CN109286016A - A kind of preparation method of big particle size single crystals ternary cathode material of lithium ion battery - Google Patents
A kind of preparation method of big particle size single crystals ternary cathode material of lithium ion battery Download PDFInfo
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- CN109286016A CN109286016A CN201810947813.XA CN201810947813A CN109286016A CN 109286016 A CN109286016 A CN 109286016A CN 201810947813 A CN201810947813 A CN 201810947813A CN 109286016 A CN109286016 A CN 109286016A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The invention discloses a kind of preparation methods of big particle size single crystals ternary cathode material of lithium ion battery.Firstly, preparing the ternary precursor Ni that D50 is 3-5um by coprecipitation1‑x‑yCoxMy(OH)2；The presoma of co-precipitation preparation is uniform by wet-mixing with lithium source, and chemical combination is dry；Finally oxygen in the mixture investment revolving burner after presoma and lithium source combination drying, will be led to, mixture is byed high temperature sintering while the rotation with revolving burner is stirred overturning in revolving burner, is reacted.This dynamic sinter enables mixture to come into full contact with oxygen, reduces Lacking oxygen, improves final agglomerated material LiNi1‑x‑yCoxMyO2Crystallinity, furthermore material recrystallizes under hot conditions in dynamic environment, it is suppressed that the reunion between particle so that each primary particle reaches uniform dispersion, so that big particle size single crystals tertiary cathode material be made.
Description
Technical field
The invention belongs to field of lithium ion battery material more particularly to ternary cathode material of lithium ion battery preparation methods.
Background technique
In recent years, quick emerge of new-energy automobile had driven the development of power battery, and proposed more to battery
Harsh requirement, while meeting safety and high circulation performance, it is necessary to have high energy density, meet electric vehicle with this
Cruising ability.In lithium ion battery, compared with negative electrode material, positive electrode restricts lithium because low gram volume and compacted density become
The principal element of ion battery high-energy density.Lithium ion tertiary cathode material, especially high-nickel material
LiNi0.8Co0.1Mn0.1O2And LiNi0.8Co0.15Al0.05O2Because gram volume is favored by researcher greatly, but three largely prepared
First positive electrode is secondary class spherical particles made of being reunited as primary particle.In this structure, there is following several places not
Foot,
First: there are more gaps between primary particle, not only reduce the compacted density of material, and material is made to compare table
Area increases, and more particle and electrolyte contacts increase the quantity of side reaction；Second: two made of being reunited as primary particle
Secondary spherical material is in pole piece manufacturing process, and when to roller, globoid is easily crushed；Third: in battery after repeatedly recycling,
The globoid being agglomerated into is easy dusting.
For problems, researcher has prepared monocrystalline lithium ion tertiary cathode material, disclosed in 2015
By the way that cosolvent and high temperature is added in the preparation method of the ternary cathode material of lithium ion battery of CN104979546A monocrystalline pattern
Calcining obtains monocrystalline ternary cathode material of lithium ion battery, but this process needs the addition of cosolvent, and needs multiple 900-
1000 DEG C of high temperature sintering, gained monocrystal material granularity is smaller, and about 1 μm of maximum particle diameter.
The preparation of CN107293744A monocrystalline tertiary cathode material disclosed in 2017, the method need adding for modifying agent
Enter, also needs 1000 DEG C or so of high temperature sintering, and monocrystalline ternary material is prepared by the method, easily occur between particle
Reunite.
Summary of the invention
The main object of the present invention be in view of the above technology aspect there are the problem of and deficiency, provide a kind of partial size it is big,
The preparation method of the big particle size single crystals ternary cathode material of lithium ion battery of even particulate dispersion.
The present invention adopts the following technical scheme that.The preparation method of big particle size single crystals ternary cathode material of lithium ion battery,
Molecular formula is LiNi1-x-yCoxMyO2, specifically use following steps:
(1) coprecipitation is used, first by nickel salt, cobalt salt and manganese salt or aluminium salt according to mole of Ni:Co:M=1-x-y:x:y
Than being made into the metal mixed salt solution that total concentration is 2M；Compound concentration is the sodium hydroxide solution of 3M；Preparing mass fraction is 16%
Ammonia spirit；Metal mixed salt solution, sodium hydroxide solution and the ammonium hydroxide of preparation are pressed into certain flow simultaneously by peristaltic pump
It being added in reaction kettle, is sufficiently stirred, reaction whole process carries out in an inert atmosphere, finally by the precipitating filtration washing of preparation,
It is dry at 100 DEG C, finally obtain the spherical or spherical ternary precursor Ni being agglomerated by primary particle1-x-yCoxMy(OH)2,
D50 is at 3-5 μm for its granularity；
(2) by the ternary precursor Ni of co-precipitation preparation1-x-yCoxMy(OH)2, lithium source, deionized water by certain mass than stirring
Mixing, then microwave drying；
(3) mixture after will be dry in step (2) is put into rotary sintering furnace, and the front end of rotary sintering furnace leads to oxygen,
Rear end waste air, mixture are stirred overturning with the rotation of revolving burner on one side in revolving burner, on one side by high temperature sintering, occur anti-
It answers.
It is prepared in step (1) according to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery
Ternary precursor Ni1-x-yCoxMy(OH)2, in which: in 0.1≤x≤0.3,0 < y≤0.3, M Al, Mn element
It is one or two kinds of.
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, lithium source is carbon in step (2)
One or more of sour lithium, lithium nitrate, lithium hydroxide, lithium acetate, and lithium ion and ternary precursor Ni in lithium source1-x- yCoxMy(OH)2Mol ratio is 1:1.01-1.08.
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, material by wet type mixing in step (2),
Ternary precursor Ni1-x-yCoxMy(OH)2Ratio with water is 1:0.3-0.5.
It is dry in step (2) to use according to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery
Microwave rapid dry process, by ternary precursor Ni1-x-yCoxMy(OH)2, lithium source, deionized water be stirred and be placed in micro-wave oven
Carry out rapid draing.
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, sintering furnace is adopted in step (3)
With rotary sintering furnace, respectively there is a blow vent in furnace body front and rear end, and front end is used to lead to oxygen, and rear end is used for waste air.
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, oxygen-supply quantity is in step (3)
0.2-0.8m3/h。
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, revolving burner turns in step (3)
Speed is 1 circle/30s-1 circle/300s, and mixture is constantly in " movement " state in sintering, is constantly stirred, overturns.
According to the preparation method of the big particle size single crystals ternary cathode material of lithium ion battery, sintering temperature in step (3)
For double sintering, first segment sintering temperature is 400-500 DEG C, sintering time 2-4h；Second segment sintering temperature is 750-800 DEG C,
Sintering time is 15-20h.
Compared with prior art, the invention has the characteristics that:
First, the presoma of preparation is spherical material made of being reunited as primary particle, and partial size D50 is 3-5 μm；Through studying
It was found that the presoma in this particle size range is easier the recrystallization that falls off between primary particle in subsequent agitation high temperature sintering,
The monocrystalline formed.
Second, when sintering at high temperature, drive the overturning of material to stir by the rotation of revolving burner, this makes material and oxygen more
Good comes into full contact with, reduce in material because contacted with oxygen it is bad caused by Lacking oxygen；Secondly, the method is constantly in material
" movement " state recrystallizes under hot conditions, it is suppressed that the reunion between particle, so that each primary particle reaches uniform
Dispersion, so that good dispersion degree is prepared, the big monocrystalline tertiary cathode material of granularity.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the tertiary cathode material of comparative example 1 of the present invention preparation.
Fig. 2 is the particle size distribution figure of the tertiary cathode material of comparative example 1 of the present invention preparation.
Fig. 3 is the scanning electron microscope (SEM) photograph of tertiary cathode material prepared by the embodiment of the present invention 2.
Fig. 4 is the particle size distribution figure of tertiary cathode material prepared by the embodiment of the present invention 2.
Specific embodiment
A kind of preparation method of big particle size single crystals ternary cathode material of lithium ion battery, molecular formula LiNi1-x- yCoxMyO2, which is characterized in that specifically includes the following steps:
(1) uses coprecipitation, first by nickel salt, cobalt salt and manganese salt or aluminium salt according to mole of Ni:Co:M=1-x-y:x:y
Than being made into the metal mixed salt solution that total concentration is 2M；Compound concentration is the sodium hydroxide solution of 3M；Preparing mass fraction is 16%
Ammonia spirit；Metal mixed salt solution, sodium hydroxide solution and the ammonium hydroxide of preparation are pressed into certain flow simultaneously by peristaltic pump
It being added in reaction kettle, is sufficiently stirred, reaction whole process carries out in an inert atmosphere, finally by the precipitating filtration washing of preparation,
It is dry at 100 DEG C, finally obtain the spherical or spherical ternary precursor Ni being agglomerated by primary particle1-x-yCoxMy(OH)2,
D50 is at 3-5 μm for its granularity；
(2) is stirred the ternary precursor Ni1-x-yCoxMy (OH) 2 of co-precipitation preparation, lithium source, deionized water by certain mass ratio
Mixing is mixed, then microwave drying；
(3) mixture after will be dry in step (2) is put into rotary sintering furnace, and the front end of rotary sintering furnace leads to oxygen,
Rear end waste air, mixture are stirred overturning with the rotation of revolving burner on one side in revolving burner, on one side by high temperature sintering, occur anti-
It answers.
Prepared ternary precursor Ni in step (1)1-x-yCoxMy(OH)2, in which: 0.1≤x≤0.3,0 <
One of y≤0.3, M TAl, Mn element is a variety of.
Lithium source is one or both of lithium carbonate, lithium nitrate, lithium hydroxide, lithium acetate in step (2), and in lithium source
Lithium ion and ternary precursor Ni1-x-yCoxMy(OH)2Mol ratio is 1:1.01-1.08.
Material by wet type mixing in step (2), ternary precursor Ni1-x-yCoxMy(OH)2Ratio with water is 1:0.3-0.5.Step
Suddenly dry in (2) to use microwave rapid dry process microwave rapid dry process, by ternary precursor Ni1-x-yCoxMy(OH)2, lithium source,
Deionized water, which is stirred to be placed in micro-wave oven, carries out rapid draing.
Oxygen-supply quantity is 0.2-0.8m in step (3)3/ h, and one end is into oxygen, other end waste air, if front end is into oxygen,
Rear end waste air.Mixture is constantly in " movement " state in sintering in step (3), is constantly stirred, and overturns.Step (3)
Middle sintering temperature is double sintering, and first segment sintering temperature is 400-500 DEG C, sintering time 2-4h；Second segment sintering temperature is
750-800 DEG C, sintering time 15-20h.
Below with LiNi0.8Co0.1Mn0.1O2For, in conjunction with the embodiments and attached drawing makees further details of retouch to the present invention
It states, embodiments of the present invention are not limited thereto.
Comparative example 1
Nickel sulfate, cobaltous sulfate, the manganese sulfate mixed salt solution that total concentration is 2M are prepared, wherein nickel, cobalt, manganese molar ratio are 8:1:1；
Prepare the sodium hydroxide solution that concentration is 3M.
It is previously added the bottom 2L liquid in 60L reaction kettle, 50 DEG C of bath temperature, by metal salt, sodium hydroxide and ammonia spirit
Three cocurrents are pumped into reaction kettle, stirring rate 500r/min, and regulation sodium hydroxide stability of flow reaction process pH is 11.5.
Continuous coprecipitation reacts 30h, to after reaction, be aged 20h.Washing and filter pressing, 100 DEG C of drying are carried out finally, precipitating to gained
Obtain the Ni spherical, granularity D50 is 3-5 μm0.8Co0.1Mn0.1(OH)2Persursor material.
By Ni0.8Co0.1Mn0.1(OH)2It is matched with lithium carbonate by 1:1.05 lithiumation, water Ni0.8Co0.1Mn0.1(OH)2Matter
0.3 times of amount is mixed, and micro-wave oven microwave drying is then passed through.By the material after drying in Muffle furnace, it is in oxygen-supply quantity
0.8m3Under conditions of/h, after 450 DEG C of sintering 2h, 800 DEG C of sintering 20h.
Embodiment 1
The Ni prepared based on comparative example 10.8Co0.1Mn0.1(OH)2, it is matched with lithium carbonate by 1:1.01 lithiumation, water is
Ni0.8Co0.1Mn0.1(OH)20.5 times of quality is mixed, and microwave drying is then passed through.
By in the material investment revolving burner after drying, converter revolving speed is 1 circle/30s, is 0.2m in oxygen-supply quantity3The condition of/h
Under, after 450 DEG C of sintering 4h, 800 DEG C of sintering 15h.
Embodiment 2
The Ni prepared based on comparative example 10.8Co0.1Mn0.1(OH)2, it is matched with lithium carbonate by 1:1.05 lithiumation, water is
Ni0.8Co0.1Mn0.1(OH)20.3 times of quality is mixed, and microwave drying is then passed through.
By in the material investment revolving burner after drying, converter revolving speed is 1 circle/120s, is 0.8m in oxygen-supply quantity3The condition of/h
Under, after 450 DEG C of sintering 2h, 800 DEG C of sintering 20h.
Embodiment 3
Ni based on comparative example preparation0.8Co0.1Mn0.1(OH)2, it is matched with lithium carbonate by 1:1.05 lithiumation, water is
Ni0.8Co0.1Mn0.1(OH)20.3 times of quality is mixed, and the microwave drying of chemical combination furnace is then passed through.
By in the material investment revolving burner after drying, converter revolving speed is 1 circle/300s, is 0.8m in oxygen-supply quantity3The condition of/h
Under, after 400 DEG C of sintering 2h, 750 DEG C of sintering 20h.
Embodiment 4
Ni based on comparative example preparation0.8Co0.1Mn0.1(OH)2, it is matched with lithium carbonate by 1:1.08 lithiumation, water is
Ni0.8Co0.1Mn0.1(OH)20.5 times of quality is mixed, and microwave drying is then passed through.
By in the material investment revolving burner after drying, converter revolving speed is 1 circle/30s, is 0.5m in oxygen-supply quantity3The condition of/h
Under, after 500 DEG C of sintering 4h, 800 DEG C of sintering 15h.
By comparison (comparative example 1 and embodiment 2 compare) discovery of Fig. 1 and Fig. 3, reached by the rotation of revolving burner to object
Material carries out stirring effect, and material is made to be in " movement " state, avoids the reunion again of the primary particle in recrystallization, prepares
Good dispersion, the big monocrystalline primary particle tertiary cathode material of granularity.In conjunction with Fig. 4 particle size distribution figure, it can be seen that embodiment 2
The monocrystalline primary particle D50 arrived is 9 μm, hence it is evident that greater than the D50 of comparative example 1.
The announcement of book according to the above description, those skilled in the art in the invention can also carry out above embodiment
Change and modification appropriate.So the invention is not limited to the specific embodiments disclosed and described above, to of the invention
Some modifications and changes should also be as falling into protection scope of the invention.In addition, although having used some spies in this specification
Fixed term, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (9)
1. a kind of preparation method of big particle size single crystals ternary cathode material of lithium ion battery, molecular formula LiNi1-x-yCoxMyO2,
It is characterized in that, specifically using following steps:
Using coprecipitation, nickel salt, cobalt salt and manganese salt or aluminium salt are matched according to the molar ratio of Ni:Co:M=1-x-y:x:y first
At metal mixed salt solution；Prepare sodium hydroxide solution；Prepare ammonia spirit；It is by peristaltic pump that the metal salt mixing of preparation is molten
Liquid, sodium hydroxide solution and ammonium hydroxide are added in reaction kettle simultaneously by certain flow, are sufficiently stirred, and react whole process in indifferent gas
It is carried out in atmosphere, dry finally by the precipitating filtration washing of preparation, final acquisition is agglomerated into spherical or spherical by primary particle
Ternary precursor Ni1-x-yCoxMy(OH)2, granularity D50 is at 3-5 μm；
By the ternary precursor Ni of co-precipitation preparation1-x-yCoxMy(OH)2, lithium source, deionized water be stirred, then microwave is dry
It is dry；
Mixture after will be dry in step (2) is put into rotary sintering furnace, and the front end of rotary sintering furnace leads to oxygen, rear end
Waste air, mixture are stirred overturning with the rotation of revolving burner on one side in revolving burner, on one side by high temperature sintering, react.
2. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Prepared ternary precursor Ni in step (1)1-x-yCoxMy(OH)2, in which: 0.1≤x≤0.3,0 y≤0.3 <,
M is one or both of Al, Mn element.
3. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
In step (2) lithium source be one or more of lithium carbonate, lithium nitrate, lithium hydroxide, lithium acetate, and in lithium source lithium ion with
Ternary precursor Ni1-x-yCoxMy(OH)2Mol ratio is 1:1.01-1.08.
4. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Material by wet type mixing in step (2), ternary precursor Ni1-x-yCoxMy(OH)2Ratio with water is 1:0.3-0.5.
5. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
It is dry in step (2) to use microwave rapid dry process, by ternary precursor Ni1-x-yCoxMy(OH)2, lithium source, deionized water stirring
Mixing, which is placed in micro-wave oven, carries out rapid draing.
6. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Sintering furnace uses rotary sintering furnace in step (3), and respectively there is a port in furnace body front and rear end, and front end is used to lead to oxygen, and rear end is used
In waste air.
7. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Oxygen-supply quantity is 0.2-0.8m in step (3)3/h。
8. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Revolving burner revolving speed is 1 circle/30s-1 circle/300s in step (3), and mixture is constantly in " movement " state, constantly quilt in sintering
Stirring overturning.
9. the preparation method of big particle size single crystals ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Sintering temperature is double sintering in step (3), and first segment sintering temperature is 400-500 DEG C, sintering time 2-4h；Second segment sintering
Temperature is 750-800 DEG C, sintering time 15-20h.
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| CN109888242A (en) * | 2019-03-12 | 2019-06-14 | 四川纳创时代新能源科技有限公司 | A kind of high-tap density cobalt nickel lithium manganate ternary material and preparation method thereof |
| CN109962234A (en) * | 2019-03-29 | 2019-07-02 | 蜂巢能源科技有限公司 | Monocrystalline positive electrode of concentration gradient and preparation method thereof |
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