CN103594716A - Method for preparing cathode material of sodium-ion battery, namely sodium vanadium fluorophosphates - Google Patents
Method for preparing cathode material of sodium-ion battery, namely sodium vanadium fluorophosphates Download PDFInfo
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- CN103594716A CN103594716A CN201310606880.2A CN201310606880A CN103594716A CN 103594716 A CN103594716 A CN 103594716A CN 201310606880 A CN201310606880 A CN 201310606880A CN 103594716 A CN103594716 A CN 103594716A
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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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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a method for preparing a cathode material of a sodium-ion battery, namely sodium vanadium fluorophosphates. The method comprises the following steps: using a vanadium source, a phosphorus source and a carbon source as main synthetic raw materials; dissolving into deionized water according to the molar ratio 1:1:1.2 of vanadium: phosphorus: carbon, heating in water bath, and continuously stirring to obtain light green pulp; after vacuum drying, grinding, then transferring into a tube furnace, preburning in an inert atmosphere at a certain temperature rise rate, cooling and then taking out to obtain black VPO4/C precursor powder; mixing the VPO4/C with NaF according to a stoichiometric ratio, ball-milling for 3 hours, sending into the tube furnace, then roasting in the inert atmosphere at the certain temperature rise rate, and cooling along with the furnace to obtain a positive active material NaVPO4F/C. According to the invention, cheap and easily-obtained pentavalent vanadium oxide or trivalent vanadium oxide is used as the main raw materials to prepare the sodium vanadium fluorophosphates cathode material through a sol gel activated auxiliary two-step high-temperature solid phase method, and the sodium vanadium fluorophosphates cathode material has the advantages of good stability, uniform particle size and good electrochemical performance. Meanwhile, the method has the advantages of simple synthesis process, short period and low cost and is convenient for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium, by collosol and gel, assist two sections of high temperature solid-state methods to prepare the method for sodium-ion battery positive electrode.The method belongs to new energy materials preparing technical field.
Background technology
At present, the research of high performance lithium ion battery and electrode material thereof is the focus of the area researches such as electrochemistry, materials chemistry, physics, and being all the sodium ion of periodic table of elements I main group and the character of lithium ion has many similarities, sodium ion is completely likely the same with lithium ion constructs a kind of widely used secondary cell.And sodium-ion battery is compared with lithium ion battery, and the cost of raw material is lower than lithium ion battery, and half-cell prtential is higher than lithium ion battery, be applicable to adopting the lower electrolyte of decomposition voltage, thereby security performance is better.
The vanadium phosphate sodium salt of mixing fluorine belongs to polyanion shaped material, and it has a kind of lattice structure that is different from Phosphoric Acid, and the two-dimensional channel of ionic conduction is provided, and is beneficial to the lifting of discharge stability and capacity.
Within 2002 .Barkert has synthesized the fluorophosphate compound (NaVPO for sodium-ion battery positive electrode first
4f).In the document, mention when doing negative material with lithium metal positive electrode NaVPO
4the charge and discharge specific capacity first of F is respectively 101mAh/g and 95mAh/g.And when doing negative pole with activated carbon, the charge and discharge specific capacity first of positive electrode is respectively 82mAh/g and 79mAh/g, discharge platform is 3.7V, and after 30 circulations of battery charging and discharging, capacity attenuation is to 50% original this NaVPO
4f material is likely as practical sodium-ion battery positive active material, but its structural stability and comprehensive electrochemical still need to be improved by suitable method.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium, adopt the methods such as sodium-ion battery positive electrode prepared by auxiliary two sections of high temperature solid-state methods and traditional high temperature solid-state method, spray drying process to compare, there is good dispersion, purity is high, dissolve fully, grain diameter evenly waits various features.
A preparation method for sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium, comprises the following steps:
(1) colloidal sol batch mixing: take pentavalent oxyvanadium compound, ammonium dihydrogen phosphate and reducing agent carbon source is raw material, by vanadium: phosphorus: the mol ratio 1:1:1.2 that goes back carbon is dissolved in 80mL deionized water, then be placed in the tank of 80 ℃ of constant temperature, stir 5-8h near dry to solution evaporation, the light green color slurry that obtains mixing;
(2) once calcining: slurry is dried in vacuum drying chamber, be then transferred in tube furnace, calcine in nitrogen atmosphere with certain programming rate, cooling rear taking-up, obtains VPO
4/ C presoma;
(3) secondary clacining: by VPO
4/ C mixes by stoichiometric proportion with NaF, and ball milling 3h sends in tube furnace, then with the roasting in nitrogen atmosphere of certain programming rate, with stove cooling, obtains positive active material NaVPO
4f/C.
Further, in described step, sodium source is one or more in sodium carbonate, sodium acid carbonate, sodium acetate, sodium nitrate, sodium fluoride;
Further, in described step, vanadium source is one or more in vanadic oxide, vanadium trioxide, vanadium dioxide, ammonium metavanadate;
Further, in described step, phosphorus source is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, triammonium phosphate, phosphorus pentoxide, phosphoric acid;
Further, in described step, fluorine source is one or more in sodium fluoride, ammonium fluoride, hydrofluoric acid;
Further, in described step, reducing agent carbon source is one or more in acetylene black, conductive black, Graphene, glucose, fructose, sucrose, soluble starch.
Further, in described step, once the temperature of calcining is 650 ℃-850 ℃, and the heat treated time is 2-10h.
Further, in described step, the temperature of secondary clacining is 650 ℃-850 ℃, and the heat treated time is 2-10h.
Further, in described step, inert gas is one or both mixing in argon gas, nitrogen, carbon monoxide, hydrogen.
The present invention be take pentavalent barium oxide cheap and easy to get or trivalent vanadium oxide and at 650-850 ℃, has been obtained fluorophosphoric acid vanadium sodium positive electrode as primary raw material activates auxiliary two step high temperature solid-state methods by collosol and gel, and has good chemical property; Synthesis technique is simple simultaneously, the cycle is short, cost is low, is convenient to large-scale production.
Accompanying drawing explanation
Fig. 1 is NaVPO prepared by the secondary clacining of embodiment 1 preparation
4the X-ray diffraction of F/C material (XRD) figure.
Fig. 2 is NaVPO prepared by the secondary clacining of embodiment 1 preparation
4the first charge-discharge figure of F/C material.
Fig. 3 is NaVPO prepared by the secondary clacining of embodiment 1 preparation
4the charge-discharge magnification curve chart of F/C material.
Embodiment
Be intended to by the following examples illustrate the present invention, rather than limitation of the invention further.
Embodiment 1:
(1) batch mixing: take pentavalent oxyvanadium compound, ammonium dihydrogen phosphate and carbon black is raw material, by vanadium: phosphorus: the mol ratio 1:1:1.2 of reducing agent carbon source element is dissolved in 80mL deionized water, then be placed in the tank of 80 ℃ of constant temperature, stir 6h near dry to solution evaporation, the light green color slurry that obtains mixing; (2) precalcining: slurry is dried in vacuum drying chamber, be then transferred in tube furnace, with the programming rates of 5 ℃ per minute 750 ℃ of preroast 5h in nitrogen atmosphere, cooling rear taking-up, obtains VPO
4/ C presoma; (3) secondary clacining: again by VPO
4/ C mixes by stoichiometric proportion with NaF, and ball milling 3h sends in tube furnace, then, with programming rate 750 ℃ of roasting 1h in nitrogen atmosphere of 5 ℃ per minute, with stove cooling, obtains positive active material NaVPO
4f/C.The X-ray diffraction analysis of products therefrom as shown in Figure 1.
Fluorophosphoric acid vanadium sodium target material, acetylene black and polytetrafluoroethylene (PTFE) binding agent of preparation are taken in the ratio of certain mass (85:5:10), put into small beaker, add appropriate absolute ethyl alcohol, after ultrasonic being uniformly dispersed, then stirring and mix well until reunite agglomerating with glass bar.The shape material of reunion is placed on glass plate and rolls and be pressed into film with glass bar, then with blunderbuss, film is made to disk, and be compressed on closely on aluminium foil with powder compressing machine, put into vacuum drying oven and take out and obtain positive plate in 120 ℃ of dry 12h.Using sodium metal sheet as negative pole, and microporous polypropylene membrane Celgard2400 is as barrier film, the NaClO that electrolyte is 1mol/L
4/ propene carbonate (PC) solution is assembled into CR2032 type button simulated battery in being full of the JMS-3X type glove box of argon gas.The simulated battery assembling at room temperature after standing 4-6h, is tested in 1.5-4.3V charging/discharging voltage scope.Test result shows: the first discharge capacity of material under the multiplying power of 0.05C is 112mAh/g, and the specific discharge capacity conservation rate from 0.05C to 0.2C is 62.6%, and occurs two constant voltage platforms near 3.7V and 3.25V voltage.The first charge-discharge curve of material and high rate performance curve are respectively as shown in Figure 2 and Figure 3.
Embodiment 2:(1) batch mixing: take trivalent vanadium oxygen compound, ammonium dihydrogen phosphate and soluble starch as raw material, by vanadium: phosphorus: the mol ratio 1:1:1.2 of reducing agent carbon source element is dissolved in 80mL deionized water, then be placed in the tank of 80 ℃ of constant temperature, stir 6h near dry to solution evaporation, the light green color slurry that obtains mixing; (2) precalcining: slurry is dried in vacuum drying chamber, be then transferred in tube furnace, with the programming rates of 5 ℃ per minute 650 ℃ of preroast 5h in nitrogen atmosphere, cooling rear taking-up, obtains VPO
4/ C presoma; (3) secondary clacining: again by VPO
4/ C mixes by stoichiometric proportion with NaF, and ball milling 3h sends in tube furnace, then, with programming rate 650 ℃ of roasting 1h in nitrogen atmosphere of 5 ℃ per minute, with stove cooling, obtains positive active material NaVPO
4f/C.Other steps are with embodiment 1.
Embodiment 3:(1) batch mixing: take pentavalent oxyvanadium compound, diammonium hydrogen phosphate and glucose as raw material, by vanadium: phosphorus: the mol ratio 1:1:1.2 of reducing agent carbon source element is dissolved in 80mL deionized water, then be placed in the tank of 80 ℃ of constant temperature, stir 6h near dry to solution evaporation, the light green color slurry that obtains mixing; (2) precalcining: slurry is dried in vacuum drying chamber, be then transferred in tube furnace, with the programming rates of 5 ℃ per minute 850 ℃ of preroast 5h in nitrogen atmosphere, cooling rear taking-up, obtains VPO
4/ C presoma; (3) secondary clacining: again by VPO
4/ C mixes by stoichiometric proportion with NaF, and ball milling 3h sends in tube furnace, then, with programming rate 850 ℃ of roasting 1h in nitrogen atmosphere of 5 ℃ per minute, with stove cooling, obtains positive active material NaVPO
4f/C.Other steps are with embodiment 1.
Claims (9)
1. a preparation method for sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium, is characterized in that, comprises following processing step:
(1) colloidal sol batch mixing: take pentavalent oxyvanadium compound, ammonium dihydrogen phosphate and reducing agent carbon source is raw material, by vanadium: phosphorus: the mol ratio 1:1:1.2 that goes back carbon is dissolved in 80mL deionized water, then be placed in the tank of 80 ℃ of constant temperature, stir 5-8h near dry to solution evaporation, the light green color slurry that obtains mixing;
(2) once calcining: slurry is dried in vacuum drying chamber, be then transferred in tube furnace, calcine in nitrogen atmosphere with certain programming rate, cooling rear taking-up, obtains VPO
4/ C presoma;
(3) secondary clacining: by VPO
4/ C mixes by stoichiometric proportion with NaF, and ball milling 3h sends in tube furnace, then with the roasting in nitrogen atmosphere of certain programming rate, with stove cooling, obtains positive active material NaVPO
4f/C.
2. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described sodium source is one or more in sodium carbonate, sodium acid carbonate, sodium acetate, sodium nitrate, sodium fluoride;
3. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described vanadium source is one or more in vanadic oxide, vanadium trioxide, vanadium dioxide, ammonium metavanadate;
4. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described phosphorus source is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, triammonium phosphate, phosphorus pentoxide, phosphoric acid;
5. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described fluorine source is one or more in sodium fluoride, ammonium fluoride, hydrofluoric acid;
6. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described reducing agent carbon source is one or more in acetylene black, conductive black, Graphene, glucose, fructose, sucrose, soluble starch.
7. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, described in it is characterized in that, once the temperature of calcining is 650 ℃-850 ℃, the heat treated time is 2-10h.
8. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described secondary clacining temperature is 650 ℃-850 ℃, and the heat treated time is 2-10h.
9. the preparation method of a kind of sodium-ion battery positive pole material fluorophosphoric acid vanadium sodium according to claim 1, is characterized in that described inert gas is one or both mixing in argon gas, nitrogen, carbon monoxide, hydrogen.
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| CN116995293A (en) * | 2023-09-27 | 2023-11-03 | 三一红象电池有限公司 | Sodium ion battery and preparation method thereof |
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