CN109546146A - Preparation method of rich lithium ternary electrode material and products thereof and application - Google Patents
Preparation method of rich lithium ternary electrode material and products thereof and application Download PDFInfo
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- CN109546146A CN109546146A CN201811548949.XA CN201811548949A CN109546146A CN 109546146 A CN109546146 A CN 109546146A CN 201811548949 A CN201811548949 A CN 201811548949A CN 109546146 A CN109546146 A CN 109546146A
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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
-
- 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
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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 relates to preparation method of a kind of rich lithium ternary electrode material and products thereof and applications, using the composition principle of MOF, with nickel salt, cobalt salt, manganese salt, terephthalic acid (TPA) and organic solvent are raw material, the method for using hydro-thermal is co-precipitated nickel cobalt manganese in the form of MOF, generates ternary precursor material；Nickel salt, cobalt salt, manganese salt molar ratio are y:y:1-x-2y, wherein the molar ratio of 0.2≤x < 1,0 < y < 0.5, nickel salt, cobalt salt, manganese salt and terephthalic acid (TPA) is 1:3, hydrothermal temperature is 150 DEG C ~ 180 DEG C, and the time is 12 hours；Product centrifugation, drying after hydro-thermal, 700 DEG C of calcinings obtain M in 5 hours in Muffle furnace3O4, by M3O4With Li2CO31:0.729 is uniformly mixed in mass ratio, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.Invention is avoided during the preparation process using precipitating reagent, so as to avoid the introducing of heteroion.
Description
Technical field
The present invention relates to a kind of lithium ion battery electrode material, in particular to a kind of preparation side of rich lithium ternary electrode material
Method and products thereof and application, specifically a kind of synthetic method using MOF prepares rich lithium ternary material.
Technical background
Lithium ion battery is a kind of energy accumulating device, has many advantages, such as that voltage is high, specific energy is big, safety is good, wide
General to be applied to various electronic products, wherein electrode material is the principal element for influencing performance of lithium ion battery.
Market-oriented anode material of lithium battery includes: cobalt acid lithium, LiMn2O4, LiFePO4 and ternary material etc. at present
Product.Wherein, the advantages such as rich lithium ternary material is high with its capacity, and production cost is low, it is considered to be energy-density lithium ion battery
The strong competitor of positive electrode.However a large number of studies show that, rich lithium ternary material is during high voltage charge and discharge, for the first time
Excessively de- lithium will lead to the destruction of material surface lattice structure to influence its chemical property, so improving rich lithium ternary material
Structure stability, improving its chemical property is the major issue currently to be solved.
The common preparation method of richness lithium ternary has hydro-thermal method, solvent-thermal method and coprecipitation at present.But with solvent heat
Method when preparing rich lithium ternary material, it is time-consuming more there are synthetic material yield is few, the problems such as higher cost.It is used in hydro-thermal method
Water is reunited seriously as the material that solvent synthesizes, and is hindered lithium ion transport, is influenced its chemical property.It is prepared using coprecipitation
When, and have the problem of ammonium hydroxide volatilization influences environment.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide a kind of preparation methods of rich lithium ternary electrode material.
Another object of the present invention is: providing a kind of rich lithium ternary electrode material product of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of richness lithium ternary electrode material has using metal
The composition principle of machine frame structure (MOF), with nickel salt, cobalt salt, manganese salt, terephthalic acid (TPA) and organic solvent are raw material, using water
The method of heat is co-precipitated nickel cobalt manganese in the form of MOF, generates ternary precursor material；Nickel salt, cobalt salt, manganese salt molar ratio are y:
Y:1-x-2y, wherein the molar ratio of 0.2≤x < 1,0 < y < 0.5, nickel salt, cobalt salt, manganese salt and terephthalic acid (TPA) is 1:3, hydro-thermal
Temperature is 150 DEG C ~ 180 DEG C, and the time is 12 hours；Product centrifugation, drying after hydro-thermal, 700 DEG C of calcinings 5 are small in Muffle furnace
When obtain M3O4, by M3O4With Li2CO31:0.729 is uniformly mixed in mass ratio, is calcined 8h at 900 DEG C in Muffle furnace, is obtained richness
Lithium ternary material.
Mechanism of the present invention: using organic solvent as solvent, nickel, cobalt, manganese is made to form co-precipitation in the form of MOF, to change
It has been apt to the agglomeration traits of rich lithium ternary material during the preparation process.
The nickel salt is one or more of nickel sulfate, nickel nitrate, nickel acetate or nickel chloride.
The cobalt salt is one or more of cobaltous sulfate, cobalt nitrate, cobalt acetate or cobalt chloride.
The manganese salt is one or more of manganese sulfate, manganese nitrate, manganese acetate or manganese chloride.
The organic solvent is one or more of n,N-Dimethylformamide, N-Methyl pyrrolidone, methanol
Mixture.
The present invention provides a kind of rich lithium ternary electrode material, is prepared according to any of the above-described the method.
The present invention provides a kind of rich lithium ternary electrode material in lithium ion battery as the application of positive electrode.
The present invention provides a kind of method that the means using synthesis MOF prepare rich lithium ternary material, this benefits
The method for using the means of synthesis MOF to prepare rich lithium ternary material has compared to original method advantage: using organic solvent as molten
Agent makes nickel cobalt manganese form co-precipitation in the form of MOF, improves the agglomeration traits of rich lithium ternary material during the preparation process, from
And improve performance.
The present invention is compared with prior art, and advantage is that the present invention using organic solvent as solvent, makes nickel, cobalt, manganese with MOF
Form formed co-precipitation, the agglomeration traits of rich lithium ternary material during the preparation process are improved, so as to improve performance.Meanwhile
The present invention is avoided during the preparation process using precipitating reagent, so as to avoid the introducing of heteroion.
Detailed description of the invention:
Fig. 1 is the first effect performance map of richness lithium ternary material obtained in embodiment 1；
Fig. 2 is the discharge-rate figure of richness lithium ternary material obtained in embodiment 1.
Specific embodiment:
The present invention is further described below by specific embodiment and in conjunction with attached drawing, but is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of richness lithium ternary electrode material, using the composition principle of MOF, with nickel salt, cobalt salt, manganese salt, to benzene two
Formic acid and organic solvent are raw material, and the method for using hydro-thermal is co-precipitated nickel cobalt manganese in the form of MOF, generate ternary precursor material
Material, wherein nickel acetate, cobalt acetate, manganese acetate are dissolved in n,N-Dimethylformamide by the molar ratio of 1:1:5 obtains solution A；It will
Terephthalic acid (TPA), which is dissolved in n,N-Dimethylformamide, obtains B solution, wherein the molar ratio of terephthalic acid (TPA) and metal salt is
3:1；B solution is slowly added drop-wise in solution A in the case of stirring, continues stirring 1 hour after being added dropwise to complete, is then transferred to water
12 hours are kept the temperature for 150 DEG C in hot kettle；Product centrifugation, drying after hydro-thermal, 700 DEG C of calcinings obtain M in 5 hours in Muffle furnace3O4,
By M3O4With Li2CO31:0.729 is uniformly mixed in mass ratio, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material
Material.
Richness obtained in the first effect performance map and Fig. 2 the present embodiment of the richness lithium ternary material as obtained in Fig. 1 the present embodiment
Shown in the discharge-rate figure of lithium ternary material, superior electrical property.
Embodiment 2
A kind of preparation method of richness lithium ternary electrode material, it is approximate with embodiment 1, wherein by nickel nitrate, cobalt nitrate, manganese nitrate
It is dissolved in n,N-Dimethylformamide by the molar ratio of 1:1:5 and obtains solution A, terephthalic acid (TPA) is dissolved in N, N- dimethyl formyl
B solution is obtained in amine, wherein the molar ratio of terephthalic acid (TPA) and metal salt is 3:1；In the case of stirring slowly by B solution
It is added drop-wise in solution A, continues stirring 1 hour after being added dropwise to complete, be then transferred in water heating kettle and keep the temperature 12 hours for 150 DEG C；After hydro-thermal
Product centrifugation, drying, 700 DEG C of calcinings obtain M in 5 hours in Muffle furnace3O4, by M3O4With Li2CO31:0.729 in mass ratio
Uniformly mixing, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.
Embodiment 3
A kind of preparation method of richness lithium ternary electrode material, it is approximate with embodiment 1, wherein by nickel acetate, cobalt acetate, manganese acetate
It is dissolved in N-Methyl pyrrolidone by the molar ratio of 1:1:5 and obtains solution A, terephthalic acid (TPA) is dissolved in N-Methyl pyrrolidone
B solution is obtained, wherein the molar ratio of terephthalic acid (TPA) and metal salt is 3:1；B solution is slowly added dropwise in the case of stirring
Into solution A, continue stirring 1 hour after being added dropwise to complete.Then it is transferred in water heating kettle and keeps the temperature 12 hours for 150 DEG C.Production after hydro-thermal
Object centrifugation, drying, 700 DEG C of calcinings obtain M in 5 hours in Muffle furnace3O4, by M3O4With Li2CO31:0.729 is uniform in mass ratio
Mixing, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.
Claims (7)
1. a kind of preparation method of richness lithium ternary electrode material, which is characterized in that former using the synthesis of metal framework structure (MOF)
Reason, using nickel salt, cobalt salt, manganese salt, terephthalic acid (TPA) and organic solvent as raw material, the method for using hydro-thermal makes nickel cobalt manganese with MOF's
Form co-precipitation, generates ternary precursor material；Nickel salt, cobalt salt, manganese salt molar ratio is y:y:1-x-2y, wherein 0.2≤x < 1,0
<y<0.5；The molar ratio of nickel salt, cobalt salt, manganese salt and terephthalic acid (TPA) is 1:3, and hydrothermal temperature is 150 DEG C ~ 180 DEG C, and the time is
12 hours；Product centrifugation, drying after hydro-thermal, 700 DEG C of calcinings obtain M in 5 hours in Muffle furnace3O4, by M3O4With Li2CO3
1:0.729 is uniformly mixed in mass ratio, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.
2. the preparation method of rich lithium ternary electrode material as described in the appended claim 1, it is characterised in that: the nickel salt is sulfuric acid
One or more of nickel, nickel nitrate, nickel acetate or nickel chloride；The cobalt salt is cobaltous sulfate, cobalt nitrate, cobalt acetate or cobalt chloride
One or more of；The manganese salt is one or more of manganese sulfate, manganese nitrate, manganese acetate or manganese chloride；It is described organic
Solvent is one or more mixtures of n,N-Dimethylformamide, N-Methyl pyrrolidone, methanol.
3. the preparation method of rich lithium ternary electrode material as stated in claim 2, it is characterised in that: by nickel acetate, cobalt acetate,
Manganese acetate is dissolved in n,N-Dimethylformamide by the molar ratio of 1:1:5 obtains solution A；Terephthalic acid (TPA) is dissolved in N, N- diformazan
B solution is obtained in base formamide, wherein the molar ratio of terephthalic acid (TPA) and metal salt is 3:1；In the case of stirring by B
Solution is slowly added drop-wise in solution A, continues stirring 1 hour after being added dropwise to complete；Then it is small that 150 DEG C of heat preservations 12 in water heating kettle are transferred to
When；The product obtained after hydro-thermal 700 DEG C of calcinings in Muffle furnace obtain M in 5 hours3O4, by M3O4With Li2CO31:0.729 in mass ratio
Uniformly mixing, calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.
4. the preparation method of rich lithium ternary electrode material as stated in claim 2, it is characterised in that: by nickel nitrate, cobalt nitrate,
Manganese nitrate is dissolved in n,N-Dimethylformamide by the molar ratio of 1:1:5 obtains solution A, and terephthalic acid (TPA) is dissolved in N, N- diformazan
B solution is obtained in base formamide, wherein the molar ratio of terephthalic acid (TPA) and metal salt is 3:1；It is in the case of stirring that B is molten
Liquid is slowly added drop-wise in solution A, continues stirring 1 hour after being added dropwise to complete；Then it is transferred in water heating kettle and keeps the temperature 12 hours for 150 DEG C；
The product obtained after hydro-thermal 700 DEG C of calcinings in Muffle furnace obtain M in 5 hours3O4, by M3O4With Li2CO31:0.729 is equal in mass ratio
Even mixing calcines 8h at 900 DEG C in Muffle furnace, obtains rich lithium ternary material.
5. the preparation method of rich lithium ternary electrode material as stated in claim 2, it is characterised in that: by nickel acetate, cobalt acetate,
Manganese acetate is dissolved in N-Methyl pyrrolidone by the molar ratio of 1:1:5 obtains solution A, and terephthalic acid (TPA) is dissolved in N- methylpyrrole
B solution is obtained in alkanone, wherein the molar ratio of terephthalic acid (TPA) and metal salt is 3:1；It is in the case of stirring that B solution is slow
Slowly it is added drop-wise in solution A, continues stirring 1 hour after being added dropwise to complete；Then it is transferred in water heating kettle and keeps the temperature 12 hours for 150 DEG C；Hydro-thermal
The product obtained afterwards 700 DEG C of calcinings in Muffle furnace obtain M in 5 hours3O4, by M3O4With Li2CO31:0.729 is uniformly mixed in mass ratio
It closes, calcines 8h at 900 DEG C in Muffle furnace, obtain rich lithium ternary material.
6. a kind of richness lithium ternary electrode material, it is characterised in that -5 any the methods are prepared according to claim 1.
7. a kind of lithium ternary electrode material rich according to claim 6 is in lithium ion battery as the application of positive electrode.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110350185A (en) * | 2019-07-09 | 2019-10-18 | 广州大学 | A kind of Fluorin doped lithium-rich anode material and the preparation method and application thereof |
| CN112928254A (en) * | 2021-01-25 | 2021-06-08 | 合肥工业大学 | Ternary positive electrode material based on NiCoMn-MOF and preparation method thereof |
| CN113184922A (en) * | 2021-04-23 | 2021-07-30 | 浙江晨阳新材料有限公司 | Sodium ion battery positive electrode material, preparation method and application |
| CN114373638A (en) * | 2022-01-19 | 2022-04-19 | 桂林电子科技大学 | Coral NiCoMn-MOF material and preparation method and application thereof |
| CN117199601A (en) * | 2023-11-01 | 2023-12-08 | 深圳汇能储能材料工程研究中心有限公司 | Regeneration method of waste nickel-cobalt-manganese ternary cathode material and cathode material |
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