CN106654298A - Negative electrode material with Sn-containing electrocatalyst of vanadium redox flow battery and preparation method for negative electrode material - Google Patents
Negative electrode material with Sn-containing electrocatalyst of vanadium redox flow battery and preparation method for negative electrode material Download PDFInfo
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- CN106654298A CN106654298A CN201610993955.0A CN201610993955A CN106654298A CN 106654298 A CN106654298 A CN 106654298A CN 201610993955 A CN201610993955 A CN 201610993955A CN 106654298 A CN106654298 A CN 106654298A
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- negative electrode
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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
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8853—Electrodeposition
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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
- H01M4/9041—Metals or alloys
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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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- 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 preparation method for a negative electrode material with a Sn-containing electrocatalyst of a vanadium redox flow battery. The preparation method adopts a chemical plating method and comprises the steps of putting a carbon base material into a sensitizing solution, soaking and taking out, and then putting into an activating solution to perform activation processing; and putting the activated carbon base material into a plating solution to be subjected to chemical plating to obtain the electrode material with the Sn-containing electrocatalyst. By modifying the Sn-containing electrocatalyst on the surface of the carbon base material through the chemical plating method, the electrode obtains high electrochemical activity and electrocatalytic activity, so that electrochemical polarity is lowered, and the voltage efficiency and energy efficiency of the battery are reduced; in addition, the method is simple and easy to operate; and the adopted material is low-cost Sn salt, so that low cost is achieved.
Description
Technical field
The invention belongs to liquid energy-storage vanadium battery field, specifically, is related to a kind of vanadium cell containing Sn elctro-catalysts and bears
Pole material and preparation method thereof.
Background technology
In recent years, wind energy and solar energy were widely developed, but were abandoned wind and abandoned the ratio of light rate and continue to increase.For
More effectively using 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, and big with power and capacity, 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 most extensive energy-storage battery of one of application prospect, increasingly
Paid close attention to by people.
Electrode is to provide the place that active material receiving and losing electrons occur electrochemical reaction as the critical material of vanadium cell,
Itself is not involved in electrochemical reaction.But, the quality of electrode performance directly influences the speed of active material electron exchange,
The working current density and energy efficiency of battery are largely affected, so as to affect the performance of whole battery system.Therefore,
Improve the active significant of electrode.
At present, it has been disclosed that patent document in mainly have for the method that improves electrode material performance：
Acid activation facture or electrochemistry anodic oxidation, to electrode material such as graphite felt acid oxidase process or electrification are carried out
Oxidation processes are learned, increases the oxygen-containing functional group of carbon fiber surface, increase its hydrophily, improved its electro-catalysis to electrode reaction and live
Property, reduce the activation polarization of battery system.Such as Yue (Yue, L., Li, W.S., Sun, Sun, F.Q., et al., Highly
hydroxylated carbon fibres as electrode materials of all-vanadium redox flow
battery.Carbon,2010,48:3079-3090) using 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.
The content of the invention
It is an object of the invention at least one in solving the problems referred to above that prior art is present.
For example, an object of the present invention is to improve the activity of vanadium battery negative electrode material so that the work electricity of vanadium cell
Current density and energy efficiency are improved.
To achieve these goals, one aspect of the present invention prepares the vanadium battery negative electrode material containing Sn elctro-catalysts there is provided a kind of
The method of material, the method comprising the steps of：Carbon basal body material is placed in the sensitizing solution containing Sn and is soaked；After immersion
Carbon basal body material is placed in activating solution carries out activation process；Carbon basal body material after activation process is washed to neutrality；Will
Carbon basal body material after washing is put into the plating solution containing Sn carries out chemical plating, obtains the vanadium cell containing Sn elctro-catalysts and bears
Pole material.
In one exemplary embodiment of the present invention, the plating solution containing Sn and the sensitizing solution containing Sn include Sn
Simple substance, SnO, SnO2, Sn halide, one or two or more kinds in stannate and Sn slaines, wherein, the Sn halide can
Think the one kind in stannous fluoride, stannous chloride, stannous bromide, stannous iodide, tin fluoride, stannic chloride, stannic bromide and stannic iodide
Or more than two kinds, can preferably be stannous chloride and/or stannic chloride.The stannate can be sodium stannate and/or potassium stannate.
The Sn slaines can be stannous sulfate, STANNOUS SULPHATE CRYSTALLINE, phosphoric acid stannous chloride, stannous pyrophosphate and phosphoric acid tin in one kind or two kinds with
On, can preferably be stannous sulfate and/or stannous pyrophosphate.
In one exemplary embodiment of the present invention, the plating solution by the stannous chloride of 4g/L～100g/L, 1g/L～
The titanium trichloride of 20g/L, the sodium citrate of 5g/L～200g/L, the disodium ethylene diamine tetraacetate of 3g/L～50g/L, 2g/L～
The sodium acetate of 20g/L and the benzene sulfonic acid composition of 0.1g/L～5g/L.
In one exemplary embodiment of the present invention, the carbon basal body material can be graphite felt, graphite cake, carbon
A kind of in paper, Graphene and carbon cloth or more than two kinds of combination.
In one exemplary embodiment of the present invention, the sensitizing solution by 5g/L～120g/L stannous chloride and 5ml/
The hydrochloric acid composition of L～500ml/L.
In one exemplary embodiment of the present invention, the activating solution is the aqueous solution containing 1g/L～30g/L palladium bichlorides.
In one exemplary embodiment of the present invention, the plating process can also include：Plating solution is adjusted with alkali
PH value is 8～9.
In one exemplary embodiment of the present invention, the alkali can for NaOH, potassium hydroxide, calcium hydroxide,
One or more combination in ammoniacal liquor.
In one exemplary embodiment of the present invention, the plating process, bath temperature can be 70 DEG C～90 DEG C.
Another aspect of the present invention provides a kind of vanadium battery negative electrode material containing Sn elctro-catalysts, the negative electrode material bag
Include carbon materials matrix and combine the elctro-catalyst containing Sn on carbon materials surface, wherein, the elctro-catalyst containing Sn is that Sn is mono-
Matter.
In one exemplary embodiment of the present invention, the carbon materials can be graphite felt, graphite cake, carbon paper, stone
A kind of in black alkene and carbon cloth or more than two kinds of combination.
In one exemplary embodiment of the present invention, the quality containing Sn elctro-catalysts accounts for carbon basal body quality of materials
Percentage (be referred to as：Mass percent is supported containing Sn elctro-catalysts) can be 0.1%～10%, preferred loading
Mass percent can be 1%～5%.
In one exemplary embodiment of the present invention, the particle size containing Sn elctro-catalysts can be 5nm～10 μ
M, grain sizes can be 10nm～1 μm.
Compared with prior art, Advantageous Effects of the invention include：
(1) present invention contains the elctro-catalyst of Sn by electroless plating method in carbon basal body surface modification so as to urge with high
Change activity, improve electrode material to V (III)/V (II) electricity to the electro catalytic activity for reacting, reduce activation polarization, improve battery
Voltage efficiency and energy efficiency.
(2) present invention makes the electrode after modification by electroless plating method in elctro-catalyst of the carbon basal body surface modification containing Sn
With higher hydrogen-evolution overpotential, suppress evolving hydrogen reaction of the battery in charge and discharge process.
(3) present invention adopts electroless plating method modified electrode, and the method is simple, easy to operate, the material for being used be price just
Suitable Sn salt, it is with low cost.
Specific embodiment
Hereinafter, by with reference to exemplary embodiment describing a kind of vanadium containing Sn elctro-catalysts of the invention in detail
Cell negative electrode material and preparation method thereof.
The method of the vanadium battery negative electrode material of the preparation containing Sn elctro-catalysts of the present invention, uses electroless plating method, the party
Method is comprised the following steps：
First, carbon basal body material is placed in the sensitizing solution containing Sn and is soaked.Here, sensitizing solution is by 5g/L～120g/L's
The hydrochloric acid composition of stannous chloride and 5ml/L～500ml/L.Carbon basal body material can be graphite felt, graphite cake, carbon paper, graphite
A kind of in alkene and carbon cloth or more than two kinds of combination.Immersion both can select to carry out at room temperature, it is also possible in heating
Under the conditions of carry out.Soak time can be 1min～30min, and the preferred time is 2min～10min.
Secondly, the carbon basal body material after immersion is placed in activating solution carries out activation process.Wherein, activating solution be containing
The aqueous solution of 1g/L～30g/L palladium bichlorides.The time of activation process can be 1min～30min, and preferred soak time is 3min
～10min.
Then, the carbon basal body material after activation process is washed to neutrality.Washing process can with deionized water or
Distilled water is carried out to carbon basal body material, and the degree of washing reaches 7.0 or so for pH value.
Finally, the carbon basal body material after washing is put into the plating solution containing Sn carries out chemical plating, obtains electro-catalysis containing Sn
The vanadium battery negative electrode material of agent.Wherein, plating solution by the stannous chloride of 4g/L～100g/L, the titanium trichloride of 1g/L～20g/L,
The sodium citrate of 5g/L～200g/L, the disodium ethylene diamine tetraacetate of 3g/L～50g/L, the sodium acetate of 2g/L～20g/L and
The benzene sulfonic acid composition of 0.1g/L～5g/L.Plating process can also include：The pH value for adjusting plating solution with alkali is 8～9, wherein,
Alkali can be one or more the combination in NaOH, potassium hydroxide, calcium hydroxide, ammoniacal liquor.As long as the addition of alkali
The pH value that plating solution can be made maintains 8～9.The temperature of plating solution can maintain 70 DEG C～90 DEG C in plating process, chemistry
The plating time can be 5s～10min.Electrode material after chemical plating can also be collected process.
In the method for preparing the vanadium battery negative electrode material containing Sn elctro-catalysts of the invention, the plating solution containing Sn and containing Sn
Sensitizing solution include Sn simple substance, SnO, SnO2, Sn halide, one or two or more kinds in stannate and Sn slaines obtain
, wherein, Sn halide can be stannous fluoride, stannous chloride, stannous bromide, stannous iodide, tin fluoride, stannic chloride, bromination
One or two or more kinds in tin and stannic iodide, can preferably be stannous chloride and/or stannic chloride.Stannate can be stannic acid
Sodium and/or potassium stannate.Sn slaines can be in stannous sulfate, STANNOUS SULPHATE CRYSTALLINE, phosphoric acid stannous chloride, stannous pyrophosphate and phosphoric acid tin
Plant or more than two kinds, can preferably be stannous sulfate and/or stannous pyrophosphate.
The vanadium battery negative electrode material containing Sn elctro-catalysts 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
A kind of in black plate, carbon paper, Graphene and carbon cloth or more than two kinds of combination.Quality percentage is supported containing Sn elctro-catalysts
Than being 0.1%～10%, preferred loading mass percent can be 1%～5%.Particle size containing Sn elctro-catalysts
Can be 5nm～10 μm, grain sizes can be 10nm～1 μm.
The exemplary embodiment of the present invention is described in further detail below in conjunction with specific example.
Embodiment 1
Chemical plating fluid is by 7.6g/L stannous chlorides, 4.5g/L titanium trichlorides, 102g/L sodium citrates, 15g/L ethylenediamine tetraacetics
Acetic acid disodium, 9.8g/L sodium acetates and 0.32g/L benzene sulfonic acids composition.The graphite felt of certain size is put into protochloride containing 40g/L
Impregnate in tin, the solution of 100ml/L hydrochloric acid, soaking at room temperature 3min, then activation process is carried out with the aqueous solution containing 2g/L palladium bichlorides
5min, it is 7 or so to wash to pH；It is then placed in carrying out chemical plating in plating solution, it is 9 to adjust plating solution pH by ammoniacal liquor, bath temperature
85 DEG C are maintained, electroless plating time is 2min.The carbon cloth of Sn modifications is finally given, using scales/electronic balance weighing supporting for Sn is determined
Amount mass ratio is 1%.
In order to test impact of the carbon cloth of Sn modifications as vanadium battery negative electrode to battery performance.Make using from embodiment 1
The graphite felt of the standby Sn modifications for obtaining, as negative electrode, is anode electrode using untreated graphite felt, assembles monocell, is entered
Row charge-discharge test.It is 3.0M and V (III)/V (IV) that both positive and negative polarity electrolyte is vanadium ion concentration for 1.6M, sulfuric acid concentration
For 1:1 V electrolyte
Comparative example 1
Using the graphite felt of Tieling Shen and the production of carbon fibre material Co., Ltd as comparative example, using unmodified graphite
Felt assembles monocell, carries out charge-discharge test.Both positive and negative polarity electrolyte be vanadium ion concentration for 1.6M, sulfuric acid concentration be 3.0M simultaneously
And V (III)/V (IV) is 1:1 V electrolyte.
The monocell that embodiment 1 is assembled and the monocell of comparative example assembling are 100mA/cm in current density2Under enter
Row charge-discharge test.
Compared with comparative example 1, the voltage efficiency and energy efficiency of the vanadium cell of embodiments in accordance with the present invention 1 respectively from
82.6% brings up to 87.5% and 77.6% brings up to 83.5%, the electricity of the battery that the electrode prepared by embodiment 1 is constituted
Pressure efficiency and energy efficiency all improve, therefore, the electro-chemical activity of the vanadium battery negative electrode material that embodiment 1 is prepared is carried
Height, the activation polarization of electrode reaction is reduced.
In sum, beneficial effects of the present invention include：
(1) present invention contains the elctro-catalyst of Sn by electroless plating method in carbon basal body surface modification so as to urge with high
Change activity, improve electrode material to V (III)/V (II) electricity to the electro catalytic activity for reacting, reduce activation polarization, improve battery
Voltage efficiency and energy efficiency.
(2) present invention makes the electrode after modification by electroless plating method in elctro-catalyst of the carbon basal body surface modification containing Sn
With higher hydrogen-evolution overpotential, suppress evolving hydrogen reaction of the battery in charge and discharge process.
(3) present invention is simple using the method for chemical plating modified electrode, easy to operate, and the material for being used is low-cost
Sn salt, it is with low cost.
Although describing the present invention already in connection with exemplary embodiment above, those of ordinary skill in the art should be clear
Chu, 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 for preparing the vanadium battery negative electrode material containing Sn elctro-catalysts, it is characterised in that methods described includes following
Step：
Carbon basal body material is placed in the sensitizing solution containing Sn and is soaked；
Carbon basal body material after immersion is placed in activating solution carries out activation process；
Carbon basal body material after activation process is washed to neutrality；
Carbon basal body material after washing is put into the plating solution containing Sn carries out chemical plating, obtains the electricity containing Sn elctro-catalysts
Pole material.
2. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that institute
Stating the plating solution containing Sn and the sensitizing solution containing Sn includes Sn simple substance, SnO, SnO2, Sn halide, stannate or Sn metals
Salt, wherein,
The Sn halide be stannous fluoride, stannous chloride, stannous bromide, stannous iodide, tin fluoride, stannic chloride, stannic bromide or
Stannic iodide；
The stannate is sodium stannate or potassium stannate；
The Sn slaines are stannous sulfate, STANNOUS SULPHATE CRYSTALLINE, phosphoric acid stannous chloride, stannous pyrophosphate or phosphoric acid tin.
3. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that institute
State plating solution by the stannous chloride of 4g/L～100g/L, the titanium trichloride of 1g/L～20g/L, the sodium citrate of 5g/L～200g/L,
The benzene sulfonic acid composition of the disodium ethylene diamine tetraacetate of 3g/L～50g/L, the sodium acetate of 2g/L～20g/L and 0.1g/L～5g/L.
4. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that institute
Carbon basal body material is stated for a kind of in graphite felt, graphite cake, carbon paper, Graphene and carbon cloth or more than two kinds of combination.
5. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that institute
State sensitizing solution to be made up of the stannous chloride of 5g/L～120g/L and the hydrochloric acid of 5ml/L～500ml/L.
6. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that institute
It is the aqueous solution containing 1g/L～30g/L palladium bichlorides to state activating solution.
7. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that
In the electroless plating step, the pH value for adjusting plating solution with alkali is 8～9.
8. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that
In the electroless plating step, bath temperature is controlled for 70 DEG C～90 DEG C.
9. a kind of vanadium battery negative electrode material containing Sn elctro-catalysts, it is characterised in that the negative electrode material includes carbon materials
Matrix and combine carbon materials surface elctro-catalyst containing Sn, wherein, the elctro-catalyst containing Sn be Sn simple substance.
10. the method that preparation according to claim 1 contains the vanadium battery negative electrode material of Sn elctro-catalysts, it is characterised in that
The carbon materials is a kind of or more than two kinds of the combination in graphite felt, graphite cake, carbon paper, Graphene and carbon cloth.
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