CN103682244A - Surface coating method for electrode material of lithium ion battery - Google Patents
Surface coating method for electrode material of lithium ion battery Download PDFInfo
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- CN103682244A CN103682244A CN201310639258.1A CN201310639258A CN103682244A CN 103682244 A CN103682244 A CN 103682244A CN 201310639258 A CN201310639258 A CN 201310639258A CN 103682244 A CN103682244 A CN 103682244A
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- electrode material
- lithium
- acid
- coating method
- ion battery
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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
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
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Abstract
The invention provides a surface coating method for an electrode material of a lithium ion battery. The surface coating method comprises the steps: co-mixing a soluble or slightly soluble lithium salt and a titanium salt with the electrode material in a liquid phase, adding an acid as a hydrolysis inhibitor of the titanium salt, fully stirring evenly, then heating and drying, allowing the surface of the electrode material powder to be coated with a compound of lithium and titanium, then carrying out high temperature calcining in an air atmosphere at the temperature of 600-1300 DEG C, and directly synthesizing one layer of lithium metatitanate (Li2TiO3) on the surface layer of the electrode material powder. After a half battery synthesized by assembling the electrode material with the surface coated with Li2TiO3 is subjected to performance testing, the electrical conductivity is found to be increased, and the electrochemical performance at high magnification is excellent. Therefore, the surface coating method for the electrode material can effectively improve the performance of the electrode material, and has simple operation which is conducive to follow-up industrial applications.
Description
Technical field
The present invention relates to a kind of surface coating method of lithium ion battery electrode material, be specifically related to a kind of with metatitanic acid lithium to the coated mode in the surface of electrode material of secondary lithium ion battery.
Background technology
Lithium ion battery, as a kind of energy storage device of existing market share maximum, has accompanied the mankind to pass by nearly two more than ten years.Its advantage is energy density high (can reach 460-600 Wh/kg), long service life (can reach more than 6 years), stable performance etc., but in order to be applied to more areas, power-equipment for example, and lithium ion battery still has many technology require study and improve.The key factor that determines performance of lithium ion battery is its electrode material, and the positive electrode of current more use is cobalt acid lithium (LiCoO
2), LiMn2O4 (LiMn
2o
4), LiFePO4 (LiFePO
4) etc., the negative material of more use is carbon, graphite, lithium titanate (Li
4ti
5o
12) etc.In these electrode materials, all there is the defect of poorly conductive in many electrode materials, and especially the lithium ion conducting rate of material is low is the large problem that most electrode materials all have, and it has had a strong impact on the chemical property of electrode material under high magnification, for example LiMn
2o
4, LiFePO
4, Li
4ti
5o
12.
In order to overcome this defect, researchers have carried out much research, have used a series of improved procedure, comprise that particle nanometer, ion doping, surface are coated etc.Wherein, surface is coated by the coated one deck conductive materials of the electrode material surface at insulation or low electric conductivity, realizes the lifting of electrode material conductivity.The coated material in the surface of current more use is carbon, coated such as original position carbon, carbon nano-tube is coated, carbon nucleocapsid structure is coated etc.But the coated mode of this class is only just by promoting the electron conduction of electrode material and not improving the inner conductive of material, so its improvement in performance is not remarkable.
The invention provides a kind of with metatitanic acid lithium (Li
2tiO
3) method of coated lithium ion battery electrode material surface, on surface, form one deck Li
2tiO
3thereby, improve the ionic conductivity of electrode material and realize the charge/discharge capacity of electrode material under high magnification and the lifting of cyclical stability.
Summary of the invention
The object of the invention is to adopt a kind of new material---L
i2tiO
3the electrode material of poorly conductive is carried out to surface and be coated, be intended to improve the ionic conductivity of electrode material, thereby the chemical property of electrode material under high magnification is significantly improved.
A surface coating method for lithium ion battery electrode material, is characterized in that, take electrode material powder as the nuclei of condensation, and titanium salt is slowly hydrolyzed and generates TiO
2h
2o, on electrode material granules surface, adds appropriate solubility lithium salts simultaneously, then after calcining at its Surface Creation one deck Li
2tiO
3form full-package structure; This technique comprises the steps:
(1) absolute ethyl alcohol and deionized water are mixed to form to 500 milliliters of solution with 1:0～0.5, electrode material powder is dropped in this solution, by magnetic stirrer approximately 1 hour, obtain mixed liquor A;
(2) in mixed liquor A, according to mass ratio Li+Ti: electrode material=1:10～40, mol ratio Li:Ti=2～3:1, the slightly soluble or the soluble compound that add lithium and titanium, and to add acid be the hydrolysis inhibitor of titanium salt, magnetic agitation is 3～5 hours simultaneously, obtains mixed liquid B;
(3) get chelating agent and join in mixed liquid B, add ammoniacal liquor and regulate pH value to 7.0, heated at constant temperature at the temperature of 40～80 ℃ then, until obtain the presoma of gel state;
(4) presoma is put into baking oven, at 120～240 ℃ of temperature, dry, gained solid is ground to powder with mortar;
(5) powder of gained in (4) is put into Muffle furnace, calcine 5～15 hours under air conditions, heating rate is 1～15 ℃/min, and heated perimeter is 600～1300 ℃, obtains with Li
2tiO
3surface coated electrode material.
Described electrode material is the positive pole of lithium ion battery, or negative material, is LiMn2O4 (LiMn
2o
4), LiFePO4 (LiFePO
4), lithium manganese phosphate (LiMnPO
4), lithium titanate (Li
4ti
5o
12), LiNiPO (LiNiPO
4), cobalt phosphate lithium (LiCoPO
4), ternary material (LiCo
1/3ni
1/3mn
1/3o
2), titanium dioxide (TiO
2) in a kind of; The particle diameter of electrode material powder is 10～500 nm, and the concentration of electrode material in ethanol/water solution is 20～100 g/500 mL.
Described slightly soluble or soluble lithium compounds are a kind of in lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate, isopropyl lithium alkoxide, long-chain or short-chain alkyl lithium.
Described soluble titanium compound is a kind of in the chloride of tetra-n-butyl titanate, tetraisopropyl titanate, titanium.
Described hydrolysis inhibitor is organic acid, or inorganic acid, be specially a kind of in nitric acid, hydrochloric acid, acetic acid, tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid, caffeic acid or its combination, wherein ethanol/water solution and sour volume ratio are 1:0.01～0.1.
The present invention is directly coated on lithium and titanium salt after electrode material surface, by calcining directly, in electrode material surface, generates Li
2tiO
3.Li
2tiO
3li can be provided
+the three-dimensional channel of migration, improves the ionic conductivity of electrode material greatly, makes prepared electrode material still can obtain excellent chemical property under high magnification.Meanwhile, Li
2tiO
3even if still can keep the stability of structure in organic electrolyte, guaranteed coated Li
2tiO
3the stability of chemical property of electrode material.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1.
Fig. 2 is the SEM figure of the embodiment of the present invention 2.
Fig. 3 is the first charge-discharge specific capacity of the embodiment of the present invention 3.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiment 1:
By 20 g particle diameters, be the LiFePO of 10 nm
4drop in 500 mL absolute ethyl alcohols, with magnetic stirrer 1 h, obtain mixed liquor.11.03 g tetra-n-butyl titanates, 4.47 g lithium nitrates are added in mixed liquor, and add 5 mL red fuming nitric acid (RFNA)s as hydrolysis inhibitor, and 25.06 g citric acids, adding ammoniacal liquor adjusting pH value is 7.0, heated at constant temperature at the temperature of 40 ℃, simultaneously magnetic agitation 3 h.Again mixed liquor is put into baking oven, at 120 ℃ of temperature, dry.Gained solid is ground to powder with mortar.The powder of gained is put into Muffle furnace, and heating rate is 15 ℃/min, in air atmosphere, at 1300 ℃, calcines 5 hours, obtains with Li
2tiO
3surface coated electrode material.
Embodiment 2:
By 100 g particle diameters, be the Li of 250 nm
4ti
5o
12drop in the solution of 250 mL absolute ethyl alcohols and the configuration of 250 mL deionized waters, with magnetic stirrer 1 h, obtain mixed liquor.10.36 g tetraisopropyl titanates, 7.21 g lithium acetates are added in mixed liquor, and add 50 mL concentrated hydrochloric acids as hydrolysis inhibitor, and 23.54 g citric acids, adding ammoniacal liquor adjusting pH value is 7.0, heated at constant temperature at the temperature of 60 ℃, simultaneously magnetic agitation 5h.Again mixed liquor is put into baking oven, at 240 ℃ of temperature, dry.Gained solid is ground to powder with mortar.The powder of gained is put into Muffle furnace, and heating rate is 1 ℃/min, in air atmosphere, at 600 ℃, calcines 15 hours, obtains with Li
2tiO
3surface coated electrode material.
Embodiment 3:
By 60 g particle diameters, be the LiMnPO of 500 nm
4drop in the solution of 400 mL absolute ethyl alcohols and the configuration of 100 mL deionized waters, with magnetic stirrer 1 h, obtain mixed liquor.6.99 g titanium tetrachlorides, 3.90 g lithium chlorides are added in mixed liquor, and add 25 mL acetic acid as hydrolysis inhibitor, and 11.03 g ethylenediamine tetra-acetic acids, adding ammoniacal liquor adjusting pH value is 7.0, heated at constant temperature at the temperature of 80 ℃, simultaneously magnetic agitation 4 h.Again mixed liquor is put into baking oven, at 180 ℃ of temperature, dry.Gained solid is ground to powder with mortar.The powder of gained is put into Muffle furnace, and heating rate is 8 ℃/min, in air atmosphere, at 900 ℃, calcines 10 hours, obtains with Li
2tiO
3surface coated electrode material.
Embodiment 4:
By 80 g particle diameters, be the TiO of 200 nm
2drop in the solution of 300 mL absolute ethyl alcohols and the configuration of 200 mL deionized waters, with magnetic stirrer 1 h, obtain mixed liquor.17.09 g tetraisopropyl titanates, 6 g lithium carbonates are added in mixed liquor, and add 35 mL nitric acid as hydrolysis inhibitor, and 38.83 g citric acids, adding ammoniacal liquor adjusting pH value is 7.0, heated at constant temperature at the temperature of 70 ℃, simultaneously magnetic agitation 4h.Again mixed liquor is put into baking oven, at 200 ℃ of temperature, dry.Gained solid is ground to powder with mortar.The powder of gained is put into Muffle furnace, and heating rate is 7 ℃/min, in air atmosphere, at 1000 ℃, calcines 11 hours, obtains with Li
2tiO
3surface coated electrode material.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (5)
1. a surface coating method for lithium ion battery electrode material, is characterized in that, take electrode material powder as the nuclei of condensation, and titanium salt is slowly hydrolyzed and generates TiO
2h
2o, on electrode material granules surface, adds appropriate solubility lithium salts simultaneously, then after calcining at its Surface Creation one deck Li
2tiO
3form full-package structure; This technique comprises the steps:
(1) absolute ethyl alcohol and deionized water are mixed to form to 500 milliliters of solution with 1:0～0.5, electrode material powder is dropped in this solution, by magnetic stirrer approximately 1 hour, obtain mixed liquor A;
(2) in mixed liquor A, according to mass ratio Li+Ti: electrode material=1:10～40, mol ratio Li:Ti=2～3:1, the slightly soluble or the soluble compound that add lithium and titanium, and to add acid be the hydrolysis inhibitor of titanium salt, magnetic agitation is 3～5 hours simultaneously, obtains mixed liquid B;
(3) get chelating agent and join in mixed liquid B, add ammoniacal liquor and regulate pH value to 7.0, heated at constant temperature at the temperature of 40～80 ℃ then, until obtain the presoma of gel state;
(4) presoma is put into baking oven, at 120～240 ℃ of temperature, dry, gained solid is ground to powder with mortar;
(5) powder of gained in (4) is put into Muffle furnace, calcine 5～15 hours under air conditions, heating rate is 1～15 ℃/min, and heated perimeter is 600～1300 ℃, obtains with Li
2tiO
3surface coated electrode material.
2. a kind of surface coating method of lithium ion battery electrode material according to claim 1, is characterized in that the positive pole that described electrode material is lithium ion battery, or negative material are LiMn2O4 (LiMn
2o
4), LiFePO4 (LiFePO
4), lithium manganese phosphate (LiMnPO
4), lithium titanate (Li
4ti
5o
12), LiNiPO (LiNiPO
4), cobalt phosphate lithium (LiCoPO
4), ternary material (LiCo
1/3ni
1/3mn
1/3o
2), titanium dioxide (TiO
2) in a kind of; The particle diameter of electrode material powder is 10～500 nm, and the concentration of electrode material in ethanol/water solution is 20～100 g/500 mL.
3. a kind of surface coating method of lithium ion battery electrode material according to claim 1, it is characterized in that, described slightly soluble or soluble lithium compounds are a kind of in lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate, isopropyl lithium alkoxide, long-chain or short-chain alkyl lithium.
4. a kind of surface coating method of lithium ion battery electrode material according to claim 1, is characterized in that, described soluble titanium compound is a kind of in the chloride of tetra-n-butyl titanate, tetraisopropyl titanate, titanium.
5. a kind of surface coating method of lithium ion battery electrode material according to claim 1, it is characterized in that, described hydrolysis inhibitor is organic acid, or inorganic acid, be specially a kind of in nitric acid, hydrochloric acid, acetic acid, tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid, caffeic acid or its combination, wherein ethanol/water solution and sour volume ratio are 1:0.01～0.1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104022276A (en) * | 2014-06-09 | 2014-09-03 | 南京航空航天大学 | Clad modified layered cathode material of lithium-ion battery and preparation method of layered cathode material |
| CN105762339A (en) * | 2016-02-22 | 2016-07-13 | 中国科学技术大学 | Modified anode material and preparation method thereof |
| CN105789606A (en) * | 2016-04-28 | 2016-07-20 | 山东玉皇新能源科技有限公司 | Preparation method of lithium titanate coated lithium ion battery nickel cobalt manganese cathode material |
| CN109904403A (en) * | 2017-12-11 | 2019-06-18 | 河南科隆新能源股份有限公司 | A kind of anode material for lithium ion battery and preparation method thereof |
| CN110061223A (en) * | 2019-05-06 | 2019-07-26 | 合肥工业大学 | A method of lithium titanate, which is prepared, based on nearly Chemical Equilibria Systems coats nickelic tertiary cathode material |
| CN110350172A (en) * | 2019-07-05 | 2019-10-18 | 贵州大学 | A kind of metatitanic acid lithium cladding lithium titanate electrode material method |
| CN111129441A (en) * | 2018-10-30 | 2020-05-08 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material and preparation method thereof, lithium ion battery cathode and lithium ion battery |
| CN112635820A (en) * | 2020-12-18 | 2021-04-09 | 中国铝业股份有限公司 | Lithiation modified rod-like ceramic filler and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104022276A (en) * | 2014-06-09 | 2014-09-03 | 南京航空航天大学 | Clad modified layered cathode material of lithium-ion battery and preparation method of layered cathode material |
| CN105762339A (en) * | 2016-02-22 | 2016-07-13 | 中国科学技术大学 | Modified anode material and preparation method thereof |
| CN105789606A (en) * | 2016-04-28 | 2016-07-20 | 山东玉皇新能源科技有限公司 | Preparation method of lithium titanate coated lithium ion battery nickel cobalt manganese cathode material |
| CN109904403A (en) * | 2017-12-11 | 2019-06-18 | 河南科隆新能源股份有限公司 | A kind of anode material for lithium ion battery and preparation method thereof |
| CN111129441A (en) * | 2018-10-30 | 2020-05-08 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material and preparation method thereof, lithium ion battery cathode and lithium ion battery |
| CN111129441B (en) * | 2018-10-30 | 2021-06-18 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material, preparation method thereof, cathode and lithium ion battery |
| CN110061223A (en) * | 2019-05-06 | 2019-07-26 | 合肥工业大学 | A method of lithium titanate, which is prepared, based on nearly Chemical Equilibria Systems coats nickelic tertiary cathode material |
| CN110061223B (en) * | 2019-05-06 | 2020-10-23 | 合肥工业大学 | Method for preparing lithium titanate-coated high-nickel ternary cathode material based on near-chemical equilibrium system |
| CN110350172A (en) * | 2019-07-05 | 2019-10-18 | 贵州大学 | A kind of metatitanic acid lithium cladding lithium titanate electrode material method |
| CN112635820A (en) * | 2020-12-18 | 2021-04-09 | 中国铝业股份有限公司 | Lithiation modified rod-like ceramic filler and its preparation method and application |
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