CN106058205A - Doped lithium nickel cobalt oxide composite cathode material and preparation method thereof - Google Patents
Doped lithium nickel cobalt oxide composite cathode material and preparation method thereof Download PDFInfo
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- CN106058205A CN106058205A CN201610624688.XA CN201610624688A CN106058205A CN 106058205 A CN106058205 A CN 106058205A CN 201610624688 A CN201610624688 A CN 201610624688A CN 106058205 A CN106058205 A CN 106058205A
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- H—ELECTRICITY
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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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- 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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Abstract
The invention discloses a doped lithium nickel cobalt oxide composite cathode material and a preparation method thereof. The preparation method comprises the following steps: (1), dissolving manganese ion raw materials in water to prepare a solution A, and dissolving a precipitator in the water to prepare a solution B; (2), adding a doped lithium nickel cobalt oxide precursor in the solution A, and adding the solution B to the solution A while stirring; after reaction is completed, filtering the mixed solution, collecting solid matters, and cleaning and drying the solid matters, thereby obtaining solids A; and (3), putting the solids A and a lithium source in an oxygen atmosphere furnace to perform high-temperature roasting, thereby obtaining products after the roasting, namely the doped lithium nickel cobalt oxide composite cathode material existing in a core-shell structure, the surface of which is coated with a spinel lithium manganate layer. According to the preparation method, a layer of spinel lithium manganate cathode material is coated on the surface of the lithium nickel cobalt oxide, so that the efficiency and the cycle life of a battery cell in use can be improved; outmost-layer spinel isolates metallic nickel from directly contacting with electrolyte, so that the stability and the safety of the battery can be effectively improved.
Description
Technical field
The present invention relates to the preparation method of anode material for lithium ion battery, particularly relate to a kind of doping type lithium nickel cobalt dioxide
Composite positive pole and preparation method thereof.
Background technology
The secondary cell that lithium ion battery is a kind of energy density height, merit metric density is high, have extended cycle life, along with fossil energy
The minimizing in source and environmental pollution serious, the most gradually plays irreplaceable effect.Along with electric automobile, intelligence
The fast development of the industries such as electrical network, the demand of lithium-ion-power cell steeply rises, simultaneously in country 13 planning, newly
Energy automobile requires that the energy density of cell is more than 2000 times more than 300Wh/kg, cycle life.This is accomplished by lithium ion
The features such as it is high that electrokinetic cell has monomer energy density, good cycling stability, and security performance is excellent.Doping type lithium nickel cobalt dioxide positive pole
The advantages such as material has that running voltage is high, specific energy big, low cost, safety are good, are highly suitable for lithium-ion-power cell body
System, is one of power type lithium-ion battery anode material with application prospect most.The nickel cobalt acid that aluminum is successfully adulterated by tesla
Lithium is applied in electrically driven treadmill, has more promoted the extensive application in electrokinetic cell of this material.
But, along with the demand of cell energy density and cell performance is gradually increased, doping type nickel cobalt
Acid lithium needs to be improved further in terms of cyclical stability and safety, and existing doping type lithium nickel cobalt dioxide material has become as system
The about bottleneck of high-energy-density electrokinetic cell development.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of doping type lithium nickel cobalt dioxide composite positive pole and preparation thereof
Method, at one layer of spinel lithium manganese oxide anode material of this lithium nickel cobalt dioxide Surface coating, improves the effect of cell during using
Rate and cycle life, outermost Spinel LiMn2O4Isolation metallic nickel directly contacts with electrolyte, can be effectively improved battery
Stability and safety；Preparation method is simple, it is easy to accomplish.
To this end, technical scheme is as follows:
The preparation method of a kind of doping type lithium nickel cobalt dioxide composite positive pole, comprises the steps:
1) manganese ion raw material is dissolved in water and is configured to solution A, molar concentration meter 0.1～2mol/L；Precipitant is dissolved in
Water is configured to solution B, and molar concentration is calculated as 0.1～2mol/L, and the major function of precipitant is that manganese ion is deposited to doping
Type lithium nickel cobalt dioxide surface；
2) by doping type lithium nickel cobalt dioxide presoma add described solution A, under agitation, mixing speed be 100～
500rpm, is added thereto to solution B；Question response completes, and filters, and collects solid content, then washs it, is dried, obtains
Solid A；
Described doping type lithium nickel cobalt dioxide presoma is LiNixCoyM1-x-yO2, based on molal weight, 0.3≤x≤0.9,0.05
≤ y≤0.3, M is Mn, any one or the most several mixture in Al, Cr, Fe, Mg, Zn, Ti；
3) by described solid A and the high-temperature roasting in oxygen atmosphere stove of lithium source, obtain roasting afterproduct, be and tie with nucleocapsid
Structure exists, and top layer is coated with the described doping type lithium nickel cobalt dioxide composite positive pole of spinel lithium manganate layer.
Further, described manganese ion raw material be in manganese sulfate, manganese nitrate and manganese acetate any one or the most several
Mixture.
Further, described precipitant is the mixed solution of ammonia and sodium hydroxide, by mol ammonia and sodium hydroxide ratio
Example is 1～20:100, or ammonia and the mixed solution of sodium carbonate, and ammonia and sodium carbonate ratio are 1～20:100 by mol.
Further, described lithium source is one or more in Lithium hydrate, lithium carbonate, lithium nitrate, Quilonorm (SKB).
Preferably, the molecular formula of doping type lithium nickel cobalt dioxide presoma is LiNi0.8Co0.1Mn0.1O2, or
LiNi0.8Co0.15Al0.05O2。
Further, step 3) temperature of described high-temperature roasting is 200～1000 DEG C, the time is 2～15h.
Further, step 3) molecular formula of spinel lithium manganate layer that obtains is Li2Mn2-xMxO4, based on molal weight, 0
≤ x≤0.1, M=Ni, B, Al, Cr, Fe, Mg, Zn, Ti；Preferably, molecular formula is Li2Mn2O4。
Further, step 3) described in the quality of spinel lithium manganate layer account for the 1 of described doping type lithium nickel cobalt dioxide gross mass
～20%.
The present invention is the doping type lithium nickel cobalt dioxide lithium ion cell positive material of synthetic kernel shell structure spinel lithium manganate cladding
Material, shows two aspects to the Main Function of doping type lithium nickel cobalt dioxide material surface coating spinelle lithium manganate material: (1) exists
In charging process, Li+From Li2Mn2O4Middle abjection, with the Li in doping type lithium nickel cobalt dioxide+Embed in negative pole, during electric discharge, Li+From negative
Pole is deviate from, and embeds MnO2In, generate Spinel LiMn2O4, during this, Li2Mn2O4In Li+Si/C negative pole is supplemented lithium
Source, improves efficiency and the safety of cell；(2) Spinel LiMn2O4It is coated on doping type lithium nickel cobalt dioxide surface, isolation
Ni metal directly contacts with electrolyte, reduces the electrolyte corrosion to lithium nickelate, and the LiMn generated2O4There is the knot of excellence
Structure stability and electrolyte have the good compatibility, are conducive to improving cyclical stability and the safety of material.Therefore, logical
Cross doping type lithium nickel cobalt dioxide Surface coating spinelle Li2Mn2O4Preparing doping type lithium nickel cobalt dioxide composite positive pole on the one hand can
To improve cyclical stability and the safety of cell, efficiency and the anti-mistake that on the other hand can improve cell put safety
Property.Coulombic efficiency first and the anti-mistake that additionally can also improve the actual effect battery using Si/C as negative material put safety.
Accompanying drawing explanation
Fig. 1 is the transmission electron micrograph of material in the embodiment of the present invention 1；
Fig. 2 is the embodiment of the present invention 1 and the cyclic curve of material in comparative example 1；
Fig. 3 is the embodiment of the present invention 1 and the DSC curve of material in comparative example 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is described in detail.
Embodiment 1
By 1.83kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2It is equipped with 1mol/L manganese sulfate molten
In the reactor of liquid, being stirred continuously, mixing speed is 500rpm, adds with 30mL/min through dosing pump in reactor
The sodium hydroxide of 0.5mol/L and the mixed solution of ammonia, ammonia and sodium hydroxide ratio are 1:20 by mol, and precipitant adds
After adding, Mn:NaOH=1:2 by mol in reactor, precipitation completely after stand 1h, filter, collect solid, by solid warp
Deionized water wash, drying.Then the solid dried is mixed 60min with Lithium hydrate, in molar ratio in high-speed mixer
1:1 mixes, then high-temperature roasting 15h under the conditions of 800 DEG C, after being cooled to room temperature, size-reduced, sieving obtains Surface coating and have point
The cobalt nickel oxide aluminum lithium composite positive pole of spar mangaic acid lithium layer.
Experimentation:
According to mass ratio, the doping type lithium nickel cobalt dioxide material being coated with spinel lithium manganate layer that the present embodiment is obtained
95%, 3%SP (conductive agent) and 2%PVDF (binding agent) join in NMP, stir and are prepared as anode sizing agent, lithium sheet, electricity
Solve liquid (the 1M LiPF containing EC/PC/DEC solute6), barrier film is assembled into button cell.
Button cell is with 0.2C electric current density constant-current charge to 4.3V, and constant-voltage charge, to 0.05C, is then discharged to 2.5V.
Note: following embodiment, comparative example the uniform the present embodiment of experimentation identical.
Comparative example 1
Directly by doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2Mix with Lithium hydrate, in molar ratio 1:
1 mixes 60min in high-speed mixer, at 800 DEG C of high-temperature roasting 15h, after being cooled to room temperature, size-reduced, sieve.
Test result is as shown in Figures 1 to 3.From figure 1 it appears that have one layer at cobalt nickel oxide aluminum lithium material Surface coating
Spinelle Li after 2nm2Mn2O4Layer, shows that the method can successfully prepare spinel lithium manganate cladding cobalt nickel oxide aluminum lithium nucleocapsid
Structure composite positive electrode；From figure 2 it can be seen that in embodiment 1, after 70 circulations, its capability retention is 93%, contrast
In example 1, after 70 circulations, its capability retention is 80%, and material has more excellent cyclical stability；From 3 it can be seen that
Compared with comparative example 1, in embodiment 1, the DSC curve peak temperature of material is 237.6 DEG C, material DSC curve in relatively comparative example 1
Peak temperature is high 4 DEG C, and material has higher safety.
Embodiment 2
By 2.01kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.1Mn0.10(OH)2It is equipped with 1mol/L manganese sulfate solution
Reactor in, be stirred continuously, mixing speed is 500rpm, adds 0.5mol/L through dosing pump with 30mL/min in reactor
Sodium hydroxide and the mixed solution of ammonia, ammonia and sodium hydroxide ratio are 1:20 by mol, after precipitant adds, instead
Answer in still Mn:NaOH=1:2 by mol, precipitation completely after stand 1h, filter, collect solid, solid is washed through deionization
Wash, dry.Then the solid dried is mixed in high-speed mixer 60min, in molar ratio 1:1 mixing, so with Lithium hydrate
After under the conditions of 800 DEG C high-temperature roasting 15h, after being cooled to room temperature, size-reduced, sieving obtains Surface coating and have spinel lithium manganate
The cobalt nickel oxide manganses lithium composite positive pole of layer.
Embodiment 3
By 1.01kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2It is equipped with 1mol/L manganese sulfate molten
In the reactor of liquid, being stirred continuously, mixing speed is 500rpm, adds with 30mL/min through dosing pump in reactor
0.5mol/L sodium hydroxide and the mixed solution of ammonia, ammonia and sodium hydroxide ratio are 1:20 by mol, and precipitant adds
After, Mn:NaOH=1:2 by mol in reactor, precipitation completely after stand 1h, filter, collect solid, by solid through going
Ionized water washing, drying.Then the solid dried is mixed 60min, in molar ratio 1:1 with Lithium hydrate in high-speed mixer
Mixing, then high-temperature roasting 15h under the conditions of 800 DEG C, after being cooled to room temperature, size-reduced, sieving obtains Surface coating and have point brilliant
The cobalt nickel oxide aluminum lithium composite positive pole of stone mangaic acid lithium layer.
Embodiment 4
By 1.83kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2Be equipped with 1mol/L manganese sulfate and
In the reactor of the mixed solution of manganese nitrate 1:2, being stirred continuously, mixing speed is 500rpm, through dosing pump with 30mL/min to
Adding 0.5mol/L sodium hydroxide and the mixed solution of ammonia in reactor, ammonia and sodium hydroxide ratio are 1 by mol:
20, after precipitant adds, Mn:NaOH=1:2 by mol in reactor, precipitation completely after stand 1h, filter, collect solid
Body, by solid through deionized water wash, drying.Then the solid dried is mixed in high-speed mixer with Lithium hydrate
60min, in molar ratio 1:1 mixing, then high-temperature roasting 15h under the conditions of 600 DEG C, after being cooled to room temperature, size-reduced, sieve
The cobalt nickel oxide aluminum lithium composite positive pole of spinel lithium manganate layer is had to Surface coating.
Embodiment 5
By 1.01kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2It is equipped with 1mol/L manganese acetate molten
In the reactor of liquid, being stirred continuously, mixing speed is 500rpm, adds with 30mL/min through dosing pump in reactor
0.5mol/L sodium hydroxide and the mixed solution of ammonia, ammonia and sodium hydroxide ratio are 1:20 by mol, and precipitant adds
After, Mn:NaOH=1:2 by mol in reactor, precipitation completely after stand 1h, filter, collect solid, by solid through going
Ionized water washing, drying.Then the solid dried is mixed 60min, in molar ratio 1:1 with Lithium hydrate in high-speed mixer
Mixing, then high-temperature roasting 15h under the conditions of 1000 DEG C, after being cooled to room temperature, size-reduced, sieving obtains Surface coating and have point brilliant
The cobalt nickel oxide aluminum lithium composite positive pole of stone mangaic acid lithium layer.
Embodiment 6
By 1.01kg doping type lithium nickel cobalt dioxide presoma Ni0.8Co0.15Al0.05(OH)2It is equipped with 1mol/L manganese nitrate molten
In the reactor of liquid, being stirred continuously, mixing speed is 500rpm, adds with 30mL/min through dosing pump in reactor
0.5mol/L sodium hydroxide and the mixed solution of ammonia, ammonia and sodium hydroxide ratio are 1:20 by mol, and precipitant adds
After, Mn:NaOH=1:2 by mol in reactor, precipitation completely after stand 1h, filter, collect solid, by solid through going
Ionized water washing, drying.Then the solid dried is mixed 60min, in molar ratio 1:1 with Lithium hydrate in high-speed mixer
Mixing, then high-temperature roasting 2h under the conditions of 1000 DEG C, after being cooled to room temperature, size-reduced, sieving obtains Surface coating and have point brilliant
The cobalt nickel oxide aluminum lithium composite positive pole of stone mangaic acid lithium layer.
Claims (10)
1. the preparation method of a doping type lithium nickel cobalt dioxide composite positive pole, it is characterised in that comprise the steps:
1) manganese ion raw material being dissolved in water and be configured to solution A, its molar concentration is 0.1～2mol/L；Precipitant is dissolved in water join
Making solution B, its molar concentration is 0.1～2mol/L；
2) doping type lithium nickel cobalt dioxide presoma being added described solution A, under agitation, mixing speed is 100～500rpm,
It is added thereto to solution B；Question response completes, and filters, and collects solid content, then washs it, is dried, obtains solid A；
Described doping type lithium nickel cobalt dioxide presoma is LiNixCoyM1-x-yO2, based on molal weight, 0.3≤x≤0.9,0.05≤y
≤ 0.3, M are Mn, any one or the most several mixture in Al, Cr, Fe, Mg, Zn, Ti；
3) by described solid A and the high-temperature roasting in oxygen atmosphere stove of lithium source, obtain roasting afterproduct, be and deposit with nucleocapsid structure
, top layer is coated with the described doping type lithium nickel cobalt dioxide composite positive pole of spinel lithium manganate layer.
2. preparation method as claimed in claim 1, it is characterised in that: described manganese ion raw material is manganese sulfate, manganese nitrate and acetic acid
Any one or the most several mixture in manganese.
3. preparation method as claimed in claim 1, it is characterised in that: described precipitant is that the mixing of ammonia and sodium hydroxide is molten
Liquid, or be the mixed solution of ammonia and sodium carbonate.
4. preparation method as claimed in claim 3, it is characterised in that: ammonia and sodium hydroxide ratio are 1～20 by mol:
100, ammonia and sodium carbonate ratio are 1～20:100.
5. preparation method as claimed in claim 1, it is characterised in that: described lithium source is Lithium hydrate, lithium carbonate, lithium nitrate and second
One or more in acid lithium.
6. preparation method as claimed in claim 1, it is characterised in that: the molecular formula of described doping type lithium nickel cobalt dioxide presoma is
LiNi0.8Co0.1Mn0.1O2, or LiNi0.8Co0.15Al0.05O2。
7. as claimed in claim 1 preparation method, it is characterised in that: step 3) temperature of described high-temperature roasting is 200～1000
DEG C, the time is 2～15h.
8. as claimed in claim 1 preparation method, it is characterised in that: step 3) molecular formula of spinel lithium manganate layer that obtains is
Li2Mn2-xMxO4, based on molal weight, 0≤x≤0.1, M=Ni, B, Al, Cr, Fe, Mg, Zn, Ti, it is preferable that molecular formula is
Li2Mn2O4。
9. as claimed in claim 1 preparation method, it is characterised in that: step 3) described in the quality of spinel lithium manganate layer account for institute
State the 1～20% of doping type lithium nickel cobalt dioxide gross mass.
10. the doping type lithium nickel cobalt dioxide composite positive pole that any one preparation method prepares in a kind such as claim 1～9.
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| WO2019041057A1 (en) | 2017-09-01 | 2019-03-07 | Universidad De Antofagasta | Manganese spinel doped with magnesium, cathode material comprising same, method for preparing same and lithium ion battery comprising same |
| CN109728375A (en) * | 2017-10-30 | 2019-05-07 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode and lithium ion battery recycled and repair the method for positive electrode, reparation |
| CN111613782A (en) * | 2020-04-21 | 2020-09-01 | 浙江锋锂新能源科技有限公司 | Shell-core structure ternary positive electrode material, preparation method thereof and all-solid-state battery |
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| WO2019041057A1 (en) | 2017-09-01 | 2019-03-07 | Universidad De Antofagasta | Manganese spinel doped with magnesium, cathode material comprising same, method for preparing same and lithium ion battery comprising same |
| CN109728375A (en) * | 2017-10-30 | 2019-05-07 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode and lithium ion battery recycled and repair the method for positive electrode, reparation |
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| US11824193B2 (en) | 2020-03-26 | 2023-11-21 | Lg Chem, Ltd. | Method of manufacturing positive electrode active material |
| CN111613782A (en) * | 2020-04-21 | 2020-09-01 | 浙江锋锂新能源科技有限公司 | Shell-core structure ternary positive electrode material, preparation method thereof and all-solid-state battery |
| CN111613782B (en) * | 2020-04-21 | 2022-09-20 | 浙江锋锂新能源科技有限公司 | Shell-core structure ternary positive electrode material, preparation method thereof and all-solid-state battery |
| CN111697216A (en) * | 2020-05-21 | 2020-09-22 | 西安交通大学 | Lithium manganate coated high nickel cobalt lithium manganate lithium ion battery positive electrode material and preparation method thereof |
| CN112736230A (en) * | 2020-12-30 | 2021-04-30 | 天目湖先进储能技术研究院有限公司 | High-voltage composite spinel-coated cathode material and preparation method thereof |
| CN113921788A (en) * | 2021-09-29 | 2022-01-11 | 蜂巢能源科技(马鞍山)有限公司 | Coated manganese-based positive electrode material and preparation method thereof |
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