CN108232147A - Nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium and preparation method thereof - Google Patents

Nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium and preparation method thereof Download PDF

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CN108232147A
CN108232147A CN201711463841.6A CN201711463841A CN108232147A CN 108232147 A CN108232147 A CN 108232147A CN 201711463841 A CN201711463841 A CN 201711463841A CN 108232147 A CN108232147 A CN 108232147A
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lithium
source
ion battery
lithium ion
cathode material
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张冉
张宏立
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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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
    • 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
    • H01M4/50—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
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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

Nickelic tertiary cathode material of lithium ion battery the invention discloses a kind of surface cladding yttrium acid lithium and preparation method thereof, preparation method includes：Nickel source, manganese source, cobalt source are dissolved in deionized water and are configured to solution A；Precipitating reagent is dissolved in deionized water and is configured to solution B；Solution A and solution B are added in reaction unit and carry out coprecipitation reaction, is aged, is filtered, washed, drying and to obtain nickel cobalt manganese presoma；Lithium source and yttrium source are dissolved in deionized water, added in nickel cobalt manganese presoma, stirring is evaporated to gel, dry mixture；Mixture is once calcined, secondary clacining is carried out after grinding uniformly, cools down, is ground up, sieved.The preparation method of the nickelic tertiary cathode material of lithium ion battery of cladding yttrium acid lithium in surface proposed by the present invention, simply, reaction condition is easily-controllable, it is reproducible, obtained covering material crystallinity is high, good dispersion improves the specific discharge capacity, circulation ability and big multiplying power charging ability of the nickelic tertiary cathode material of lithium ion battery.

Description

The nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium and its preparation Method
Technical field
Lithium ion battery the present invention relates to technical field of lithium ion more particularly to a kind of surface cladding yttrium acid lithium is high Nickel tertiary cathode material and preparation method thereof.
Background technology
With the development of new-energy automobile, lithium ion battery becomes the most promising energy storage device of electric vehicle. In lithium ion battery important component, positive electrode occupies leading factor, determines chemical property, the thermal stability of battery And security performance, more account for more than the 40% of battery cost.At present, course continuation mileage problem becomes the bottle of new-energy automobile development Neck, therefore the battery for developing high-energy density is extremely urgent.It, can be significantly using nickelic ternary as the lithium ion battery of positive electrode The energy density of battery is improved, also becomes the Research Emphasis of domestic and international each Li electricity companies.But high-nickel material is limited by storage item The shortcomings of part, poor circulation and poor thermal stability, limits it and commercially produces.
The chemical substance stablized by coating one layer of chemical property on the nickelic positive electrode surface of lithium ion battery, inhibits to follow Erosions of the HF to electrode material during ring reduces the side reaction between active material and electrolyte, and stabilized electrodes structure can be big Amplitude improves energy density, circulation ability and the high rate charge-discharge ability of battery.Usually using metal oxide such as Al2O3、 TiO2Deng progress surface cladding, but these materials may form doping rather than clad at high temperature with material of main part；In addition Coat inactive metal phosphate such as FePO4、AlPO4, but the electrochemically inactive material of these low electronics, poorly conductive carries out table When bread covers, material surface can coat one layer of megohmite insulant and hinder Li+Diffusion, therefore influence its discharge capacity.Some researchs Person uses the nickelic tertiary cathode material of lithium ion fast ion conducting material surface coated lithium ion battery, such as number of patent application In the patent document of 107069006A, a kind of side for improving the nickelic tertiary cathode material chemical property of lithium ion battery is disclosed Method, in the surface coated fast Lithium Ionic Conducting Materials Li of nickelic tertiary cathode material chemical property3PO4, the material after coating modification Material improves discharge capacity, improves the high rate performance of nickelic tertiary cathode material compared with uncoated material.
In the research of coating modification, have no using LiYO2To lithium ion battery, nickelic tertiary cathode material carries out surface packet It covers.
Invention content
Technical problems based on background technology, the present invention propose a kind of lithium ion battery of surface cladding yttrium acid lithium Nickelic tertiary cathode material and preparation method thereof, the method is simple, easy control of reaction conditions, reproducible, is prepared Covering material crystallinity it is high, particle dispersion is good, improve the nickelic tertiary cathode material of lithium ion battery specific discharge capacity, Circulation ability and big multiplying power charging ability.
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, it nickel source, manganese source, cobalt source is dissolved in deionized water is configured to solution A；Precipitating reagent is dissolved in deionized water and is matched Solution B is made；Solution A and solution B are added in reaction unit and carry out coprecipitation reaction, is aged, filters, washes after reaction It washs, be dried to obtain nickel cobalt manganese presoma；
S2, lithium source and yttrium source are dissolved in deionized water, then added in the nickel cobalt manganese presoma in S1, is stirred It is even, gel is evaporated to, is dried to obtain mixture；
S3, the mixture in S2 is once calcined, secondary clacining is carried out after grinding uniformly, be down to ground after room temperature Sieve obtains the nickelic tertiary cathode material of lithium ion battery of the surface cladding yttrium acid lithium.
Preferably, in S1, in solution A, nickel source, manganese source, cobalt source total mol concentration be 0.8-2.0mol/L.
Preferably, nickel source, manganese source, cobalt source total mol concentration be 1mol/L.
Preferably, nickel source, cobalt source, the molar ratio of manganese source are x：y：1-x-y, wherein, 0.5≤x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1.
Preferably, in S1, the precipitating reagent is sodium hydroxide, one or two kinds of mixture in sodium carbonate.
Preferably, in S1, nickel source, cobalt source, the total mole number of manganese source and precipitating reagent the ratio between molal quantity be 1：1-1：2.
Preferably, the nickel source is the mixture of one or more of nickel sulfate, nickel acetate, nickel nitrate；The manganese Source is manganese sulfate, one or more mixtures in manganese acetate, manganese nitrate；The cobalt source is cobaltous sulfate, cobalt acetate, cobalt nitrate In one or more mixtures.
Preferably, in S1, solution A and solution B is added drop-wise to simultaneously in reaction kettle and carry out coprecipitation reaction, it is molten being added dropwise During liquid A and solution B, the pH value with ammonium hydroxide regulation system is 7-11；The coprecipitation reaction carries out under nitrogen atmosphere, The temperature of coprecipitation reaction is 35-55 DEG C, time 4-12h.
Preferably, in S1, digestion time 6-12h.
Preferably, in S2, the lithium source for lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate, lithium chloride, lithium fluoride, One or more mixtures in lithium phosphate, lithium hydrogen phosphate, lithium dihydrogen phosphate；The yttrium source is yttrium nitrate, yttrium oxide, acetic acid One or more mixtures in yttrium.
Preferably, in S2, magnetic force is sufficiently stirred 30-60min and is uniformly mixed.
Preferably, in S2, magnetic agitation is evaporated to gel at 60-90 DEG C.
Preferably, in S2, the drying is vacuum drying, and vacuum drying temperature is 60-100 DEG C, time 6- 24h。
Preferably, the concrete technology of S3 is：By the mixture in S2 under air or oxygen atmosphere, with 3-5 DEG C/min liters Warm rate is heated to 400-550 DEG C of heat preservation 3-8h, and 700-900 DEG C is heated to the heating rate of 3-5 DEG C/min after grinding uniformly 10-16h is kept the temperature, is ground up, sieved to obtain the nickelic tertiary cathode material of lithium ion battery of the surface cladding yttrium acid lithium after being down to room temperature Material.
Preferably, the preparation method of the nickelic tertiary cathode material of lithium ion battery of the surface cladding yttrium acid lithium, including Following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water, are configured to the solution A of a concentration of 1mol/L；By hydroxide Sodium or sodium carbonate, which are dissolved in deionized water, is configured to solution B；Solution A and solution B are instilled into reaction kettle simultaneously using peristaltic pump Middle carry out coprecipitation reaction, is aged 6-12h after reaction, is filtered, washed later, drying to obtain nickel cobalt manganese presoma； It is 7-11 to be added dropwise during solution A and solution B with the pH value of ammonium hydroxide regulation system, and the coprecipitation reaction need to be in closed nitrogen Atmosphere encloses lower progress, and temperature is 35-55 DEG C, reaction time 4-12h；
S2, lithium source and yttrium source are dissolved in deionized water obtain mixed solution successively, the nickel cobalt manganese presoma in S1 is equal It is even to be scattered in container, above-mentioned mixed solution is added dropwise, and magnetic force is sufficiently stirred 30-60min, after mixing, in 60-90 Magnetic agitation is evaporated to gel at DEG C, places into vacuum drying chamber, and dry 6-24h obtains mixture at 60-100 DEG C；
S3, by the mixture obtained in S2 under air/oxygen atmosphere, be heated to the heating rate of 3-5 DEG C/min 400-550 DEG C, and 3-8h is kept the temperature at this temperature, 700-900 is heated to the heating rate of 3-5 DEG C/min again after grinding uniformly DEG C, 10-16h is kept the temperature at this temperature, and it is high to be down to the lithium ion battery being ground up, sieved after room temperature to get yttrium acid lithium is coated to surface Nickel tertiary cathode material.
Preferably, the surface has in the nickelic ternary electrode material of lithium ion battery of yttrium acid lithium clad, yttrium acid lithium Quality be nickelic ternary electrode quality of materials 0.5-10wt%.
Preferably, the chemical formula of the nickelic tertiary cathode material of the lithium ion battery is LiNixCoyMn1-x-yO2, wherein 0.5 ≤ x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1；The nickel cobalt manganese presoma is (NixCoyMn1-x-y)(OH)2、 (NixCoyMn1-x-y) CO3、(NixCoyMn1-x-y)C2O4In one kind, wherein 0.5≤x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1.
The nickelic tertiary cathode material of lithium ion battery of a kind of surface cladding yttrium acid lithium that the present invention also proposes, using described The preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium is prepared.
The present invention useful achievement be：
1st, the present invention carries out surface coating modification in nickelic ternary material, and electrolyte and active material can be hindered by reducing Between the contact area that contacts, mitigate erosions of the HF to electrode material, effectively reduce the generation of positive electrode surface adverse reaction, Reduce Charge-transfer resistance of the battery in charge and discharge process, hence it is evident that improve following for the nickelic tertiary cathode material of lithium ion battery Ring stability and high rate performance；
2nd, the present invention is in nickelic tertiary cathode material Surface Creation lithium ion fast ion conducting material LiYO2, it is this soon from Sub- conductor material is used as Li in itself+Conductor material, have higher lithium ion conducting rate, improve lithium ion in solid state electrode Transmission efficiency between liquid electrolyte, significantly improve the nickelic tertiary cathode material of lithium ion battery specific discharge capacity and Big multiplying power discharging property；
3rd, the present invention under liquid phase environment using surface cladding is carried out, and method is simple, reproducible, and can prepare has The nickelic tertiary cathode material of lithium ion battery of equal yttrium acid lithium clad；
4th, the present invention directly coats on presoma, and avoiding nickel cobalt manganese oxidate for lithium and being contacted with water causes material surface alkali Property raising, be unfavorable for storing；Double sintering is avoided to reduce energy consumption to nickel cobalt manganese oxidate for lithium structural damage simultaneously.
Description of the drawings
Fig. 1 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by the embodiment of the present invention 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2The XRD diagram of positive electrode；
Fig. 2 is the nickelic ternary of lithium ion battery that surface prepared by the embodiment of the present invention 2 coats 1wt% yttrium acid lithiums LiNi0.8Co0.1Mn0.1O2The SEM figures of positive electrode；
Fig. 3 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by the embodiment of the present invention 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2Cycle performance curve graph of the positive electrode under 1C multiplying powers；
Fig. 4 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by the embodiment of the present invention 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2The high rate performance curve graph of positive electrode.
Specific embodiment
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
Prepare LiNi of the surface without cladding0.8Co0.1Mn0.1O2Tertiary cathode material includes the following steps：
S1, it is 8 in molar ratio by nickel acetate, cobalt acetate, manganese acetate：1：1 be dissolved in deionized water be configured to it is a concentration of The solution A of 1mol/L；NaOH is dissolved in the solution B that 1mol/L is configured in deionized water；Using peristaltic pump by solution A and solution B instills progress coprecipitation reaction 6h in reaction kettle simultaneously, wherein, during solution A and solution B is added dropwise, adjusted with ammonium hydroxide The pH value of system is 10, persistently leads to N during coprecipitation reaction2, temperature is 50 DEG C, is aged 12h after reaction, later mistake Filter, washing, drying to obtain nickel cobalt manganese presoma, i.e. (Ni0.8Co0.1Mn0.1)(OH)2Presoma；
S2, it LiOH is dissolved in deionized water obtains solution, then (the Ni by 15g0.8Co0.1Mn0.1)(OH)2Presoma is equal It is even to be scattered in container, (Ni then is added dropwise in above-mentioned solution0.8Co0.1Mn0.1)(OH)2In presoma, and magnetic force fully stirs 60min is mixed, after mixing, magnetic force heating stirring is evaporated to gel at 85 DEG C, places into vacuum drying chamber with 100 DEG C Temperature drying 12h obtains mixture；
S3, by the mixture in S2 under oxygen atmosphere, be heated to 450 DEG C with the heating rate of 5 DEG C/min, and warm herein The lower heat preservation 6h of degree, is heated to 800 DEG C with the heating rate of 5 DEG C/min again after grinding uniformly, keeps the temperature 12h at this temperature, be down to It is ground up, sieved after room temperature to get to LiNi of the surface without cladding0.8Co0.1Mn0.1O2Positive electrode.
Embodiment 2
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, it is 8 in molar ratio by nickel acetate, cobalt acetate, manganese acetate:1:1 be dissolved in deionized water be configured to it is a concentration of The solution A of 1mol/L；NaOH is dissolved in the solution B that 1mol/L is configured in deionized water；Using peristaltic pump by solution A and solution B instills progress coprecipitation reaction 6h in reaction kettle simultaneously, wherein, during solution A and solution B is added dropwise, adjusted with ammonium hydroxide The pH value of system is 10, persistently leads to N during coprecipitation reaction2, temperature is 50 DEG C, is aged 12h after reaction, later mistake Filter, washing, drying to obtain nickel cobalt manganese presoma, i.e. (Ni0.8Co0.1Mn0.1)(OH)2Presoma；
S2, according to yttrium acid lithium：Nickelic tertiary cathode material mass ratio is 1：100, by LiOH, lithium acetate be dissolved in successively from Solution, the then (Ni by 15g are obtained in sub- water0.8Co0.1Mn0.1)(OH)2Presoma is dispersed in container, then will be above-mentioned (Ni is added dropwise in solution0.8Co0.1Mn0.1)(OH)2In presoma, and magnetic force is sufficiently stirred 60min, after mixing, at 85 DEG C Lower magnetic force heating stirring is evaporated to gel, places into vacuum drying chamber and obtains mixture with 100 DEG C of temperature drying 12h；
S3, by the mixture in S2 under oxygen atmosphere, be heated to 450 DEG C, and in this temperature with 5 DEG C/min heating rates Lower heat preservation 6h is heated to 800 DEG C with same heating rate again after grinding uniformly, 12h is kept the temperature at this temperature, after being down to room temperature It is ground up, sieved to coat the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium to surface, i.e. surface coats yttrium acid lithium LiNi0.8Co0.1Mn0.1O2Positive electrode.
By being coated with, drying, positive electrode prepared by embodiment 1 and embodiment 2 is dressed up into button cell, constant current is carried out and fills Discharge test.
Fig. 1 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by embodiment 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2The XRD diagram of positive electrode；As shown in Figure 1, between the material after cladding (006) and (012), (018) there is apparent tear peak between (110), no miscellaneous peak, material stratiform well-formed, cladding yttrium acid lithium is not to positive electrode Main body has destruction.
Fig. 2 is the nickelic ternary of lithium ion battery that surface prepared by the embodiment of the present invention 2 coats 1wt% yttrium acid lithiums LiNi0.8Co0.1Mn0.1O2The SEM figures of positive electrode；As shown in Figure 2, material granule keeps good spherical morphology, and yttrium acid lithium is not The sphere pattern of material is destroyed, particle surface has yttrium acid lithium particle.
Fig. 3 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by embodiment 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2Cycle performance curve graph of the positive electrode under 1C multiplying powers；By Fig. 3 it is found that table in embodiment 2 Bread covers the nickelic ternary LiNi of lithium ion battery of 1wt% yttrium acid lithiums0.8Co0.1Mn0.1O2It discharges for the first time under positive electrode 1C multiplying powers Specific capacity is from uncoated LiNi0.8Co0.1Mn0.1O2The 186.6mAhg of tertiary cathode material-1It improves to 195.1mAhg-1, improve 8.5mAhg-1, for cycle after 50 weeks, capacity retention ratio is increased to 95.1% by 75.5% before；
Fig. 4 is lithium ion battery nickelic ternary of the surface without cladding yttrium acid lithium prepared by embodiment 1 LiNi0.8Co0.1Mn0.1O2The lithium ion battery of surface cladding 1wt% yttrium acid lithiums prepared by positive electrode and embodiment 2 is nickelic Ternary LiNi0.8Co0.1Mn0.1O2The high rate performance curve graph of positive electrode, as shown in Figure 4, surface coats in embodiment 2 The nickelic ternary LiNi of lithium ion battery of 1wt% yttrium acid lithiums0.8Co0.1Mn0.1O2Positive electrode specific discharge capacity under high magnification 5C By 183.4mAhg-1It improves to 158.1mAhg-1, improve 25.3mAhg-1, greatly improve LiNi0.8Co0.1Mn0.1O2Three First big multiplying power discharging property of positive electrode.
Embodiment 3
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, it nickel source, manganese source, cobalt source is dissolved in deionized water is configured to solution A；Precipitating reagent is dissolved in deionized water and is matched Solution B is made；Solution A and solution B are added in reaction unit and carry out coprecipitation reaction, is aged, filters, washes after reaction It washs, be dried to obtain nickel cobalt manganese presoma；
S2, lithium source and yttrium source are dissolved in deionized water, then added in the nickel cobalt manganese presoma in S1, is stirred It is even, gel is evaporated to, is dried to obtain mixture；
S3, the mixture in S2 is once calcined, secondary clacining is carried out after grinding uniformly, be down to ground after room temperature Sieve obtains the nickelic tertiary cathode material of lithium ion battery of the surface cladding yttrium acid lithium.
Embodiment 4
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water, are configured to the solution A of a concentration of 1mol/L；By sodium carbonate It is dissolved in deionized water and is configured to solution B；Solution A and solution B are instilled in reaction kettle simultaneously using peristaltic pump and are co-precipitated Reaction during solution A and solution B is added dropwise, is 11 with the pH value of ammonium hydroxide regulation system, is aged 6h after reaction, it After be filtered, washed, drying to obtain nickel cobalt manganese presoma；The coprecipitation reaction need to carry out under closed nitrogen atmosphere, temperature It is 55 DEG C to spend, reaction time 4h；
S2, lithium source and yttrium source are dissolved in deionized water obtain mixed solution successively, the nickel cobalt manganese presoma in S1 is equal It is even to be scattered in container, above-mentioned mixed solution is added dropwise, and magnetic force is sufficiently stirred 30min, after mixing, the magnetic at 90 DEG C Power stirring is evaporated to gel, places into vacuum drying chamber, dry at 60 DEG C to obtain mixture for 24 hours；
S3, by the mixture obtained in S2 under air atmosphere, be heated to 400 DEG C with the heating rate of 5 DEG C/min, and 8h is kept the temperature at this temperature, the heating rate of 5 DEG C/min is heated to 900 DEG C again after grinding uniformly, keeps the temperature 10h at this temperature, It is ground up, sieved to coat the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium to surface after being down to room temperature.
Embodiment 5
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water, are configured to the solution A of a concentration of 1mol/L；By hydroxide Sodium, which is dissolved in deionized water, is configured to solution B；Solution A and solution B instilled simultaneously in reaction kettle using peristaltic pump carry out it is coprecipitated It forms sediment and reacts, the pH value that ammonium hydroxide regulation system is used during solution A and solution B is added dropwise is 7, is aged 12h after reaction, it After be filtered, washed, drying to obtain nickel cobalt manganese presoma；The coprecipitation reaction need to carry out under closed nitrogen atmosphere, temperature It is 35 DEG C to spend, reaction time 12h；
S2, lithium source and yttrium source are dissolved in deionized water obtain mixed solution successively, the nickel cobalt manganese presoma in S1 is equal It is even to be scattered in container, above-mentioned mixed solution is added dropwise, and magnetic force is sufficiently stirred 60min, after mixing, the magnetic at 60 DEG C Power stirring is evaporated to gel, places into vacuum drying chamber, and dry 6h obtains mixture at 100 DEG C；
S3, by the mixture obtained in S2 under oxygen atmosphere, be heated to 550 DEG C with the heating rate of 3 DEG C/min, and 3h is kept the temperature at this temperature, the heating rate of 3 DEG C/min is heated to 700 DEG C again after grinding uniformly, keeps the temperature 16h at this temperature, It is ground up, sieved to coat the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium to surface after being down to room temperature.
Embodiment 6
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water are configured to solution A, wherein, nickel source, manganese source, cobalt source it is total Molar concentration is 2.0mol/L, and nickel source, cobalt source, the molar ratio of manganese source are 0.6：0.3：0.1, the nickel source is nickel sulfate, described Manganese source is manganese nitrate, and the cobalt source is cobaltous sulfate；Precipitating reagent is dissolved in deionized water and is configured to solution B, wherein, the precipitation Agent is sodium carbonate；Solution A and solution B are added drop-wise to simultaneously in reaction kettle and carry out coprecipitation reaction, wherein, be added dropwise solution A and With the pH value of ammonium hydroxide regulation system be 7 during solution B, nickel source, cobalt source, the total mole number of manganese source and precipitating reagent molal quantity The ratio between be 1：1, it is aged 12h after reaction, is filtered, washed, is dried to obtain nickel cobalt manganese presoma；The coprecipitation reaction is in nitrogen Atmosphere encloses lower progress, and the temperature of coprecipitation reaction is 35 DEG C, time 12h；The nickel cobalt manganese presoma is (Ni0.6Co0.3Mn0.1)CO3；
S2, lithium source and yttrium source are dissolved in deionized water, wherein, the lithium source is lithium carbonate；The yttrium source is yttrium nitrate, Then it adds in the nickel cobalt manganese presoma in S1, magnetic force is sufficiently stirred 60min and is uniformly mixed, and magnetic agitation is evaporated at 60 DEG C Gel, vacuum drying obtain mixture, and vacuum drying temperature is 100 DEG C, time 6h；
S3, by the mixture in S2 under oxygen atmosphere, with 3 DEG C/min heating rates be heated to 550 DEG C heat preservation 3h, grinding 700 DEG C of heat preservation 16h are heated to the heating rate of 5 DEG C/min after uniformly, are ground up, sieved to obtain the surface packet after being down to room temperature Cover the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium；Lithium ion battery of the surface with yttrium acid lithium clad is nickelic In ternary electrode material, the quality of yttrium acid lithium is the 0.5wt% of nickelic ternary electrode quality of materials；The lithium ion battery is nickelic The chemical formula of tertiary cathode material is LiNi0.6Co0.3Mn0.1O2。
Embodiment 7
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water are configured to solution A, wherein, nickel source, manganese source, cobalt source it is total Molar concentration is 0.8mol/L, and nickel source, cobalt source, the molar ratio of manganese source are 0.8：0.1：0.1, the nickel source is nickel acetate, described Manganese source is manganese sulfate, and the cobalt source is cobalt acetate, the mixture of cobalt nitrate, and the mass ratio of cobalt acetate, cobalt nitrate is 3：2；It will Precipitating reagent, which is dissolved in deionized water, is configured to solution B, wherein, the precipitating reagent is sodium hydroxide；By solution A and solution B simultaneously It is added drop-wise in reaction kettle and carries out coprecipitation reaction, wherein, with ammonium hydroxide regulation system during solution A and solution B is added dropwise PH value is 11, nickel source, cobalt source, the total mole number of manganese source and precipitating reagent the ratio between molal quantity be 1：2, after reaction be aged 6h, It is filtered, washed, is dried to obtain nickel cobalt manganese presoma；The coprecipitation reaction carries out under nitrogen atmosphere, the temperature of coprecipitation reaction It is 55 DEG C to spend, time 4h；The nickel cobalt manganese presoma is (Ni0.8Co0.1Mn0.1)(OH)2；
S2, lithium source and yttrium source are dissolved in deionized water, wherein, the lithium source is lithium hydroxide；The yttrium source is oxidation Then yttrium is added in the nickel cobalt manganese presoma in S1, magnetic force is sufficiently stirred 30min and is uniformly mixed, and magnetic agitation is steamed at 90 DEG C Gel is sent to, vacuum drying obtains mixture, and vacuum drying temperature is 60 DEG C, and the time is for 24 hours；
S3, by the mixture in S2 under air atmosphere, with 5 DEG C/min heating rates be heated to 400 DEG C heat preservation 8h, grinding 900 DEG C of heat preservation 10h are heated to the heating rate of 3 DEG C/min after uniformly, are ground up, sieved to obtain the surface packet after being down to room temperature Cover the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium；Lithium ion battery of the surface with yttrium acid lithium clad is nickelic In ternary electrode material, the quality of yttrium acid lithium is the 10wt% of nickelic ternary electrode quality of materials；The lithium ion battery is nickelic The chemical formula of tertiary cathode material is LiNi0.8Co0.1Mn0.1O2。
Embodiment 8
A kind of preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium proposed by the present invention, Include the following steps：
S1, nickel source, manganese source, cobalt source are dissolved in deionized water are configured to solution A, wherein, nickel source, manganese source, cobalt source it is total Molar concentration is 1mol/L, and nickel source, cobalt source, the molar ratio of manganese source are 0.7：0.1：0.2, the nickel source for nickel sulfate, nickel acetate, The mixture of nickel nitrate, and the mass ratio of nickel sulfate, nickel acetate, nickel nitrate is 3:2:1, the manganese source for manganese sulfate, manganese acetate, The mixture of manganese nitrate, and the mass ratio of manganese sulfate, manganese acetate, manganese nitrate is 3:5:2, the cobalt source for cobaltous sulfate, cobalt acetate, The mixture of cobalt nitrate, and the mass ratio of cobaltous sulfate, cobalt acetate, cobalt nitrate is 3:5:2；Precipitating reagent is dissolved in deionized water and is matched Solution B is made, wherein, the precipitating reagent is sodium hydroxide, the mixture of sodium carbonate, and the mass ratio of sodium hydroxide, sodium carbonate It is 3:2；Solution A and solution B are added drop-wise to simultaneously in reaction kettle and carry out coprecipitation reaction, wherein, solution A and solution B is being added dropwise During with the pH value of ammonium hydroxide regulation system be 10, nickel source, cobalt source, the total mole number of manganese source and precipitating reagent the ratio between molal quantity It is 1：1.5, it is aged 10h after reaction, is filtered, washed, is dried to obtain nickel cobalt manganese presoma；The coprecipitation reaction is in nitrogen It is carried out under atmosphere, the temperature of coprecipitation reaction is 50 DEG C, time 10h；The nickel cobalt manganese presoma is (Ni0.7Co0.1Mn0.2) CO3；
S2, lithium source and yttrium source are dissolved in deionized water, wherein, the lithium source is lithium nitrate, lithium acetate, lithium chloride it is mixed Object is closed, and the mass ratio of lithium nitrate, lithium acetate, lithium chloride is 4:6:1；The yttrium source is yttrium nitrate, then adds in the nickel in S1 In cobalt manganese presoma, magnetic force is sufficiently stirred 50min and is uniformly mixed, and magnetic agitation is evaporated to gel at 80 DEG C, vacuum drying Mixture is obtained, vacuum drying temperature is 80 DEG C, time 10h；
S3, by the mixture in S2 under air atmosphere, with 4 DEG C/min heating rates be heated to 500 DEG C heat preservation 6h, grinding 850 DEG C of heat preservation 15h are heated to the heating rate of 4 DEG C/min after uniformly, are ground up, sieved to obtain the surface packet after being down to room temperature Cover the nickelic tertiary cathode material of lithium ion battery of yttrium acid lithium；Lithium ion battery of the surface with yttrium acid lithium clad is nickelic In ternary electrode material, the quality of yttrium acid lithium is the 8wt% of nickelic ternary electrode quality of materials；The lithium ion battery nickelic three The chemical formula of first positive electrode is LiNi0.7Co0.1Mn0.2O2。
The invention also provides a kind of nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium, using described The preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium is prepared.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (10)

  1. A kind of 1. preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium, which is characterized in that packet Include following steps：
    S1, it nickel source, manganese source, cobalt source is dissolved in deionized water is configured to solution A；Precipitating reagent is dissolved in deionized water and is configured to Solution B；Solution A and solution B are added in reaction unit and carry out coprecipitation reaction, is aged, is filtered, washed, does after reaction It is dry to obtain nickel cobalt manganese presoma；
    S2, lithium source and yttrium source are dissolved in deionized water, then add in the nickel cobalt manganese presoma in S1, be uniformly mixed, Gel is evaporated to, is dried to obtain mixture；
    S3, the mixture in S2 is once calcined, carries out secondary clacining after grinding uniformly, be ground up, sieved after being down to room temperature To the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium.
  2. 2. the preparation method of the nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium according to claim 1, It is characterized in that, in S1, in solution A, nickel source, manganese source, cobalt source total mol concentration be 0.8-2.0mol/L；Preferably, Nickel source, manganese source, cobalt source total mol concentration be 1mol/L；Preferably, nickel source, cobalt source, the molar ratio of manganese source are x：y：1-x-y, Wherein, 0.5≤x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1.
  3. 3. the preparation side of the nickelic tertiary cathode material of lithium ion battery of cladding yttrium acid lithium in surface according to claim 1 or claim 2 Method, which is characterized in that in S1, the precipitating reagent is sodium hydroxide, one or two kinds of mixture in sodium carbonate.
  4. 4. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-3 surface cladding yttrium acid lithiums Preparation method, which is characterized in that in S1, nickel source, cobalt source, the total mole number of manganese source and precipitating reagent the ratio between molal quantity be 1：1- 1：2；Preferably, the nickel source is the mixture of one or more of nickel sulfate, nickel acetate, nickel nitrate；The manganese source is One or more mixtures in manganese sulfate, manganese acetate, manganese nitrate；The cobalt source is cobaltous sulfate, in cobalt acetate, cobalt nitrate One or more mixtures.
  5. 5. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-4 surface cladding yttrium acid lithiums Preparation method, which is characterized in that in S1, solution A and solution B are added drop-wise to simultaneously in reaction kettle and carry out coprecipitation reaction, During solution A and solution B is added dropwise, the pH value with ammonium hydroxide regulation system is 7-11；The coprecipitation reaction is in nitrogen atmosphere Lower progress, the temperature of coprecipitation reaction is 35-55 DEG C, time 4-12h.
  6. 6. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-5 surface cladding yttrium acid lithiums Preparation method, which is characterized in that in S2, the lithium source is lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate, lithium chloride, fluorine Change one or more mixtures in lithium, lithium phosphate, lithium hydrogen phosphate, lithium dihydrogen phosphate；The yttrium source is yttrium nitrate, oxidation One or more mixtures in yttrium, yttrium acetate.
  7. 7. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-6 surface cladding yttrium acid lithiums Preparation method, which is characterized in that the concrete technology of S3 is：By the mixture in S2 under air or oxygen atmosphere, with 3-5 DEG C/ Min heating rates are heated to 400-550 DEG C of heat preservation 3-8h, and 700- is heated to the heating rate of 3-5 DEG C/min after grinding uniformly 900 DEG C of heat preservation 10-16h are ground up, sieved to obtain the nickelic ternary of lithium ion battery of the surface cladding yttrium acid lithium after being down to room temperature Positive electrode.
  8. 8. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-7 surface cladding yttrium acid lithiums Preparation method, which is characterized in that the surface has in the nickelic ternary electrode material of lithium ion battery of yttrium acid lithium clad, yttrium The quality of sour lithium is the 0.5-10wt% of nickelic ternary electrode quality of materials.
  9. 9. according to the nickelic tertiary cathode material of lithium ion battery of any one of the claim 1-8 surface cladding yttrium acid lithiums Preparation method, which is characterized in that the chemical formula of the nickelic tertiary cathode material of lithium ion battery is LiNixCoyMn1-x-yO2, In 0.5≤x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1；The nickel cobalt manganese presoma is (NixCoyMn1-x-y)(OH)2、 (NixCoyMn1-x-y)CO3、(NixCoyMn1-x-y)C2O4In one kind, wherein 0.5≤x ＜ 1,0 ＜ y≤0.5,0 ＜ x+y ＜ 1.
  10. 10. a kind of nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium, which is characterized in that will using such as right The preparation method of the nickelic tertiary cathode material of lithium ion battery of any one of 1-9 surfaces cladding yttrium acid lithium is asked to prepare and Into.
CN201711463841.6A 2017-12-28 2017-12-28 Nickelic tertiary cathode material of lithium ion battery of surface cladding yttrium acid lithium and preparation method thereof Pending CN108232147A (en)

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CN110518221A (en) * 2019-09-05 2019-11-29 中南大学 A kind of method that anti-solvent method prepares lithium metasilicate cladding nickel-cobalt lithium manganate cathode material
CN110752362A (en) * 2019-10-31 2020-02-04 贵州中伟资源循环产业发展有限公司 Ternary precursor coated with magnesium and preparation method thereof
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CN113097461A (en) * 2021-03-29 2021-07-09 清华大学 Ternary cathode material @ yttrium oxide core-shell structure composite material and preparation method thereof
CN113629232A (en) * 2021-08-06 2021-11-09 浙江帕瓦新能源股份有限公司 Modified low-cobalt ternary positive electrode material precursor and positive electrode material
CN113839025A (en) * 2021-09-24 2021-12-24 四川朗晟新能源科技有限公司 High-nickel ternary cathode material of lithium ion battery and modification method thereof
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CN108232182A (en) * 2016-12-13 2018-06-29 天津国安盟固利新材料科技股份有限公司 A kind of modified nickel-cobalt lithium manganate cathode material and preparation method thereof
CN109638232A (en) * 2018-10-25 2019-04-16 宁夏汉尧石墨烯储能材料科技有限公司 A kind of preparation method of cladded type ternary cobalt nickel oxide manganses lithium anode material
CN109360983A (en) * 2018-10-29 2019-02-19 合肥国轩高科动力能源有限公司 A kind of nickelic tertiary cathode material of modification and its preparation method and application
CN109360983B (en) * 2018-10-29 2021-08-06 合肥国轩高科动力能源有限公司 Modified high-nickel ternary cathode material and preparation method and application thereof
CN109244433A (en) * 2018-11-15 2019-01-18 合肥国轩高科动力能源有限公司 A kind of Y adulterates the preparation method of high nickel cobalt lithium manganate
CN109509875A (en) * 2018-11-26 2019-03-22 合肥国轩高科动力能源有限公司 A kind of high-rate type monocrystalline nickel-cobalt lithium manganate cathode material and preparation method thereof
CN109509875B (en) * 2018-11-26 2021-09-10 合肥国轩高科动力能源有限公司 High-rate single crystal lithium nickel cobalt manganese oxide cathode material and preparation method thereof
CN109713275A (en) * 2018-12-28 2019-05-03 天能电池(芜湖)有限公司 Lithium ion battery nickel cobalt aluminium tertiary cathode material method of modifying
CN112186177A (en) * 2019-07-04 2021-01-05 丰田自动车株式会社 Nonaqueous electrolyte secondary battery and positive electrode active material
CN110233261A (en) * 2019-07-08 2019-09-13 甘肃大象能源科技有限公司 A kind of preparation method and lithium ion battery of monocrystalline ternary anode material of lithium battery
CN110518221B (en) * 2019-09-05 2022-04-15 中南大学 Method for preparing lithium silicate coated lithium nickel cobalt manganese oxide positive electrode material by anti-solvent method
CN110518221A (en) * 2019-09-05 2019-11-29 中南大学 A kind of method that anti-solvent method prepares lithium metasilicate cladding nickel-cobalt lithium manganate cathode material
CN110752362A (en) * 2019-10-31 2020-02-04 贵州中伟资源循环产业发展有限公司 Ternary precursor coated with magnesium and preparation method thereof
CN113097461A (en) * 2021-03-29 2021-07-09 清华大学 Ternary cathode material @ yttrium oxide core-shell structure composite material and preparation method thereof
CN113097461B (en) * 2021-03-29 2022-03-29 清华大学 Ternary cathode material @ yttrium oxide core-shell structure composite material and preparation method thereof
CN113629232A (en) * 2021-08-06 2021-11-09 浙江帕瓦新能源股份有限公司 Modified low-cobalt ternary positive electrode material precursor and positive electrode material
CN113839025A (en) * 2021-09-24 2021-12-24 四川朗晟新能源科技有限公司 High-nickel ternary cathode material of lithium ion battery and modification method thereof
CN113839025B (en) * 2021-09-24 2023-06-16 四川朗晟新能源科技有限公司 High-nickel ternary positive electrode material of lithium ion battery and modification method thereof
CN114538532A (en) * 2022-01-11 2022-05-27 宜宾锂宝新材料有限公司 Preparation method of high-nickel ternary cathode material and prepared high-nickel ternary cathode material
CN114538532B (en) * 2022-01-11 2024-03-22 宜宾锂宝新材料有限公司 Preparation method of high-nickel ternary cathode material and prepared high-nickel ternary cathode material
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