CN110444752A - Extended-life lithium ion battery tertiary cathode material and its preparation method and application - Google Patents
Extended-life lithium ion battery tertiary cathode material and its preparation method and application Download PDFInfo
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- CN110444752A CN110444752A CN201910741094.0A CN201910741094A CN110444752A CN 110444752 A CN110444752 A CN 110444752A CN 201910741094 A CN201910741094 A CN 201910741094A CN 110444752 A CN110444752 A CN 110444752A
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- 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
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- 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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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- 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
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a kind of extended-life lithium ion battery tertiary cathode materials, including the ternary material as substrate and are coated on the polymeric PTC materials layer on the ternary material surface, wherein the macromolecule includes havingThe polycarboxylic acids esters high-molecular compound of structure.The present invention also provides the preparation method and applications of the extended-life lithium ion battery tertiary cathode material.Extended-life lithium ion battery tertiary cathode material of the invention has good mechanical property and excellent capacitance characteristic, and simply, the capacitor material that can be used as business is promoted the use of for cheap, preparation.
Description
Technical field
The present invention relates to electrode material technical fields, and in particular to a kind of extended-life lithium ion battery tertiary cathode material and
Preparation method and application.
Background technique
In recent years, as the demand of electric car, hybrid vehicle and scale energy storage is increasing, people to lithium from
More stringent requirements are proposed for the energy density and cost of sub- battery, on the one hand need to increase substantially positive electrode specific capacity and
Specific energy, while also to reduce the demand to cobalt.In this context, tertiary cathode material causes the extensive concern of people.Three
First positive electrode has LiNi1-x-yCoxMyO2The chemical composition of (1 >=x >=0,1 >=y >=0, x+y < 1, M=Mn, Al), including mesh
Before in common NCM811, NCM622, NCM523, NCM111 and NCA.On the one hand the outstanding advantages of this kind of material are to greatly reduce
Demand to cobalt has apparent price advantage, it is often more important that, the specific capacity of material is also obviously improved, can
To reach 200mAh g-1More than, there is important application value and prospect in the lithium ion battery of the following high-energy density, be
For the ideal positive electrode of mixed type power electric motor car.
However, the currently used tertiary cathode material of lithium ion battery contains relatively high Ni mostly, it is especially therein
Ni4+ has very strong oxidisability, apparent interface side reaction can be aoxidized and induced when directly contacting with electrolyte, generation has
The ingredients such as machine acid further corrode tertiary cathode material, and the Ni of tertiary cathode material is on the one hand caused to dissolve, and structure is destroyed, simultaneously
The raising of electrode/electrolyte interface resistance is also resulted in, leads to the qualitative surely circulation of this kind of material, thermal stability and big high rate performance not
Reach, in this sense, improve the interface stability of ternary material have to its following extensive scale application it is important
Application value and development prospect.In fact, in recent years people ternary cathode material of lithium ion battery surface and interface modification and
Modified aspect is done a lot of work, and inorganic carbon material cladding, oxide, phosphide cladding and organic conductive polymerization are mostly concentrated on
Object cladding etc..Carbon coating is mainly used for improving the electron conduction of material, to the side for inhibiting electrode/electrolyte interfacial reaction
It helps less；The cladding of oxide and phosphide helps to reduce the interfacial reaction of electrode/electrolyte, but inorganic material brittleness is big,
Clad is unevenly and continuous, is easily broken in electrode charge and discharge process, therefore the effect of this kind of material is limited, conductive polymer
Son can realize the protection to tertiary cathode material while improving electrodic electron electric conductivity, but this kind of material is anti-oxidant steady
Qualitative difference, nitrogen-atoms and Ni are mutually rented between Co, Mn there is no chemical bond, therefore improvement is also undesirable.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, a kind of extended-life lithium ion battery tertiary cathode material is provided
Material and preparation method thereof, which needs not move through high-temperature process, and low in cost, low energy consumption, and raw material is easy to obtain, technique
Process is simple, environmentally friendly, can not only effectively realize to the uniform cladding and coating thickness regulation of positive electrode surface, also hold
Easily realize large-scale production.
In order to solve the above-mentioned technical problems, the present invention provides a kind of extended-life lithium ion battery tertiary cathode material, packets
The polymeric PTC materials layer for including the ternary material as substrate and being coated on the ternary material surface, wherein the macromolecule
Including havingThe polycarboxylic acids esters high-molecular compound of structure.
Further, the polycarboxylic acids esters high-molecular compound is selected from polymethyl methacrylate, polymethylacrylic acid
Ethyl ester, polybutyl methacrylate, polyisobutyl methacrylate, vinyl chloride methacrylate copolymer, polymethyl
One in acid glycidyl ester, polyhydroxypropyl methaciylate and poly- (2,2,2- trifluoroethyl methacrylate) similar structures
Kind is a variety of.
Further, the macromolecule further includes above-mentioned polycarboxylic acids esters high-molecular compound and other common high score attached bags
It covers material to be used in mixed way, such as Kynoar (PVDF), polyvinyl fluoride (PVF) etc..
Further, the ternary material has LiNi1-x-yCoxMyO2(1 >=x >=0,1 >=y >=0, x+y < 1, M=Mn,
Al chemical composition).
Further, the ternary material is selected from one of NCM811, NCM622, NCM523, NCM111 and NCA or two
Kind or more mixture.
Further, the polymeric PTC materials layer material and ternary material and weight ratio be 0.2~5%.
Another aspect of the present invention additionally provides the preparation method of the extended-life lithium ion battery tertiary cathode material, packet
Include following steps:
S1, the macromolecule is dissolved in solvent, obtains Polymer Solution；
S2, the tertiary cathode material is dipped in the Polymer Solution, heating stirring to solvent is volatilized completely；It takes out
Tertiary cathode material, it is dry to get the extended-life lithium ion battery tertiary cathode material.
Further, the solvent is selected from ethyl alcohol, glycerol, ethylene glycol, methanol, n,N dimethylformamide, N- methylpyrrole
One of alkanone, isopropanol, dimethyl sulfoxide, acetone or two or more mixtures.
Further, the temperature of the heating is 30~200 DEG C.
Further, the drying is to dry under vacuum conditions, and drying time is 1~10 hour, drying temperature 80
~200 DEG C.
The present invention also provides extended-life lithium ion battery tertiary cathode material the answering in field of lithium ion battery
With.
Beneficial effects of the present invention:
1. the present invention utilizes simple Liquid Coating Technology, uniform organic coating can be formd on positive electrode surface
Layer, and coating thickness can be regulated and controled by adjusting the concentration of solution and the method for dosage；In clad in carboxylate
Oxygen atom can establish strong chemical bond interaction, covered effect between the metal ion on active material particle surface
It is good；Wellability between this polycarboxylate clad and carbonate solution is good, and interface impedance is small；The electrification of this polycarboxylate
Stability is good, and decomposition voltage is up to 4.6V or more, can inhibit the side reaction of positive electrode and electrolyte；This close packet
Coating helps to inhibit the dissolution of metal cation in the electrolytic solution, protects surface and the structural stability of positive electrode.
2. product cyclical stability that the present invention obtains and it is forthright again obtained apparent improvement, while the invention method is not required to
To pass through high-temperature process, low in cost, low energy consumption, and raw material is easy to obtain, and process flow is simple, and it is environmentally friendly, it is easy to accomplish
Large-scale production.
Detailed description of the invention
Fig. 1 is the first charge-discharge figure of embodiment 1,2,3 and comparative example 1；
Fig. 2 is the circulation figure of embodiment 1,2,3 and comparative example 1；
Fig. 3 is the 1C circulation figure of embodiment 1,2,3,4,5,6 and comparative example 1,2,3；
Fig. 4 is ac impedance spectroscopy after embodiment 1,2,3 and the circulation of comparative example 1；
The electron microscope of Fig. 5 comparative example 1；
The electron microscope of Fig. 6 embodiment 1；
Fig. 7 embodiment 1 coats preparation technology flow chart and battery process preparation flow.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
This example provides a kind of monocrystalline LiNi0.8Co0.1Mn0.1O2Modifying interface and preparation method, specifically include following step
It is rapid:
(a) 0.05g polymethyl methacrylate (PMMA) heating is dissolved in 10g acetone solvent (molecular sieve water removal), is stirred
2h is mixed, uniform solution is formed.
(b) 2g monocrystalline LiNi is taken0.8Co0.1Mn0.1O2Active material is slowly added in PMMA solution under the conditions of 30 DEG C, not
Solution is heated straight solvent under constant agitation and volatilized completely by the stirring stopped.
(c) powder product for obtaining above-mentioned steps in a vacuum drying oven, temperature control 60 DEG C aging 8 hours, obtain
The ternary clad anode material for being 2.5% to PMMA covering amount.
The present invention also provides application of this cladded type tertiary cathode material in lithium ion battery, and above-mentioned steps are obtained
Coating modification monocrystalline tertiary cathode material carry out battery film-making process, the assembled battery in dry chamber, at room temperature carry out electricity
Chemical property test.All batteries carry out test 1C loop test after first being enclosed with 0.1C electric current chemical conversion 5 and multiplying power tests (0.5C
It is at full charge, discharge test successively is carried out 0.5,1,2,5,10,20, medium and small multiplying power 0.1C and 0.2C is filled in phase same multiplying
It puts)
Embodiment 2
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike take 0.03g polyethyl methacrylate (PEMA) to be dissolved in 10g toluene solvant
Coating modification is carried out, the ternary clad anode material that PEMA covering amount is 1.5% is obtained.
Embodiment 3
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike take the different ethyl ester of 0.04g polymethylacrylic acid to be dissolved in 10g toluene solvant to carry out
Coating modification obtains the different ethyl ester ternary clad anode material of polymethylacrylic acid that covering amount is 2.0%.
Embodiment 4
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike take 0.04g vinyl chloride methacrylate copolymer to be dissolved in 10g dimethyl sulfoxide
Coating modification is carried out in solvent, obtains the vinyl chloride methacrylate copolymer ternary clad anode material that covering amount is 2.0%
Material.
Embodiment 5
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike take 0.04g polyhydroxypropyl methaciylate to be dissolved in 10g dimethylsulfoxide solvent
Coating modification is carried out, the polyhydroxypropyl methaciylate ternary clad anode material that covering amount is 2.0% is obtained.
Embodiment 6
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike 0.02g PMMA and 0.02gPVDF are dissolved in 10g N-Methyl pyrrolidone
Coating modification is carried out, takes 0.04g polyhydroxypropyl methaciylate to be dissolved in 10g dimethyl sulfoxide in acetone solvent (molecular sieve water removal) molten
Coating modification is carried out in agent, obtains PMMA the and PVDF mixing clad anode material that covering amount is 2.0%.
Embodiment 7
This example provides a kind of cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2The preparation method of positive electrode, preparation process
With it is almost the same in embodiment 1, unlike by 0.02g PMMA be dissolved in acetone to tertiary cathode material carry out cladding change
Property, then 0.02gPVDF is dissolved in 10g N-Methyl pyrrolidone and carries out coating modification, obtain PMMA and PVDF double-coating amount
For 2.0% cladding ternary monocrystalline positive electrode.
Comparative example 1
Comparative example 1 provides a kind of no cladded type monocrystalline LiNi0.8Co0.1Mn0.1O2Anode, the material carry out button cell system
Piece process, assembled battery in dry chamber, carries out electrochemical property test at room temperature.All batteries are first with 0.1C electric current chemical conversion 5
Carried out after circle test 1C loop test and multiplying power test (0.5C is at full charge, successively carries out electric discharge survey 0.5,1,2,5,10,20
Examination, medium and small multiplying power 0.1C and 0.2C is in the charge and discharge of phase same multiplying).
Comparative example 2
Comparative example 2 provides a kind of PVDF cladding monocrystalline LiNi0.8Co0.1Mn0.1O2In material, preparation process and embodiment 1
It is almost the same, unlike by 0.06g PVDF be dissolved in N-Methyl pyrrolidone to tertiary cathode material carry out cladding change
Property, it obtains the PVDF that covering amount is 3.0% and coats tertiary cathode material, test condition is identical as comparative example 1.
It will be seen from figure 1 that the first charge-discharge capacity of the polycarboxylate cladding ternary material of different embodiments preparations and
Coulombic efficiency improves, it is often more important that, the high rate performance for the ternary material that in Fig. 2 prepared by these embodiments obtains
It is obviously improved, still has very high capacity retention ratio under the conditions of the material 10C that especially prepared by embodiment 1, it is shown that excellent
Rate charge-discharge property.
Fig. 3 compared the cycle performance for the tertiary cathode material that different comparative examples and embodiment obtain, it can be seen that use
The cycle performance of the tertiary cathode material of polycarboxylate clad is obviously improved, after 100 circulations, polycarboxylate cladding
The capacity retention ratio of modified material is significantly more than PVDF cladding and uncoated tertiary cathode material.
Fig. 4 compared the impedance behavior of the polycarboxylate cladding ternary material of different embodiment preparations, compared with comparative example,
The electrochemical impedance of material is decreased obviously.
Fig. 5 and Fig. 6 compared the material morphology of comparative example 1 and embodiment 1, it can be seen that the organic material in embodiment surface
Material cladding continuous uniform helps to improve and improves tertiary cathode using this kind of distinctive functionality advantage of polycarboxylate clad
Macroscopical electrochemical properties of material.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of extended-life lithium ion battery tertiary cathode material, which is characterized in that including as substrate ternary material and
It is coated on the polymeric PTC materials layer on the ternary material surface, wherein the macromolecule includes havingStructure
Polycarboxylic acids esters high-molecular compound.
2. extended-life lithium ion battery tertiary cathode material as described in claim 1, which is characterized in that the polycarboxylic acids esters
High-molecular compound is selected from polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate, polymethyl
Sour isobutyl ester, vinyl chloride methacrylate copolymer, poly (glycidyl methacrylate), polyhydroxypropyl methaciylate with
And the middle one or more of poly- (2,2,2- trifluoroethyl methacrylate) similar structures.
3. extended-life lithium ion battery tertiary cathode material as described in claim 1, which is characterized in that the ternary material tool
There is LiNi1-x-yCoxMyO2The chemical composition of (1 >=x >=0,1 >=y >=0, x+y < 1, M=Mn, Al).
4. extended-life lithium ion battery tertiary cathode material as claimed in claim 3, which is characterized in that the ternary material choosing
From one or more mixtures of NCM811, NCM622, NCM523, NCM111 and NCA.
5. extended-life lithium ion battery tertiary cathode material as described in claim 1, which is characterized in that the polymeric PTC materials
Layer material and ternary material and weight ratio be 0.2~5%.
6. the preparation method of described in any item extended-life lithium ion battery tertiary cathode materials according to claim 1~5, special
Sign is, comprising the following steps:
S1, the macromolecule is dissolved in solvent, obtains Polymer Solution；
S2, the tertiary cathode material is dipped in the Polymer Solution, heating stirring to solvent is volatilized completely；Take out ternary
Positive electrode, it is dry to get the extended-life lithium ion battery tertiary cathode material.
7. the preparation method of extended-life lithium ion battery tertiary cathode material as claimed in claim 6, which is characterized in that described
Solvent is selected from ethyl alcohol, glycerol, ethylene glycol, methanol, and n,N dimethylformamide, N-Methyl pyrrolidone, isopropanol, dimethyl are sub-
One of sulfone, acetone or two or more mixtures.
8. the preparation method of extended-life lithium ion battery tertiary cathode material as claimed in claim 6, which is characterized in that described
The temperature of heating is 30~200 DEG C.
9. the preparation method of extended-life lithium ion battery tertiary cathode material as claimed in claim 6, which is characterized in that described
Dry to dry under vacuum conditions, drying time is 1~10 hour, and drying temperature is 80~200 DEG C.
10. the described in any item extended-life lithium ion battery tertiary cathode materials of Claims 1 to 5 are in field of lithium ion battery
Application.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111211299A (en) * | 2020-01-07 | 2020-05-29 | 中南大学 | Modified lithium ion battery positive electrode material coated with strong electronegative organic matter layer and preparation method thereof |
| CN112436121A (en) * | 2020-11-24 | 2021-03-02 | 上海华谊（集团）公司 | Composite material with core-shell structure and preparation method thereof |
| CN116750802A (en) * | 2023-08-21 | 2023-09-15 | 中节能万润股份有限公司 | Preparation method and application of layered oxide sodium ion battery positive electrode material |
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| CN116750802A (en) * | 2023-08-21 | 2023-09-15 | 中节能万润股份有限公司 | Preparation method and application of layered oxide sodium ion battery positive electrode material |
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| CN110444752B (en) | 2021-07-20 |
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