CN108075122A - A kind of preparation method of lithium ion battery composite cathode material - Google Patents
A kind of preparation method of lithium ion battery composite cathode material Download PDFInfo
- Publication number
- CN108075122A CN108075122A CN201711338809.5A CN201711338809A CN108075122A CN 108075122 A CN108075122 A CN 108075122A CN 201711338809 A CN201711338809 A CN 201711338809A CN 108075122 A CN108075122 A CN 108075122A
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- Prior art keywords
- lithium ion
- ion battery
- lithium
- citric acid
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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
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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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- 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 present invention provides a kind of preparation method of lithium ion battery composite cathode material, by using Li1.3Ti1.7Al0.3(PO4)3Coating modification is carried out to lithium ion cell positive with carbon, effectively increases the electrical conductivity and high rate performance of lithium ion battery.Li1.3Ti1.7Al0.3(PO4)3It is a kind of lithium fast-ionic conductor, can effectively shortens the transmission range of lithium ion in positive electrode, improves the electrical conductivity of lithium ion in composite positive pole, and then improve the charge-discharge magnification performance of lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery composite cathode material.
Background technology
At present, lithium ion battery is widely used to the electronic equipments such as mobile phone, notebook, digital camera and electric vehicle
On, as market increasingly increases the demand of lithium ion battery, to lithium ion battery in charge-discharge velocity, security performance and cycling
Requirement in performance is also higher and higher.
Anode material for lithium-ion batteries has vital influence to the performance of lithium battery, at present, common lithium-ion electric
Pond positive electrode there are stability of material in cyclic process it is poor, with electrolyte occur side reaction, high rate performance is bad the problems such as, table
It is one of current most effective method of modifying that bread, which covers,.However, traditional positive electrode surface cladding generally use single substance,
Such as carbon coating, although electronic conductivity can be improved, ionic conductivity cannot be improved；In addition, common covering material is such as
ZrO2、MgO、V2O5、Al2O3Metal oxides is waited not have lithium ion conduction characteristic, abjection and insertion of the clad to lithium ion
Process has certain inhibition.
The content of the invention
The present invention for background technology there are the defects of, it is proposed that a kind of preparation side of lithium ion battery composite cathode material
Method.The present invention uses Li1.3Ti1.7Al0.3(PO4)3With carbon to lithium ion cell positive carry out coating modification, effectively increase lithium from
The electrical conductivity and high rate performance of sub- battery.
Technical scheme is as follows：
A kind of preparation method of lithium ion battery composite cathode material, specifically includes following steps：
Step 1, according to molar ratio Li：Al：Ti：P=1.3：0.3：1.7：3 ratio weighs lithium source, Al sources, Ti sources and phosphorus
Source；
Step 2 adds in citric acid in ethylene glycol, stirs evenly, preparation obtains the ethylene glycol solution of citric acid；
Step 3 adds in the Ti sources that step 1 weighs in the ethylene glycol solution for the citric acid that step 2 is prepared, at 60~90 DEG C
Under be uniformly mixed, obtain mixed liquor A；
Step 4 adds in citric acid in deionized water, prepares and obtains the citric acid that mass fraction is 60wt%~90wt%
Aqueous solution；Then lithium source, Al sources and phosphorus source step 1 weighed is added in the aqueous citric acid solution prepared, and is stirred evenly, is obtained
Mixed liquid B；
Step 5, under conditions of stirring, mixed liquid B that step 4 is prepared is added in the mixed liquor A that step 3 is prepared, so
0.5~2h is stirred at 40~70 DEG C afterwards, obtains colloidal sol；
Step 6, according to mass ratio Ti sources：Organic carbon source：Anode active material of lithium ion battery=1：(1~5)：(10~
300) ratio adds in anode active material of lithium ion battery and organic carbon source in the colloidal sol obtained to step 5, then using super
After 0.5~1.5h of sound cell crushing instrument ultrasonic disperse, it is heated to 100~200 DEG C and 1~2h is kept at 100~200 DEG C, with
Water removal and ethylene glycol equal solvent are removed, forms gel；Wherein, the ultrasonic power of ultrasonic cell disintegration instrument is 400~500W；
Step 7, the gel for obtaining step 6 are placed in silica crucible, are then placed in tube furnace in inert gas atmosphere
Under be warming up to 400~500 DEG C and keep 4~8h, then cool to room temperature with the furnace, take out, obtained product is ground to powder shaped；
Then obtained powder is placed in tube furnace, is warming up to 700~900 DEG C and keeps 2~3h, after the completion of reaction, furnace cooling
To room temperature, take out, you can obtain the lithium ion battery composite cathode material.
Further, lithium source described in step 1 for lithium carbonate, lithium acetate, lithium hydroxide, lithium nitrate, lithium sulfate, lithia,
One or more in lithium fluoride；The Ti sources are butyl titanate or isopropyl titanate；Phosphorus source is ammonium dihydrogen phosphate or phosphorus
Sour diammonium hydrogen；The Al sources are aluminum nitrate, ANN aluminium nitrate nonahydrate or aluminium hydroxide.
Further, in the ethylene glycol solution of citric acid described in step 2 citric acid mass concentration for 0.08g/mL~
0.2g/mL。
Further, the molar ratio of Ti sources and citric acid is 1 in step 3：(2~5).
Further, the mass ratio of lithium source described in step 4 and citric acid is 1：(0.5~20).
Further, anode active material of lithium ion battery described in step 6 is cobalt acid lithium, lithium nickelate, LiMn2O4, nickel mangaic acid
One or more in the positive electrodes such as lithium, nickle cobalt lithium manganate, LiFePO4.
Further, organic carbon source described in step 6 is glucose, in sucrose, phenolic resin, epoxy resin, polyethylene
It is one or more.
Beneficial effects of the present invention are：
The present invention provides a kind of preparation method of lithium ion battery composite cathode material, by using Li1.3Ti1.7Al0.3
(PO4)3Coating modification is carried out to lithium ion cell positive with carbon, effectively increases the electrical conductivity and high rate performance of lithium ion battery.
Li1.3Ti1.7Al0.3(PO4)3It is a kind of lithium fast-ionic conductor, can effectively shortens the transmission range of lithium ion in positive electrode, carry
The electrical conductivity of lithium ion in high composite positive pole, and then improve the charge-discharge magnification performance of lithium ion battery.
Description of the drawings
Fig. 1 is the lithium ion battery composite cathode material and uncoated LiCoO that the embodiment of the present invention obtains2Positive electrode
Assemble the high rate performance test curve of obtained lithium ion battery；
Fig. 2 is the lithium ion battery composite cathode material and uncoated LiCoO that the embodiment of the present invention obtains2Positive electrode
Assemble the EIS figures of obtained lithium ion battery.
Specific embodiment
With reference to the accompanying drawings and examples, technical scheme is described in detail.
Embodiment
A kind of preparation method of cobalt acid lithium composite positive pole, specifically includes following steps：
Step 1, with Ti (OC4H9)4、LiNO3·H2O、Al(NO3)3·9H2O and NH4H2PO4For raw material, according to
Li1.3Ti1.7Al0.3(PO4)3Stoichiometric ratio, weigh 5.786g Ti (OC4H9)4, 0.897g LiNO3·H2O,1.126gAl
(NO3)3·9H2O and 3.451gNH4H2PO4；
Step 2 first adds in 8g citric acids in 100mL ethylene glycol, stirs evenly, obtains the ethylene glycol solution of citric acid；
Then 5.786gTi (OC step 1 weighed4H9)4It adds in the ethylene glycol solution for the citric acid prepared, is stirred at 90 DEG C
2h treats that white insoluble matter is completely dissolved, obtains mixed liquor A；
Step 3 adds in 15g citric acids in 20mL distilled water, and preparation obtains the aqueous citric acid solution of saturation, stirs evenly
Afterwards, 0.897gLiNO step 1 weighed3·H2O、1.126gAl(NO3)3·9H2O and 3.451gNH4H2PO4Add in saturation
It in aqueous citric acid solution, stirs evenly, obtains mixed liquid B；
Step 4, under conditions of stirring, mixed liquid B that step 3 is prepared is added in the mixed liquor A that step 2 is prepared,
1h is stirred at 70 DEG C, obtains colloidal sol；
65.31g anode active material of lithium ion battery LiCoO is added in step 5, the colloidal sol obtained in step 42With
9.116g organic carbon source sucrose, then using ultrasonic cell disintegration instrument ultrasonic disperse 1.5h after, be heated to 150 DEG C and at 150 DEG C
Lower holding 2h to remove water removal and ethylene glycol equal solvent, forms gel；Wherein, the ultrasonic power of ultrasonic cell disintegration instrument is 500W；
Step 6, the gel for obtaining step 5 are placed in silica crucible, are then placed in tube furnace and are risen under an argon atmosphere
Temperature is to 500 DEG C and keeps 8h, then cools to room temperature with the furnace, takes out, and obtained product is ground to powder shaped；Then will obtain again
Powder be placed in tube furnace, be warming up to 700 DEG C under an argon atmosphere and keep 2h, after the completion of reaction, cool to room temperature with the furnace,
It takes out, you can obtain the cobalt acid lithium composite positive pole.
The lithium ion battery composite cathode material that embodiment is obtained and traditional anode active material of lithium ion battery
LiCoO2Lithium ion battery is assembled, is tested for the property comparison.Fig. 1 is that the lithium ion battery that the embodiment of the present invention obtains is compound just
Pole material and uncoated LiCoO2The high rate performance test curve for the lithium ion battery that positive electrode assembles；It can by Fig. 1
Know, under 3V~4.5V, 0.2C, 0.5C, 1C, 2C difference discharge-rate, the battery of embodiment anode composite assembling, discharge ratio
Capacity is above the battery of traditional anode assembling, shows using Li1.3Ti1.7Al0.3(PO4)3With carbon to lithium ion cell positive into
Row coating modification effectively improves the high rate performance of lithium cobaltate cathode material under high voltages.
Fig. 2 is the lithium ion battery composite cathode material and uncoated LiCoO that the embodiment of the present invention obtains2Positive electrode
Obtained lithium ion battery is assembled under 3V~4.5V, 0.2C charge-discharge magnifications, the energy Qwest figure EIS figures after one circle of Xun Huan.
As shown in Figure 2, the value of X-axis (real impedance) is corresponded at first semicircle inflection point and lithium ion passes through active material particle in Fig. 2
The diffusive migration of surface insulation layer is related, this process can use a RSEI/CSEIParallel circuit represents (RSEIIt is moved for lithium ion diffusion
The resistance of SEI films is crossed by Mobile Communication), lithium ion passes through SEI films in the lithium ion battery of composite positive pole that embodiment obtains assembling
Resistance reduce, show that composite positive pole provided by the invention can effectively improve the ionic conductivity of interface.
Claims (5)
1. a kind of preparation method of lithium ion battery composite cathode material, comprises the following steps：
Step 1, according to molar ratio Li：Al：Ti：P=1.3：0.3：1.7：3 ratio weighs lithium source, Al sources, Ti sources and phosphorus source；
Step 2 adds in citric acid in ethylene glycol, stirs evenly, preparation obtains the ethylene glycol solution of citric acid；
Step 3 adds in the Ti sources that step 1 weighs in the ethylene glycol solution for the citric acid that step 2 is prepared, and is stirred at 60~90 DEG C
It mixes uniformly mixed, obtains mixed liquor A；
Step 4 adds in citric acid in deionized water, and it is water-soluble that preparation obtains the citric acid that mass fraction is 60wt%~90wt%
Liquid；Then lithium source, Al sources and phosphorus source step 1 weighed is added in the aqueous citric acid solution prepared, and is stirred evenly, is mixed
Liquid B；
Step 5, under conditions of stirring, mixed liquid B that step 4 is prepared is added in the mixed liquor A that step 3 is prepared, Ran Hou
0.5~2h is stirred at 40~70 DEG C, obtains colloidal sol；
Step 6, according to mass ratio Ti sources：Organic carbon source：Anode active material of lithium ion battery=1：(1~5)：(10~300)
Ratio, anode active material of lithium ion battery and organic carbon source are added in the colloidal sol obtained to step 5, it is then thin using ultrasound
After born of the same parents crush 0.5~1.5h of instrument ultrasonic disperse, it is heated to 100~200 DEG C and 1~2h is kept at 100~200 DEG C, formed solidifying
Glue；Wherein, the ultrasonic power of ultrasonic cell disintegration instrument is 400~500W；
Step 7, the gel for obtaining step 6 are placed in tube furnace, are warming up to 400~500 DEG C under inert gas atmosphere and are protected
4~8h is held, then cools to room temperature with the furnace, is taken out, obtained product is ground to powder shaped；Then obtained powder is placed in pipe
In formula stove, it is warming up to 700~900 DEG C and keeps 2~3h, after the completion of reaction, cool to room temperature with the furnace, take out, you can obtain institute
State lithium ion battery composite cathode material.
2. the preparation method of lithium ion battery composite cathode material according to claim 1, which is characterized in that step 2 institute
The mass concentration for stating citric acid in the ethylene glycol solution of citric acid is 0.08g/mL~0.2g/mL；Ti sources and citric acid in step 3
Molar ratio be 1：(2~5).
3. the preparation method of lithium ion battery composite cathode material according to claim 1, which is characterized in that step 4 institute
The mass ratio for stating lithium source and citric acid is 1：(0.5~20).
4. the preparation method of lithium ion battery composite cathode material according to claim 1, which is characterized in that step 6 institute
Anode active material of lithium ion battery is stated as in cobalt acid lithium, lithium nickelate, LiMn2O4, nickel ion doped, nickle cobalt lithium manganate, LiFePO4
One or more.
5. the preparation method of lithium ion battery composite cathode material according to claim 1, which is characterized in that step 6 institute
Organic carbon source is stated as the one or more in glucose, sucrose, phenolic resin, epoxy resin, polyethylene.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807902A (en) * | 2018-06-12 | 2018-11-13 | 奇瑞汽车股份有限公司 | A kind of lithium sulfur battery anode material and preparation method thereof |
| CN109088061A (en) * | 2018-08-02 | 2018-12-25 | 成都宏焘新材料有限公司 | A kind of modified nickle cobalt lithium manganate electrode material and preparation method thereof |
| CN110858643A (en) * | 2018-08-24 | 2020-03-03 | 湖南杉杉新能源有限公司 | Fast ion conductor modified lithium ion battery cathode material and preparation method thereof |
| CN111600014A (en) * | 2020-05-26 | 2020-08-28 | 宁波容百新能源科技股份有限公司 | Modified high-specific-capacity high-nickel ternary cathode material and preparation method thereof |
| CN111848151A (en) * | 2020-08-10 | 2020-10-30 | 西安航空学院 | Titanium magnesium aluminum lithium phosphate LAMTP single-phase ceramic wave-absorbing material and preparation method and application thereof |
| CN114057235A (en) * | 2021-10-27 | 2022-02-18 | 荆门市格林美新材料有限公司 | Method for coating LATP (LATP-activated copper phosphate) by nickel-cobalt-manganese ternary precursor |
| CN114824280A (en) * | 2022-06-27 | 2022-07-29 | 蚂蚁新能源科技(天津)有限公司 | Composite positive electrode material for lithium ion battery dry-method electrode and preparation method and application thereof |
| CN114824227A (en) * | 2022-05-16 | 2022-07-29 | 上海屹锂新能源科技有限公司 | Double-layer coated positive electrode composite material and preparation method and application thereof |
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| CN111848151A (en) * | 2020-08-10 | 2020-10-30 | 西安航空学院 | Titanium magnesium aluminum lithium phosphate LAMTP single-phase ceramic wave-absorbing material and preparation method and application thereof |
| CN114057235A (en) * | 2021-10-27 | 2022-02-18 | 荆门市格林美新材料有限公司 | Method for coating LATP (LATP-activated copper phosphate) by nickel-cobalt-manganese ternary precursor |
| CN114824227A (en) * | 2022-05-16 | 2022-07-29 | 上海屹锂新能源科技有限公司 | Double-layer coated positive electrode composite material and preparation method and application thereof |
| CN114824227B (en) * | 2022-05-16 | 2023-09-12 | 上海屹锂新能源科技有限公司 | Double-layer coated positive electrode composite material and preparation method and application thereof |
| CN114824280A (en) * | 2022-06-27 | 2022-07-29 | 蚂蚁新能源科技(天津)有限公司 | Composite positive electrode material for lithium ion battery dry-method electrode and preparation method and application thereof |
| CN114824280B (en) * | 2022-06-27 | 2022-09-06 | 蚂蚁新能源科技(天津)有限公司 | Composite positive electrode material for lithium ion battery dry-method electrode and preparation method and application thereof |
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