CN103825027A - Preparation method of porous spherical positive material (lithium vanadyl phosphate) for lithium ion battery - Google Patents
Preparation method of porous spherical positive material (lithium vanadyl phosphate) for lithium ion battery Download PDFInfo
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- CN103825027A CN103825027A CN201410101030.1A CN201410101030A CN103825027A CN 103825027 A CN103825027 A CN 103825027A CN 201410101030 A CN201410101030 A CN 201410101030A CN 103825027 A CN103825027 A CN 103825027A
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- lithium
- ion battery
- vanadyl
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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 porous spherical positive material (lithium vanadyl phosphate) for a lithium ion battery. The preparation method comprises the steps of firstly, dissolving a lithium source, a vanadium source, a phosphorus source and a reducing agent into deionized water according to the molar ratio of lithium to vanadium to phosphorus to the reducing agent of 1:1:1:1-5; secondly, placing mixed liquid in a water bath kettle at 70-80 DEG C and stirring for 2-6h for forming solution; thirdly, regulating pH value of the solution to be 1-14; fourthly, drying and granulating the solution through a spraying and drying method; and fifthly, placing a lithium vanadyl phosphate precursor into a tubular sintering furnace and sintering at 300-600 DEG C for 6-10h in a non-reducing atmosphere. The positive material (lithium vanadyl phosphate) has high specific surface area, is beneficial to sufficient immersion of electrolyte, can shorten the ion transmission path and facilitates lithium ion transmission, and besides, the processability and the rate capability of the positive material are improved.
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 spray drying technology that adopts and prepare porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium (LiVOPO
4) method, belong to technical field of lithium ion.
Background technology
In recent years, many researcher's reports, polyanion type compound has good performance as anode material for lithium-ion batteries, very likely become anode material for lithium-ion batteries of new generation, especially transition metal phosphate, except current potential is high and ionic conductivity well, also show good electrochemical properties and thermal stability, wherein LiVOPO
4research get more and more people's extensive concerning.LiVOPO
4be a kind of Olivine-type Cathode Material in Li-ion Batteries, there is higher discharge platform (3.95Vvs Li/Li
+), theoretical specific capacity is 159mAh/g, its energy density compares LiFePO
4slightly high; And China's vanadium resource is abundant, reserves occupy third place in the world, and raw material wide material sources are with low cost; Therefore LiVOPO
4it is a high-voltage lithium ion positive electrode with very large potential value.
LiVOPO
4although have higher energy density, its electronic conductivity is lower, has seriously limited its chemical property in the time of large multiplying power discharging.CN101807691A and CN101841027A all disclose lithium position sodium-doped and rare-earth-doped modification LiVOPO
4to improve the method for its high rate performance, but it is only to improve material property from modification doping aspect, does not still have the LiVOPO of special microscopic appearance at present by preparation
4improve the report of its chemical property.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, and a kind of preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium simple to operate is provided, and the chemical property of gained vanadyl phosphate lithium is more excellent.
The technical scheme that the present invention solves its technical problem employing is that a kind of preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium, comprises the following steps:
(1) ratio that is 1:1:1:1-5 by lithium source, vanadium source, phosphorus source, reducing agent according to the mol ratio of elemental lithium, v element, P elements and reducing agent is dissolved in deionized water, and the concentration of controlling vanadium metal ion is 0.01-2molL
-1(preferably 0.05-1.5 molL
-1, more preferably 0.1-1 molL
-1, further preferred 0.2-0.3 molL
-1);
(2) step (1) gained mixed liquor is placed in to 70-80 ℃ of water-bath and stirs 2-6h, form solution;
(3) step (2) gained solution is regulated to no matter acidity or alkaline solution of pH to 1-14(, after being dried through spraying, all can obtain spherical vanadyl phosphate lithium presoma, but the output of acid-base pair vanadyl phosphate lithium has impact, acid mistake by force or alkaline mistake under strong condition, the amount of product is all less);
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, obtain vanadyl phosphate lithium (LiVOPO
4) presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, 300-600 ℃ of sintering 6-10h under irreducibility atmosphere, cool to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium (LiVOPO
4).
Further, described lithium source is the one in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride.
Further, described vanadium source is the one in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl.
Further, described phosphorus source is the one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
Further, described reducing agent is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
Further, in step (4), the dry intake air temperature of described spraying is at 200-260 ℃, and the dry peristaltic pump rotating speed of spraying is at 700-1800rpm/min, and spraying drying air fan rotating speed is at 40-150HZ.
Further, in step (5), described irreducibility atmosphere is the mist of argon gas, nitrogen, air or helium or non-reducing gas and inert gas.
The positive pole material phosphoric acid vanadyl lithium that the present invention prepares is through the HTHP of spray dryer, moment nucleation and follow-up cyclone collection product can form the uniform spherical presoma of pattern, due to vanadyl phosphate lithium sintering in oxidizing atmosphere, in course of reaction, there is carbon dioxide, the gases such as ammonia generate and discharge, therefore prepared vanadyl phosphate lithium material is that surface has the coated porous spherical particles of carbon, its porous spherical structure has higher specific area, be conducive to the abundant infiltration of electrolyte, can shorten ion transfer path, be conducive to the transmission of lithium ion, processing characteristics improves simultaneously, carbon-coating is coated on the surface of material, can improve the electron conduction of material, its special porous spherical microscopic appearance can improve the high rate performance of material greatly, the porous spherical anode material for lithium-ion batteries LiVOPO that uses the present invention to prepare
4there is good chemical property.
Accompanying drawing explanation
fig. 1 is the XRD figure of the embodiment of the present invention 1 gained porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium;
Fig. 2 is the SEM diffraction pattern of the embodiment of the present invention 1 gained porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium;
Fig. 3 is the 1C first charge-discharge curve chart that uses the assembled battery of the embodiment of the present invention 1 gained porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium institute.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.The embodiment of the present invention is used to provide a further understanding of the present invention, for explaining the present invention, but is not construed as limiting the invention.
Embodiment 1
The present embodiment comprises the following steps:
(1) take lithium nitrate 0.025mol, vanadic oxide 0.0125mol, ammonium dihydrogen phosphate 0.025mol, oxalic acid 0.035mol, is mixed, and is dissolved in the deionized water of 200mL;
(2) step (1) gained solution is placed in to 80 ℃ of thermostat water bath mechanical agitation 4h, forms blue solution;
(3) step (2) gained solution being regulated to pH is 7;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, described spraying is dry, and intake air temperature is 260 ℃, and peristaltic pump rotating speed is 1000rpm/min, and rotation speed of fan is 60HZ, obtains LiVOPO
4presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, under air atmosphere, in 450 ℃ of sintering 8h, is then naturally cooled to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: take the obtained vanadyl phosphate lithium anode material of 0.24g the present embodiment, 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 take metal lithium sheet as negative pole, take 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 discharge specific capacity is 151.3mAh/g, and 1C first discharge specific capacity is 130.4mAh/g.
The XRD of the present embodiment gained porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium schemes as shown in Figure 1; The SEM diffraction pattern of the present embodiment gained porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium as shown in Figure 2; The 1C first charge-discharge curve of the battery that the porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium that uses the present embodiment to prepare is assembled as shown in Figure 3.
Embodiment 2
The present embodiment comprises the following steps:
(1) take lithium carbonate 0.005mol, ammonium metavanadate 0.01mol, diammonium hydrogen phosphate 0.01mol, citric acid 0.02mol, is mixed, and is dissolved in the deionized water of 200mL;
(2) step (1) gained solution is placed in to 80 ℃ of thermostat water bath mechanical agitation 2h, forms homogeneous blue solution;
(3) step (2) gained solution is regulated to pH to 1;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, described spraying is dry: intake air temperature is 200 ℃, and peristaltic pump rotating speed is 1200rpm/min, and rotation speed of fan is under 80HZ, to spray to be dried, and obtains LiVOPO
4presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, under air atmosphere, in 350 ℃ of sintering 8h, is then naturally cooled to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the fluorophosphoric acid vanadium lithium anode material 0.24g that takes the present embodiment 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 take metal lithium sheet as negative pole, take 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 discharge specific capacity is 136.6mAh/g, and 1C first discharge specific capacity is 108.4mAh/g.
Embodiment 3
The present embodiment comprises the following steps:
(1) take lithium hydroxide 0.1mol, vanadic oxide 0.05mol, diammonium hydrogen phosphate 0.1mol, ethanedioic acid 0.5mol, is mixed, and is dissolved in the deionized water of 500mL;
(2) step (1) gained solution is placed in to 80 ℃ of water-bath mechanical agitation 6h, forms homogeneous blue solution;
(3) step (2) gained solution is regulated to pH to 9;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, described spraying is dry: intake air temperature is 220 ℃, and peristaltic pump rotating speed is 1800rpm/min, and rotation speed of fan is 100HZ, obtains LiVOPO
4presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, under air atmosphere, in 550 ℃ of sintering 9h, is then naturally cooled to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the fluorophosphoric acid vanadium lithium anode material 0.24g that takes the present embodiment 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 take metal lithium sheet as negative pole, take 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 discharge specific capacity is 137.2mAh/g, and 1C first discharge specific capacity is 104.6mAh/g.
Embodiment 4
The present embodiment comprises the following steps:
(1) take lithium fluoride 0.2mol, vanadium trioxide 0.1mol, diammonium hydrogen phosphate 0.2mol, oxalic acid 0.2mol, is mixed, and is dissolved in the deionized water of 200mL;
(2) step (1) gained solution is placed in to 80 ℃ of water-bath mechanical agitation 4h, forms homogeneous blue solution;
(3) step (2) gained solution is regulated to pH to 5;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, described spraying is dry: intake air temperature is 240 ℃, and peristaltic pump rotating speed is 700rpm/min, and rotation speed of fan is 40HZ, obtains LiVOPO
4presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, under air atmosphere, in 600 ℃ of sintering 6h, is then naturally cooled to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the fluorophosphoric acid vanadium lithium anode material 0.24g that takes the present embodiment 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 take metal lithium sheet as negative pole, take 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 discharge specific capacity is 137.6mAh/g, and 1C first discharge specific capacity is 105.5mAh/g.
Embodiment 5
The present embodiment comprises the following steps:
(1) take lithium chloride 0.05mol, vanadic oxide 0.025mol, diammonium hydrogen phosphate 0.05mol, ascorbic acid 0.2mol, is mixed, and is dissolved in the deionized water of 200mL;
(2) step (1) gained solution is placed in to 80 ℃ of thermostat water bath mechanical agitation 3h, forms homogeneous blue solution;
(3) step (2) gained solution is regulated to pH to 14;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, described spraying is dry: intake air temperature is 250 ℃, and peristaltic pump rotating speed is 1400rpm/min, and rotation speed of fan is 150HZ, obtains LiVOPO
4presoma;
(5) by step (4) gained vanadyl phosphate lithium (LiVOPO
4) presoma is placed in pipe type sintering furnace, under air atmosphere, in 300 ℃ of sintering 10h, is then naturally cooled to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
The assembling of battery: the fluorophosphoric acid vanadium 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 take metal lithium sheet as negative pole, take 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 103.8mAh/g, and 1C first discharge specific capacity is 68.6mAh/g.
Claims (7)
1. a preparation method for porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium, is characterized in that, comprises the following steps:
(1) ratio that is 1:1:1:1-5 by lithium source, vanadium source, phosphorus source, reducing agent according to the mol ratio of elemental lithium, v element, P elements and reducing agent is dissolved in deionized water, and the concentration of controlling vanadium metal ion is 0.01-2molL
-1;
(2) step (1) gained mixed liquor is placed in to 70-80 ℃ of water-bath and stirs 2-6h, form solution;
(3) step (2) gained solution is regulated to pH to 1-14;
(4) step (3) gained solution is carried out to drying-granulating by spray-dired method, obtain vanadyl phosphate lithium presoma;
(5) step (4) gained vanadyl phosphate lithium presoma is placed in to pipe type sintering furnace, 300-600 ℃ of sintering 6-10h under irreducibility atmosphere, cool to room temperature, obtains porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium.
2. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1, is characterized in that, in step (1), the concentration of controlling vanadium metal ion is 0.05-1.5 molL
-1.
3. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 2, is characterized in that, the concentration of controlling vanadium metal ion is 0.1-1 molL
-1.
4. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 3, is characterized in that, the concentration of controlling vanadium metal ion is 0.2-0.3 molL
-1.
5. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1, it is characterized in that, in step (1), described lithium source is the one in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride; Described vanadium source is the one in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl; Described phosphorus source is the one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid; Described reducing agent is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
6. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1, it is characterized in that, in step (4), the dry intake air temperature of described spraying is at 200-260 ℃, the dry peristaltic pump rotating speed of spraying is at 700-1800rpm/min, and spraying drying air fan rotating speed is at 40-150HZ.
7. the preparation method of porous spherical lithium ion battery positive pole material phosphoric acid vanadyl lithium according to claim 1, it is characterized in that, in step (5), described irreducibility atmosphere is the mist of argon gas, nitrogen, air or helium or non-reducing gas and inert gas.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104600253A (en) * | 2014-12-31 | 2015-05-06 | 北京鼎能开源电池科技股份有限公司 | Preparation method of ammonium oxovanadium phosphate crystals |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102034979A (en) * | 2009-09-29 | 2011-04-27 | Tdk株式会社 | Method of manufacturing active material and method of manufacturing lithium-ion secondary battery |
-
2014
- 2014-03-19 CN CN201410101030.1A patent/CN103825027A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN102034979A (en) * | 2009-09-29 | 2011-04-27 | Tdk株式会社 | Method of manufacturing active material and method of manufacturing lithium-ion secondary battery |
Non-Patent Citations (1)
| Title |
|---|
| BABOO JOSEPH PAUL ET AL.: "Enhanced storage capacities in carbon-coated triclinic-LiVOPO4 cathode with porous structure for Li-ion batteries.", 《ECS ELECTROCHEMISTRY LETTERS》, vol. 1, no. 4, 24 August 2012 (2012-08-24), pages 63 - 1 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104600253A (en) * | 2014-12-31 | 2015-05-06 | 北京鼎能开源电池科技股份有限公司 | Preparation method of ammonium oxovanadium phosphate crystals |
| 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 |
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