CN103972476A - Preparation method of positive electrode material, phosphoric acid oxygen vanadium lithium, of lithium ion battery - Google Patents
Preparation method of positive electrode material, phosphoric acid oxygen vanadium lithium, of lithium ion battery Download PDFInfo
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- CN103972476A CN103972476A CN201410207594.3A CN201410207594A CN103972476A CN 103972476 A CN103972476 A CN 103972476A CN 201410207594 A CN201410207594 A CN 201410207594A CN 103972476 A CN103972476 A CN 103972476A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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
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Abstract
The invention discloses a preparation method of a positive electrode material, phosphoric acid oxygen vanadium lithium, of a lithium ion battery. The preparation method comprises the following steps: (1) mixing a lithium source, a vanadium source and a phosphorus source in water according to the atom ratio of LiVOPO4, and adding a reduction agent to obtain a mixed solution; (2) stirring the mixed solution in thermostatic water bath at 60-100 DEG C; (3) regulating the pH to 6-9; (4) transferring the mixed solution into a vacuum freeze drier, and carrying out freeze drying on the mixed solution at -10 to -50 DEGC and with the vacuum degree of 5Pa-30Pa for 24-72 hours so as to obtain a phosphoric acid oxygen vanadium lithium precursor; and (5) taking out the phosphoric acid oxygen vanadium lithium precursor obtained in the step (4), uniformly grinding, pressing the ground phosphoric acid oxygen vanadium lithium precursor to obtain pieces, sintering the pieces in a tubular sintering furnace at 300-600 DEG C under a non-reducing atmosphere for 1-30 hours, and cooling to indoor temperature so as to obtain the positive electrode material, phosphoric acid oxygen vanadium lithium. The preparation method provided by the invention has the advantages that the positive electrode material, LiVOPO4, is prepared through a vacuum freeze drying technology, the preparation process is simple, and the operation is easy.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, especially relate to a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium.
Background technology
LiVOPO
4be a kind of Olivine-type Cathode Material in Li-ion Batteries, belong to phosphate-based positive electrode, at V
4+/ V
5+on the basis of oxidation-reduction pair, there is higher charge and discharge platform (3.95V vs Li by the inductive effect of polyanion
+) and higher theoretical specific capacity (156mAh/g), its energy density be 616Wh/Kg, higher than business-like lithium iron phosphate positive material (598Wh/Kg), and vanadyl phosphate lithium has advantages such as voltage platform is stable, Stability Analysis of Structures, fail safe is good, raw material is cheap, in the manufacture of lithium-ion-power cell, show larger potentiality.
LiVOPO
4although there is above advantage, the electronic conductivity that it is lower, has seriously limited its chemical property in the time of high rate charge-discharge.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, and the preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium that a kind of high rate performance is better, chemical property is more excellent is provided.
The technical scheme that the present invention solves its technical problem employing is that a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium, comprises the following steps:
(1) by lithium source, vanadium source, phosphorus source according to LiOVPO
4atom ratio be mixed in water, add reducing agent, the mol ratio of described reducing agent and vanadium ion is the preferred 2-8:1 of 1-10:1(), obtain mixed liquor; Control the concentration of metal ion in mixed liquor at 0.01-1mol L
-1(preferably 0.1-0.4 mol L
-1) between;
(2) step (1) gained mixed liquor is placed in to 60-100 DEG C of (preferably 80-90 DEG C) water bath with thermostatic control and stirs, form uniform solution, colloidal sol or suspension-turbid liquid;
(3) step (2) gained solution, colloidal sol or suspension-turbid liquid are regulated to pH to 6-9;
(4) step (3) gained solution, colloidal sol or suspension-turbid liquid being transferred in vacuum freeze drier, is that-10 DEG C ~-50 DEG C (preferably-30 DEG C ~-40 DEG C), vacuum degrees are freeze drying 24 ~ 72h under 5Pa ~ 30Pa in temperature, obtains vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is taken out, grinding is even, compressing tablet is placed in pipe type sintering furnace, in lower 300 DEG C ~ 600 DEG C preferred 6-10h of sintering 1-30h(of non-reduced atmosphere), cool to room temperature, obtains vanadyl phosphate lithium anode material.
Further, in step (1), described lithium source is one or more in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium chloride.
Further, in step (1), described vanadium source is one or more in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl.
Further, in step (1), described phosphorus source is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
Further, in step (1), described reducing agent is one or more in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
Further, in step (5), described non-reduced atmosphere is the one in argon gas, nitrogen, air, helium.
The prepared lithium ion battery positive pole material phosphoric acid vanadyl of the present invention lithium microscopic appearance is nano-sheet structure.Nano-sheet structure can shorten the evolving path of lithium ion, accelerates its diffusion rate, improves its high rate performance; Larger specific area can make active material fully contact with electrolyte, and can provide more lithium ion can embed site, and the chemical property of material is improved significantly.
The present invention utilizes Freeze Drying Technique to prepare lithium ion battery positive pole material phosphoric acid vanadyl lithium, and preparation process is simple, easy to operate, and products obtained therefrom microscopic appearance is to form by nanometer sheet is stacking, chemical property excellence.
Brief description of the drawings
Fig. 1 is the SEM diffraction pattern of gained lithium ion battery positive pole material phosphoric acid vanadyl lithium in the embodiment of the present invention 2;
Fig. 2 is the 1C first charge-discharge curve of gained lithium ion battery positive pole material phosphoric acid vanadyl lithium in the embodiment of the present invention 2.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) take lithium hydroxide 0.01mol, vanadic oxide 0.005mol, diammonium hydrogen phosphate 0.01mol, is dissolved in the deionized water of 300mL, adds citric acid 0.02mol, obtains mixed liquor;
(2) step (1) gained mixed liquor is placed in to 80 DEG C of water-baths, mechanical agitation is to forming homogeneous green solution;
(3) step (2) gained solution is regulated to pH=6;
(4) step (3) gained solution is transferred in vacuum freeze drier ,-30 DEG C, 5Pa freeze drying 24h, obtain vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is fully ground to uniform powder in agate mortar, compressing tablet is placed in pipe type sintering furnace, under air atmosphere, in 600 DEG C of sintering 6h, be then naturally cooled to room temperature, obtain lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the vanadyl phosphate lithium anode material that takes 0.24g gained, add 0.03g Super-P to make conductive agent and 0.03g PVDF(HSV-900) make binding agent, after fully grinding, add NMP to disperse to mix, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/L LiPF
6/ EC: DMC: EMC(volume ratio 1: 1: 1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed to its charge/discharge capacity and high rate performance in 3.0V～4.5V voltage range, and wherein 0.1C first discharge specific capacity is 140mAh/g, and 1C first discharge specific capacity is 112.8mAh/g.
Embodiment 2
The present embodiment comprises the following steps:
(1) take lithium nitrate 0.1mol, vanadic oxide 0.05mol, ammonium dihydrogen phosphate 0.1mol, is dissolved in the deionized water of 500mL, then adds oxalic acid 0.5mol, obtains mixed liquor;
(2) step (1) gained mixed liquor is placed in to 80 DEG C of waters bath with thermostatic control and stirs, form homogeneous blue solution;
(3) step (2) gained solution is regulated to pH=7;
(4) step (3) gained solution is transferred in vacuum freeze drier ,-50 DEG C, 15Pa freeze drying 36h, obtain vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is fully ground to uniform powder in agate mortar, compressing tablet is placed in pipe type sintering furnace, under air atmosphere, in 450 DEG C of sintering 10h, be then naturally cooled to room temperature, obtain lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the lithium ion battery positive pole material phosphoric acid vanadyl lithium that takes 0.24g gained, add 0.03g Super-P to make conductive agent and 0.03g PVDF(HSV-900) make binding agent, after fully grinding, add NMP 2mL to disperse to mix, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/L LiPF
6/ EC: DMC: EMC(volume ratio 1: 1: 1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed to its charge/discharge capacity and high rate performance in 3.0V～4.5V voltage range, and wherein 0.1C first discharge specific capacity is 146mAh/g, and 1C first discharge specific capacity is 130mAh/g.
Embodiment 3
The present embodiment comprises the following steps:
(1) take lithium fluoride 0.01mol, vanadic oxide 0.005mol, ammonium phosphate 0.01mol, is dissolved in the deionized water of 100mL, then adds citric acid 0.02mol, obtains mixed liquor;
(2) step (1) gained mixed liquor is placed in to 100 DEG C of water-baths, mechanical agitation is to forming homogeneous blue solution;
(3) step (2) gained solution is regulated to pH=9;
(4) step (3) gained solution is transferred in vacuum freeze drier ,-50 DEG C, 30Pa freeze drying 72h, obtain vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is fully ground to uniform powder in agate mortar, compressing tablet is placed in pipe type sintering furnace, under nitrogen atmosphere, in 350 DEG C of sintering 10h, be then naturally cooled to room temperature, obtain lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the vanadyl phosphate lithium anode material that takes 0.24g gained, add 0.03g Super-P to make conductive agent and 0.03g PVDF(HSV-900) make binding agent, after fully grinding, add NMP to disperse to mix, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/L LiPF
6/ EC: DMC: EMC(volume ratio 1: 1: 1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed to its charge/discharge capacity and high rate performance in 3.0V～4.5V voltage range, wherein 0.1C first charge-discharge specific capacity is 150.5mAh/g, and 1C first discharge specific capacity is 132mAh/g.
Embodiment 4
The present embodiment comprises the following steps:
(1) take lithium fluoride 0.01mol, ammonium metavanadate 0.01mol, diammonium hydrogen phosphate 0.01mol, is dissolved in the deionized water of 100mL, then adds citric acid 0.08mol, obtains mixed liquor;
(2) step (1) gained mixed liquor is placed in to 80 DEG C of water-baths, mechanical agitation is to forming homogeneous green solution;
(3) step (2) gained solution is regulated to pH=8;
(4) step (3) gained solution is transferred in vacuum freeze drier ,-40 DEG C, 15Pa freeze drying 48h, obtain vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is fully ground to uniform powder in agate mortar, compressing tablet is placed in pipe type sintering furnace, under air atmosphere, in 400 DEG C of sintering 24h, be then naturally cooled to room temperature, obtain lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the vanadyl phosphate lithium anode material that takes 0.24g gained, add 0.03g Super-P to make conductive agent and 0.03g PVDF(HSV-900) make binding agent, after fully grinding, add NMP to disperse to mix, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/L LiPF
6/ EC: DMC: EMC(volume ratio 1: 1: 1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed to its charge/discharge capacity and high rate performance in 3.0V～4.5V voltage range, wherein 0.1C first charge-discharge specific capacity is 148.5mAh/g, and 1C first discharge specific capacity is 131.5mAh/g.
Embodiment 5
The present embodiment comprises the following steps:
(1) take lithium nitrate 0.1mol, vanadic oxide 0.05mol, diammonium hydrogen phosphate 0.1mol, is dissolved in the deionized water of 2000mL, then adds oxalic acid 0.5mol, obtains mixed liquor;
(2) step (1) gained mixed liquor is placed in to 80 DEG C of water-bath mechanical agitation, forms homogeneous blue solution;
(3) step (2) gained solution is regulated to pH=7;
(4) step (3) gained solution is gone in vacuum freeze drier ,-30 DEG C, 20Pa freeze drying 36h, obtain vanadyl phosphate lithium presoma;
(5) vanadyl phosphate lithium presoma is fully ground to uniform powder in agate mortar, compressing tablet is placed in pipe type sintering furnace, under air atmosphere, in 550 DEG C of sintering 10h, be then naturally cooled to room temperature, obtain lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the vanadyl phosphate lithium anode material that takes 0.24g gained, add 0.03g Super-P to make conductive agent and 0.03g PVDF(HSV-900) make binding agent, after fully grinding, add NMP 2mL to disperse to mix, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/L LiPF
6/ EC: DMC: EMC(volume ratio 1: 1: 1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed to its charge/discharge capacity and high rate performance in 3.0V～4.5V voltage range, and wherein 0.1C first discharge specific capacity is 143.5mAh/g, and 1C first discharge specific capacity is 124mAh/g.
Reference examples (example 1 in CN103682339A)
Take vanadic oxide 1.22g, ammonium dihydrogen phosphate 15.42g, oxalic acid 2.6g, lithium hydroxide 1.00g and ascorbic acid 3.00g, be dissolved in the deionized water of 150mL, return stirring taking frequency as 40KHZ ultrasonic wave aid dispersion 4h in 60 DEG C of water-baths, obtains uniform solution; Get 45mL solution and be transferred to 100mL counteracting tank, in 250 DEG C clear up reaction 30h after naturally lower the temperature, after taking out, adopt three washing and filterings of deionized water, then adopt successively twice washing and filtering of ethanol, acetone, filter cake is placed in to 80 DEG C of dry 6h of vacuum drying chamber, obtains vanadyl phosphate lithium presoma, in 95%Ar+5%O2 atmosphere in 450 DEG C of sintering 1h, had the vanadyl phosphate lithium of " hollow ball " structure, particle diameter is 5 μ m-20 μ m.
The assembling of battery: the vanadyl phosphate lithium that takes 0.4g gained, add 0.05g conductive carbon black (Super-P) to make conductive agent and 0.05g PVDF(HSV900) make binding agent, after fully grinding, add 0.8g NMP to disperse to mix, slurry film-making on aluminium foil after sizing mixing evenly, in anaerobism glove box taking metal lithium sheet as negative pole, taking Celgard 2300 as barrier film, 1mol/LLiPF6/EC: DMC: EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, 0.1C first discharge specific capacity is 138.9mAh/g, after 50 circulations, capability retention is 86%, 1C first discharge specific capacity is 110.3mAh/g.
By obtaining in reference examples, the charge/discharge capacity of the prepared material of the present invention is higher than reference examples.The prepared nano-sheet vanadyl phosphate lithium of the present invention shows excellent chemical property, is mainly because the primary particle size of prepared material is nanoscale, can provide shorter the evolving path for the diffusion of lithium ion; Nano material has larger specific area can make active material and electrolyte fully infiltrate, and can provide and more can embed lithium ion site simultaneously.
Claims (10)
1. a preparation method for lithium ion battery positive pole material phosphoric acid vanadyl lithium, is characterized in that, comprises the following steps:
(1) by lithium source, vanadium source, phosphorus source according to LiOVPO
4atom ratio be mixed in water, add reducing agent, the mol ratio of described reducing agent and vanadium ion is 1-10:1, obtains mixed liquor; Control the concentration of metal ion in mixed liquor at 0.01-1mol L
-1between;
(2) step (1) gained mixed liquor is placed in to 60-100 DEG C of water bath with thermostatic control and stirs, form uniform solution, colloidal sol or suspension-turbid liquid;
(3) step (2) gained solution, colloidal sol or suspension-turbid liquid are regulated to pH to 6-9;
(4) step (3) gained solution, colloidal sol or suspension-turbid liquid being transferred in vacuum freeze drier, is that-10 DEG C ~-50 DEG C, vacuum degree are freeze drying 24 ~ 72h under 5Pa ~ 30Pa in temperature, obtains vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is taken out, grinding is even, compressing tablet is placed in pipe type sintering furnace, and in lower 300 DEG C ~ 600 DEG C sintering 1-30h of non-reduced atmosphere, cool to room temperature, obtains vanadyl phosphate lithium anode material.
2. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1, is characterized in that, in step (1), the mol ratio of described reducing agent and vanadium ion is 2-8:1.
3. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, is characterized in that, in step (1), the concentration of controlling metal ion in mixed liquor is 0.1-0.4 mol L
-1.
4. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, is characterized in that, in step (2), mixed liquor is placed in to 80-90 DEG C of water bath with thermostatic control and stirs.
5. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, is characterized in that, in step (4), vacuum freeze drying temperature is-30 DEG C ~-40 DEG C; In step (5), by vanadyl phosphate lithium presoma sintering 6-10h under non-reduced atmosphere.
6. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, it is characterized in that, in step (1), described lithium source is one or more in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, lithium chloride.
7. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2 is characterized in that, in step (1), described vanadium source is one or more in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl.
8. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, is characterized in that, in step (1), described phosphorus source is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
9. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, it is characterized in that, in step (1), described reducing agent is one or more in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
10. the preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1 and 2, is characterized in that, in step (5), described non-reduced atmosphere is the one in argon gas, nitrogen, air, helium.
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| CN106654186A (en) * | 2016-10-14 | 2017-05-10 | 南京工业大学 | Large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof |
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| CN107706380A (en) * | 2017-09-27 | 2018-02-16 | 郴州博太超细石墨股份有限公司 | A kind of method that phosphoric acid vanadium lithium/grapheme composite positive electrode material is prepared in Metal Substrate |
| CN107706379A (en) * | 2017-09-27 | 2018-02-16 | 郴州博太超细石墨股份有限公司 | A kind of preparation method of phosphoric acid vanadium lithium/graphene/carbon composite positive pole |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106654186A (en) * | 2016-10-14 | 2017-05-10 | 南京工业大学 | Large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof |
| CN106784809A (en) * | 2016-11-18 | 2017-05-31 | 山东精工电子科技有限公司 | A kind of LiVOPO4/LiMPO4/ C composite material of core-shell structure and preparation method |
| CN107845783A (en) * | 2017-09-15 | 2018-03-27 | 深圳市德方纳米科技股份有限公司 | Nanometer vanadyl phosphate lithium anode material and preparation method thereof, lithium ion battery |
| CN107845783B (en) * | 2017-09-15 | 2020-07-14 | 深圳市德方纳米科技股份有限公司 | Nano lithium vanadyl phosphate cathode material, preparation method thereof and lithium ion battery |
| CN107706380A (en) * | 2017-09-27 | 2018-02-16 | 郴州博太超细石墨股份有限公司 | A kind of method that phosphoric acid vanadium lithium/grapheme composite positive electrode material is prepared in Metal Substrate |
| CN107706379A (en) * | 2017-09-27 | 2018-02-16 | 郴州博太超细石墨股份有限公司 | A kind of preparation method of phosphoric acid vanadium lithium/graphene/carbon composite positive pole |
| CN107706380B (en) * | 2017-09-27 | 2020-06-12 | 郴州博太超细石墨股份有限公司 | Method for preparing lithium vanadium phosphate/graphene composite cathode material on metal base |
| CN108461740A (en) * | 2018-03-26 | 2018-08-28 | 西北工业大学 | A kind of LiVOPO4Nickelic tertiary cathode material of lithium ion battery of cladding and its preparation method and application |
| WO2023236595A1 (en) * | 2022-06-10 | 2023-12-14 | 广东邦普循环科技有限公司 | Method for preparing positive electrode material from waste livopo4 battery |
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Application publication date: 20140806 |