CN103928683B - The preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure - Google Patents
The preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure Download PDFInfo
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- CN103928683B CN103928683B CN201410179765.6A CN201410179765A CN103928683B CN 103928683 B CN103928683 B CN 103928683B CN 201410179765 A CN201410179765 A CN 201410179765A CN 103928683 B CN103928683 B CN 103928683B
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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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- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
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- 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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Abstract
The preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure, comprise the following steps: the ratio that lithium source, vanadium source, phosphorus source are 1:1:1 with the mol ratio of lithium ion, vanadium ion, phosphate anion by (1) mixes, soluble in water together with reducing agent; (2) regulate pH value of solution to 6-9; (3) solution is moved in autoclave, adds thermal response 10-72h in 200-400 DEG C, obtain homogeneous colloidal sol; (4) colloidal sol is taken out filtration, vacuum 60-120 DEG C of oven dry, obtains presoma; (5) presoma is placed in sintering furnace, under non-reducing atmosphere in 300-600 DEG C sintering 2-15h, subsequently under oxygen atmosphere in 200-400 DEG C of heat treatment 0.1-4.0h, finally naturally cool to room temperature.Material phosphoric acid vanadyl lithium of the present invention, core is LiVOPO
4, shell is the V with nano thickness
2o
5thin layer, structure is special, electrochemical performance.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium, particularly relate to a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure.
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, be there is by the inductive effect of polyanion higher charge and discharge platform (3.95VvsLi
+) and higher theoretical specific capacity (156mAh/g), energy density is 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, its lower electronic conductivity, seriously limits its chemical property when high rate charge-discharge.Due to LiVOPO
4sintering atmosphere general in atmosphere, chemical reaction is violent, makes traditional carbon coated lose meaning to the method improving electronic conductivity improving on this material.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure, to improve the chemical property of lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure, comprises the following steps:
(1) ratio being 1:1:1 by lithium source, vanadium source, phosphorus source with the mol ratio of lithium ion, vanadium ion, phosphate anion mixes, soluble in water together with reducing agent, controls the concentration of vanadium metal ion at 0.005-0.5molL
-1between; The mol ratio of described reducing agent and vanadium ion is 5-1:1;
(2) solution of step (1) gained is regulated pH to 6-9;
(3) solution of step (2) gained is moved in autoclave, adds thermal response 10-72h in 200-400 DEG C, obtain homogeneous colloidal sol;
(4) colloidal sol of step (3) gained is taken out filtration, vacuum 60-120 DEG C of oven dry, obtains LiVOPO
4presoma;
(5) presoma of step (4) gained is placed in sintering furnace, in 300-600 DEG C of sintering 2-15h under non-reducing atmosphere, subsequently under oxygen atmosphere in 200-400 DEG C of heat treatment 0.1-4.0h, finally naturally cool to room temperature, obtain the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure.
Further, in step (1), described lithium source is one or more in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, 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, vanadyl oxalate.
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-reducing atmosphere is argon gas, nitrogen, air or helium.
Vanadic oxide is a kind of layered oxide lithium ion battery anode material, though its voltage platform is low, its electronic conductivity is higher by (10
-2~ 10
-3and circulation ratio performance is all better than LiVOPO S/cm),
4positive electrode.Material is in the improvement of microstructure, Core-shell structure material has bilayer or sandwich construction, its inside and outside enrichment heterogeneity respectively, make the functional realiey compound of core and shell with complementary, the design concept of nucleocapsid structure is applied in lithium ion battery material by the present invention, by the stratiform V with nano thickness
2o
5be coated on LiVOPO uniformly
4electrode material is peripheral, improves its chemical property.
The present invention utilizes solwution method to prepare the lithium ion battery positive pole material phosphoric acid vanadyl lithium with nucleocapsid structure, and the core of gained Core-shell structure material is the LiVOPO with high electrochemical platform
4, the shell of Core-shell structure material is the V with nano thickness
2o
5thin layer, its conductivity is higher, and self has electro-chemical activity again, not only can improve the conductivity of material monolithic, and can provide more Lithium-ion embeding site, increases the energy density of material.
The lithium ion battery positive pole material phosphoric acid vanadyl lithium with nucleocapsid structure of the present invention's synthesis has good structural stability and excellent chemical property.
Accompanying drawing explanation
Fig. 1 is 0.05C, 0.1C, 1C first charge-discharge curve of gained sample in the embodiment of the present invention 1;
Fig. 2 is the cycle graph of the electrochemistry high rate performance of gained sample in the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Take lithium fluoride 0.01mol, vanadic oxide 0.005mol, diammonium hydrogen phosphate 0.01mol, citric acid 0.02mol, they are dissolved in the deionized water of 500mL together, form homogeneous blue solution, regulate the pH=7 of solution; Solution is gone in autoclave, add thermal response 12h in 250 DEG C, obtain homogeneous colloidal sol, gained colloidal sol is taken out and filters, by filtration product 80 DEG C of oven dry in vacuum drying oven; After oven dry powder is ground in agate mortar, be placed in sintering furnace, in air atmosphere in 450 DEG C of sintering 8h, then 350 DEG C of heat treatment 1h under oxygen atmosphere, finally naturally cool to room temperature, obtain the lithium ion battery positive pole material phosphoric acid vanadyl lithium with nucleocapsid structure that vanadic oxide is coated.
The assembling of battery: the lithium vanadyl phosphate anode material taking 0.24g gained, add 0.03gSuper-P and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, NMP dispersion mixing is added after abundant grinding, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, be negative pole with metal lithium sheet in anaerobism glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed its charge/discharge capacity and high rate performance in 2.0 ~ 4.5V voltage range, 0.05C, 0.1C, 1C first charge-discharge curve as shown in Figure 1, the cycle graph of electrochemistry high rate performance as shown in Figure 2,0.05C first discharge specific capacity is 144.6mAh/g, 0.1C first charge-discharge specific capacity be 143.5mAh/g, 1C first discharge specific capacity is 107mAh/g.
Embodiment 2
Take lithium hydroxide 0.02mol, vanadic oxide 0.01mol, diammonium hydrogen phosphate 0.02mol, citric acid 0.02mol, they are dissolved in the deionized water of 500mL together, form homogeneous green solution, regulate the pH=6 of solution; Solution is gone in autoclave, add thermal response 10h in 300 DEG C, obtain homogeneous colloidal sol; Gained colloidal sol is taken out and filters, by filtration product 120 DEG C of oven dry in vacuum drying oven; After oven dry powder is ground in agate mortar, be placed in sintering furnace, under an argon atmosphere in 500 DEG C of sintering 15h, then 200 DEG C of heat treatment 4h under oxygen atmosphere, finally naturally cool to room temperature, the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure must be had.
The assembling of battery: the lithium vanadyl phosphate anode material taking 0.24g gained, add 0.03gSuper-P and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, NMP dispersion mixing is added after abundant grinding, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, be negative pole with metal lithium sheet in anaerobism glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed its charge/discharge capacity and high rate performance in 2.0 ~ 4.5V voltage range, wherein 0.05C first electric specific capacity be 123.7mAh/g, 0.1C first discharge specific capacity is 119.5mAh/g, 1C first discharge specific capacity is 99.5mAh/g.
Embodiment 3
Take lithium fluoride 0.05mol, ammonium metavanadate 0.05mol, diammonium hydrogen phosphate 0.05mol, citric acid 0.2mol, they are dissolved in the deionized water of 2000mL together, form homogeneous green solution, regulate the pH=9 of solution; Then solution is gone in autoclave, add thermal response 72h in 200 DEG C, obtain anti-homogeneous colloidal sol; Gained colloidal sol is taken out and filters, by filtration product 60 DEG C of oven dry in vacuum drying oven; After oven dry powder is ground in agate mortar, be placed in sintering furnace, in air atmosphere in 300 DEG C of sintering 6h, then 400 DEG C of heat treatment 0.1h under oxygen atmosphere, finally naturally cool to room temperature, the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure must be had.
The assembling of battery: the lithium vanadyl phosphate anode material taking 0.24g gained, add 0.03gSuper-P and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, NMP dispersion mixing is added after abundant grinding, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, be negative pole with metal lithium sheet in anaerobism glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed its charge/discharge capacity and high rate performance in 2.0 ~ 4.5V voltage range, wherein 0.05C first discharge specific capacity is 133.2mAh/g, 0.1C first charge-discharge specific capacity is 137.5mAh/g, 1C first discharge specific capacity is 93.5mAh/g.
Embodiment 4
Take lithium nitrate 0.1mol, vanadic oxide 0.05mol, diammonium hydrogen phosphate 0.1mol, oxalic acid 0.3mol, they are dissolved in the deionized water of 1000mL together, form homogeneous blue solution, regulate the pH=8 of solution; Then solution is gone in autoclave, add thermal response 36h in 400 DEG C, obtain homogeneous colloidal sol; Gained colloidal sol is taken out and filters, by filtration product 80 DEG C of oven dry in vacuum drying oven; After oven dry powder is ground in agate mortar, be placed in sintering furnace, in a nitrogen atmosphere in 600 DEG C of sintering 2h, then 350 DEG C of heat treatment 2h under oxygen atmosphere, finally naturally cool to room temperature, obtain the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure.
The assembling of battery: the lithium vanadyl phosphate anode material taking the vanadic oxide finishing of 0.24g gained, add 0.03gSuper-P and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, NMP2mL dispersion mixing is added after abundant grinding, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, be negative pole with metal lithium sheet in anaerobism glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed its charge/discharge capacity and high rate performance in 2.0 ~ 4.5V voltage range, wherein 0.05C first discharge specific capacity is 117.6mAh/g, 0.1C first discharge specific capacity is 105.5mAh/g, 1C first discharge specific capacity is 83.5mAh/g.
Embodiment 5
Take lithium nitrate 0.05mol, vanadic oxide 0.025mol, diammonium hydrogen phosphate 0.05mol, oxalic acid 0.2mol, they are dissolved in the deionized water of 1500mL together, form homogeneous blue solution, regulate the pH=7 of solution; Then solution is gone in autoclave, add thermal response 20h in 270 DEG C, obtain homogeneous colloidal sol; Gained colloidal sol is taken out and filters, by filtration product 80 DEG C of oven dry in vacuum drying oven; After oven dry powder is ground in agate mortar, be placed in sintering furnace, in air atmosphere in 550 DEG C of sintering 18h, then 250 DEG C of heat treatment 1.5h under oxygen atmosphere, finally naturally cool to room temperature, obtain the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure.
The assembling of battery: the lithium ion battery positive pole material phosphoric acid vanadyl lithium taking the vanadic oxide finishing of 0.24g gained, add 0.03gSuper-P and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, NMP2mL dispersion mixing is added after abundant grinding, size mixing to after evenly on the thick aluminium foil of 16um slurry be made into positive plate, be negative pole with metal lithium sheet in anaerobism glove box, take Celgard2300 as barrier film, 1mol/LLiPF
6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025, battery is surveyed its charge/discharge capacity and high rate performance in 2.0 ~ 4.5V voltage range, wherein 0.05C first discharge specific capacity is 105.8mAh/g, 0.1C first discharge specific capacity is 98.6mAh/g, 1C first discharge specific capacity is 83.5mAh/g.
Claims (5)
1. a preparation method for the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure, is characterized in that, comprise the following steps:
(1) ratio being 1:1:1 by lithium source, vanadium source, phosphorus source with the mol ratio of lithium ion, vanadium ion, phosphate anion mixes, soluble in water together with reducing agent, controls the concentration of vanadium metal ion at 0.005-0.5molL
-1between; The mol ratio of described reducing agent and vanadium ion is 5-1:1;
(2) solution of step (1) gained is regulated pH to 6-9;
(3) solution of step (2) gained is moved in autoclave, adds thermal response 10-72h in 200-400 DEG C, obtain homogeneous colloidal sol;
(4) colloidal sol of step (3) gained is taken out filtration, vacuum 60-120 DEG C of oven dry, obtains LiVOPO
4presoma;
(5) presoma of step (4) gained is placed in sintering furnace, under non-reducing atmosphere in 300-600 DEG C sintering 2-15h, subsequently under oxygen atmosphere in 200-400 DEG C of heat treatment 0.1-4.0h, finally naturally cool to room temperature, obtaining shell is V
2o
5the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure;
In step (5), described non-reducing atmosphere is argon gas, nitrogen, air or helium.
2. the preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure according to claim 1, 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 hydroxide, lithium acetate, lithium chloride.
3. the preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure according to claim 1 and 2, it is characterized in that, in step (1), described vanadium source is one or more in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, vanadyl oxalate.
4. the preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure according to claim 1 and 2, it 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.
5. the preparation method of the lithium ion battery positive pole material phosphoric acid vanadyl lithium of nucleocapsid structure 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.
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CN106876669B (en) * | 2016-12-23 | 2019-10-18 | 山东精工电子科技有限公司 | A kind of crystallite LiVOPO4-LiMPO4-TiO2Complex lithium electric material and preparation method |
CN106654218A (en) * | 2017-01-11 | 2017-05-10 | 湖南文理学院 | Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and 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 |
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 |
CN113555537B (en) * | 2021-06-11 | 2024-02-23 | 惠州锂威新能源科技有限公司 | Positive electrode material, preparation method thereof, positive electrode plate and lithium ion battery |
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CN101734637A (en) * | 2008-11-20 | 2010-06-16 | 中国科学院理化技术研究所 | Preparation method of anode material vanadium-lithium phosphate powder for lithium ion battery |
CN102363523A (en) * | 2010-06-18 | 2012-02-29 | Tdk株式会社 | Active material, electrode containing same, lithium-ion secondary battery with electrode, and method of manufacturing active material |
US20130330261A1 (en) * | 2008-09-30 | 2013-12-12 | Tdk Corporation | Active material and positive electrode and lithium-ion second battery using same |
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US20130330261A1 (en) * | 2008-09-30 | 2013-12-12 | Tdk Corporation | Active material and positive electrode and lithium-ion second battery using same |
CN101734637A (en) * | 2008-11-20 | 2010-06-16 | 中国科学院理化技术研究所 | Preparation method of anode material vanadium-lithium phosphate powder for lithium ion battery |
CN102363523A (en) * | 2010-06-18 | 2012-02-29 | Tdk株式会社 | Active material, electrode containing same, lithium-ion secondary battery with electrode, and method of manufacturing active material |
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