CN103682319A - Constant high temperature circulation NCM 523 (nickel cobalt manganese acid lithium) ternary material and preparation method thereof - Google Patents

Constant high temperature circulation NCM 523 (nickel cobalt manganese acid lithium) ternary material and preparation method thereof Download PDF

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CN103682319A
CN103682319A CN201310726770.XA CN201310726770A CN103682319A CN 103682319 A CN103682319 A CN 103682319A CN 201310726770 A CN201310726770 A CN 201310726770A CN 103682319 A CN103682319 A CN 103682319A
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high temperature
ternary material
lithium manganate
temperature circulation
nickle cobalt
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衡凯
赵志兵
王燕舞
万国莉
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LANZHOU JINLI ENERGY SCIENCE AND TECHNOLOGY Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • YGENERAL 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
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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10Energy storage using batteries

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Abstract

The invention relates to a preparation method of a constant high temperature circulation NCM 523 (nickel cobalt manganese acid lithium) ternary material for a lithium ion battery. The chemical formula of the constant high temperature circulation NCM 523 ternary material is Li(1+x)Ni0.5Co0.2Mn0.3AlxO2, wherein x is 0.02-0.1. According to the method, aluminum salt and oxide thereof are added in material sintering, a dry process is adopted to uniformly mix, then sintering is performed, high-temperature performance of NCM 523 is increased by admixing Al ions, so that the problems of worse high-temperature cycle performance and high-temperature storage performance of nickel cobalt manganese acid lithium are effectively solved; as the dry-process is adopted to admix, prepared NCM 523 cathode material has the advantages of large specific capacity, good cycle performance, stable quality, low cost, simple preparation technology and little pollution, does not produce waste water, and is easy for industrialization.

Description

Long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material and preparation method thereof
Technical field
The invention belongs to new energy materials preparing technical field, relate to the preparation method for the long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material of lithium ion battery.
 
Background technology
In order progressively to solve energy shortage and the atmosphere polluting problem of restriction Economic Development, the advantages such as operating voltage is high because having for lithium ion battery, energy density is large, have extended cycle life, pollute less, memory-less effect, volume are little, lightweight, non-environmental-pollution, on technology, production, market, obtain fast development in recent years, formed a large novel industry.
Anode material nickel cobalt manganic acid lithium NCM523 ternary material for lithium ion battery has the advantages such as voltage platform is high, specific capacity is large, normal-temperature circulating performance is good, energy density is high, self discharge is little, but this material charge and discharge cycles capacity attenuation at 55 ℃ of temperature is fast, and memory property is poor.By nickle cobalt lithium manganate NCM523 ternary material is carried out to metal ion mixing, improve the structural stability of material, within the scope of 3.0~4.3V, with 0.2C electric current, discharge and recharge, more than specific capacity can reach 153mAh/g, high temperature circulation conservation rate is compared pure phase material and is all improved and improves with high-temperature storage performance.
Summary of the invention
In view of above-mentioned, the object of the invention is to provide a kind of long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material.
Another object of the present invention is to provide the method for preparing long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material.The method adopts dry mixed to carry out Al ion doping to nickle cobalt lithium manganate NCM523 ternary material, has improved stability and the high-temperature behavior of material, has especially improved normal high temperature circulation conservation rate and the high-temperature storage performance of material.
The object of the invention is to complete like this:
A long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material, is characterized in that: chemical expression is Li 1+xni 0.5co 0.2mn 0.3al xo 2, 0.02≤x≤0.10 wherein.
Prepare a kind of method of growing high temperature circulation nickle cobalt lithium manganate NCM523 ternary material described in claim 1, it is characterized in that, comprise the following steps:
(1) by the salting liquid of nickel, cobalt, manganese ternary, according to Ni:Co:Mn mol ratio, be that 5:2:3 mixes, in reactor, add nickelous sulfate, cobaltous sulfate, manganese sulfate solution, insert and in aqueous slkali, carry out coprecipitation reaction, the pH value 11~12 of mixed solution, temperature 50 C, continuous stirring reaction ageing 12 hours after 8 hours, washs, filters, is drying to obtain presoma (Ni with pure water 0.5co 0.2mn 0.3) OH;
(2) presoma (the Ni (1) step being obtained 0.5co 0.2mn 0.3) after OH sieves, 400~600 ℃ of temperature lower calcinations 4~10 hours, obtain oxidation of precursor thing (Ni 0.5co 0.2mn 0.3) 2o;
(3) by the (2) oxidation of precursor thing (Ni of gained of step 0.5co 0.2mn 0.3) 2o, after sieving with battery-level lithium carbonate or lithium hydroxide and activated aluminum salt or oxide according to Li:Ni 0.5co 0.2mn 0.3: mole proportioning of Al=(1+x): 1:x, 0.02≤x≤0.10 wherein, and with batch mixer, adopt dry mixed mode fully to mix under certain rotating speed;
(4) the mixture (3) step being obtained packs saggar compacting into, and in air atmosphere, at 900~950 ℃ of temperature, heated at constant temperature 12 ~ 20h carries out calcination, and after completing, naturally cooling 8~12h takes out powder pulverizing, sieves;
(5) it is floating that the powder (4) step being obtained packs saggar into, and in air atmosphere, at 800~850 ℃ of temperature, heated at constant temperature 6 ~ 12h carries out roasting, and after completing, naturally cold rear taking-up powder sieves, and obtains long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material Li 1+xni 0.5co 0.2mn 0.3al xo 2.
Presoma (the Ni of above-mentioned steps in (1) 0.5co 0.2mn 0.3) OH is spherical or class is spherical.
The battery-level lithium carbonate of above-mentioned steps in (3) or the mean particle size range of lithium hydroxide are 5 μ m~7 μ m.
The activated aluminum salt of above-mentioned steps in (3) or oxide are at least aluminum nitrate, aluminum sulfate, aluminum acetate, a kind of in aluminium acetate, γ type aluminium oxide, aluminium hydroxide partially, and particle size range is 25nm~5 μ m.
The above-mentioned steps (3) rotating speed of middle batch mixer is 30~300 revs/min, and the dry mixed time is 1~4 hour.
 
Advantage of the present invention:
The present invention adopts dry mixed to carry out Al ion doping to nickle cobalt lithium manganate NCM523 ternary material.The ternary material performance of preparation has that large, the normal high temperature cyclic performance of specific capacity is good, stay in grade, cost are low; Process for producing is simple, with low cost, be easy to accomplish scale production.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material in the present invention.
Fig. 2 is the stereoscan photograph of 1000 times of the amplifications of long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material in the present invention.
Fig. 3 is the stereoscan photograph of 5000 times of the amplifications of long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material in the present invention.
Fig. 4 is that in the present invention, long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material and common nickle cobalt lithium manganate NCM523 ternary material (example 2 and comparative example) voltage under 55 ℃ of conditions are that 3.0-4.3V, 0.2C discharge and recharge lower circulation cyclic curve figure.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail:
comparative example
By Ni:Co:Mn mol ratio, be 5:2:3 be 1mol/L nickelous sulfate, cobaltous sulfate, manganese sulfate solution to adding metal molar concentration in reactor, add the soda bath of 10mol/L and the NH of 10mol/L simultaneously 4 +solution, controls the pH value 11~12 of mixed solution, temperature 50 C, and continuous stirring reaction ageing 12 hours after 8 hours, the control of noting pH value in ageing process pH value when reacting is consistent.Then filter, wash, dry and obtain (Ni 0.5co 0.2mn 0.3) OH presoma, this ternary precursor particle mean size (D50) is 10.8 μ m, specific area 7.27m 2/ g.
By presoma (Ni obtained above 0.5co 0.2mn 0.3) after OH sieves, 450 ℃ of temperature lower calcinations 6 hours, obtain oxidation of precursor thing (Ni 0.5co 0.2mn 0.3) 2o, this forerunner's oxide body particle mean size (D50) is 9.3 μ m, specific area 40.2m 2/ g.By the oxidation of precursor thing (Ni obtaining 0.5co 0.2mn 0.3) 2o is that 6 μ m battery-level lithium carbonates are according to Li:Ni with particle mean size after sieving 0.5co 0.2mn 0.3mole proportioning of=1.06:1 adopts dry mixed mode fully to mix.
Pack mixture obtained above into saggar compacting, in air atmosphere, at 930 ℃ of temperature, heated at constant temperature is carried out calcination in 16 hours, and after completing, naturally cooling 8h takes out powder pulverizing, sieves.It is floating that the powder obtaining packs saggar into, and in air atmosphere, at 830 ℃ of temperature, heated at constant temperature is carried out roasting in 6 hours, and after completing, naturally cold rear taking-up powder sieves, and obtains LiNi 0.5co 0.2mn 0.3o 2.The specific area of this nickle cobalt lithium manganate is 0.23m 2/ g, average grain diameter (D50) is 11.56 μ m.
Resulting nickel-cobalt lithium manganate material is made into button cell, detects its electrical property, material gram volume reaches 157.8mA/g, and 50 circulation conservation rates are 86.88% at 55 ℃, high temperature storage conservation rate 89.2%.
example 1:
By the oxidation of precursor thing (Ni obtaining in comparative example 0.5co 0.2mn 0.3) 2o is that 6 μ m battery-level lithium carbonates, the particle mean size aluminium hydroxide that is 200nm is according to Li:Ni with particle mean size after sieving 0.5co 0.2mn 0.3: mole proportioning of Al=1.02:1:0.02 adopts dry mixed mode fully to mix.
Pack mixture obtained above into saggar compacting, in air atmosphere, at 950 ℃ of temperature, heated at constant temperature is carried out calcination in 18 hours, and after completing, naturally cooling 10h takes out powder pulverizing, sieves.
Pack powder obtained above into saggar floating, in air atmosphere, at 810 ℃ of temperature, heated at constant temperature is carried out roasting in 6 hours, and after completing, naturally cold rear taking-up powder sieves, and obtains long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material Li 1.02ni 0.5co 0.2mn 0.3al 0.02o 2.The specific area of this nickle cobalt lithium manganate is 0.38m 2/ g, average grain diameter (D50) is 11.25 μ m.
Resulting nickel-cobalt lithium manganate material is made into button cell, detects its electrical property, material gram volume reaches 156.8mA/g, and 50 circulation conservation rates are 92.1% at 55 ℃, and high temperature storage conservation rate 93.5% performance index are excellent.
example 2:
By the oxidation of precursor thing (Ni obtaining in comparative example 0.5co 0.2mn 0.3) 2o is that 6 μ m battery-level lithium carbonates, the particle mean size aluminium oxide that is 50nm is according to Li:Ni with particle mean size after sieving 0.5co 0.2mn 0.3: mole proportioning of Al=1.05:1:0.05 adopts dry mixed mode fully to mix.
Pack mixture obtained above into saggar compacting, in air atmosphere, at 930 ℃ of temperature, heated at constant temperature is carried out calcination in 15 hours, and after completing, naturally cooling 8h takes out powder pulverizing, sieves.
Pack powder obtained above into saggar floating, in air atmosphere, at 830 ℃ of temperature, heated at constant temperature is carried out roasting in 8 hours, and after completing, naturally cold rear taking-up powder sieves, and obtains long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material Li 1.05ni 0.5co 0.2mn 0.3al 0.05o 2.The specific area of this nickle cobalt lithium manganate is 0.27m 2/ g, average grain diameter (D50) is 11.88 μ m.
Resulting nickel-cobalt lithium manganate material is made into button cell, detects its electrical property, material gram volume reaches 155.9mA/g, and 50 circulation conservation rates are 96.4% at 55 ℃, high temperature storage conservation rate 94.8%, and performance index are excellent.
example 3:
By the oxidation of precursor thing (Ni obtaining in comparative example 0.5co 0.2mn 0.3) 2o is that 6 μ m battery-level lithium carbonates, particle mean size are that the aluminum nitrate of 1.8 μ m is according to Li:Ni with particle mean size after sieving 0.5co 0.2mn 0.3: mole proportioning of Al=1.08:1:0.08 adopts dry mixed mode fully to mix.
Pack mixture obtained above into saggar compacting, in air atmosphere, at 910 ℃ of temperature, heated at constant temperature is carried out calcination in 14 hours, and after completing, naturally cooling 7h takes out powder pulverizing, sieves.
Pack powder obtained above into saggar floating, in air atmosphere, at 850 ℃ of temperature, heated at constant temperature is carried out roasting in 8 hours, and after completing, naturally cold rear taking-up powder sieves, and obtains long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material Li 1.08ni 0.5co 0.2mn 0.3al 0.08o 2.The specific area of this nickle cobalt lithium manganate is 0.20m 2/ g, average grain diameter (D50) is 12.25 μ m.
Resulting nickel-cobalt lithium manganate material is made into button cell, detects its electrical property, material gram volume reaches 153.1mA/g, and 50 circulation conservation rates are 97.5% at 55 ℃, and high temperature storage conservation rate 95.8% performance index are excellent.
Will comparative example, example 1, example 2, example 3in resulting positive electrode adopt Japanese DMAX2400 type X-ray diffractometer carry out structural analysis (CuK target, tube voltage is 40kV, electric current is 150mA, 10 o~100 o, step-length 0.02 o), Fig. 1 is comparative example, example 1, example 2, example 3resulting positive electrode XRD figure, as shown in Figure 1 after the nickle cobalt lithium manganate NCM523 of Al ion doping without dephasign, advantages of good crystallization.
Fig. 2 is example 2the stereoscan photograph of resulting long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material, multiplication factor is 1000 times.
Fig. 3 is example 2the stereoscan photograph of resulting long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material, multiplication factor is 5000 times.
Will comparative example, example 1, example 2, example 3in resulting positive electrode to adopt negative pole be lithium sheet, concentration is 1mol/lLiPF 6electrolyte, thickness are that the barrier film of 16 μ m Clegard2000 is made 2016 simulation button cells, adopt blue electric cell tester to test.Fig. 4 is example 1, example 2, example 3with comparative exampleit is cyclic curve figure under 3.0-4.3V, 0.2C rate charge-discharge that resulting positive electrode is made after 2016 simulation button cells voltage under 55 ℃ of conditions, as shown in Figure 4 charge and discharge cycles under 55 ℃ of hot conditionss example 1, example 2, example 3with comparative example50 times circulation conservation rate is respectively 92.1%, 96.4%, 97.5%, 86.88%, example 1, example 2, example 3the circulation conservation rate of material under 55 ℃ of hot conditionss significantly better than comparative examplematerial, so doped with Al ion of the present invention has played vital effect for the high-temperature behavior of improving nickle cobalt lithium manganate NCM523 material.

Claims (6)

1. a long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material, is characterized in that: chemical expression is Li 1+xni 0.5co 0.2mn 0.3al xo 2, 0.02≤x≤0.10 wherein.
2. prepare a kind of method of growing high temperature circulation nickle cobalt lithium manganate NCM523 ternary material described in claim 1, it is characterized in that, comprise the following steps:
(1) by the salting liquid of nickel, cobalt, manganese ternary, according to Ni:Co:Mn mol ratio, be that 5:2:3 mixes, in reactor, add nickelous sulfate, cobaltous sulfate, manganese sulfate solution, insert and in aqueous slkali, carry out coprecipitation reaction, the pH value 11~12 of mixed solution, temperature 50 C, continuous stirring reaction ageing 12 hours after 8 hours, washs, filters, is drying to obtain presoma (Ni with pure water 0.5co 0.2mn 0.3) OH;
(2) presoma (the Ni (1) step being obtained 0.5co 0.2mn 0.3) after OH sieves, 400~600 ℃ of temperature lower calcinations 4~10 hours, obtain oxidation of precursor thing (Ni 0.5co 0.2mn 0.3) 2o;
(3) by the (2) oxidation of precursor thing (Ni of gained of step 0.5co 0.2mn 0.3) 2o, after sieving with battery-level lithium carbonate or lithium hydroxide and activated aluminum salt or oxide according to Li:Ni 0.5co 0.2mn 0.3: mole proportioning of Al=(1+x): 1:x, 0.02≤x≤0.10 wherein, and with batch mixer, adopt dry mixed mode fully to mix under certain rotating speed;
(4) the mixture (3) step being obtained packs saggar compacting into, and in air atmosphere, at 900~950 ℃ of temperature, heated at constant temperature 12 ~ 20h carries out calcination, and after completing, naturally cooling 8~12h takes out powder pulverizing, sieves;
(5) it is floating that the powder (4) step being obtained packs saggar into, and in air atmosphere, at 800~850 ℃ of temperature, heated at constant temperature 6 ~ 12h carries out roasting, and after completing, naturally cold rear taking-up powder sieves, and obtains long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material Li 1+xni 0.5co 0.2mn 0.3al xo 2.
3. a kind of method of preparing long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material as claimed in claim 2, is characterized in that: the presoma (Ni of described step in (1) 0.5co 0.2mn 0.3) OH is spherical or class is spherical.
4. a kind of method of preparing long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material as claimed in claim 2, is characterized in that: the battery-level lithium carbonate of described step in (3) or the mean particle size range of lithium hydroxide are 5 μ m~7 μ m.
5. a kind of method of preparing long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material as claimed in claim 2, it is characterized in that: the activated aluminum salt of described step in (3) or oxide are at least aluminum nitrate, aluminum sulfate, aluminum acetate, a kind of in aluminium acetate, γ type aluminium oxide, aluminium hydroxide partially, and particle size range is 25nm~5 μ m.
6. a kind of method of preparing long high temperature circulation nickle cobalt lithium manganate NCM523 ternary material as claimed in claim 1, is characterized in that: the described step (3) rotating speed of middle batch mixer is 30~300 revs/min, and the dry mixed time is 1~4 hour.
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CN105118985A (en) * 2015-08-27 2015-12-02 北大先行科技产业有限公司 Lithium ion battery positive electrode material with adjustable crystalline grain size and preparation method thereof
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Application publication date: 20140326