CN105591106A - Sodium-ion battery positive pole material and preparation method thereof - Google Patents
Sodium-ion battery positive pole material and preparation method thereof Download PDFInfo
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- CN105591106A CN105591106A CN201610157842.7A CN201610157842A CN105591106A CN 105591106 A CN105591106 A CN 105591106A CN 201610157842 A CN201610157842 A CN 201610157842A CN 105591106 A CN105591106 A CN 105591106A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/582—Halogenides
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a sodium-ion battery positive pole material with the composition being NaFe0.5Mn0.5SO4F. The invention further discloses a preparation method of the sodium-ion battery positive pole material. MnSO4.H2O, FeSO4.H2O and NaF are heated in a sealed state for a reaction in the presence of an additive, and the sodium-ion battery positive pole material NaFe0.5Mn0.5SO4F is obtained. The first-time reversible capacity of the sodium-ion battery positive pole material can reach 130 mAh/g, and the sodium-ion battery positive pole material has the good circulation performance and the wide application prospect. The preparation method is simple, easy to control and beneficial to achieving large-scale industrial production.
Description
Technical field
The present invention relates to chargeable battery positive electrode in energy and material, especially a kind of sodium ion electricityPond positive electrode and preparation method thereof.
Background technology
Along with the consumption of fossil energy and the discharge of carbon dioxide increasing, environmental problem and energySource crisis is day by day serious, and chemical energy storage is more and more subject to the mankind's attention. Lithium ion battery is because of toolThere are the features such as high voltage, large capacity, long-life and security performance are good, make it from portable electronicEquipment, energy-storage battery to the many-sides such as electric automobile have been shown wide application prospect, but oneDawn lithium ion battery by large-scale application in electric automobile and energy storage device, limited lithium on the earthResource cannot meet large-scale application requirement like this at all.
Sodium and lithium are of the same clan, have similar electrochemical properties, compared with lithium ion battery, sodium fromSub-battery has many potential advantages such as aboundresources, cost be low, is suitable for extensive energy storage,Will become a kind of new green environment protection energy-storage battery that has development prospect, market prospects veryWide.
Anode material of lithium-ion battery mainly contains carbon back negative material, oxide and sulfide negative poleMaterial, alloy type negative material and organic compound negative material, these negative materials have higherStorage sodium capacity and good cycle performance, as anode material of lithium-ion battery Ni3S2'sSpecific capacity is higher than 400mAh/g, Na2C8H4O4The specific capacity of negative material after 50 circulationsStill remain on 258mAh/g.
Sodium-ion battery positive electrode is the key of the development of restriction sodium-ion battery and business application,Exploitation and develop new sodium-ion battery positive electrode and become the development of current sodium-ion batteryFor urgent problem. At present, sodium-ion battery positive electrode mainly contain transition metal oxide andPolyanionic compound. As Doff etc. prepares Na0.44MnO4Sodium-ion battery positive electrode,Under 0.1C electric current first discharge capacity in about 100mAh/g; The solid-phase synthesis such as XiaThe NaCrO of synthetic layer structure2Positive electrode, discharge capacity is 110mAh/g; Seung-MinOh etc. are by displacement olivine LiFePO4In Li, obtain olive and pull the NaFePO of stone type4SodiumIon battery positive electrode. In addition, also have some Patent Application Publications some sodium-ion batteriesPositive electrode, there is the shortcoming that discharge capacity is low or preparation method is complicated in these materials. For exampleCN103985851A discloses a kind of sodium-ion battery positive electrode, comprise conductive additive andNa3-xM2LO6, M be a kind of in Fe, Co, Ni, Cu, Zn, Mg, V, Cr orSeveral; L is one or more in Sb, Te, Nb, Bi, P. The head of this positive electrodeAll discharge capacities are not high, and preparation is comparatively complicated, and reaction temperature is high, is unfavorable for commercial Application.
Summary of the invention
First object of the present invention is to provide a kind of sodium-ion battery positive electrode.
Second object of the present invention is to provide the preparation of above-mentioned sodium-ion battery positive electrodeMethod.
For realizing above-mentioned first object, the present invention adopts following content:
A kind of sodium-ion battery positive electrode, the consisting of of this sodium-ion battery positive electrodeNaFe0.5Mn0.5SO4F。
For realizing above-mentioned second object, the present invention adopts following content:
The preparation method of above-mentioned sodium-ion battery positive electrode, by by MnSO4·H2O、FeSO4·H2O and NaF, under the existence of auxiliary agent, heat and react under sealing state,Obtain sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F；
Described auxiliary agent is water-soluble polyhydroxy organic matter;
Described MnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is 1:1:(2.0-4.0);
The reaction temperature of described reaction is 200-350 DEG C.
Further, described MnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is1：1：2.5。
Auxiliary agent is used to provide polyhydroxy environment, and reaction can be carried out smoothly, has partially catalyzed agent to doWith. Preferably, described auxiliary agent is one or more in glycerine, citric acid, ethylene glycolMixture.
Further, the reaction time of described reaction is 2-10h.
Further, after described reaction completes, use CH2Cl2Washing, dry, obtain sodium ionCell positive material NaFe0.5Mn0.5SO4F。
Those skilled in the art can be according to the commercially available purchase of condition MnSO4·H2O and FeSO4·H2O，Or according to existing preparation method's preparation. Be preferably in situ preparation MnSO4·H2O andFeSO4·H2O, has good activity like this.
Further, described MnSO4·H2O is by MnSO4·4H2O saturated solution is closeUnder envelope state, heat, add wherein ethanol, stir, cooling, obtain MnSO4·H2O。
Preferably, preparation MnSO4·H2Reaction temperature when O is 80-200 DEG C, the reaction timeBe no less than 1 hour.
Further, described in, be by FeSO4·7H2O saturated solution is under sealing state and inertiaIn atmosphere protection, heat, add wherein ethanol, stir, cooling, obtain FeSO4·H2O。
Preferably, preparation FeSO4·H2Reaction temperature when O is 100-300 DEG C, when reactionBetween be no less than 1 hour.
The present invention has the following advantages:
1, sodium-ion battery positive electrode of the present invention first reversible capacity can reach 130mAh/g,And there is good cycle performance, have wide practical use.
2, preparation method of the present invention is simple, only needs a step just can make, and is easy to control, and hasBe beneficial to and realize large-scale industrial production.
Brief description of the drawings
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the first two circulation volume song of ten weeks of the sodium-ion battery positive electrode of embodiment 1Line.
Fig. 2 is the SEM figure of the sodium-ion battery positive electrode of embodiment 2.
Detailed description of the invention
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiment, the present invention is done into oneThe explanation of step. It will be appreciated by those skilled in the art that specifically described content is explanation belowProperty and nonrestrictive, should not limit the scope of the invention with this.
Embodiment 1
A preparation method for sodium-ion battery positive electrode, comprises the following steps:
1) accurately take appropriate MnSO4·4H2O solid, is mixed with saturated by deionized waterSolution seals in polytetrafluoroethyltank tank, is heated to 120 DEG C, is incubated 4 hours, adds suitableAmount ethanol, fully stirs, and obtains MnSO4·H2O solid;
2) accurately take appropriate FeSO4·7H2O solid, is mixed with saturated by deionized waterSolution, under high-purity argon gas protection, seals in polytetrafluoroethyltank tank, is heated to 250 DEG C, protectsTemperature 4 hours, adds appropriate ethanol, fully stirs, and obtains FeSO4·H2O solid;
3) by the MnSO of preparation4·H2O solid, MnSO4·H2O solid is pressed MnSO4·H2O：FeSO4·H2The ratio of O:NaF=1:1:2.5 (mol ratio) is mixed, and adds sweet in right amountOil after ultrasonic wave disperses to mix, adds thermal response 6 hours, use in 300 DEG C under sealing stateCH2Cl2Washing, dry, obtain sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
Performance test:
By the sodium-ion battery positive electrode NaFe of preparation0.5Mn0.5SO4F and acetylene black, poly-fourPVF mixes by the mass ratio of about 85:10:5, is pressed into thickness is about with film laminatorThe film of 1mm, is placed in baking oven and fully dries in 120 DEG C, and intercepting surface area is 1cm2'sCircular membrane, is compressed on stainless (steel) wire, makes Electrode.
Using Electrode as positive pole, taking sodium metal as to electrode, Celgard2300 micropore is poly-Propylene film is barrier film, taking be dissolved in volume ratio as EC (ethylene carbonate)/DMC of 1:1 (1,2-dimethyl carbonate) 1mol/LNaClO4For electrolyte, be full of the glove box of argon gasIn be assembled into CR2032 type button cell.
Button cell is placed on battery test system and tests its room temperature charge-discharge performance, discharge and rechargeElectric current is 0.1C, and charging/discharging voltage scope is that 4.2V is to 1.5V (vs.N).
Fig. 1 is the first two circulation volume song of ten weeks of the sodium-ion battery positive electrode of embodiment 1Line. After tested, reversible specific discharge capacity is 138mAh/g first, after 20 circulations,Discharge capacity is 125mAh/g.
Comparative example 1
With embodiment 1, difference is: described MnSO4·H2O、FeSO4·H2O and NaFMol ratio be 1.5:1:5. Discovery can not make sodium-ion battery positive electrodeNaFe0.5Mn0.5SO4F。
Comparative example 2
With embodiment 1, difference is: described MnSO4·H2O、FeSO4·H2O and NaFMol ratio be 1:1.2:1. Discovery can not make sodium-ion battery positive electrodeNaFe0.5Mn0.5SO4F。
Comparative example 3
With embodiment 1, difference is: step 3) in, reaction temperature is 150 DEG C. Find notCan make sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
Comparative example 4
With embodiment 1, difference is: step 3) in, reaction temperature is 400 DEG C. Find notCan make sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
Embodiment 2
A preparation method for sodium-ion battery positive electrode, comprises the following steps:
1) accurately take appropriate MnSO4·4H2O solid, is mixed with saturated by deionized waterSolution seals in polytetrafluoroethyltank tank, is heated to 150 DEG C, is incubated 3 hours, adds suitableAmount ethanol, fully stirs, and obtains MnSO4·H2O solid;
2) accurately take appropriate FeSO4·7H2O solid, is mixed with saturated by deionized waterSolution, under high-purity argon gas protection, seals in polytetrafluoroethyltank tank, is heated to 280 DEG C, protectsTemperature 3 hours, adds appropriate ethanol, fully stirs, and obtains MnSO4·H2O solid;
3) by the MnSO of preparation4·H2O solid, MnSO4·H2O solid is pressed MnSO4·H2O：FeSO4·H2The ratio of O:NaF=1:1:2.5 (mol ratio), adds appropriate citric acid,Ultrasonic wave adds thermal response 4 hours in 320 DEG C after disperseing to mix under sealing state, uses CH2Cl2Washing, dry, obtain sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
Fig. 2 is the SEM figure of the sodium-ion battery positive electrode of embodiment 2.
Performance test:
The sodium-ion battery positive electrode NaFe of preparation0.5Mn0.5SO4F and acetylene black, polytetrafluoroEthene mixes by the mass ratio of about 85:10:5, is pressed into thickness is about 1 with film laminatorThe film of mm, is placed in baking oven and fully dries in 120 DEG C, and intercepting surface area is 1cm2'sCircular membrane, is compressed on stainless (steel) wire, makes Electrode.
Using Electrode as positive pole, taking sodium metal as to electrode, Celgard2300 micropore is poly-Propylene film is barrier film, to be dissolved in volume ratio as EC (ethylene carbonate)/DMC (1, the 2-of 1: 1Dimethyl carbonate) 1mol/LNaClO4For electrolyte, in the glove box that is full of argon gas, fillBe made into CR2032 type button cell.
Button cell is placed on battery test system and tests its room temperature charge-discharge performance, discharge and rechargeElectric current is 0.5C, and charging/discharging voltage scope is that 4.2V is to 1.5V (vs.N).
After tested, reversible specific discharge capacity is 121mAh/g first, after 20 circulations,Discharge capacity is 106mAh/g.
Embodiment 3
A preparation method for sodium-ion battery positive electrode, comprises the following steps:
1) accurately take appropriate MnSO4·4H2O solid, is mixed with saturated by deionized waterSolution seals in polytetrafluoroethyltank tank, is heated to 120 DEG C, is incubated 6 hours, adds suitableAmount ethanol, fully stirs, and obtains MnSO4·H2O solid;
2) accurately take appropriate FeSO4·7H2O solid, is mixed with saturated by deionized waterSolution, under high-purity argon gas protection, seals in polytetrafluoroethyltank tank, is heated to 220 DEG C, protectsTemperature 6 hours, adds appropriate ethanol, fully stirs, and obtains MnSO4·H2O solid;
3) by the MnSO of preparation4·H2O solid, MnSO4·H2O solid is pressed MnSO4·H2O：FeSO4·H2The ratio of O:NaF=1:1:2.5 (mol ratio), adds proper amount of glycol, superSound wave adds thermal response 8 hours in 260 DEG C after disperseing to mix under sealing state, uses CH2Cl2Washing, dry, obtain sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
Performance test:
The sodium-ion battery positive electrode NaFe of preparation0.5Mn0.5SO4F and acetylene black, polytetrafluoroEthene mixes by the mass ratio of about 85:10:5, is pressed into thickness is about 1 with film laminatorThe film of mm, is placed in baking oven and fully dries in 120 DEG C, and intercepting surface area is 1cm2'sCircular membrane, is compressed on stainless (steel) wire, makes Electrode.
Using Electrode as positive pole, taking sodium metal as to electrode, Celgard2300 micropore is poly-Propylene film is barrier film, to be dissolved in volume ratio as EC (ethylene carbonate)/DMC (1, the 2-of 1: 1Dimethyl carbonate) 1mol/LNaClO4For electrolyte, in the glove box that is full of argon gas, fillBe made into CR2032 type button cell.
Button cell is placed on battery test system and tests its room temperature charge-discharge performance, discharge and rechargeElectric current is 1.0C, and charging/discharging voltage scope is that 4.2V is to 1.5V (vs.N).
After tested, reversible specific discharge capacity is 114mAh/g first, after 20 circulations,Discharge capacity is 93mAh/g.
Embodiment 4
With embodiment 1, difference is: step 1) in, reaction temperature is 80 DEG C, when reactionBetween be 1.5h; Step 2) in, reaction temperature is 100 DEG C, the reaction time is 1.5h; Step3) in, described MnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is 1:1:2;Auxiliary agent is the mixture (volume ratio 1:1) of glycerine and citric acid; Reaction temperature is 200 DEG C,Reaction time is 10h.
After tested, performance is similar to Example 1.
Embodiment 5
With embodiment 1, difference is: step 1) in, reaction temperature is 200 DEG C, when reactionBetween be 8h; Step 2) in, reaction temperature is 300 DEG C, the reaction time is 7h; Step 3)In, described MnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is 1:1:4;Auxiliary agent is the mixture (volume ratio 1:2) of glycerine and ethylene glycol; Reaction temperature is 350 DEG C,Reaction time is 2h.
After tested, performance is similar to Example 1.
Obviously, the above embodiment of the present invention is only the act for clearly illustrating that the present invention doesExample, and be not the restriction to embodiments of the present invention, for the ordinary skill in affiliated fieldPersonnel, can also make other multi-form variation or change on the basis of the above descriptionMoving, cannot give all embodiments exhaustively here, everyly belong to technical side of the present inventionThe apparent variation that case is extended out or the still row in protection scope of the present invention of variation.
Claims (10)
1. a sodium-ion battery positive electrode, is characterized in that, described sodium-ion battery justUtmost point material consist of NaFe0.5Mn0.5SO4F。
2. the preparation method of sodium-ion battery positive electrode as claimed in claim 1, its spyLevy and be, by by MnSO4·H2O、FeSO4·H2O and NaF under the existence of auxiliary agent,Under sealing state, heat and react, obtain sodium-ion battery positive electrodeNaFe0.5Mn0.5SO4F；
Described auxiliary agent is water-soluble polyhydroxy organic matter;
Described MnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is 1:1:(2.0-4.0);
The reaction temperature of described reaction is 200-350 DEG C.
3. preparation method according to claim 2, is characterized in that, described inMnSO4·H2O、FeSO4·H2The mol ratio of O and NaF is 1:1:2.5.
4. preparation method according to claim 2, is characterized in that, described auxiliary agent isThe mixture of one or more in glycerine, citric acid, ethylene glycol.
5. preparation method according to claim 2, is characterized in that, described reactionReaction time is 2-10h.
6. preparation method according to claim 2, is characterized in that, described inMnSO4·H2O is by MnSO4·4H2O saturated solution heats under sealing state, Xiang QiIn add ethanol, stir, cooling, obtain MnSO4·H2O。
7. preparation method according to claim 6, is characterized in that, preparationMnSO4·H2Reaction temperature when O is 80-200 DEG C.
8. preparation method according to claim 2, is characterized in that, described in be byFeSO4·7H2O saturated solution heats under sealing state He in inert atmosphere protection, whereinAdd ethanol, stir, cooling, obtain FeSO4·H2O。
9. preparation method according to claim 8, is characterized in that, preparation FeSO4·H2OTime reaction temperature be 100-300 DEG C.
10. preparation method according to claim 2, is characterized in that, after having reacted,Use CH2Cl2Washing, dry, obtain sodium-ion battery positive electrode NaFe0.5Mn0.5SO4F。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110931784A (en) * | 2019-12-09 | 2020-03-27 | 苏州大学 | Iron-based sodium-ion battery positive electrode material and preparation method thereof |
| CN111063871A (en) * | 2019-12-09 | 2020-04-24 | 苏州大学 | Sodium ion full cell and preparation method thereof |
| CN115125069A (en) * | 2022-08-12 | 2022-09-30 | 芜湖天弋能源科技有限公司 | Acid washing detergent for positive electrode material of sodium-ion battery and application thereof |
| CN117239138A (en) * | 2023-11-15 | 2023-12-15 | 华北电力大学 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
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2016
- 2016-03-18 CN CN201610157842.7A patent/CN105591106A/en active Pending
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| PRABEER BARPANDA等: "Structural, Transport, and Electrochemical Investigation of Novel AMSO4F (A = Na, Li; M = Fe, Co, Ni, Mn) Metal Fluorosulphates Prepared Using Low Temperature Synthesis Routes", 《INORG. CHEM.》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110931784A (en) * | 2019-12-09 | 2020-03-27 | 苏州大学 | Iron-based sodium-ion battery positive electrode material and preparation method thereof |
| CN111063871A (en) * | 2019-12-09 | 2020-04-24 | 苏州大学 | Sodium ion full cell and preparation method thereof |
| CN110931784B (en) * | 2019-12-09 | 2020-11-24 | 苏州大学 | Iron-based sodium-ion battery positive electrode material and preparation method thereof |
| CN111063871B (en) * | 2019-12-09 | 2020-11-24 | 苏州大学 | Sodium ion full cell and preparation method thereof |
| CN115125069A (en) * | 2022-08-12 | 2022-09-30 | 芜湖天弋能源科技有限公司 | Acid washing detergent for positive electrode material of sodium-ion battery and application thereof |
| CN115125069B (en) * | 2022-08-12 | 2023-11-14 | 芜湖天弋能源科技有限公司 | Acid washing detergent for positive electrode material of sodium ion battery and application thereof |
| CN117239138A (en) * | 2023-11-15 | 2023-12-15 | 华北电力大学 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
| CN117239138B (en) * | 2023-11-15 | 2024-01-23 | 华北电力大学 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
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