CN103996852A - Preparation method of novel nano lithium vanadium phosphate positive electrode material - Google Patents
Preparation method of novel nano lithium vanadium phosphate positive electrode material Download PDFInfo
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- CN103996852A CN103996852A CN201410230396.9A CN201410230396A CN103996852A CN 103996852 A CN103996852 A CN 103996852A CN 201410230396 A CN201410230396 A CN 201410230396A CN 103996852 A CN103996852 A CN 103996852A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—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
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of a novel nano lithium vanadium phosphate positive electrode material. The preparation method is characterized in that a precursor is prepared by combining a liquid phase method and a solid phase method. The preparation method comprises the steps of dissolving a vanadium source, a lithium source and a phosphorus source into deinoized water according to a given molar ratio, adding a small amount of a dispersing agent, namely polyethylene glycol (PEG), dropwise adding a certain amount of a complexing agent, namely ethylenediamine tetraacetic acid (EDTA), and continuously stirring the mixture to form a stable complex; transferring the obtained solution into a high-pressure reaction kettle to carry out hydrothermal reaction, and cooling a product to obtain the lithium vanadium phosphate precursor; calcining the obtained precursor in an inert environment at a high temperature, and cooling the precursor to obtain the carbon-coated nano lithium vanadium phosphate. The preparation method is simple, the reaction process is easy to control, and the prepared product has advantages of high crystallization degree, uniformity in granularity distribution, excellent electrochemical property and the like.
Description
Technical field
The invention belongs to technical field of lithium ion, relate in particular to a kind of preparation method of novel nano vanadium phosphate cathode material.
Background technology
Follow global warming, the problems such as traditional non-renewable energy resources shortage day by day serious, appearance that need a kind of novel Green Chemistry energy improves this situation.Lithium ion battery is high owing to having specific energy, the extensive concern have extended cycle life, environmental protection, the plurality of advantages such as safe and reliable enjoying countries in the world.Lithium ion battery has been widely used in portable set power supply, hybrid vehicle and large-scale energy storage device at present.
Anode material for lithium-ion batteries is key and the core of battery, studies at present more have cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4 and ternary material.Cobalt acid lithium is expensive and toxicity is large, and LiMn2O4 thermal stability is poor, and the synthesis step of lithium nickelate is loaded down with trivial details, and LiFePO4 specific capacity is low, and ternary material fail safe is poor, and phosphoric acid alum lithium anode material not only theoretical specific capacity up to 197mAh ﹒ g
-1, and Heat stability is good, can be in wider temperature range steady operation, therefore become the main direction of studying of Olivine-type Cathode Material in Li-ion Batteries.Research discovery, the phosphoric acid alum lithium of nanostructure has higher specific area, can provide more embedding-Tuo embedding passage for lithium ion; In addition, its unique nano-scale can shorten the diffusion length of lithium ion effectively, significantly improves the migration rate of lithium ion, thereby shows good chemical property.
In recent years, existing a large amount of report relates to the preparation method of phosphoric acid vanadium lithium, mainly contains high temperature solid-state method, carbothermic method and sol-gel process.Comparatively speaking, about hydro thermal method, prepare the report of phosphoric acid vanadium lithium fewer.Although phosphoric acid vanadium lithium process prepared by high temperature solid-state method is simple, its product particle size is larger, and chemical property is poor; Material tap density prepared by carbothermic method is lower; Although it is less that sol-gel process is prepared size, the good phosphoric acid alum of chemical property lithium, its synthesis technique is too complicated, and process is wayward, is not suitable for large-scale production.And the vanadium phosphate cathode material that hydro thermal method makes not only particle size distribution is even, Stability Analysis of Structures, and there is more excellent chemical property.Recently, researcher utilizes surfactant SDS (dodecyl sodium sulfate), prepares nanometer phosphoric acid vanadium lithium under hydrothermal condition.But the SDS post-processed of its use is more difficult, is not suitable for suitability for industrialized production.Nanometer phosphoric acid alum lithium preparation method involved in the present invention is simply efficient, consuming time shorter, and meets the requirement of Green Chemistry, and the product degree of crystallinity finally making is high, even particle size distribution, and chemical property is good.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of novel nano phosphoric acid alum lithium anode material, described method is for vanadium source, lithium source, phosphorus source are joined and obtain mixed liquor in deionized water according to certain molar ratio, then adds a certain amount of dispersant PEG, complexing agent EDTA to form uniform and stable solution in mixed liquor.By hydro-thermal reaction, prepare Powdered presoma, subsequently to its high-temperature calcination, obtain the coated nanometer phosphoric acid alum lithium material of carbon.Nanometer phosphoric acid alum lithium preparation method involved in the present invention is simply efficient, and product degree of crystallinity is high, even particle size distribution, and chemical property is good.
For achieving the above object, technical scheme of the present invention is as follows:
A preparation method for novel nano vanadium phosphate cathode material, is characterized in that: processing step is:
(1) vanadium source, lithium source, phosphorus source are dissolved in to deionized water under electric stirring, form solution
i, wherein the molar ratio in vanadium source, lithium source, phosphorus source is 2:3:3;
(2) to solution
iin add PEG, form solution
iI,wherein the molar ratio in PEG and lithium source is 0.02～0.1:1;
(3) to solution
iIin add EDTA, obtain solution
iII, lithium source and EDTA molar ratio are 3:1.0～3.5;
(4) by solution
iIIproceed to containing in teflon-lined autoclave, after hydro-thermal reaction 4～12 h of 150～190 ℃ of excess temperatures, obtain solution
iV;
(5) by solution
iVbe cooled to suction filtration after room temperature, gained filter cake grinds and obtains pulverous presoma after vacuumize 10 h under 80 ℃ of conditions;
(6) under the protection of inert gas, the Muffle furnace that Powdered presoma is placed in to 700～950 ℃ is calcined 7～12 h, can obtain nanometer phosphoric acid vanadium lithium after cooling.
According to the preparation method of described a kind of novel nano vanadium phosphate cathode material, described vanadium source is the mixture of a kind of in vanadic oxide, ammonium metavanadate or two kinds.
According to the preparation method of described a kind of novel nano vanadium phosphate cathode material, described lithium source is the mixture of a kind of in lithium hydroxide, lithium carbonate, lithium acetate or two kinds or three kinds.
According to the preparation method of described a kind of novel nano vanadium phosphate cathode material, described phosphorus source is the mixture of a kind of in phosphoric acid, ammonium dihydrogen phosphate or two kinds.
According to the preparation method of described a kind of novel nano vanadium phosphate cathode material, described PEG is polyethylene glycol, and its molecular weight is 2000.
According to described in a kind of preparation method of novel nano vanadium phosphate cathode material, described EDTA is ethylenediamine tetra-acetic acid.
According to the preparation method of described a kind of novel nano vanadium phosphate cathode material, the inert gas in step (6) is a kind of in nitrogen or argon gas.
The present invention has the following advantages:
(1) simple, the course of reaction of preparation method is easy to control, and meets the requirement of Green Chemistry, is applicable to large-scale industrialization and produces;
(2) the raw material wide material sources that the present invention relates to, cheap;
(3) dispersant PEG can improve the dispersiveness of lithium ion in solution, vanadium ion and phosphate radical effectively, reduces the generation of agglomeration;
(4) complexing agent EDTA can with lithium ion, vanadium ion and phosphate radical generation complex reaction in solution, be conducive to form uniform and stable phosphoric acid vanadium lithium presoma.In addition, EDTA can also provide coated carbon source for phosphoric acid vanadium lithium material, improves the conductivity of material;
(5) utilize hydro thermal method to prepare phosphoric acid alum lithium presoma, be conducive to form particle less, the product of even particle size distribution;
(6) the nanometer phosphoric acid alum lithium anode material Stability Analysis of Structures of preparing, degree of crystallinity is high, even particle size distribution, chemical property is good.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the sample of embodiment 1 preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph of the sample of embodiment 1 preparation.
Fig. 3 is the charge and discharge cycles resolution chart of the sample of embodiment 1 preparation.
Embodiment
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the invention will be further elaborated and explanation.
Embodiment 1
The preparation method of nanometer vanadium phosphate cathode material is as follows.
Take respectively 3.64 g vanadic oxides, 2.22g lithium carbonate and 2.94 g phosphoric acid, the inferior deionized water for stirring 1h that is added to 17.6g, the PEG2000 that adds subsequently 1.2g, stirring 0.5～1 h to PEG dissolves completely, the EDTA that adds again 10.23 g, electric stirring 1～2 H-shaped becomes uniform and stable solution.By solution go to 25 mL containing teflon-lined autoclave, 150 ℃ of insulation 12 h obtain phosphoric acid vanadium lithium precursor solution.Solid precursor after collecting is placed in to 950 ℃ of Muffle furnaces that are full of nitrogen, and calcining 7h obtains the coated nanometer phosphoric acid vanadium lithium material of carbon.
Nanometer phosphoric acid vanadium lithium material prepared by the present invention of take is example, and its structure is determined by X-ray diffractometer and scanning electron microscopy.As shown in Figure 1, what X ray diffracting spectrum demonstration obtained is the phosphoric acid vanadium lithium of pure phase, and crystallinity is better.As shown in Figure 2, nanometer phosphoric acid vanadium lithium particle has the pattern of homogeneous, and its diameter is 60～70 nanometers.The nanometer phosphoric acid vanadium lithium making of usining is made button cell as anode material for lithium-ion batteries, carries out the test of lithium ion battery charge-discharge performance.As shown in Figure 3, under the current density of 0.1C, the discharge capacity first of battery is up to 124 mAh/g, and after the charge-discharge test of 20 weeks, the capability retention of battery, up to 95%, shows good chemical property.
Embodiment 2
The preparation method of nanometer vanadium phosphate cathode material is as follows.
Take respectively deionized water for stirring 1 h that 3.64 g vanadic oxides, 2.22 g lithium carbonates and 2.94 g phosphoric acid are added to 17.6g successively, the PEG2000 that adds subsequently 6 g, stirring 0.5～1h to PEG dissolves completely, the EDTA that adds again 2.92g, electric stirring 1～2 H-shaped becomes uniform and stable solution.By solution go to 25 mL containing teflon-lined autoclave, 190 ℃ of insulation 4 h obtain phosphoric acid vanadium lithium precursor solution.Solid precursor after collecting is placed in to 700 ℃ of Muffle furnaces that are full of nitrogen, and calcining 12 h obtain the coated nanometer phosphoric acid vanadium lithium material of carbon.
The sample that the present embodiment is made carries out X-ray diffraction successively, the test of scanning electron microscopy and chemical property, and result shows: sample is the nanometer phosphoric acid vanadium lithium of single thing phase, its crystallinity is better, even particle size, diameter, in 70 nanometer left and right, has good chemical property simultaneously.
Claims (7)
1. a preparation method for novel nano vanadium phosphate cathode material, is characterized in that: processing step is:
(1) vanadium source, lithium source, phosphorus source are dissolved in to deionized water under electric stirring, form solution
i, wherein the molar ratio in vanadium source, lithium source, phosphorus source is 2:3:3;
(2) to solution
iin add PEG, form solution
iI,wherein the molar ratio in PEG and lithium source is 0.02～0.1:1;
(3) to solution
iIin add EDTA, obtain solution
iII, lithium source and EDTA molar ratio are 3:1.0～3.5;
(4) by solution
iIIproceed to containing in teflon-lined autoclave, after hydro-thermal reaction 4～12 h of 150～190 ℃ of excess temperatures, obtain solution
iV;
(5) by solution
iVbe cooled to suction filtration after room temperature, gained filter cake grinds and obtains pulverous presoma after vacuumize 10 h under 80 ℃ of conditions;
(6) under the protection of inert gas, the Muffle furnace that Powdered presoma is placed in to 700～950 ℃ is calcined 7～12 h, can obtain nanometer phosphoric acid vanadium lithium after cooling.
2. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: described vanadium source is the mixture of a kind of in vanadic oxide, ammonium metavanadate or two kinds.
3. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: described lithium source is the mixture of a kind of in lithium hydroxide, lithium carbonate, lithium acetate or two kinds or three kinds.
4. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: described phosphorus source is the mixture of a kind of in phosphoric acid, ammonium dihydrogen phosphate or two kinds.
5. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: described in step (2), PEG is polyethylene glycol, its molecular weight is 2000.
6. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: the described EDTA of step (3) is ethylenediamine tetra-acetic acid.
7. according to the preparation method of a kind of novel nano vanadium phosphate cathode material described in claims 1, it is characterized in that: the inert gas in step (6) is a kind of in nitrogen or argon gas.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104269530A (en) * | 2014-09-30 | 2015-01-07 | 中南大学 | Method for hydro-thermal synthesis of lithium iron phosphate-lithium vanadium phosphate composite material |
| CN104538626A (en) * | 2014-12-23 | 2015-04-22 | 山东精工电子科技有限公司 | Preparation method of cobalt-doped lithium vanadium phosphate positive material |
| CN106410157A (en) * | 2016-11-08 | 2017-02-15 | 桑顿新能源科技有限公司 | High-magnification long-service-life anode material and preparation method thereof |
| CN107093726A (en) * | 2017-05-02 | 2017-08-25 | 安庆师范大学 | A kind of method for improving lithium ion battery electrode material chemical property |
| CN111180716A (en) * | 2020-02-17 | 2020-05-19 | 成都其其小数科技有限公司 | Bismuth phosphate positive electrode material with good conductivity for lithium battery and preparation method |
| CN115483383A (en) * | 2022-09-30 | 2022-12-16 | 陕西科技大学 | Barium titanate coated ternary cathode material and preparation method and application thereof |
| CN117410579A (en) * | 2023-12-14 | 2024-01-16 | 湖南大学 | Preparation method and application of high-performance lithium ion battery for energy storage |
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| CN102447109A (en) * | 2011-12-10 | 2012-05-09 | 桂林理工大学 | Method for preparing lithium vanadium phosphate and lithium manganese phosphate composite anode material through rheological phase reaction |
| CN102738463A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source |
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2014
- 2014-05-28 CN CN201410230396.9A patent/CN103996852A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2009032808A1 (en) * | 2007-09-06 | 2009-03-12 | Valence Technology, Inc. | Method of making active materials for use in secondary electrochemical cells |
| CN102447109A (en) * | 2011-12-10 | 2012-05-09 | 桂林理工大学 | Method for preparing lithium vanadium phosphate and lithium manganese phosphate composite anode material through rheological phase reaction |
| CN102738463A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104269530A (en) * | 2014-09-30 | 2015-01-07 | 中南大学 | Method for hydro-thermal synthesis of lithium iron phosphate-lithium vanadium phosphate composite material |
| CN104538626A (en) * | 2014-12-23 | 2015-04-22 | 山东精工电子科技有限公司 | Preparation method of cobalt-doped lithium vanadium phosphate positive material |
| CN106410157A (en) * | 2016-11-08 | 2017-02-15 | 桑顿新能源科技有限公司 | High-magnification long-service-life anode material and preparation method thereof |
| CN107093726A (en) * | 2017-05-02 | 2017-08-25 | 安庆师范大学 | A kind of method for improving lithium ion battery electrode material chemical property |
| CN111180716A (en) * | 2020-02-17 | 2020-05-19 | 成都其其小数科技有限公司 | Bismuth phosphate positive electrode material with good conductivity for lithium battery and preparation method |
| CN115483383A (en) * | 2022-09-30 | 2022-12-16 | 陕西科技大学 | Barium titanate coated ternary cathode material and preparation method and application thereof |
| CN117410579A (en) * | 2023-12-14 | 2024-01-16 | 湖南大学 | Preparation method and application of high-performance lithium ion battery for energy storage |
| CN117410579B (en) * | 2023-12-14 | 2024-03-12 | 湖南大学 | Preparation method and application of high-performance lithium ion battery for energy storage |
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Application publication date: 20140820 |