CN108461740A - A kind of LiVOPO4Nickelic tertiary cathode material of lithium ion battery of cladding and its preparation method and application - Google Patents
A kind of LiVOPO4Nickelic tertiary cathode material of lithium ion battery of cladding and its preparation method and application Download PDFInfo
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- CN108461740A CN108461740A CN201810251247.9A CN201810251247A CN108461740A CN 108461740 A CN108461740 A CN 108461740A CN 201810251247 A CN201810251247 A CN 201810251247A CN 108461740 A CN108461740 A CN 108461740A
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- lithium ion
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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
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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
- H01M4/48—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
- 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
- H01M4/50—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
- 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
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of LiVOPO4The preparation method of the nickelic tertiary cathode material of lithium ion battery of cladding, includes the following steps：By NH4VO3, (NH4)2HPO4And LiNO3In molar ratio 1：1：1.05 ratio is add to deionized water, 75~80 DEG C of heating water baths and stir 15~30min make it dissolve, be added ascorbic acid stir 4~6h；Base material is added in solution made from S1, is spray-dried, is sintered 6~10h in air atmosphere at 400~600 DEG C；Or, stirring solution made from S1 to doing, it is sintered 6~10h at 400~600 DEG C, will be added in ball grinder together with sintered product and base material, 50~100r/min ball milling 30min, wherein sintered product account for the 1~5% of base material quality；Compared with prior art, the present invention assists solwution method or ball-milling method to coat LiVOPO in substrate using spray drying4, high power capacity, high circulation, high magnification, ionic conductivity height, the excellent ternary cathode material of lithium ion battery of security performance has been made.
Description
Technical field
The invention belongs to electrochemical technology fields, more particularly to a kind of LiVOPO4The lithium ion battery nickelic three of cladding
First positive electrode and its preparation method and application.
Background technology
Lithium ion battery is widely used in portable electronic product, the fields such as electric vehicle.People are to its security performance, electricity
More stringent requirements are proposed for pond service life, battery capacity.In lithium ion battery, positive electrode is its most important component part,
It is also the key for determining performance of lithium ion battery.
Currently, commercial positive electrode is still with LiCoO2Based on, but the rare of cobalt resource leads to that it is expensive, and have
The unfavorable factors such as poison, thermal stability difference limit it and further apply.Ternary material (NCA and NCM) has both LiCoO2、LiMnO2
And LiNiO2The advantages of.Moreover, some researches show that, the increase of the Ni contents in ternary system therewith, the gram volume of material also phase
It should increase.Therefore, nickelic ternary material is considered as the novel anode material for most having application prospect.
However, with the increase of Ni contents, Li+And Ni2+Mixing is also more serious, causes cyclical stability poor, for the first time not
Reversible capacity is high.And the lithium salts of excess surface can absorb water and CO in air2, it is that material surface structure is destroyed；Surface is high
The Ni of valence state4+It can accelerate electrolyte decomposition, decomposition product can accelerate electrode material structural damage, steady so as to cause circulating battery
Qualitative decline, security performance decline.
The Chinese patent of Publication No. CN101308925A：A kind of preparation of the nickelic ternary material of metal oxide cladding
Method utilizes TiO2、Al2O3、MgO2And Cr2O3Etc. claddings nickelic ternary material, completely cut off nickelic ternary material and electrolyte
Contact, improves the cyclical stability of battery, but used metal oxide is inert material, ionic conductivity is not high, makes just
The capacity and high rate performance of pole material decline.
Invention content
In order to solve the deficiencies in the prior art, the present invention provides a kind of LiVOPO4The lithium ion battery nickelic three of cladding
The preparation method of first positive electrode, this method can produce high power capacity, high circulation, high magnification and the excellent lithium ion of security performance
Battery tertiary cathode material.
Specifically, LiVOPO provided by the invention4The preparation method of the nickelic tertiary cathode material of lithium ion battery of cladding,
Include the following steps：
S1：By NH4VO3, (NH4)2HPO4And LiNO3In molar ratio 1：1：1.05 ratio is add to deionized water,
75~80 DEG C of heating water baths and stir 15~30min make it dissolve, be added ascorbic acid stir 4~6h；
Wherein, ascorbic acid and NH4VO3The molar ratio of middle V element is 2：1；
S2：Base material is added in solution made from S1, is spray-dried, in air atmosphere at 400~600 DEG C
It is sintered 6~10h；Or,
Solution made from S1 is stirred to dry, 6~10h of sintering at 400~600 DEG C, by sintered product and base material one
It rises and is added in ball grinder, 50~100r/min ball milling 30min, wherein sintered product account for the 1~5% of base material quality；
The chemical formula of the base material is：LiNixCoyMn1-x-yO2, wherein 0.5≤x<1,0<y<1, and x+y<1；
Or LiNixCoyAl1-x-yO2, wherein 0.8≤x<1,0<y<1, and x+y<1.
The present invention also provides the LiVOPO that above-mentioned preparation method is prepared4The nickelic ternary of lithium ion battery of cladding is just
Pole material.
The present invention also provides above-mentioned LiVOPO4The nickelic tertiary cathode material of lithium ion battery of cladding is in lithium ion battery
In application.
Compared with prior art, the beneficial effects of the present invention are：
The present invention is with LiVOPO4For clad ascorbic acid is selected with nickelic ternary material (NCA and NCM) for substrate not
It is only used as reducing agent, the function being also complexed, by controlling the ratio of ascorbic acid and middle V, and it is molten to combine spray drying to assist
Liquid method or ball-milling method are coated, and the nickelic tertiary cathode material of lithium ion battery that clad accounts for substrate quality 1~5% is obtained,
Structure and morphology characterization is carried out to the tertiary cathode material being prepared using scanning electron microscope, is finding prepared ternary just
Upper LiVOPO is successfully coated on the material of pole4；And XRD test results show that prepared positive electrode crystal structure does not occur
Prodigious variation.Through electro-chemical test, tertiary cathode material prepared by this method be a kind of high power capacity, high circulation, high magnification, from
Electron conductivity is high, the excellent ternary cathode material of lithium ion battery of security performance.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Surface prepared by Fig. 1 embodiment of the present invention 3 coats LiVOPO4Lithium ion battery nickelic tertiary cathode material
SEM photograph.
Specific implementation mode
In order to enable those skilled in the art to more fully understand, technical scheme of the present invention is practiced, with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
Unless otherwise defined, the hereinafter used all technical terms for being and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.Unless otherwise specified, it the various raw materials used in the following embodiment of the present invention, reagent, instrument and sets
It is standby to be commercially available by market or be prepared by existing method.
Embodiment 1
S1：Take NH4VO31.1698g, (NH4)2HPO41.3105g, LiNO30.7239g, be added to 200mL go from
In sub- water, 80 DEG C of heating water baths simultaneously stir 30min and make it dissolve, be added 3.5226g ascorbic acid as reducing agent be complexed
6h is stirred in agent；
S2：By the LiNi of 168.88g0.6Co0.2Mn0.2O2It is added in solution made from S1, is spray-dried, in air
600 DEG C of sintering 8h, obtain target product, it is about 1% that wherein clad, which accounts for substrate quality, obtains LiVOPO4The lithium ion of cladding
The nickelic tertiary cathode material of battery.
Embodiment 2
S1：Take NH4VO30.4095g, (NH4)2HPO40.4587g, LiNO30.2534g, be added to 200mL go from
In sub- water, 80 DEG C of heating water baths simultaneously stir 30min and make it dissolve, and 1.2329g ascorbic acid is added and stirs 6h；
S2：By the LiNi of 11.8216g0.8Co0.1Mn0.1O2It is added in solution made from S1, is spray-dried, in air
500 DEG C of sintering 8h, it is about 5% that wherein clad, which accounts for substrate quality, obtains LiVOPO4The nickelic ternary of lithium ion battery of cladding is just
Pole material.
Embodiment 3
S1：Take NH4VO31.1698g, (NH4)2HPO41.3105g, LiNO30.7239g, be added to 200mL go from
In sub- water, 80 DEG C of heating water baths simultaneously stir 30min and make it dissolve, and 3.5226g ascorbic acid is added and stirs 6h；
S2：Solution made from S1 is stirred to dry, 8h is sintered at 525 DEG C, obtains sintered product, take 1g sintered products with
50g LiNi0.8Co0.15Al0.05O2Mixing, is added in ball grinder, 100r/min ball milling 30min, wherein sintered product together
The 2% of base material quality is accounted for, LiVOPO is obtained4The nickelic tertiary cathode material of lithium ion battery of cladding.
Further, in order to further test the electric property of the tertiary cathode material, we take 80mg embodiments respectively
1~3 LiVOPO prepared4The nickelic tertiary cathode material of lithium ion battery, 10mg PVDF and the 10mg conductive blacks of cladding
It is configured to slurry, and is coated on aluminium foil with 200 μm of height faces of scraper, and dries and forms tertiary cathode piece.Positive plate is rushed
It is pressed into the pole piece of a diameter of 12mm, and lithium ion battery is prepared into using conventional method, then in 25 DEG C, 0.5C charge-discharge magnifications
Under be tested for the property, specific performance test result is as shown in table 1：
The performance test results of 1 each tertiary cathode material of table
As can be seen from Table 1, by LiVOPO4The nickelic tertiary cathode material of cladding not only has and recycles well surely
Qualitative and higher coulombic efficiency for the first time, and there is higher specific capacity.It is a kind of high performance lithium ion cell positive material
Material.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.Embodiment described above is only to absolutely prove the present invention
And the preferred embodiment lifted, protection domain are without being limited thereto.Those skilled in the art institute on the basis of the present invention
The equivalent substitute of work or transformation, within protection scope of the present invention, protection scope of the present invention is subject to claims.
Claims (3)
1. a kind of LiVOPO4The preparation method of the nickelic tertiary cathode material of lithium ion battery of cladding, which is characterized in that including such as
Lower step：
S1：By NH4VO3, (NH4)2HPO4And LiNO3In molar ratio 1：1：1.05 ratio is add to deionized water, 75~
80 DEG C of heating water baths and stir 15~30min make it dissolve, be added ascorbic acid, stir 4~6h；
Wherein, ascorbic acid and NH4VO3The molar ratio of middle V element is 2：1；
S2：Base material is added in solution made from S1, is spray-dried, 6 are sintered at 400~600 DEG C in air atmosphere
~10h；Or,
Solution made from S1 is stirred to doing, 6~10h is sintered at 400~600 DEG C, sintered product is added together with base material
Enter into ball grinder, 50~100r/min ball milling 30min, wherein sintered product account for the 1~5% of base material quality；
The chemical formula of the base material is：LiNixCoyMn1-x-yO2, wherein 0.5≤x<1,0<y<1, and x+y<1；
Or LiNixCoyAl1-x-yO2, wherein 0.8≤x<1,0<y<1, and x+y<1.
2. the LiVOPO that preparation method according to claim 1 is prepared4The nickelic tertiary cathode of lithium ion battery of cladding
Material.
3. LiVOPO according to claim 24The nickelic tertiary cathode material of lithium ion battery of cladding is in lithium ion battery
Application.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109713252A (en) * | 2018-11-30 | 2019-05-03 | 高点(深圳)科技有限公司 | The high nickelic tertiary cathode material and its preparation method and application of electrical property consistency |
| CN117038996A (en) * | 2023-10-10 | 2023-11-10 | 浙江帕瓦新能源股份有限公司 | α-NaVOPO 4 Coated sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
| WO2024113626A1 (en) * | 2022-11-30 | 2024-06-06 | 格林美（无锡）能源材料有限公司 | High-nickel ternary positive electrode material using lithium fast-ion conductor as coating layer, preparation method therefor, and application thereof |
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| CN106784726A (en) * | 2017-01-18 | 2017-05-31 | 长安大学 | Vanadyl phosphate lithium is modified lithium-rich manganese-based layered lithium ion battery positive electrode and preparation method thereof |
| CN107275584A (en) * | 2016-03-30 | 2017-10-20 | Tdk株式会社 | Positive electrode active material for lithium ion secondary battery and use its lithium ion secondary battery anode and lithium rechargeable battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109713252A (en) * | 2018-11-30 | 2019-05-03 | 高点(深圳)科技有限公司 | The high nickelic tertiary cathode material and its preparation method and application of electrical property consistency |
| WO2024113626A1 (en) * | 2022-11-30 | 2024-06-06 | 格林美（无锡）能源材料有限公司 | High-nickel ternary positive electrode material using lithium fast-ion conductor as coating layer, preparation method therefor, and application thereof |
| CN117038996A (en) * | 2023-10-10 | 2023-11-10 | 浙江帕瓦新能源股份有限公司 | α-NaVOPO 4 Coated sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
| CN117038996B (en) * | 2023-10-10 | 2024-01-23 | 浙江帕瓦新能源股份有限公司 | α-NaVOPO 4 Coated sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
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Application publication date: 20180828 |