kind of carbon element class electrode material treatment fluid; To overcome the deficiency of prior art; Use this treatment fluid to handle electrode material, can improve the electro-chemical activity of electrode material, improve the right invertibity of negative electricity; Reduce the hydrogen-evolution overpotential of negative electrode, can also significantly improve the charge-discharge performance of the battery that uses this processing rear electrode simultaneously.
For this reason; Carbon electrode material treating agent provided by the invention comprises following raw material: rare earth compound, ethylenediamine tetra-acetic acid; And proper amount of solvent, wherein rare earth compound accounts for the 1-5% of inorganic agent total weight, and ethylenediamine tetra-acetic acid accounts for the 0.5-3% of inorganic agent total weight.
In specific embodiment provided by the invention, said rare earth compound can be lanthanum chloride, lanthana, yttrium nitrate or cerium oxide, and the solvent of employing is selected from that (hereinafter is with H by ethanol, sulfuric acid, deionized water
2O representes) and the group formed of nitric acid in one or more.
Inorganic agent provided by the invention can further include the ammonium chloride of 0-3% and/or the urea of 0-3%.
In the specific embodiment provided by the invention, this inorganic agent is by cerium oxide (CeO
2) 2.682%, H
2O 53.648%, and ethanol 42.328% and ethylenediamine tetra-acetic acid 1.342% are formed; Perhaps this inorganic agent is by lanthana 2.817%, H
2O 89.206%, and ethylenediamine tetra-acetic acid 0.939% and ethanol 7.038% are formed; Perhaps said inorganic agent is by yttrium nitrate (Y (NO
3)
36H
2O) 1%, H
2O 95%, ethylenediamine tetra-acetic acid 1%, and the concentrated sulfuric acid 1% and urea 2% are formed; Perhaps by lanthanum chloride 3%, ethanol 90%, ammonium chloride 3%, red fuming nitric acid (RFNA) 0.5%, urea 3% and ethylenediamine tetra-acetic acid 0.5% are formed this inorganic agent.
The present invention also provides a kind of processing method of carbon element class electrode material; This method adopts inorganic agent provided by the invention to soak said carbon element class electrode material at normal temperatures; Usually can soak 3-10 hour, the electrode material after will soaking then is 60-100 ℃ of oven dry, and washed with de-ionized water is used in the oven dry back; Dry again oven dry, the electrode material after can obtaining handling.
The present invention also provides a kind of battery, and it adopts the vanadium ion sulfuric acid solution as electrolyte, makes electrode by the electrode material of handling through inorganic agent provided by the invention, and this electrode material both can be used as the positive pole of battery, also can be used as the negative pole of battery.
The electrode of battery provided by the invention has passed through the processing of electrode material processing method provided by the invention.
Use carbon element class electrode material treatment fluid provided by the invention to handle carbon element class electrode material, can improve the electro-chemical activity of carbon element class electrode material, improve the right invertibity of negative electricity, reduce the hydrogen-evolution overpotential of negative electrode.Can significantly improve simultaneously the charge-discharge performance of battery.Simultaneously, carbon element class electrode material processing method provided by the invention, simple, do not need the support of main equipment, easy to utilize.
Description of drawings
Fig. 1 is the cyclic voltammogram of graphite felt electrode in vanadium redox battery negative pole electrolyte before and after handling.
Fig. 2 is the cyclic voltammogram of the graphite felt before and after handling in the anodal electrolyte of vanadium cell.
Fig. 3 is that battery 1,2,3 is at 50mA/cm
2Charging and discharging curve figure under the current density.
Fig. 4 is that battery 1,4,5 is at 50mA/cm
2Charging and discharging curve figure under the current density.
Fig. 5 is that battery 6 is at 50mA/cm
2The charging and discharging curve figure of the 1st, 10,20 and 30 circulation under the current density.
Embodiment
To do further detailed explanation to goal of the invention of the present invention, technical scheme and beneficial effect below.
Be noted that following detailed description all is an exemplary, being intended to provides further explanation to desired the present invention.Unless otherwise, all technology used of this paper and scientific terminology have with the present invention under the identical meanings of those of ordinary skill common sense of technical field.
Inventor of the present invention be intended to study a kind of can be when improving carbon element class electrode material electro-chemical activity; Improve the right invertibity of negative electricity; And the electrode inorganic agent of the hydrogen-evolution overpotential of reduction negative electrode, this inorganic agent is by raw material rare earth compound, ethylenediamine tetra-acetic acid, and solvent composition; The electrode material of handling through this inorganic agent has the electro-chemical activity height, and negative electricity is to plurality of advantages such as invertibity are strong.
In a kind of embodiment of the present invention, above-mentioned raw materials is by rare earth compound, ethylenediamine tetra-acetic acid, and an amount of solvent composition.The content of wherein said rare earth compound is 1-5%, and said ethylenediamine tetra-acetic acid content is 0.5-3%.
In specific embodiment provided by the invention, said rare earth compound can be lanthanum chloride, lanthana, yttrium nitrate or cerium oxide.Though the specific embodiment of the invention adopts above-mentioned rare earth compound, those skilled in the art should know, the rare earth compound that every skin contains the d electronic structure can be applied among the present invention.
The solvent that adopts can be selected from ethanol, the concentrated sulfuric acid, deionized water or red fuming nitric acid (RFNA), perhaps the arbitrary mixture in them.
Inorganic agent provided by the invention can further include the ammonium chloride of 0-3% and/or the urea of 0-3%.The inventor finds, add these ammonium chlorides or urea after, inorganic agent has enhancing to a certain degree to the treatment effect of electrode material.
In the specific embodiment provided by the invention, this inorganic agent is by cerium oxide (CeO
2) 2.682%, H
2O 53.648%, and ethanol 42.328% and ethylenediamine tetra-acetic acid 1.342% are formed; Perhaps by lanthana 2.817%, H
2O 89.206%, and ethylenediamine tetra-acetic acid 0.939% and ethanol 7.038% are formed; Perhaps by yttrium nitrate (Y (NO
3)
36H
2O) 1%, H
2O95%, ethylenediamine tetra-acetic acid 1%, the concentrated sulfuric acid 1% and urea 2% are formed; Perhaps by lanthanum chloride 3%, ethanol 90%, ammonium chloride 3%, red fuming nitric acid (RFNA) 0.5%, urea 3% and ethylenediamine tetra-acetic acid 0.5% are formed.
In embodiment of the present invention; The method that electrode material is handled is to adopt the prepared inorganic agent of the present invention to soak electrode material 3-10h at normal temperatures; Electrode material after soaking is dried 3-10h at 60-100 ℃; Washed with de-ionized water is used in the oven dry back, selects suitable temperature to carry out the drying oven dry down or according to the concrete condition of electrode material at 120 ℃ again.
In a kind of embodiment of the present invention, a kind of battery is provided, by the vanadium ion sulfuric acid solution as electrolyte, by adopting electrode material after above-mentioned inorganic agent is handled as electrode.
One, to the processing of carbon element class electrode material
Embodiment 1:
The carbon electrode material treating agent raw material: lanthanum chloride 3%, ethanol 90%, ammonium chloride 3%, red fuming nitric acid (RFNA) 0.5%, urea 3%, EDTA 0.5%.
Carbon element class electrode material processing method: with the above-mentioned raw materials mixing and stirring, prepared inorganic agent soaked electrode material 3 hours at normal temperatures, and then electrode material is used washed with de-ionized water after 80 ℃ of oven dry, and is dry down at 120 ℃ at last.
The raw material of carbon electrode material treating agent: lanthana 2.817%, H
2O 89.206%, and EDTA 0.939%, ethanol 7.038%.
The electrode material processing method: with the above-mentioned raw materials mixing and stirring, soaked electrode material at normal temperatures 5 hours, then electrode material is used washed with de-ionized water after 60 ℃ of oven dry, and is dry down at 120 ℃ at last.
Carbon electrode material treating agent raw material: yttrium nitrate (Y (NO
3)
36H
2O) 1%, H
2O 95%, and EDTA 1%, the concentrated sulfuric acid 1%, urea 2%.
The processing method of electrode material: with the above-mentioned raw materials mixing and stirring, soaked electrode material at normal temperatures 10 hours, then electrode material is used washed with de-ionized water after 100 ℃ of oven dry, and is dry down at 120 ℃ at last.
Embodiment 4
The raw material of carbon electrode material treating agent: cerium oxide 2.682%, H
2O 53.648%, ethanol 42.328%, and EDTA 1.342%.
The processing method of electrode material: as above raw materials mix stirs, and soaks electrode material 5h at normal temperatures, and then electrode material is used washed with de-ionized water after 100 ℃ of oven dry, and is dry down at 120 ℃ at last.
Two, embodiment 1-4 gained electrode material is tested
1. cyclic voltammetric test:
Electrode is selected for use: adopt three-electrode system; (1) embodiment of the invention 1 makes the graphite felt of inorganic agent before and after handling (available from Liaoyang Jin Gu High Seience Technology Co., Ltd.; Graphite felt thickness is 5mm) be work electrode; (2) platinum electrode is to electrode, and (3) saturated calomel electrode electrode (saturated KCl solution) is a reference electrode, forms three-electrode system through Luggin capillary.
Electrolyte is selected for use: it is 0.9mol/L V that negative pole electrolyte adopts total V density
2+And V
3+Mixed electrolytic solution (V
2+And V
3+Mol ratio is 1: 1)+3.0mol/L H
2SO
4, anodal electrolyte adopts 1.6mol/L V (IV)+3.0mol/L H
2SO
4
On CS350 type electrochemical workstation, carry out electro-chemical test, sweep speed is 5mv/s.
As shown in Figure 1, former felt (undressed graphite felt) V occurs at-0.423V
2+/ V
3+The oxidation peak that electricity is right, corresponding reduction peak is not obvious, and this is because the higher V that flooded of hydrogen-evolution overpotential
2+/ V
3+The reduction peak that electricity is right; And greatly reduced hydrogen-evolution overpotential through the graphite felt after the inorganic agent processing provided by the invention, reduced evolving hydrogen reaction, V
2+/ V
3+The right redox peak-to-peak current potential of electricity is respectively-0.423V and-0.564V, and the spike potential difference is 0.141V, V
2+/ V
3+Electricity is better to the redox peak symmetry on the graphite felt electrode after the processing, and V is described
2+/ V
3+Electricity is better to the invertibity on the graphite felt electrode after the processing.
The redox peak that in Fig. 2, occurs is corresponding to V (IV)/right redox reaction of V (V) electricity, and the V of former felt (IV)/V (V) redox peak-to-peak current potential is respectively 1.709V and 0.455V, and the spike potential difference is 1.254V; Graphite felt V after the processing (IV)/V (V) redox peak-to-peak current potential is respectively 1.598V and 0.571V; The spike potential difference is 1.027V; Graphite felt after the processing is than the little 227mV of spike potential of former felt, and peak current improves, and the electro-chemical activity of the graphite felt electrode after the processing improves.
Like Fig. 1 and shown in Figure 2, through the graphite felt that carbon electrode material treating agent of the present invention is handled, its negative electricity is to V
2+/ V
3+Invertibity, and electro-chemical activity all is significantly improved.
2. dynamic battery test:
The battery that the electrode material of embodiment 2 and the processing of embodiment 3 gained inorganic agents is formed carries out the dynamic battery test.
In Fig. 3, battery 1 is for to make the battery that both positive and negative polarity assembles respectively with undressed Liaoyang Jin Gu graphite felt (thickness is 5mm);
The battery that battery 3 assembles as both positive and negative polarity respectively for the graphite felt of handling through the embodiment of the invention 2 prepared carbon electrode material treating agent;
In Fig. 4, battery 4 is for the graphite felt of handling through the embodiment of the invention 3 prepared carbon electrode material treating agent is done negative pole, former felt is made the anodal battery that assembles;
Battery 5 assembles battery as both positive and negative polarity respectively for the graphite felt of handling through the embodiment of the invention 3 prepared carbon electrode material treating agent.
The battery effective area is 7 * 8cm
2, positive pole and negative pole are respectively with 70mL 1.6mol/LV (III)/V (IV)+3.0mol/L H
2SO
4Electrolyte, barrier film are nafion 115 films, at 50mA/cm
2Test under the current density.
Fig. 3 shows and adopts embodiment 2 gained inorganic agents to handle the front and back graphite felt at 50mA/cm
2Charging and discharging curve figure under the current density.Wherein, curve 1 is the charging and discharging curve of battery 1, and curve 2 is the charging and discharging curve of battery 2, and curve 3 is the charging and discharging curve of battery 3.
Fig. 4 shows and adopts embodiment 3 to handle the front and back graphite felt at 50mA/cm
2Charging and discharging curve figure under the current density.Wherein, curve 1 is the charging and discharging curve of battery 1, and curve 2 is the charging and discharging curve of battery 4, and curve 3 is the charging and discharging curve of battery 5.
From Fig. 3 and Fig. 4, can obviously find out; Under the identical situation of current density; One termination electrode obviously is longer than all undressed battery 1 of two end electrodes through the time that discharges and recharges of the battery 2,4 that carbon electrode material treating agent of the present invention is handled, the time that discharges and recharges of the battery 3,5 that two end electrodes is all handled through carbon electrode material treating agent of the present invention obviously be longer than battery have only a termination electrode through carbon electrode material treating agent of the present invention handle 2,4.
Therefore, in battery, use the electrode after carbon electrode material treating agent of the present invention is handled, can significantly improve the charge-discharge performance of battery.
The inventor has further carried out dynamic electrode test to the battery 6 that the electrode material inorganic agent that makes through embodiment 4 was handled, and test result is as shown in Figure 5.
To pass through the prepared carbon electrode material treating agent of the embodiment of the invention 4 handles back Liaoyang Jin Gu graphite felt (thickness is 5mm) and does both positive and negative polarity respectively and be assembled into battery 6.
The battery effective area is 7 * 8cm
2, positive pole and negative pole are respectively with 70mL 1.4mol/LV (III)/V (IV)+3.0mol/L H
2SO
4Electrolyte, barrier film are nafion 115 films, at 50mA/cm
2Carry out 30 cycle charge-discharges under the current density.
Fig. 5 shows battery 6 at 50mA/cm
2The charging and discharging curve figure of the 1st, 10,20,30 circulation under the current density.1 is the 1st charging and discharging curve figure among the figure; 2 is the 10th charging and discharging curve figure among the figure; 3 is the 20th charging and discharging curve figure among the figure; 4 is the 30th charging and discharging curve figure.
Can know battery 6 the 1-30 time cycle charge-discharge from Fig. 5, the voltage platform of battery, charge/discharge capacity do not have variation basically, explain that the electrode that the present invention handles has cyclical stability preferably.
In sum, use the treatment fluid of carbon element class electrode material of the present invention to handle electrode material, can improve the electro-chemical activity of carbon element class electrode material, improve the right invertibity of negative electricity, reduce the hydrogen-evolution overpotential of negative electrode.Can significantly improve simultaneously the charge-discharge performance of the battery that uses this processing rear electrode.Simultaneously, the processing method of carbon element class electrode material of the present invention, this method is simple, is easy to promote.
The foregoing description only is being example by the vanadium ion sulfuric acid solution as the battery of electrolyte.But it will be understood by those skilled in the art that through the electrode material that inorganic agent provided by the invention was handled and to be applied in sodium polysulfide flow battery or the full chrome liquor galvanic battery.
More than explanation is merely preferred implementation of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a battery is characterized in that, said battery adopts the vanadium ion sulfuric acid solution as electrolyte, adopts the graphite felt of handling through inorganic agent as electrode; Said inorganic agent comprises following raw material: rare earth compound, and ethylenediamine tetra-acetic acid and solvent, the weight percentage of wherein said rare earth compound are 1-5%, the weight percentage of said ethylenediamine tetra-acetic acid is 0.5-3%; Said rare earth compound is lanthanum chloride, lanthana, yttrium nitrate or cerium oxide, and said solvent is selected from one or more in the group of being made up of ethanol, nitric acid, sulfuric acid and deionized water; The said method of handling through inorganic agent is: soaked at normal temperatures graphite felt 3-10 hour with said inorganic agent; Graphite felt after soaking was dried 3-10 hour at 60-100 ℃; Washed with de-ionized water, drying are used in the oven dry back.
2. battery according to claim 1 is characterized in that said inorganic agent further comprises ammonium chloride and/or urea, and the quality percentage composition of said ammonium chloride and/or urea all≤3%.
3. battery according to claim 1; It is characterized in that; Said inorganic agent is 2.682% cerium oxide by weight percentage; Weight percentage is 53.648% deionized water, and weight percentage is that 42.328% ethanol and weight percentage are that 1.342% ethylenediamine tetra-acetic acid is formed.
4. battery according to claim 1; It is characterized in that; Said inorganic agent is 2.817% lanthana by weight percentage; Weight percentage is 89.206% deionized water, and weight percentage is that 0.939% ethylenediamine tetra-acetic acid and weight percentage are that 7.038% ethanol is formed.
5. battery according to claim 2 is characterized in that, said inorganic agent is 1% yttrium nitrate Y (NO by weight percentage
3)
36H
2O, weight percentage are 95% deionized water, and weight percentage is 1% ethylenediamine tetra-acetic acid, and weight percentage is that 1% sulfuric acid and weight percentage are that 2% urea is formed.
6. battery according to claim 2; It is characterized in that; Said inorganic agent is 3% lanthanum chloride by weight percentage, and weight percentage is 90% ethanol, and weight percentage is 3% ammonium chloride; Weight percentage is 0.5% nitric acid, and weight percentage is that 3% urea and weight percentage are that 0.5% ethylenediamine tetra-acetic acid is formed.
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| CN103000897B (en) * | 2012-12-12 | 2015-06-03 | 大力电工襄阳股份有限公司 | Method and device for removing fragments in electrode material |
| CN108461758B (en) * | 2018-04-24 | 2020-12-29 | 中南大学 | Cathode electrode for all-vanadium redox flow battery, preparation method of cathode electrode and all-vanadium redox flow battery |
| CN109411772A (en) * | 2018-10-17 | 2019-03-01 | 无锡威孚高科技集团股份有限公司 | A kind of processing method for catalyst of fuel batter with proton exchange film |
| CN112768705A (en) * | 2021-01-19 | 2021-05-07 | 江苏大学 | Sectional type electrode for liquid-liquid type eutectic solvent electrolyte flow battery |
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| CN1597774A (en) * | 2004-08-12 | 2005-03-23 | 上海交通大学 | Preparation process for composite of rare earth modified carbon-fibre / epoxy resin |
| CN101651201A (en) * | 2009-08-19 | 2010-02-17 | 湖南维邦新能源有限公司 | Electrode materials and all-vanadium redox flow battery containing electrode materials |
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| CN1597774A (en) * | 2004-08-12 | 2005-03-23 | 上海交通大学 | Preparation process for composite of rare earth modified carbon-fibre / epoxy resin |
| CN101651201A (en) * | 2009-08-19 | 2010-02-17 | 湖南维邦新能源有限公司 | Electrode materials and all-vanadium redox flow battery containing electrode materials |
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