CN104538626A - Preparation method of cobalt-doped lithium vanadium phosphate positive material - Google Patents
Preparation method of cobalt-doped lithium vanadium phosphate positive material Download PDFInfo
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- CN104538626A CN104538626A CN201410808014.6A CN201410808014A CN104538626A CN 104538626 A CN104538626 A CN 104538626A CN 201410808014 A CN201410808014 A CN 201410808014A CN 104538626 A CN104538626 A CN 104538626A
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- cobalt
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
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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 cobalt-doped lithium vanadium phosphate positive material. The preparation method comprises the following steps of: (1) dissolving a lithium source, a vanadium source, a phosphorus source and a cobalt source into deionized water according to the substance ratio of 3:2:3:(0.05-0.2) to form a solution A; (2) adding a complexing agent to the solution A according to the substance ratio of the complexing agent to the lithium source of 3:(1.0-3.5) while continuously stirring electrically to form a uniform solution B; (3) transferring the solution B into a high-pressure reaction kettle which contains a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 80-150 DEG C for 6-12 hours to obtain a solution C; (4) sequentially carrying out suction filtration and drying on a product contained in the solution C to obtain a cobalt-doped lithium vanadium phosphate precursor; (5) placing the cobalt-doped lithium vanadium phosphate precursor into a muffle furnace under the protection of an inert gas, and calcining at high temperature of 550-700 DEG C for 8-12 hours to obtain the cobalt-doped lithium vanadium phosphate positive material.
Description
Technical field
The present invention relates to a kind of technical field of lithium batteries, particularly relate to a kind of preparation method of vanadium phosphate cathode material of cobalt doped.
Background technology
As everyone knows, lithium battery has the advantages such as environmental protection, specific capacity are high, safe and reliable, memory-less effect.From the appearance of the first item commercial Li-ion battery nineties in last century, people are just to which creating keen interest.In recent decades, people deepen continuously for the theoretical research of lithium battery and commercial operations, and lithium electrical travelling industry obtains develop rapidly.At present, lithium battery has been widely used in hybrid vehicle, portable set and large-scale energy storage device.
Positive electrode is key and the core of lithium ion battery, and the performance that decide battery is good and bad.At present, on market, modal positive electrode mainly contains: the acid of LiFePO4, nickle cobalt lithium manganate, cobalt lithium, lithium nickelate, LiMn2O4.LiFePO 4 material specific capacity is lower; Nickel-cobalt lithium manganate material fail safe is poor; Cobalt acid lithium material is expensive; Lithium nickelate materials synthesis difficulty; Lithium manganate material poor heat stability.At present, lithium vanadium phosphate material is because specific capacity is up to 197mAh ﹒ g
-1, the cheap and better heat stability of the prices of raw and semifnished materials, obtains the extensive concern of researcher.But simple lithium vanadium phosphate material conductivity is poor, limit its application in field of batteries.Research finds, the coated conductivity waiting modifying and decorating means significantly can increase lithium vanadium phosphate material of adulterating, makes it have higher specific discharge capacity and more stable cycle performance.
Summary of the invention
The object of this invention is to provide a kind of can increase lithium vanadium phosphate material conductivity, improve specific discharge capacity and strengthen the preparation method of the vanadium phosphate cathode material of the cobalt doped of cycle performance.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of vanadium phosphate cathode material of cobalt doped, it is characterized in that: comprise the following steps: lithium source, vanadium source, phosphorus source, cobalt source are 3:2:3:(0.05-0.2 according to thing mass ratio by (1)) ratio be dissolved in deionized water, form solution A; (2) continuing under electric stirring, is 3:(1.0 ~ 3.5 by complexing agent according to the ratio with above-mentioned lithium source substance amount) ratio add above-mentioned solution A, form homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 6 ~ 12h of 80 ~ 150 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 550 ~ 700 DEG C of high-temperature calcination 8 ~ 12 h, obtain the vanadium phosphate cathode material of cobalt doped.
In the method, comprise the following steps: the ratio that lithium source, vanadium source, phosphorus source, cobalt source are 3:2:3:0.1 according to thing mass ratio by (1) is dissolved in deionized water, form solution A; (2), under continuing electric stirring, complexing agent is added above-mentioned solution A according to the ratio that the ratio with above-mentioned lithium source substance amount is 3:2, forms homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 10h of 100 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 600 DEG C of high-temperature calcination 10 h, obtain the vanadium phosphate cathode material of cobalt doped.
In the method, described lithium source is lithium hydroxide, lithium carbonate, lithium acetate a kind of monomer wherein or the mixture of a few person.
In the method, described vanadium source is vanadic oxide, ammonium metavanadate a kind of monomer wherein or both mixtures.
In the method, described phosphorus source is one or several mixture of phosphoric acid, ammonium dihydrogen phosphate.
In the method, described cobalt source is cobalt acetate.
In the method, described complexing agent is glycine, ethylenediamine tetra-acetic acid, one or several mixture tartaric.
In the method, described inert gas is nitrogen, the one of argon gas or two kinds of mists.
Advantageous effect of the present invention is: preparation method's environmental protection of (1) material, and synthesis technique is simple and be easy to operation and control, and this be that the production application of reality provides stronger operability, is convenient to large-scale industrial production;
(2) lithium source, vanadium source, phosphorus source and cobalt source can combine by complexing agent effectively, this presoma for acquisition stable homogeneous provides favourable condition, and in addition, complexing agent is after high-temperature calcination, formed at material surface and stabilize carbon coating layer, enhance the conductivity of material;
(3) material utilizing hydro thermal method obtained has the advantages such as Stability Analysis of Structures, particle diameter are less, has excellent specific discharge capacity and cycle performance simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the vanadium phosphate cathode material of cobalt doped prepared by specific embodiment 1;
Fig. 2 is the cycle performance curve of the vanadium phosphate cathode material of cobalt doped prepared by specific embodiment 2.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
As shown in Figure 1, 2, a kind of preparation method of vanadium phosphate cathode material of cobalt doped, is characterized in that: comprise the following steps in the present invention:
(1) be 3:2:3:(0.05-0.2 by lithium source, vanadium source, phosphorus source, cobalt source according to thing mass ratio) ratio be dissolved in deionized water, form solution A; (2) continuing under electric stirring, is 3:(1.0 ~ 3.5 by complexing agent according to the ratio with above-mentioned lithium source substance amount) ratio add above-mentioned solution A, form homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 6 ~ 12h of 80 ~ 150 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 550 ~ 700 DEG C of high-temperature calcination 8 ~ 12 h, obtain the vanadium phosphate cathode material of cobalt doped.
In the present embodiment, comprise the following steps: the ratio that lithium source, vanadium source, phosphorus source, cobalt source are 3:2:3:0.1 according to thing mass ratio by (1) is dissolved in deionized water, form solution A; (2), under continuing electric stirring, complexing agent is added above-mentioned solution A according to the ratio that the ratio with above-mentioned lithium source substance amount is 3:2, forms homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 10h of 100 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 600 DEG C of high-temperature calcination 10 h, obtain the vanadium phosphate cathode material of cobalt doped.In the present embodiment, described lithium source is lithium hydroxide, lithium carbonate, lithium acetate a kind of monomer wherein or the mixture of a few person.In the present embodiment, described vanadium source is vanadic oxide, ammonium metavanadate a kind of monomer wherein or both mixtures.In the present embodiment, described phosphorus source is one or several mixture of phosphoric acid, ammonium dihydrogen phosphate.In the present embodiment, described cobalt source is cobalt acetate.In the present embodiment, described complexing agent is glycine, ethylenediamine tetra-acetic acid, one or several mixture tartaric.In the present embodiment, described inert gas is nitrogen, the one of argon gas or two kinds of mists.
Embodiment 1
The preparation method of the vanadium phosphate cathode material of cobalt doped: take 2.21 g lithium carbonates respectively; 2.33 g ammonium metavanadate; the ammonium dihydrogen phosphate of 3.45 g and the cobalt acetate of 0.059 g; be dissolved in after mixing in deionized water; the glycine of 0.25g is added wherein under mechanical agitation; proceed in the autoclave of polytetrafluoro liner after dissolving completely and react 6h at 150 DEG C; suction filtration; drying obtains the phosphoric acid vanadium lithium presoma of cobalt doped; this presoma is placed in the Muffle furnace under nitrogen protection, and 550 DEG C of calcining 12h obtain the lithium vanadium phosphate material of cobalt doped.
The sample topography that above-mentioned steps obtains is as Fig. 1, can find out that from scanning electron microscope (SEM) photograph the lithium vanadium phosphate material particle diameter of obtained cobalt doped is less, larger grain diameter is at about 1-1.5um, less grain diameter is at below 1um, reach Nano grade, therefore battery can have excellent chemical property; Using the active material making button cell of the lithium vanadium phosphate material of obtained cobalt doped as anode material of lithium battery, the discharge cycles curve of battery is as Fig. 2, and the first discharge specific capacity of battery reaches 162mAhg
-1, after 50 circulations, the specific discharge capacity of battery remains on 150.1 mAhg
-1, conservation rate is 92.6%, has shown comparatively stable chemical property.
Embodiment 2
The preparation method of the vanadium phosphate cathode material of cobalt doped: take 1.25 g lithium hydroxides respectively; 3.64 g vanadic oxide; the phosphoric acid of 2.94g and the cobalt acetate of 2.35 g; be dissolved in after mixing in deionized water; the tartaric acid of 5.25g is added wherein under mechanical agitation; proceed in the autoclave of polytetrafluoro liner after dissolving completely and react 12h at 80 DEG C; suction filtration; drying obtains the phosphoric acid vanadium lithium presoma of cobalt doped; this presoma is placed in the Muffle furnace under nitrogen protection, and 700 DEG C of calcining 8h obtain the lithium vanadium phosphate material of cobalt doped.
Carry out scanning electron microscopic observation to the lithium vanadium phosphate material of obtained cobalt doped, result shows, and the particle of this material is less, particle diameter is at about 1um, make button cell with this material, test result shows, the material that this embodiment obtains has higher specific discharge capacity and stable cycle performance equally.
Claims (8)
1. a preparation method for the vanadium phosphate cathode material of cobalt doped, is characterized in that: comprise the following steps:
(1) be 3:2:3:(0.05-0.2 by lithium source, vanadium source, phosphorus source, cobalt source according to thing mass ratio) ratio be dissolved in deionized water, form solution A; (2) continuing under electric stirring, is 3:(1.0 ~ 3.5 by complexing agent according to the ratio with above-mentioned lithium source substance amount) ratio add above-mentioned solution A, form homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 6 ~ 12h of 80 ~ 150 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 550 ~ 700 DEG C of high-temperature calcination 8 ~ 12 h, obtain the vanadium phosphate cathode material of cobalt doped.
2. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 1, it is characterized in that: comprise the following steps: the ratio that lithium source, vanadium source, phosphorus source, cobalt source are 3:2:3:0.1 according to thing mass ratio by (1) is dissolved in deionized water, form solution A; (2), under continuing electric stirring, complexing agent is added above-mentioned solution A according to the ratio that the ratio with above-mentioned lithium source substance amount is 3:2, forms homogeneous solution B; (3) above-mentioned solution B is proceeded in the autoclave containing polytetrafluoro liner, obtain solution C through the hydro-thermal reaction 10h of 100 DEG C; (4) product in above-mentioned solution C is carried out suction filtration successively, dry, obtain the presoma of the phosphoric acid vanadium lithium of cobalt doped; (5) under inert gas shielding, above-mentioned presoma is placed in Muffle furnace, 600 DEG C of high-temperature calcination 10 h, obtain the vanadium phosphate cathode material of cobalt doped.
3. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 2, it is characterized in that: described lithium source is lithium hydroxide, lithium carbonate, lithium acetate a kind of monomer wherein or the mixture of a few person.
4. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 3, it is characterized in that: described vanadium source is vanadic oxide, ammonium metavanadate a kind of monomer wherein or both mixtures.
5. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 4, it is characterized in that: described phosphorus source is one or several mixture of phosphoric acid, ammonium dihydrogen phosphate.
6. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 5, it is characterized in that: described cobalt source is cobalt acetate.
7. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 6, it is characterized in that: described complexing agent is glycine, ethylenediamine tetra-acetic acid, one or several mixture tartaric.
8. according to the preparation method of the vanadium phosphate cathode material of a kind of cobalt doped described in claims 7, it is characterized in that: described inert gas is nitrogen, the one of argon gas or two kinds of mists.
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Cited By (6)
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| CN105036103A (en) * | 2015-08-03 | 2015-11-11 | 山东威能环保电源科技股份有限公司 | Preparation method of cuboid lithium battery anode lithium ferric manganese phosphate material |
| CN105552358A (en) * | 2016-02-03 | 2016-05-04 | 三峡大学 | Preparation method of chromium-doped Li<3>VO<4>/C anode material for lithium-ion battery |
| CN106169570A (en) * | 2016-08-25 | 2016-11-30 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of doped with metal elements lithium ion battery vanadium phosphate cathode material |
| CN106450297A (en) * | 2016-10-11 | 2017-02-22 | 安徽师范大学 | Nearly cubic lithium vanadium phosphate and preparation method thereof, lithium-ion battery and positive electrode of lithium-ion battery |
| CN108493449A (en) * | 2018-03-20 | 2018-09-04 | 苏州大学 | A kind of method of controllable preparation manganese fluorophosphate sodium positive electrode |
| CN110668505A (en) * | 2019-09-24 | 2020-01-10 | 烟台大学 | Cobalt-containing two-dimensional accordion-shaped nanosheet material and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036103A (en) * | 2015-08-03 | 2015-11-11 | 山东威能环保电源科技股份有限公司 | Preparation method of cuboid lithium battery anode lithium ferric manganese phosphate material |
| CN105036103B (en) * | 2015-08-03 | 2017-08-01 | 山东威能环保电源科技股份有限公司 | A kind of preparation method of cuboid-type anode material of lithium battery lithium ferric manganese phosphate |
| CN105552358A (en) * | 2016-02-03 | 2016-05-04 | 三峡大学 | Preparation method of chromium-doped Li<3>VO<4>/C anode material for lithium-ion battery |
| CN106169570A (en) * | 2016-08-25 | 2016-11-30 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of doped with metal elements lithium ion battery vanadium phosphate cathode material |
| CN106450297A (en) * | 2016-10-11 | 2017-02-22 | 安徽师范大学 | Nearly cubic lithium vanadium phosphate and preparation method thereof, lithium-ion battery and positive electrode of lithium-ion battery |
| CN106450297B (en) * | 2016-10-11 | 2019-08-13 | 安徽师范大学 | Nearly cube phosphoric acid vanadium lithium and preparation method thereof, lithium ion battery and its anode |
| CN108493449A (en) * | 2018-03-20 | 2018-09-04 | 苏州大学 | A kind of method of controllable preparation manganese fluorophosphate sodium positive electrode |
| CN110668505A (en) * | 2019-09-24 | 2020-01-10 | 烟台大学 | Cobalt-containing two-dimensional accordion-shaped nanosheet material and preparation method and application thereof |
| CN110668505B (en) * | 2019-09-24 | 2022-04-26 | 烟台大学 | Cobalt-containing two-dimensional accordion-shaped nanosheet material and preparation method and application thereof |
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Application publication date: 20150422 |