CN106571452A - Lithium ion battery positive electrode material and preparation method thereof - Google Patents
Lithium ion battery positive electrode material and preparation method thereof Download PDFInfo
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- CN106571452A CN106571452A CN201610954211.8A CN201610954211A CN106571452A CN 106571452 A CN106571452 A CN 106571452A CN 201610954211 A CN201610954211 A CN 201610954211A CN 106571452 A CN106571452 A CN 106571452A
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- lithium
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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
-
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 discloses a lithium ion battery positive electrode material and a preparation method thereof. The preparation method comprises the following steps: 1, dispersing a titanium source in a dispersant, adding lithium cobaltate and water, uniformly mixing the titanium source, the dispersant, lithium cobaltate and water, and drying the obtained solution to obtain a precursor; and 2, heating and reacting the precursor in nitrogen or ammonia gas atmosphere to prepare titanium nitride coated lithium cobaltate, wherein a mass ratio of titanium in the titanium source to the dispersant to lithium cobaltate to water is 1:(500-5000):(50-1000):(50-1000). The lithium ion battery positive electrode material is formed through coating the surface of lithium cobaltate with a compact and uniform titanium nitride passivation film, and can prevent direct contact of an active material and an electrolyte in order to reduce dissolving of cobalt in the electrolyte, so the capacity retention rate and the cycle stability are well improved.
Description
Technical field
The invention belongs to lithium ion battery manufacture field, more particularly to a kind of anode material for lithium-ion batteries and its preparation
Method.
Background technology
In recent years, lithium ion battery because specific energy is high, have extended cycle life, self discharge is little, safe and reliable, environmental protection etc.
Many advantages and the deep extensive concern by various circles of society.And cobalt acid lithium has and prepares simple, volume energy density in electrokinetic cell
Greatly, safety and the advantages of excellent high rate performance by it is believed that being electrokinetic cell cost performance highest positive electrode.But cobalt is sour
Lithium cycle performance under high voltages is unsatisfactory, and the decay of capacity is mainly due to the cobalt dissolving institute in cobalt acid lithium under high voltage
Cause, the Fluohydric acid. in electrolyte can react with cobalt acid lithium, and cobalt can dissolve and cause structural instability and capacity
Loss.
Chem.Mater.7 (2005) 5603-5605, the colloidal sol and cobalt acid lithium mix homogeneously of aluminium oxide after, sprayed
It is dried, in LiCoO after drying calcining2Surface forms one layer of Al2O3Clad, improve the cyclical stability of material.In electric current
Density is 0.05mA/cm2After circulation 10 times, Al2O3The LiCoO of cladding2The capacity of material is that (first capacity is 158mAh/g
172mAh/g)；And under the same terms, pure phase LiCoO2Capacity only have 115mAh/g (first capacity be 169mAh/g).It is this
Method for coating improves well LiCoO2Cyclical stability, but the method uses alumina sol and spray drying side
Method, preparation process complexity is loaded down with trivial details, is not easy to commercial production.
The 10-16 of Journal of Power Sources 322 (2016), by sputtering in business cobalt acid lithium table
Face has successfully coated the clad of one layer of lithium phosphate.The high voltage cycle of material is improve well by this coating modification
Performance.After 1.0C multiplying powers, 3.0-4.5 voltage ranges interior circulation 100 times, its capability retention reaches 79.3% to the material, and
Uncoated LiCoO2Capability retention only has 46.2% after 100 circulations.The clad of product prepared by injection cladding process
It is uniform and granule is less, but the preparation process of the method is more complicated, and production cost is high, is not easy to commercial production.
In LiCoO2Surface coating layer of metal compound type passivating film can prevent active material and electrolyte from directly connecing
Touch, reduce cobalt dissolving in the electrolytic solution, the capacitance loss caused so as to avoid structural instability improves specific capacity
Energy and cyclical stability.
The Chinese invention patent of Publication No. CN103700846A discloses a kind of lithium ion battery cladding lithium cobaltate cathode
Material and preparation method, this positive electrode includes following raw material：Butyl titanate, cobalt acid lithium and dehydrated alcohol.Making step
For：Calculated by stoichiometric proportion, butyl titanate is weighed, in being dissolved in dehydrated alcohol；Then by cobalt acid lithium be added to dissolved with
In the ethanol solution of butyl titanate, stir four hours；Heating is evaporated dehydrated alcohol, and five hours, grinding are sintered at 400 DEG C
And obtain the lithium cobaltate cathode material of coated by titanium dioxide after over-molecular sieve.But TiO2As anode material for lithium-ion batteries
Have the disadvantage poorly conductive.
The content of the invention
The invention provides a kind of preparation method is simple, be evenly coated and electrochemical performance lithium ion cell positive
Material, the lithium ion battery circulation volume conservation rate of preparation is high, improves specific capacity performance and cyclical stability.
A kind of preparation method of anode material for lithium-ion batteries, comprises the following steps：
(1) titanium source is dispersed in dispersant, is subsequently adding cobalt acid lithium (LiCoO2) and water is mixed, drying obtains forerunner
Body；
(2) reacting by heating under presoma being placed in into nitrogen or ammonia atmosphere, is obtained the cobalt acid lithium of titanium nitride (TiN) cladding,
The mass ratio of titanium wherein, in titanium source, dispersant, cobalt acid lithium and water is 1: 500～5000: 50～1000: 50
～1000.The ratio of various materials is groped optimization and is obtained by experiment, and wherein the amount of titanium source is only needed seldom, and titanium source is in nitrogen or ammonia
Heating under atmosphere produces titanium nitride, is coated on cobalt acid lithium surface.
Preferably, the titanium source is the one kind in butyl titanate, tetraethyl titanate or isopropyl titanate or mixing.
Preferably, the dispersant is the one kind in ethanol, propanol, isopropanol or acetone or mixing.
Preferably, heating means be with the ramp of 2～8 DEG C/min to 400～700 DEG C, then heated at constant temperature 3～
9h.Acquisition is groped by experiment the time required to reaction temperature and heating.
Invention further provides anode material for lithium-ion batteries prepared by described preparation method.
Preferably, described anode material for lithium-ion batteries, the quality of titanium nitride clad for cobalt acid lithium 0.13%～
2.6%.
Present invention also offers lithium ion battery prepared by the anode material for lithium-ion batteries.
Anode material for lithium-ion batteries of the present invention by one layer of dense uniform of cobalt acid lithium Surface coating nitridation Ti passivation, lithium
Ion battery electrolyte salt LiPF6 runs into the water of trace will hydrolyze generation HF, and HF can be further exacerbated by the decomposition of LiPF6,
Simultaneously HF also can be lost in cobalt with cobalt acid lithium reaction, and on the one hand this layer of nitridation Ti passivation can avoid active material and electrolyte
Directly contact, prior is that TiN can react with the HF in electrolyte, and micro HF is consumed, and is existed so as to reduce cobalt
Dissolving in electrolyte, improves well capability retention and cyclical stability.
Description of the drawings
Fig. 1 is the TEM testing result figures that titanium nitride prepared by embodiment 1 coats lithium cobaltate cathode material；
Fig. 2 is the XRD testing result figures that titanium nitride prepared by embodiment 1 coats lithium cobaltate cathode material；
Fig. 3 is that the titanium nitride prepared using embodiment 1 coats lithium ion battery cyclicity obtained in lithium cobaltate cathode material
Can testing result figure.
Specific embodiment
Embodiment 1
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 5000: 1000: 1000
Ratio.
(1) 0.0047g tetraethyl titanates are distributed in 6.3mL ethanol, are subsequently adding 1.0g cobalt acid lithiums powder and 1mL goes
Ionized water, mix homogeneously, drying obtains presoma；
(2) by the presoma for obtaining in nitrogen atmosphere with 2 DEG C/min ramps to 400 DEG C and constant temperature 3 hours, then
Room temperature is naturally cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Matter
The 0.13% of amount.
Products therefrom is detected with TEM (transmission electron microscope), as a result as shown in figure 1, LiCoO2Outside one layer of titanium nitride of cladding,
It is evenly coated, and the thickness of titanium nitride clad is about 30nm.
Products therefrom is detected with XRD (X-ray diffraction), testing result is as shown in Figure 2, it can be seen that after titanium nitride cladding
The structure of cobalt acid lithium is not destroyed.
Embodiment 2
Titanium nitride cladding lithium cobaltate cathode material obtained in embodiment 1 is gathered into inclined difluoro with conductive carbon black and binding agent respectively
Ethylene (PVDF) 8: 1: 1 mix homogeneously in mass ratio, are coated on aluminium foil, and after being dried anode pole piece is cut into, dry in 120 DEG C of vacuum
Dry 24 hours.It is to electrode, by electrolyte LiPF with lithium metal6Salt be dissolved in mass ratio be 1: 1: 1 ethylene carbonate (EC)/
Electrolyte is formed in the mixed solution of dimethyl carbonate (DMC)/Ethyl methyl carbonate (EMC), the concentration of electrolyte is 1mol/L,
CR2016 button cells are assembled in argon glove box.
Electrochemical property test is carried out using Wuhan indigo plant electricity CT2001A types cell tester, charging/discharging voltage scope is
3.0V～4.5V (vs.Li+/ Li), test result is (the cycle performance curve of 1.0C multiplying powers) as shown in Figure 3, with the gained of embodiment 1
Used as the battery of positive electrode, first discharge specific capacity is 174.6mAh/g to cobalt acid lithium, and Jing is circulated for 150 times after titanium nitride cladding
Afterwards, capacity still has 167.8mAh/g, and capability retention is 96.1%；And as a comparison using uncoated cobalt acid lithium as positive pole
The battery of material, first discharge specific capacity is close to experimental group, but the capacity Jing after 150 circulations is 81.8mAh/g, and capacity is protected
Holdup is 47.8%.With uncoated LiCoO2Compare, LiCoO is coated with titanium nitride2As the lithium ion battery of positive electrode
Specific capacity performance and cyclical stability are improved significantly.
Embodiment 3
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 500: 50: 50 ratio.
(1) 0.095g tetraethyl titanates are distributed in 12.7mL acetone, are subsequently adding 1.0g cobalt acid lithiums powder and 1.0mL
Deionized water, mix homogeneously, drying obtains presoma；
(2) by the presoma for obtaining in nitrogen atmosphere with 5 DEG C/min ramps to 500 DEG C and constant temperature 3 hours, then
Room temperature is naturally cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Matter
The 2.6% of amount.
Embodiment 4
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 4000: 500: 400 ratio
Example.
(1) 0.0118g isopropyl titanates are distributed in 10mL ethanol, are subsequently adding 1.0g cobalt acid lithiums powder and 0.8mL goes
Ionized water, mix homogeneously, drying obtains presoma；
(2) by the presoma for obtaining in ammonia atmosphere with 8 DEG C/min ramps to 600 DEG C and constant temperature 9 hours, then
Room temperature is naturally cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Matter
The 0.26% of amount.
Embodiment 5
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 1000: 200: 100 ratio
Example.
(1) 0.296g isopropyl titanates are distributed in 6.3mL acetone, are subsequently adding 1.0g cobalt acid lithiums powder and 0.5mL goes
Ionized water, mix homogeneously, drying obtains presoma；
(2) by the presoma nitrogen atmosphere for obtaining with 5 DEG C/min ramps to 500 DEG C and constant temperature 9 hours, then from
Room temperature is so cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Quality
0.65%.
Embodiment 6
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 2000: 100：100 ratio
Example.
(1) 0.0708g butyl titanates are distributed in 25.4mL acetone, be subsequently adding 1.0g cobalt acid lithiums powder and
1.0mL deionized waters, mix homogeneously, drying obtains presoma；
(2) by the presoma for obtaining in ammonia atmosphere with 3 DEG C/min ramps to 700 DEG C and constant temperature 6 hours, then from
Room temperature is so cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Quality
1.3%.
Embodiment 7
Calculate in mass ratio, i.e. titanium in titanium source: dispersant: LiCoO2: deionized water is 1: 3000: 70:60 ratio.
(1) 0.101g butyl titanates are distributed in 54.3mL ethanol, be subsequently adding 1.0g cobalt acid lithiums powder and
0.86mL deionized waters, mix homogeneously, drying obtains presoma；
(2) by the presoma for obtaining in ammonia atmosphere with 6 DEG C/min ramps to 400 DEG C and constant temperature 8 hours, then
Room temperature is naturally cooled to, titanium nitride cladding LiCoO of the present invention is obtained2Product, the wherein quality of titanium nitride clad are LiCoO2Matter
The 1.95% of amount.
Claims (8)
1. a kind of preparation method of anode material for lithium-ion batteries, it is characterised in that comprise the following steps：
(1) titanium source is dispersed in dispersant, is subsequently adding cobalt acid lithium and water is mixed, drying obtains presoma；
(2) reacting by heating under presoma being placed in into nitrogen or ammonia atmosphere, is obtained the cobalt acid lithium of titanium nitride cladding,
The mass ratio of titanium wherein, in titanium source, dispersant, cobalt acid lithium and water is 1: 500～5000: 50～1000: 50～
1000。
2. preparation method as claimed in claim 1, it is characterised in that the titanium source be butyl titanate, tetraethyl titanate or
One kind or mixing in isopropyl titanate.
3. preparation method as claimed in claim 1, it is characterised in that the dispersant is ethanol, propanol, isopropanol or acetone
In one kind or mixing.
4. preparation method as claimed in claim 1, it is characterised in that heating means be with the ramp of 2～8 DEG C/min extremely
400～700 DEG C, then 3～9h of heated at constant temperature.
5. the anode material for lithium-ion batteries for being prepared by the arbitrary described preparation method of Claims 1 to 4.
6. anode material for lithium-ion batteries as claimed in claim 5, it is characterised in that the quality of titanium nitride clad is cobalt acid
The 0.13%～2.6% of lithium.
7. the lithium ion battery that prepared by anode material for lithium-ion batteries as claimed in claim 5.
8. the lithium ion battery that prepared by anode material for lithium-ion batteries as claimed in claim 6.
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Cited By (8)
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| CN108336315A (en) * | 2017-12-11 | 2018-07-27 | 浙江天能能源科技股份有限公司 | A kind of preparation method of the lithium ion battery nickel lithium manganate cathode material of coating modification |
| CN109698380A (en) * | 2018-12-28 | 2019-04-30 | 天能电池(芜湖)有限公司 | A kind of high-capacity lithium ion power battery and its material preparation process |
| CN111320214A (en) * | 2020-02-27 | 2020-06-23 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
| CN111435747A (en) * | 2020-01-17 | 2020-07-21 | 蜂巢能源科技有限公司 | Cobalt-free layered cathode material, preparation method thereof and lithium ion battery |
| CN112174222A (en) * | 2020-08-27 | 2021-01-05 | 浙江美都海创锂电科技有限公司 | TiN-coated nickel-cobalt-manganese ternary positive electrode material and preparation method thereof |
| CN112467121A (en) * | 2020-12-03 | 2021-03-09 | 珠海冠宇电池股份有限公司 | Positive plate and preparation method and application thereof |
| CN113097458A (en) * | 2021-03-29 | 2021-07-09 | 清华大学 | Ternary cathode material @ titanium nitride core-shell structure composite material and preparation method thereof |
| CN113277568A (en) * | 2021-05-14 | 2021-08-20 | 浙江中金格派锂电产业股份有限公司 | Preparation method of high-conductivity lithium cobalt oxide positive electrode material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108336315A (en) * | 2017-12-11 | 2018-07-27 | 浙江天能能源科技股份有限公司 | A kind of preparation method of the lithium ion battery nickel lithium manganate cathode material of coating modification |
| CN109698380A (en) * | 2018-12-28 | 2019-04-30 | 天能电池(芜湖)有限公司 | A kind of high-capacity lithium ion power battery and its material preparation process |
| CN111435747A (en) * | 2020-01-17 | 2020-07-21 | 蜂巢能源科技有限公司 | Cobalt-free layered cathode material, preparation method thereof and lithium ion battery |
| WO2021143373A1 (en) * | 2020-01-17 | 2021-07-22 | 蜂巢能源科技有限公司 | Cobalt-free layered positive electrode material and preparation method therefor, and lithium-ion battery |
| EP3972017A4 (en) * | 2020-01-17 | 2023-07-19 | Svolt Energy Technology Co., Ltd | Cobalt-free layered positive electrode material and preparation method therefor, and lithium-ion battery |
| CN111320214A (en) * | 2020-02-27 | 2020-06-23 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
| CN111320214B (en) * | 2020-02-27 | 2022-07-08 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
| CN112174222A (en) * | 2020-08-27 | 2021-01-05 | 浙江美都海创锂电科技有限公司 | TiN-coated nickel-cobalt-manganese ternary positive electrode material and preparation method thereof |
| CN112467121A (en) * | 2020-12-03 | 2021-03-09 | 珠海冠宇电池股份有限公司 | Positive plate and preparation method and application thereof |
| CN113097458A (en) * | 2021-03-29 | 2021-07-09 | 清华大学 | Ternary cathode material @ titanium nitride core-shell structure composite material and preparation method thereof |
| CN113277568A (en) * | 2021-05-14 | 2021-08-20 | 浙江中金格派锂电产业股份有限公司 | Preparation method of high-conductivity lithium cobalt oxide positive electrode material |
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Application publication date: 20170419 |