CN106410218A - Sn electric catalyst vanadium cell negative electrode material and preparation method thereof - Google Patents
Sn electric catalyst vanadium cell negative electrode material and preparation method thereof Download PDFInfo
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- CN106410218A CN106410218A CN201610992634.9A CN201610992634A CN106410218A CN 106410218 A CN106410218 A CN 106410218A CN 201610992634 A CN201610992634 A CN 201610992634A CN 106410218 A CN106410218 A CN 106410218A
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- catalyst
- elctro
- negative electrode
- electrode material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides a Sn electric catalyst vanadium cell negative electrode material and preparation method thereof. The method puts charcoal element base body material as work electrode, in Sn containing ion deposit liquid carries out direct current electrochemical deposition, resulting in a Sn containing electric catalyst vanadium cell negative electrode material, wherein, the Sn containing ion acts as Sn2+, Sn4+ and SnO32- middle one sort or two sorts and above. The method via electric chemical theory deposit method on charcoal element base body repairs the Sn containing electric catalyst, puts electrode to keep high electric chemical theory activity, represses electric chemical theory electric polarization, raises cell electric pressure function rate and energy producing rate. The method prepares by easy step, takes easy to hand operate, and the held material is inexpensive Sn salt, and the preparation cost amounts low.
Description
Technical field
The invention belongs to liquid energy-storage vanadium battery field, specifically, it is related to one kind and is contained using electrochemical deposition method preparation
The method of the vanadium battery negative electrode material of Sn elctro-catalyst.
Background technology
In recent years, wind energy and solar energy were widely developed, but abandoned wind and abandon the ratio of light rate and continue to increase.For
More effectively utilize wind energy and solar energy, people are to the demand of large-scale energy storage device more and more stronger.Vanadium cell is because of it
Power output and capacity are separate, have power and capacity is big, service life cycle is long, and energy efficiency is high, depth discharge and recharge
Performance is good, the advantages of security performance is high, therefore it is considered to be the extensive energy-storage battery of most one of application prospect, increasingly
Paid close attention to by people.
Electrode, as the critical material of vanadium cell, is the place providing active material receiving and losing electrons that electrochemical reaction occurs,
Itself is not involved in electrochemical reaction.But, the quality of electrode performance, directly influence the speed of active material electron exchange,
Largely affect working current density and the energy efficiency of battery, thus affecting the performance of whole battery system.Therefore,
The activity improving electrode is significant.
At present it has been disclosed that patent document in mainly have for the method improving electrode material performance：
Acid activation facture or electrochemistry anodic oxidation, carry out acid oxidase process or electrification to electrode material such as graphite felt
Learn oxidation processes, increase the oxygen-containing functional group of carbon fiber surface, increase its hydrophily, improve it and electro-catalysis of electrode reaction is lived
Property, reduce the activation polarization of battery system.As (Yue, L., Li, W.S., Sun, Sun, F.Q., et al., the Highly such as Yue
hydroxylated carbon fibres as electrode materials of all-vanadium redox flow
battery.Carbon,2010,48:3079-3090) adopt sulfuric acid and nitric acid mixed processing graphite felt；(Li, the X.G. such as Li；
Liu,S.Q.；Tan,N.；et al.,Characteristics of graphite felt electrode
electrochemically oxidized for vanadium redox battery application,
Transactions of Nonferrous Metals Society of China,2007,17:Using electrification in 195-199)
Learn anodized graphite felt.
Content of the invention
It is an object of the invention to solving at least one in the problems referred to above that prior art exists.
For example, an object of the present invention is to improve the electro-chemical activity of vanadium battery negative electrode material so that vanadium cell
Working current density and energy efficiency are improved.
To achieve these goals, one aspect of the present invention provides a kind of vanadium battery negative electrode material prepared containing Sn elctro-catalyst
The method of material, the method comprising the steps of：Using carbon basal body material as working electrode, in the deposition liquid containing Sn ion
Carry out direct current electrochemical deposition, obtain the vanadium battery negative electrode material containing Sn elctro-catalyst.Wherein, described ion containing Sn can be
Sn2+、Sn4+And SnO3 2-One of or more than two kinds.
In one exemplary embodiment of the present invention, the described deposition liquid containing Sn ion can be by drawing in deposition liquid
Enter Sn simple substance, SnO, SnO2, Sn halide, one of stannate and Sn slaine or two kinds achieved above.
In one exemplary embodiment of the present invention, in the described deposition liquid containing Sn ion, the concentration containing Sn ion is permissible
For 0.05mol/L～1.0mol/L, preferred concentration is 0.1mol/L～0.8mol/L.
In one exemplary embodiment of the present invention, wherein, described Sn halide can be stannous fluoride, protochloride
One of tin, stannous bromide, stannous iodide, tin fluoride, stannic chloride, stannic bromide and stannic iodide or more than two kinds, preferably may be used
Think stannous chloride and/or stannic chloride.Described stannate can be sodium stannate and/or potassium stannate.Described Sn slaine can be
One of stannous sulfate, STANNOUS SULPHATE CRYSTALLINE, phosphoric acid stannous chloride, stannous pyrophosphate and phosphoric acid tin or more than two kinds, can preferably be sulphur
Sour stannous and/or stannous pyrophosphate.
In one exemplary embodiment of the present invention, described elctro-catalyst containing Sn can be Sn simple substance.
In one exemplary embodiment of the present invention, described direct current electrochemical deposition process current density can be 5mA/
cm2～100mA/cm2, preferably current density is 10mA/cm2～50mA/cm2；Sedimentation time can be 5s～20min, preferably heavy
The long-pending time is 10s～1min.
In one exemplary embodiment of the present invention, the temperature of described direct current electrochemical deposition process can for 20 DEG C～
100 DEG C, 30 DEG C～80 DEG C of preferred range.
In one exemplary embodiment of the present invention, described carbon materials can be graphite felt, graphite cake, carbon paper, stone
The combination of one of black alkene and carbon cloth or more than two kinds.
Another aspect of the present invention provides a kind of vanadium battery negative electrode material containing Sn elctro-catalyst, described negative electrode material bag
Include the carbon materials matrix and combination elctro-catalyst containing Sn on carbon materials surface, wherein, described elctro-catalyst containing Sn is that Sn is mono-
Matter.
In one exemplary embodiment of the present invention, described carbon materials can be graphite felt, graphite cake, carbon paper, stone
The combination of one of black alkene and carbon cloth or more than two kinds.
In one exemplary embodiment of the present invention, the described quality containing Sn elctro-catalyst accounts for carbon basal body quality of materials
Percentage (be referred to as：Support mass percent containing Sn elctro-catalyst) can be 0.1%～10%, preferably loading
Mass percent can be 1%～5%.
In one exemplary embodiment of the present invention, the described particle size containing Sn elctro-catalyst can be 5nm～10 μ
M, grain sizes can be 10nm～1 μm.
Compared with prior art, the Advantageous Effects of the present invention include：
(1) present invention contains the elctro-catalyst of Sn so as to have height by electrochemical deposition method in carbon basal body surface modification
Catalysis activity, improve the electro catalytic activity to V (III)/V (II) electricity to reaction for the vanadium cell electrode material, reduce electrochemistry pole
Change, improve voltage efficiency and the energy efficiency of vanadium cell.
(2) present invention adopts electrochemical deposition method modified electrode, and the method is simple, easy to operate, and the material being used is
Low-cost Sn salt, with low cost.
Specific embodiment
Hereinafter, a kind of vanadium cell containing Sn elctro-catalyst of the present invention will be described in detail with reference to exemplary embodiment
Negative material and preparation method thereof.
The preparation of the present invention contains the vanadium battery negative electrode material of Sn elctro-catalyst, uses electrochemical deposition method, the method
Operation principle can sketch and be：After energising, in solution, obtain electronics containing tin ion in carbon basal body material surface, be reduced to
Tin simple substance, then directly deposits in carbon basal body material surface.
The method that the preparation of the present invention contains the vanadium battery negative electrode material of Sn elctro-catalyst comprises the following steps：With carbon basal body
, as working electrode, Sn plate, graphite cake or platinized platinum are electrochemical as to electrode, carrying out direct current in the deposition liquid containing Sn ion for material
Learn deposition, obtain the vanadium battery negative electrode material containing Sn elctro-catalyst.Wherein, described ion containing Sn can be Sn2+、Sn4+With
SnO3 2-One of or more than two kinds.Containing Sn ion deposition liquid in containing Sn ion concentration can for 0.05mol/L～
1.0mol/L, preferred concentration is 0.1mol/L～0.8mol/L.Carbon basal body material can be graphite felt, graphite cake, carbon paper, stone
The combination of one of black alkene and carbon cloth or more than two kinds.Wherein, the elctro-catalyst containing Sn being obtained by the method is permissible
For Sn simple substance.
Electrodeposit liquid containing Sn ion can be by introducing Sn simple substance, SnO, SnO in deposition liquid2, Sn halide, stannic acid
One of salt and Sn slaine or two kinds achieved above.Wherein, Sn halide can be stannous fluoride, stannous chloride, bromination
One of stannous, stannous iodide, tin fluoride, stannic chloride, stannic bromide and stannic iodide or more than two kinds, can preferably be chlorination
Stannous and/or stannic chloride.Stannate can be sodium stannate and/or potassium stannate.Sn slaine can for stannous sulfate, STANNOUS SULPHATE CRYSTALLINE,
One of phosphoric acid stannous chloride, stannous pyrophosphate and phosphoric acid tin or more than two kinds, can preferably be stannous sulfate and/or pyrophosphoric acid
Stannous.
In direct current electrochemical deposition process, the current density of employing is too low, and for example current density is less than 5mA/cm2When, meeting
Cause that the speed of electro-deposition Sn simple substance is too low, deposition effect is poor；According to current density too high when, such as current density is high
In 100mA/cm2When, the excessive velocities of electro-deposition Sn simple substance can be caused, and then make the combination of Sn simple substance and carbon basal body material
Power is less, easy to fall off, and when current density is too high, also easily burns carbon basal body material.Therefore, electric current is close in the present invention
Degree can be 5mA/cm2～100mA/cm2, preferably current density can be 10mA/cm2～50mA/cm2；Sedimentation time can be
5s～20min, the preferred deposition time can be 10s～1min.
Similarly, when the temperature of electrodeposit liquid in direct current electrochemical deposition process is too low, such as when temperature is less than 20 DEG C,
Sn simple substance can be caused to be difficult in carbon basal body deposited on materials；When the temperature depositing liquid is too high, for example temperature is higher than 100 DEG C
When, the Sn simple substance short texture that electro-deposition obtains can be caused, the adhesion and carbon basal body material between is little, easy to fall off.Therefore,
The temperature of electrodeposit liquid can be 20 DEG C～100 DEG C in the present invention, 30 DEG C～80 DEG C of preferred range.
In the method for the vanadium battery negative electrode material containing Sn elctro-catalyst in the preparation according to the present invention, can also include：Will
Vanadium battery negative electrode material after direct current electrochemical deposition is collected processing.Can be entered using distilled water, deionized water equal solvent
Row washing.Process can also be dried after washing.
The vanadium battery negative electrode material containing Sn elctro-catalyst of the present invention can include carbon materials matrix and combine in carbon
The elctro-catalyst containing Sn of material surface, wherein, elctro-catalyst containing Sn is Sn simple substance.Wherein, carbon materials can be graphite felt, stone
The combination of one of black plate, carbon paper, Graphene and carbon cloth or more than two kinds.Support percent mass containing Sn elctro-catalyst
Ratio can be 0.1%～10%, and preferably loading mass percent can be 1%～5%.Particle size containing Sn elctro-catalyst
Can be 5nm～10 μm, grain sizes can be 10nm～1 μm.
The exemplary embodiment of the present invention to be described in further detail below in conjunction with specific example.
Embodiment 1
Configuration consists of stannous sulfate, the sulfuric acid of 140g/L, the gelatin of 5.5g/L, the cresols of 7g/L and the 40g/L of 40g/L
Sodium sulphate electric depositing solution (referred to as deposition liquid).
Using graphite felt as working electrode, it is pure tin plate to electrode, bath temperature maintains 30 DEG C, using DC electrodeposition,
Wherein, current density is 10mA/cm2.
Deposition 1min after take out graphite felt, and deionized water clean after be dried, obtain Sn simple substance modification graphite felt.
Using scales/electronic balance weighing, the mass percent that supports of Sn simple substance is 1%.
Embodiment 2
Configuration consists of sodium stannate, the hydrogen peroxide of the NaOH of 12g/L, the sodium acetate of 20g/L and 2ml/L of 80g/L
(30%) electric depositing solution.
Using graphite felt as working electrode, it is pure tin plate to electrode, bath temperature maintains 80 DEG C, using DC electrodeposition,
Wherein, current density is 15mA/cm2.
Deposition 2min after take out graphite felt, and deionized water clean after be dried, obtain Sn simple substance modification graphite felt.
Using scales/electronic balance weighing, the mass percent that supports of Sn simple substance is 2%.
Embodiment 3
Configuration consists of stannic chloride, the sulfuric acid of 140g/L, the gelatin of 5.5g/L, the cresols of 7g/L and the 40g/L's of 40g/L
The electric depositing solution of sodium sulphate.
Using carbon cloth as working electrode, it is pure tin plate to electrode, bath temperature maintains 30 DEG C, using DC electrodeposition, its
In, current density is 20mA/cm2.
Deposition 2min after take out carbon cloth, and deionized water clean after be dried, obtain Sn simple substance modification carbon cloth.
Using scales/electronic balance weighing, the mass percent that supports of Sn simple substance is 3%.
Embodiment 4
Configuration consist of the stannous sulfate of 70g/L, the sulfuric acid of 180g/L, the gelatin of 1.0g/L, the cresols of 2.0g/L and
The electric depositing solution of the sodium sulphate of 10g/L.
Using carbon paper as working electrode, it is pure tin plate to electrode, bath temperature maintains 40 DEG C, using DC electrodeposition, its
In, current density is 35mA/cm2.
Deposition 3min after take out carbon paper, and deionized water clean after be dried, obtain Sn simple substance modification carbon paper.
Using scales/electronic balance weighing, the mass percent that supports of Sn simple substance is 4%.
Embodiment 5
Configuration consist of the stannic chloride of 20g/L, the phosphoric acid stannous chloride of 80g/L, the sulfuric acid of 140.0g/L, the gelatin of 0.8g/L,
The electric depositing solution of the sodium sulphate of the cresols of 1.5g/L and 8g/L.
Using graphite felt as working electrode, it is pure tin plate to electrode, bath temperature maintains 40 DEG C, using DC electrodeposition,
Wherein, current density is 40mA/cm2.
Deposition 3min after take out graphite felt, and deionized water clean after be dried, obtain Sn simple substance modification graphite felt.
Using scales/electronic balance weighing, the mass percent that supports of Sn simple substance is 5%.
In order to test carbon basal body material impact to battery performance as vanadium battery negative electrode of Sn simple substance modification.From enforcement
The carbon basal body material that the Sn simple substance for preparing in example 1～5 is modified as negative electrode, using untreated corresponding carbon
Matrix material is anode electrode, assembles monocell, carries out charge-discharge test.In positive and negative electrode electrolyte, the concentration of vanadium ion is
1.6mol/L, the concentration of sulfuric acid are 3.0mol/L, and V (III)/V (IV) is 1:1.
Comparative example
The graphite felt being produced using Tieling Shen and carbon fibre material Co., Ltd as a comparison case, using unmodified graphite
Felt assembles monocell, carries out charge-discharge test.In positive and negative electrode electrolyte, the concentration of vanadium ion is 1.6mol/L, the concentration of sulfuric acid
For 3.0mol/L, and V (III)/V (IV) is 1:1.
The monocell of the monocell of embodiment 1～5 assembling and comparative example assembling is 100mA/cm in current density2Under survey
Test result is shown in Table 1.
The monocell of the different negative material assembling of table 1 runs the Performance comparision of 50 circulations
| Embodiment | Average current efficiency | Average voltage efficiencies | Average energy efficiency |
| Comparative example | 95.62% | 82.20% | 78.60% |
| Embodiment 1 | 95.88% | 87.40% | 83.80% |
| Embodiment 2 | 95.80% | 88.10% | 84.40% |
| Embodiment 3 | 95.83% | 88.80% | 85.10% |
| Embodiment 4 | 95.56% | 87.90% | 84.00% |
| Embodiment 5 | 95.80% | 87.80% | 84.10% |
As can be known from Table 1, compared with unmodified graphite felt, the monocell that graphite felt that surface modification has Sn simple substance assembles
Voltage efficiency be 88.00% ± 1.00% and energy efficiency be 84.00% ± 0.50%, all improve 5.0%～6.0%.
And, surface modification has the carbon cloth of Sn simple substance and the voltage efficiency of the monocell of carbon paper assembling to be respectively 88.80% He
87.90%, energy efficiency is respectively 85.10% and 84.00%.Therefore, by electrodeposition process obtain containing Sn elctro-catalyst
Vanadium battery negative electrode material can improve vanadium battery negative electrode material to V (III)/electro-chemical activity to reaction for V (II) electricity, reduces electricity
The activation polarization of pole reaction.
In sum, beneficial effects of the present invention include：
(1) present invention modifies the elctro-catalyst containing Sn so as to have by electrochemical deposition method in carbon basal body material surface
There is high catalysis activity, improve electrode material to V (III)/electro-chemical activity to reaction for V (II) electricity, reduce activation polarization,
Thus improving voltage efficiency and the energy efficiency of vanadium cell.
(2) the electrode modification method of the present invention is simple, easy to operate, and the material being used is low-cost Sn salt, cost
Cheap.
Although describing the present invention already in connection with specific illustrative embodiment above, those of ordinary skill in the art should
This understands, in the case of without departing from spirit and scope by the claims, can carry out various modifications to above-described embodiment.
Claims (10)
1. a kind of method preparing the vanadium battery negative electrode material containing Sn elctro-catalyst is it is characterised in that methods described is with carbon base
Body material, as working electrode, carries out direct current electrochemical deposition in the deposition liquid containing Sn ion, obtains containing Sn elctro-catalyst
Vanadium battery negative electrode material, wherein, described ion containing Sn is Sn2+、Sn4+And SnO3 2-One of or more than two kinds.
2. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
State the combination that carbon basal body material is one of graphite felt, graphite cake, carbon paper, Graphene and carbon cloth or more than two kinds.
3. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
State the deposition liquid containing Sn ion to pass through to introduce Sn simple substance, SnO, SnO in deposition liquid2, Sn halide, stannate and Sn slaine
One of or two kinds achieved above.
4. according to claim 3 preparation containing Sn elctro-catalyst vanadium battery negative electrode material method it is characterised in that
Described Sn halide be stannous fluoride, stannous chloride, stannous bromide, stannous iodide, tin fluoride, stannic chloride, stannic bromide and
One of stannic iodide or more than two kinds；
Described stannate is sodium stannate and/or potassium stannate；
Described Sn slaine be one of stannous sulfate, STANNOUS SULPHATE CRYSTALLINE, phosphoric acid stannous chloride, stannous pyrophosphate and phosphoric acid tin or two kinds with
On.
5. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
Stating the concentration containing Sn ion in the deposition liquid containing Sn ion is 0.05mol/L～1.0mol/L.
6. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
Stating elctro-catalyst containing Sn is Sn simple substance.
7. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
The current density stating direct current electrochemical deposition process is 5mA/cm2～100mA/cm2.
8. the method for the vanadium battery negative electrode material containing Sn elctro-catalyst for the preparation according to claim 1 is it is characterised in that institute
The temperature stating direct current electrochemical deposition is 20 DEG C～100 DEG C.
9. a kind of vanadium battery negative electrode material containing Sn elctro-catalyst is it is characterised in that described negative electrode material includes carbon materials
The matrix and combination elctro-catalyst containing Sn on carbon materials surface, wherein, described elctro-catalyst containing Sn is Sn simple substance.
10. according to claim 1 preparation containing Sn elctro-catalyst vanadium battery negative electrode material method it is characterised in that
Described carbon materials is the combination of one of graphite felt, graphite cake, carbon paper, Graphene and carbon cloth or more than two kinds.
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Cited By (1)
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| CN116031424A (en) * | 2023-03-24 | 2023-04-28 | 南方科技大学 | Flow battery composite electrode, preparation method thereof and flow battery |
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Application publication date: 20170215 |