CN108172799A - A kind of tertiary cathode material of nucleocapsid structure lithium ion battery and preparation method thereof - Google Patents
A kind of tertiary cathode material of nucleocapsid structure lithium ion battery and preparation method thereof Download PDFInfo
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- CN108172799A CN108172799A CN201711454528.6A CN201711454528A CN108172799A CN 108172799 A CN108172799 A CN 108172799A CN 201711454528 A CN201711454528 A CN 201711454528A CN 108172799 A CN108172799 A CN 108172799A
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery, includes the following steps, 1)Prepare nickel salt, cobalt salt, manganese salt, aluminium salt Diversity solution;2)Under protective atmosphere, Diversity solution is added to ammonium hydroxide and sodium hydroxide cocurrent in the reaction unit containing bottom liquid, is carried out coprecipitation reaction and is obtained the hydroxide precursor of NCM;3)Being passed through carbon dioxide gas causes NCM presomas surface to form one layer of aluminium hydroxide clad;4)Above-mentioned presoma is filtered, is washed, dry after add in lithium source carry out being thermally treated resulting in the NCM materials that surface is coated with aluminium oxide.The presoma even pore distribution of nucleocapsid produced by the present invention, spacing is moderate, large specific surface area.Presoma obtained and lithium salts are further processed to obtain anode material for lithium-ion batteries, high charge-discharge specific capacity, long circulating stability energy and good high rate performance can be shown.
Description
Technical field
The present invention relates to a kind of lithium ion battery positive electrode more particularly to a kind of nucleocapsid structure lithium ion battery three
First positive electrode and preparation method.
Background technology
At present, fossil fuel is still main for electric resources.However as the mankind unreasonable exploitation and utilization, fossil
Energy day is becoming tight, environmental pollution getting worse.Therefore, new cleaning resource and regenerative resource, such as sun are developed and used
Energy, wind energy, tide energy etc. become the task of top priority.But then, the normal operation of power grid needs the power generation of steady and continuous, too
Positive energy, wind energy, tide energy etc. are restricted by factors such as weather, place and times, are significantly limited it and on a large scale should
With with it is universal.In order to solve this problem, extensive electrochemical energy storage technology becomes an important field of research.Wherein, two
Primary cell becomes the only selection of extensive storing up electricity due to having higher energy density and transformation efficiency, and cycle life
Long and with highest energy density lithium ion battery is considered as most promising secondary cell.
According to the planning of current country, the energy density positive to the year two thousand twenty reaches 250mAh/g or even arrives 300mAh/g's
Energy density index, then the electrode material system of present commercial applications can not all be realized, therefore just need larger technology
Reform.By taking electric vehicle as an example, to run farther, must just there are the higher energy content of battery and continuation of the journey, just be widely used at present
The needs for meeting development have been difficult to for the LFP of power battery.And ternary battery higher energy density and is followed compared to having
Ring performance becomes the only selection of battery system.
Place of the positive electrode as storage lithium ion main inside current lithium ion battery, performance directly affect lithium
The performance of ion battery.However as the continuous improvement of capacity, this gesture of the high rate performance and bad stability of tertiary cathode material
The big hidden danger that lithium ion battery is hindered to advance must be become.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide it is a kind of it is simple for process, reproducible,
Of low cost, environmental-friendly nucleocapsid structure lithium ion battery positive electrode and preparation method thereof.
In order to solve the above technical problems, technical solution proposed by the present invention is:The three of a kind of nucleocapsid structure lithium ion battery
The preparation method of first positive electrode, it is characterised in that:Include the following steps, 1)Prepare nickel salt, cobalt salt, manganese salt, aluminium salt it is polynary
Mixed solution;
2)Under protective atmosphere, by step 1)Diversity solution and ammonium hydroxide and sodium hydroxide cocurrent be added to containing bottom liquid
Reaction unit in, adjust flow, pH, ammonium root concentration, rotating speed, temperature and carry out before coprecipitation reaction obtains the hydroxide of NCM
Drive body;In the present invention, bottom liquid is sodium hydroxide and the mixed liquor of ammonium hydroxide.
3)Stop adding in sodium hydroxide, ammonium hydroxide and complex solution, be passed through carbon dioxide gas and cause NCM presomas surface shape
Into one layer of aluminium hydroxide clad;
4)Above-mentioned presoma is filtered, is washed, dry after add in lithium source and carry out being thermally treated resulting in surface and be coated with aluminium oxide
NCM materials.
The presoma even pore distribution of nucleocapsid produced by the present invention, spacing is moderate, large specific surface area.By made from
Presoma is further processed to obtain anode material for lithium-ion batteries with lithium salts, and it is steady can to show high charge-discharge specific capacity, long circulating
Qualitative energy and good high rate performance.In addition, the method for the present invention is simple for process, reproducible, of low cost, environmental-friendly.
Aluminium salt is directly dissolved in complex solution by the present invention, is uniformly adhered in the form of meta-aluminic acid root at a high ph
NCM presomas surface, being passed through carbon dioxide gas later can be in the homogeneous precipitation of presoma surface, and then it is good to obtain compactness
And consistent protective film.Later by being filtered, washed, drying.Heat treatment removes the nucleocapsid that the impurity in presoma obtains
Positive electrode.
Aluminium oxide as good ion conductor, be uniformly coated on ternary material surface be conducive to lithium ion uniformly from
All directions deintercalation.And its chemical property is stablized, and one layer of stable interface is formd between electrolyte and positive electrode, is avoided
Electrolytic corrosion positive electrode and the stabilization for advantageously ensuring that structure.Not only ensure that capacity, but can improve material circulation performance, times
The problems such as rate poor performance.
In the present invention, the nickel salt is at least one of nickel nitrate, nickel chloride, nickel acetate, nickel sulfate, preferably sulphur
Sour nickel or nickel chloride.The manganese salt is at least one of manganese nitrate, manganese chloride, manganese acetate, manganese sulfate, preferably sulfuric acid
Manganese or manganese chloride;The cobalt salt is at least one of cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate, preferably sulfuric acid
Cobalt, cobalt chloride;The aluminium salt is at least one of aluminum sulfate, aluminium chloride, aluminum nitrate, aluminium acetate, preferably aluminum sulfate, chlorine
Change aluminium.
In the present invention, step 1)Described in the nickel of Diversity solution, cobalt, manganese element molar ratio be 8:1:1.Step 1)
Described in the molar ratio of aluminium and cobalt or manganese be 1:20-3:10.Not only it can guarantee material capacity under the ratio, but also be conducive in particle
Surface forms the clad that even compact and thickness are suitble to.Wherein step 1)Described in the optimum mole ratio of aluminium and cobalt or manganese be
1:10-1:5。
In the present invention, step 2)The charging rate of middle Diversity solution is 90-150ml/min;Sodium hydroxide charging speed
It spends for 30-70ml/min;Ammonium hydroxide charging rate is 5-40ml/min.Wherein, step 2)The charging rate of middle Diversity solution
For 100-140ml/min;Sodium hydroxide charging rate is 40-60ml/min;Ammonium hydroxide charging rate is the 10-30ml/min ranges
The endoparticle speed of growth is stablized, good sphericity.
In the present invention, step 1)The total ion concentration of middle Diversity solution is 1mol/L-1.5mol/L, and sodium hydroxide is molten
Liquid a concentration of 7.5-10mol/L, ammonia concn 6-8mol/L.Step 2)The PH of middle coprecipitation reaction be 10-12, ammonium root from
A concentration of 5-9g/L of son;Reaction temperature is 50-60 °C, speed of agitator 200-300r/min.
In the present invention, step 4)Middle addition lithium source carries out heat treatment as lithium salts:Ternary precursor=1.05:1 mixing, in oxygen
2-4h first is pre-sintered at 300-500 °C under gas atmosphere, then is warming up to 800-1000 °C of sintering 10-16h.In the present invention, pre-burning
Junction temperature is 300oC-500 oC.Under the collaboration of aforementioned condition, then coordinate the sintering temperature, anode material obtained can be made
The even pore distribution of material, spacing is moderate, and porosity is high, large specific surface area, good conductivity.
A kind of positive electrode of nucleocapsid structure lithium ion battery in the present invention is also provided, is made by above-mentioned preparation method,
The material is nucleocapsid, and kernel is NCM ternary materials, and shell is aluminium oxide, and for lithium ion battery ternary precursor and
Positive electrode.The D50 granularities of the kernel of the positive electrode are 8-12um, and the thickness of alumina-coated layer is 50-500nm.
The ternary precursor and anode material spherical degree of a kind of nucleocapsid of invention are good, even particle distribution,
There are higher specific surface area and tap density, and alumina layer is suitble to the transmission of lithium ion, be conducive to stablize electrolyte and anode
The interface of material can effectively improve the cyclical stability and high rate performance of material, and preparation method is simple, easily controllable, fit
Close industrialization production.
Compared with prior art, the advantage of the invention is that:
1)The present invention is directly dissolved in aluminium salt in material solution, and meta-aluminic acid is converted by the amphotericity and its of aluminium hydroxide
The property of root.It is made to be then converted to aluminium hydroxide by the effect of carbon dioxide later and obtain the presoma of nucleocapsid.
2)The positive electrode of alumina-coated is obtained by sintering.Stable interface can be formed by alumina-coated layer,
Positive electrode is avoided by electrolytic corrosion, and aluminium oxide is conducive to the diffusion transport of lithium ion as good ion conductor.It will
The material is used as the anode of lithium ion battery, has excellent electric property.
3)In preparation method of the present invention, assisted by the conditions such as the aluminium salt and material rate, pH, ammonium root concentration, rotating speed
With under, alumina-coated layer can be controlled in suitable range, and then other electrifications can also be improved while guaranteed capacity
Learn performance.
4)The positive electrode of the present invention can be used for preparing steady with high specific discharge capacity, excellent high rate performance and long circulating
The lithium ion battery of qualitative energy.
5)The present invention the carbon material method for preparing operation is simple and reliable, it is reproducible, operability is strong, it is environmental-friendly, into
This is cheap, has wide industrial applications prospect.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of nucleocapsid structure lithium ion battery positive electrode made from embodiment 1(SEM).
Fig. 2 is the transmission electron microscope picture of nucleocapsid structure lithium ion battery positive electrode made from embodiment 1(TEM).
Specific embodiment
For the ease of understanding the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter 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.
Embodiment
The present embodiment provides a kind of preparation method of nucleocapsid structure lithium ion battery tertiary cathode material, including following step
Suddenly:
Step 1), according to Ni:Co:Mn=8:1:1:The ratio of 0.1-0.2 prepare nickel salt, cobalt salt, manganese salt, aluminium salt Diversity
Solution, total ion concentration 1mol/L-1.5mol/L;
2), the sodium hydroxide cocurrent of mixed solution obtained above and 6-8mol/L ammonium hydroxide and 7.5-10mol/L is added to and is contained
In the reaction unit for having bottom liquid, the charging rate for adjusting mixing complex solution is 100-140ml/min, sodium hydroxide charging rate
It is 10-30ml/min for 40-60ml/min, ammonium hydroxide charging rate.Reaction temperature is 50-60 °C, rotating speed 200-400r/min.
PH is 10-12, and a concentration of 5-9g/L of ammonium ion carries out coprecipitation reaction and obtains hydroxide precursor.
3), stop adding in sodium hydroxide, ammonium hydroxide and complex solution, be passed through carbon dioxide gas and cause NCM presomas surface
Form one layer of aluminium hydroxide clad;
4), above-mentioned presoma is centrifuged, washed and is dried, and takes lithium salts:Ternary precursor=1.05:1 mixing, in oxygen
2-4h first is pre-sintered at 400-450 °C under atmosphere, then is warming up to 800-1000 °C of sintering 10-16h to get to the nucleocapsid knot
The ternary material of structure.
Embodiment 1
The sulfate liquor that total concentration of metal ions is 1.5mol/L is configured(Ni:Co:Mn:Al=8:1:1:0.2).It will be above-mentioned mixed
It closes solution to be added in the reaction kettle containing ammonium hydroxide and sodium hydroxide mixed liquor together with ammonium hydroxide and sodium hydroxide, adjusts reaction kettle and turn
Speed is 300r/min, and temperature is 55 degree.Mother liquor ammonium root a concentration of 6-8g/L, pH 12 are adjusted, is made in solution by evenly mixing
Nickel, cobalt, manganese comes out according to chemical dosage ratio co-precipitation.Stop adding in raw material, and be passed through carbon dioxide gas later.Finally
Above-mentioned presoma is filtered, wash, is dried.Finally take lithium hydroxide:Presoma=1.05:1, under oxygen atmosphere first
3h is pre-sintered at 400-450 °C, then is warming up to 800-1000 °C of sintering 14h to get to the ternary material of the nucleocapsid.
The material of nucleocapsid manufactured in the present embodiment is used as working electrode, lithium piece is to electrode, is assembled into button electricity
Chemical property under the multiplying power of 1C, is tested in pond.In the present embodiment, the scanning electricity of nucleocapsid structure lithium ion battery positive electrode
Mirror figure(SEM)As shown in Figure 1.In the present embodiment, the transmission electron microscope picture of nucleocapsid structure lithium ion battery positive electrode(TEM)Such as figure
Shown in 2.
By test result it is found that lithium electricity prepared by this example is just having good chemical property;It is first under the multiplying power of 1C
It is 88% to enclose coulombic efficiency, after 100 circle of cycle, remains to keep the specific capacity of 160mA/g.
Comparative example 1
The sulfate liquor that total concentration of metal ions is 1.5mol/L is configured(Ni:Co:Mn=8:1:1), by above-mentioned solution together with ammonia
Water and sodium hydroxide are added in the reaction kettle containing sodium hydroxide and ammonia water mixture, and it is 300r/ to adjust reaction kettle rotating speed
Min, temperature are 55 degree.Adjust mother liquor ammonium root a concentration of 6-8g/L, pH 12, make each component in solution by evenly mixing by
It is come out according to chemical dosage ratio co-precipitation.Lithium hydroxide is taken later:Presoma=1.05:1, first in 400- under oxygen atmosphere
450 °C of pre-sintering 3h, then 800-1000 °C of sintering 14h is warming up to get to spheral anode material.
Spheroidal material manufactured in the present embodiment is used as working electrode, lithium piece is to electrode, button cell is assembled into, in 1C
Multiplying power under, test chemical property.
By test result it is found that the lithium electricity anode chemical property of this example preparation is poor;Under the multiplying power of 1C, first circle coulomb
Efficiency is 73%, after 100 circle of cycle, is only capable of keeping the specific capacity of 110mA/g.
Claims (10)
1. a kind of preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery, it is characterised in that:Include the following steps,
1)Prepare nickel salt, cobalt salt, manganese salt, aluminium salt Diversity solution;
2)Under protective atmosphere, by step 1)Diversity solution and ammonium hydroxide and sodium hydroxide cocurrent be added to containing bottom liquid
Reaction unit in, adjust flow, pH, ammonium root concentration, rotating speed, temperature and carry out before coprecipitation reaction obtains the hydroxide of NCM
Drive body;
3)Stop adding in sodium hydroxide, ammonium hydroxide and complex solution, be passed through carbon dioxide gas and NCM presomas surface is caused to form one
Layer aluminium hydroxide clad;
4)Above-mentioned presoma is filtered, is washed, dry after add in lithium source and carry out being thermally treated resulting in surface and be coated with aluminium oxide
NCM materials.
2. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:The nickel salt is at least one of nickel nitrate, nickel chloride, nickel acetate, nickel sulfate;The manganese salt is manganese nitrate, chlorine
Change at least one of manganese, manganese acetate, manganese sulfate;The cobalt salt is cobalt nitrate, cobalt chloride, cobalt acetate, in cobaltous sulfate extremely
Few one kind;The aluminium salt is at least one of aluminum sulfate, aluminium chloride, aluminum nitrate, aluminium acetate.
3. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 1)Described in the nickel of Diversity solution, cobalt, manganese element molar ratio be 8:1:1.
4. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 1)Described in the molar ratio of aluminium and cobalt or manganese be 1:20-3:10.
5. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 2)The charging rate of middle Diversity solution is 90-150ml/min;Sodium hydroxide charging rate is 30-70ml/
min;Ammonium hydroxide charging rate is 5-40ml/min.
6. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 1)The total ion concentration of middle Diversity solution is 1mol/L-1.5mol/L, concentration of sodium hydroxide solution 7.5-
10mol/L, ammonia concn 6-8mol/L.
7. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 2)The PH of middle coprecipitation reaction is 10-12, a concentration of 5-9g/L of ammonium ion;Reaction temperature is 50-60 °C, is stirred
Mix rotating speed is 200-400r/min.
8. the preparation method of the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 1, feature exist
In:Step 4)Middle addition lithium source carries out heat treatment as lithium salts:Ternary precursor=1.05:1 mixing, first exists under oxygen atmosphere
300-500 °C of pre-sintering 2-4h, then it is warming up to 700-1000 °C of sintering 10-16h.
9. a kind of tertiary cathode material that nucleocapsid structure lithium ion battery is made such as claim 1-9 any one of them preparation methods
Material, it is characterised in that:The material is nucleocapsid, and kernel is NCM ternary materials, and shell is aluminium oxide, and for lithium-ion electric
Pond ternary precursor and positive electrode.
10. the tertiary cathode material of nucleocapsid structure lithium ion battery according to claim 9, it is characterised in that:Kernel
D50 granularities are 8-12um, and the thickness of alumina-coated layer is 50-500nm.
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