CN105322194A - Multifunctional negative material and application thereof in all-vanadium redox flow battery - Google Patents
Multifunctional negative material and application thereof in all-vanadium redox flow battery Download PDFInfo
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- CN105322194A CN105322194A CN201410371296.8A CN201410371296A CN105322194A CN 105322194 A CN105322194 A CN 105322194A CN 201410371296 A CN201410371296 A CN 201410371296A CN 105322194 A CN105322194 A CN 105322194A
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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
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- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a multifunctional negative material. A carbon material is taken as a matrix; the surface of the material is modified by an electrocatalyst containing Pb; the electrocatalyst containing the Pb is one/two or more of a Pb simple substance, PbO<2> or lead sulfate; and the deposit rate of the electrocatalyst containing the Pb on the matrix is 0.05wt% to 80wt% of that of the multifunctional negative material. The electrode is applicable to a negative electrode of an all-vanadium redox flow battery; the electrocatalytic activity and the electrochemical reversibility of the electrode material on a V<2+>/V<3+> redox reaction can be improved; the charge transfer resistance is reduced; the multifunctional negative material has high hydrogen evolution over-potential; a hydrogen evolution reaction can be inhibited; the service lifetime of the battery is prolonged; and the charge and discharge capacity of the battery can also be improved. According to the multifunctional negative material, the voltage efficiency and the energy efficiency of the all-vanadium redox flow battery are improved, so that the working current density of the all-vanadium redox flow battery is improved; and the weight, the size and the cost of the battery with the same output power are greatly reduced.
Description
Technical field
The present invention relates to the liquid flow energy storage battery field in chemical energy storage technology, particularly the electrode of all-vanadium flow battery.
Background technology
All-vanadium flow battery has power output because of it and capacity is separate, and system is flexible; Energy efficiency is high, and the life-span is long, operation stability and reliability high, self discharge is low; The addressing degree of freedom is large, pollution-free, safeguard simple, operation cost is low, fail safe advantages of higher, in scale energy storage, there is vast potential for future development, be considered to the effective ways solving the renewable energy system randomness such as solar energy, wind energy and intermittent unstable state feature, in renewable energy power generation and intelligent grid construction, have great demand.
At present, restricting the business-like main restriction of all-vanadium flow battery is exactly Cost Problems.Reduce its cost, main solution has two: one to be the cost reducing each critical material, as the cost of amberplex, electrolyte, pole dual-pole board; One for improving the working current density of battery operation.Because the raising of working current density can improve the power density of battery, namely larger power stage can be realized with same pile, but also floor space and the space of energy-storage system can be reduced, improve the mobility of its adaptive capacity to environment and system, the application of expansion liquid flow energy storage battery.But the raising of working current density can cause the reduction of voltage efficiency and energy efficiency.In order to improve the working current density of battery under the prerequisite not reducing energy efficiency, just needing to reduce battery polarization as much as possible, i.e. ohmic polarization, electrochemical polarization and concentration polarization, reducing voltage loss.
Electrode is as one of the critical component of liquid flow energy storage battery, and the impact of its performance on liquid flow energy storage battery is very big.The electro catalytic activity of electrode directly determines the intrinsic reaction rate of electrochemical reaction, affects working current density and the energy efficiency of battery largely.
In tradition flow battery, both positive and negative polarity uses identical carbon materials, and uses identical method of modifying to go to process electrode material.And in fact, because the redox reaction on both positive and negative polarity is different, the electro catalytic activity that material with carbon element aligns cathode oxidation reduction electricity right is also different, therefore positive and negative pole material should be treated with a certain discrimination.Research shows the positive pole polarization of all-vanadium flow battery and not quite, its electrochemical polarization is primarily of negative pole polarization composition, and the modification therefore for positive pole has little significance, and research emphasis should be placed in negative pole modification.
In addition, all-vanadium flow battery operationally, when working especially at higher current densities, negative pole is easy to occur evolving hydrogen reaction, the hydrogen atom being adsorbed on electrode surface can infiltrate electrode and spread in electrode, causes the infringement such as hydrogen blister, hydrogen embrittlement, has a strong impact on the working life of battery.Therefore, the generation of evolving hydrogen reaction will be avoided as far as possible.
For reducing liquid flow energy storage battery electrochemical polarization and suppressing the method for evolving hydrogen reaction to mainly contain in current published patent documentation:
(1) to electrode material as graphite felt, carbon paper etc. carry out oxidation modification process, oxygen-containing functional group is modified at carbon fiber surface, improve the electro catalytic activity of electrode, reduce the electrochemical polarization of battery, graphite felt is carried out to the method for electrochemical oxidation disclosed in patent CN101465417A and CN101182678A.
(2) to electrode material as graphite felt, carbon paper etc. carry out metalized, i.e. modified metal ion on carbon fiber surface, as (Sun, B.T. such as Sun; Skyllas-Kazacos, M.ChemicalModificationandElectrochemicalBehaviorofGraphi teFiberinAcidicVanadiumSolution.Electrochim.Acta1991,36,513-517.) on carbon fiber surface, modified Mn
2+, Te
4+, In
3+and Ir
3+deng, find Ir
3+there is most effect to the raising of the electro catalytic activity of electrode material, but cause the high expensive of electrode, so and be not suitable for large-scale application due to the use of noble metal.
(3) some redox reaction current potentials are added in the electrolytic solution lower than V
2+/ V
3+other elements of reaction potential, as Cr
3+, Zn
2+deng (patent WO2011136256A1), the method limits the local overcharge of negative pole to suppress the generation of side reaction by the simple chargeable capacity improving negative pole.But owing to occurring even without overcharge, evolving hydrogen reaction also can along with V
2+/ V
3+reaction is carried out simultaneously, and therefore the method can't reduce liberation of hydrogen.
Summary of the invention
The present invention aims to provide a kind of multi-functional negative material and the application in all-vanadium flow battery thereof.
For achieving the above object, the technical solution used in the present invention is:
A kind of multi-functional negative material, described multi-functional negative material is using carbon materials as matrix, has containing Pb eelctro-catalyst in its finishing, is Pb simple substance, PbO containing Pb eelctro-catalyst
2or one or two or more kinds in lead sulfate;
Described is 0.05 ~ 80wt% of multi-functional negative material containing the deposition of Pb eelctro-catalyst on matrix.
Described is 0.05 ~ 20wt% of multi-functional negative material containing the deposition of Pb eelctro-catalyst on matrix, is more preferably 0.1 ~ 10wt%.
The described particle size containing Pb eelctro-catalyst is 1nm ~ 5 μm, preferably, is 2 ~ 500nm.
Described carbon materials is a kind of in carbon felt, graphite felt, carbon paper or carbon cloth or the complex of more than two kinds in them.
The mode of described modification can be one in physical absorption, chemical deposition or two kinds.
Described multi-functional negative material can be used as all-vanadium flow battery negative pole in all-vanadium flow battery.
Described multi-functional negative material is prepared by infusion process:
By carbon basal body material soaking in the inorganic or organic solution being dissolved with finite concentration brown lead oxide, Pb slaine, stir or take out after ultrasonic disperse, put into drying box dry.Dried carbon basal body material directly can be used as the negative pole of all-vanadium flow battery, also can be warming up to 400 ~ 800 DEG C under an inert atmosphere, logical H
2isothermal reaction 0.1-3h, by Pb
2+or Pb
4+be reduced into Pb, then be cooled to room temperature under an inert atmosphere and make all-vanadium flow battery negative pole electrode material.
Described Pb slaine is lead sulfate, plumbi nitras or lead acetate, is preferably plumbi nitras or lead acetate;
Described inorganic solution is water, nitric acid or sulfuric acid solution;
Described organic solution is glycerol or acetum;
Described inert gas is a kind of in nitrogen, argon gas or helium or their mist.
Alternatively, described high electrocatalytic active electrode is prepared by electrochemical deposition method:
Pb in electric depositing solution
2+or Pb
4+concentration is 0.001-0.2M, and carbon basal body material, as work electrode, is Pb plate, graphite cake or platinum electrode to electrode, and adopt direct current chemical deposition, current density is 2 ~ 200mA/cm
2, preferably, be 10 ~ 80mA/cm
2; Sedimentation time is 2s ~ 30min, preferably, is 5s ~ 1min.
Described multi-functional negative material can be used as all-vanadium flow battery negative pole in all-vanadium flow battery.
Tool of the present invention has the following advantages:
(1) adopt multi-functional negative material of the present invention, because carbon material surface has supported Pb eelctro-catalyst, improve overpotential of hydrogen evolution, can liberation of hydrogen be suppressed, reduce side reaction, extend battery service life.
(2) adopt multi-functional negative material of the present invention, because carbon material surface has supported nanometer Pb eelctro-catalyst, improve electrode material V
2+/ V
3+the electro catalytic activity of redox reaction and electrochemical reversibility, reduce charge-transfer resistance, improves voltage efficiency and the energy efficiency of all-vanadium flow battery.
(3) adopt multi-functional negative material of the present invention, in charge and discharge process, except there is V in negative pole
2+/ V
3+outside redox reaction, also Pb/PbSO can be there is
4redox reaction, the charge/discharge capacity of battery can be improved.
(4) electrode preparation method of the present invention is simple, and the material used is the Pb slaine that carbon materials cheap and easy to get and price are very not expensive, has commercialization application value.
Accompanying drawing explanation
Fig. 1 is the cyclic voltammetry curve figure of carbon felt in Pb modified carbon felt and comparative example 1 in the embodiment of the present invention 1, sweep speed: 10mV/s;
Fig. 2 is the voltage efficiency of all-vanadium flow monocell when different current density adopting electrode in negative pole and comparative example 1 in the embodiment of the present invention 1;
Fig. 3 is the energy efficiency of all-vanadium flow monocell when different current density adopting electrode in negative pole and comparative example 1 in the embodiment of the present invention 1.
Embodiment
Below by specific embodiment in detail the present invention is described in detail.
Embodiment 1
The graphite felt of certain size is immersed in 0.02MPb (NO
3)
2hNO
3in solution, take out after ultrasonic disperse 30min, put into drying box 105 DEG C of dry 10h, then will be supported with Pb (NO
3)
3graphite felt in nitrogen atmosphere, be warming up to 600 DEG C, pass into H
2isothermal reaction 1h, by Pb
2+be reduced into Pb, then be cooled to room temperature in a nitrogen atmosphere, use scales/electronic balance weighing to determine that the loading mass ratio of Pb is 2%.
For the electro-chemical activity of test vanadium ion oxidation-reduction pair on Pb modification graphite felt surface, cyclic voltammetry is carried out to Pb modification graphite felt prepared by embodiment 1.Modify graphite felt as work electrode using Pb, atresia graphite cake is as to electrode, and saturated calomel electrode is as reference electrode, and the electro-chemical test instrument of employing is the CHI612 type electrochemical workstation of Shanghai Chen Hua company.Compound concentration is 0.05MV
2++ 0.05MV
3++ 3MH
2sO
4electrolyte, to V
2+/ V
3+electricity is studied the electro-chemical activity modifying graphite felt surface at Pb, and sweep limits is respectively-1.0V ~ 0V, and sweep speed is 10mV/s.In the present embodiment, Pb modifies the cyclic voltammetry curve of graphite felt as shown in Figure 1, compares Pb and to modify in graphite felt and comparative example V in unmodified graphite felt
2+/ V
3+electrochemical oxidation, reduction peak position and peak current size known, Pb modify graphite felt there is compared with graphite felt unmodified in comparative example the electro catalytic activity and electrochemical reversibility that significantly improve.
The Pb of preparation from embodiment 1 modify graphite felt cut be of a size of 8cm × 6cm × 0.5cm graphite felt as negative pole, use the graphite felt of unmodified Pb to be assembled into monocell as positive pole, carry out charge-discharge performance test.Anode electrolyte is 1.5MVO
2+3MH
2sO
4solution 60ml, electrolyte liquid is 1.5MV
3+3MH
2sO
4solution 60ml.It is at 80-160mA/cm
2time voltage efficiency and energy efficiency as shown in Figures 2 and 3, therefrom can find out, compared with graphite felt unmodified in comparative example 1, in the present embodiment, Pb modifies the voltage efficiency of graphite felt monocell at 80mA/cm
2current density under brought up to 89.4% from 77.4%, energy efficiency can reach 84%; At 120mA/cm
2high current density under voltage efficiency brought up to 84.6% from 71.6%, energy efficiency also can reach 80%.In addition, compared with comparative example, the charge/discharge capacity of the present embodiment improves 3%.
Comparative example 1
Adopt graphite felt that German SGL company produces as comparative example, this graphite felt, without any process, cuts the graphite felt being of a size of 8cm × 6cm × 0.5cm and is assembled into monocell as both positive and negative polarity, carry out charge-discharge performance test.Anode electrolyte is 1.5MVO
2+3MH
2sO
4solution 60ml, electrolyte liquid is 1.5MV
3+3MH
2sO
4solution 60ml.Its voltage efficiency under different current density and energy efficiency are as shown in Figures 2 and 3.
Embodiment 2
The carbon felt of certain size is immersed in the aqueous solution of 0.05M lead acetate, takes out after ultrasonic disperse 30min, put into drying box 100 DEG C of dry 10h, then the carbon felt being supported with lead acetate is warming up to 600 DEG C in nitrogen atmosphere, passes into H
2isothermal reaction 2h, by Pb
2+be reduced into Pb, then be cooled to room temperature in a nitrogen atmosphere, use scales/electronic balance weighing to determine that the loading mass ratio of Pb is 5%.This negative material not only has high electrocatalytic active, can reduce the electrochemical polarization of liquid flow energy storage battery, improves the working current density of battery, also improves the charge/discharge capacity of battery.
Monocell assembling evaluation and test condition is with embodiment 1, and difference from Example 1 is: adopt the present embodiment Pb modified carbon felt as the all-vanadium flow battery of negative pole, current density is 80mA/cm
2time, voltage efficiency and energy efficiency are respectively 89.3% and 84.5%; Current density brings up to 120mA/cm
2time, voltage efficiency and energy efficiency still remain on 84.7% and 80.8%.Charge/discharge capacity improves 10% with unmodified carbon felt ratio.
Embodiment 3
The carbon paper of certain size is immersed in 0.1MPb (NO
3)
2hNO
3in solution, take out after ultrasonic disperse 30min, put into drying box 105 DEG C of dry 10h, then will be supported with Pb (NO
3)
2carbon paper in nitrogen atmosphere, be warming up to 600 DEG C, pass into H
2isothermal reaction 1h, makes Pb (NO
3)
2decomposition-reduction becomes Pb, is then cooled to room temperature, uses scales/electronic balance weighing to determine that the loading mass ratio of Pb is 10%.This negative material not only has high electrocatalytic active, can reduce the electrochemical polarization of liquid flow energy storage battery, improves the working current density of battery, also improves the charge/discharge capacity of battery.
Monocell assembling evaluation and test condition is with embodiment 1, and difference from Example 1 is: adopt the present embodiment Pb to modify the all-vanadium flow battery of carbon paper as negative pole, current density is 80mA/cm
2time, voltage efficiency and energy efficiency are respectively 84.3% and 80.1%, and charge/discharge capacity improves 15% with unmodified carbon paper ratio.
Embodiment 4
The graphite felt of certain size is immersed in 0.01MPbSO
4h
2sO
4in solution, take out after ultrasonic disperse 60min, put into drying box 120 DEG C of dry 10h, use scales/electronic balance weighing to determine PbSO
4loading mass ratio be 1%.This negative material not only has high electrocatalytic active, can reduce the electrochemical polarization of liquid flow energy storage battery, improves the working current density of battery, can also improve the charge/discharge capacity of battery.
Monocell assembling evaluation and test condition is with embodiment 1, and difference from Example 1 is: adopt the present embodiment Pb to modify the all-vanadium flow battery of graphite felt as negative pole, current density is 80mA/cm
2time, voltage efficiency and energy efficiency are respectively 87.3% and 82.8%; Current density brings up to 120mA/cm
2time, voltage efficiency and energy efficiency still remain on 82.7% and 79.4%.Charge/discharge capacity improves 2% with unmodified graphite felt ratio.
Claims (6)
1. a multi-functional negative material, is characterized in that: described multi-functional negative material is using carbon materials as matrix, has containing Pb eelctro-catalyst in its finishing, is Pb simple substance, PbO containing Pb eelctro-catalyst
2or one or two or more kinds in lead sulfate;
Described is 0.05 ~ 80wt% of multi-functional negative material containing the deposition of Pb eelctro-catalyst on matrix.
2. multi-functional negative material according to claim 1, is characterized in that: described is 0.05 ~ 20wt% of multi-functional negative material containing the deposition of Pb eelctro-catalyst on matrix, is more preferably 0.1 ~ 10wt%.
3. multi-functional negative material according to claim 1, is characterized in that: the described particle size containing Pb eelctro-catalyst is 1nm ~ 5 μm, preferably, is 2 ~ 500nm.
4. multi-functional negative material according to claim 1, is characterized in that: described carbon materials is a kind of in carbon felt, graphite felt, carbon paper or carbon cloth or the complex of more than two kinds in them.
5. multi-functional negative material according to claim 1, is characterized in that: the mode of described modification can be one in physical absorption, chemical deposition or two kinds.
6. an application for the arbitrary described multi-functional negative material of claim 1-5, is characterized in that: described multi-functional negative material can be used as all-vanadium flow battery negative pole in all-vanadium flow battery.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107039670A (en) * | 2017-03-14 | 2017-08-11 | 香港科技大学 | Electric fuel energy storage new method and system |
| CN114256466A (en) * | 2020-09-25 | 2022-03-29 | 中国科学院金属研究所 | Negative electrode material for hydrogen evolution inhibition type vanadium battery and preparation method thereof |
| CN114628702A (en) * | 2020-12-10 | 2022-06-14 | 中国科学院大连化学物理研究所 | Difunctional cathode and application thereof as cathode of all-vanadium redox flow battery |
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| JPS59117067A (en) * | 1982-12-22 | 1984-07-06 | Pentel Kk | Production method of air pole |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107039670A (en) * | 2017-03-14 | 2017-08-11 | 香港科技大学 | Electric fuel energy storage new method and system |
| CN114256466A (en) * | 2020-09-25 | 2022-03-29 | 中国科学院金属研究所 | Negative electrode material for hydrogen evolution inhibition type vanadium battery and preparation method thereof |
| CN114628702A (en) * | 2020-12-10 | 2022-06-14 | 中国科学院大连化学物理研究所 | Difunctional cathode and application thereof as cathode of all-vanadium redox flow battery |
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Application publication date: 20160210 |
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