CN105161705B - A kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material and preparation method thereof - Google Patents
A kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material and preparation method thereof Download PDFInfo
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- 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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- 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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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode materials and preparation method thereof, belong to electrochemical technology field.The positive electrode includes nickle cobalt lithium manganate and the lithium manganese phosphate for being coated on the nickle cobalt lithium manganate surface, and the chemical formula of the nickle cobalt lithium manganate is LiNixCoyMnzO2, wherein x+y+z=1,0.25≤x≤0.6,0.1≤y≤0.4,0.2≤z≤0.5.The preparation process of the material is simple, of low cost, environmental-friendly, is easy to industrialized production；The nickel-cobalt lithium manganate cathode material of lithium manganese phosphate cladding prepared by the present invention especially significantly improves nickel cobalt mangaic acid high voltage compared with uncoated nickle cobalt lithium manganate（4.4V）Lower cyclical stability；Lithium manganese phosphate has higher voltage as positive electrode in itself simultaneously（4.1V）, nickel-cobalt lithium manganate material surface lithium ion conduction is promoted after cladding, improves its high rate performance.
Description
Technical field
The present invention relates to electrochemical technology field, more particularly to anode material for lithium-ion batteries, further to a kind of phosphorus
Sour manganese lithium cladding nickel-cobalt lithium manganate cathode material and preparation method thereof.
Background technology
With becoming increasingly conspicuous for the energy and environmental problem, lithium ion battery is as a kind of energy storage of clean and effective with turning
Medium is changed, has obtained the research and attention of more and more people.Lithium ion battery is widely used in mobile phone, laptop, photograph
The portable mobile apparatus such as machine；It is also lithium ion battery that very powerful and exceedingly arrogant New-energy electric vehicle master is to be used at present.
The anode material for lithium-ion batteries of current commodity mainly has cobalt acid lithium, LiMn2O4, LiFePO4 and nickel cobalt mangaic acid
Lithium.Wherein cobalt acid lithium is of high cost, and there are security risks during overcharge；Layered lithium manganate structural stability is poor, spinel-type manganese
Sour lithium specific capacity is low, and high temperature lower structure stability has much room for improvement.LiFePO4 poor processability, tap density is low, energy density
It is low.Compared with above-mentioned material, nickel-cobalt lithium manganate material have it is at low cost, high-temperature behavior is good, energy density is high and processing performance is excellent
The advantages that good, nickle cobalt lithium manganate comprehensive performance are higher than above-mentioned positive electrode.But the high rate capability of nickle cobalt lithium manganate and Xun Huan are steady
It is qualitative rate is accounted for compared with high market cobalt acid lithium it is poor.It is to improve its electrification that cobalt nickel lithium manganate ternary material, which is surface modified,
Learn a kind of effective approach of performance.Application No. 201410250912.4 uses carbon-coating nickel cobalt manganic acid lithium, after cladding
Improve the high rate performance and cyclical stability of positive electrode.Application No. 201310312317.4 is using fluorapatite to nickel cobalt
LiMn2O4 is coated, and the cyclical stability of material is improved.
The modification nickel-cobalt lithium manganate material that development cost is low, easily promotes, with improve the cyclical stability of nickle cobalt lithium manganate and
High rate performance is significant in electrochemical field.
The content of the invention
It is an object of the invention to provide a kind of lithium manganese phosphates to coat nickel-cobalt lithium manganate cathode material and preparation method thereof, with
Improve the cyclical stability and high rate performance of nickle cobalt lithium manganate.Another object of the present invention is to provide lithium manganese phosphate cladding nickel cobalt
Application of the manganate cathode material for lithium in lithium rechargeable battery.Lithium manganese phosphate cladding nickle cobalt lithium manganate anode prepared by the present invention
Material has many advantages, such as that cyclical stability and high rate performance are excellent, preparation method is inexpensive, is easy to industrialized production.
The technical scheme is that：
A kind of lithium manganese phosphate coats nickel-cobalt lithium manganate cathode material, including nickle cobalt lithium manganate and is coated on the nickel cobalt mangaic acid
The lithium manganese phosphate on lithium surface, the chemical formula of the nickle cobalt lithium manganate is LiNixCoyMnzO2, wherein x+y+z=1,0.25≤x≤
0.6,0.1≤y≤0.4,0.2≤z≤0.5.
Preferably, the mass fraction of the lithium manganese phosphate is 0.5%-1.5%.Lithium manganese phosphate poorly conductive, cladding
Amount can excessively cause nickel-cobalt lithium manganate material electric conductivity sharp-decay, the very few uniform bag that can not realize lithium manganese phosphate of covering amount
It covers, it is impossible to effectively prevent corrosion of the hydrofluoric acid to surface of active material in electrolyte, and then nickel-cobalt lithium manganate material is caused to follow
Ring stability is decayed.In the range and avoid the attenuation of materials conductive performance that from can effectively preventing nickel-cobalt lithium manganate material simultaneously
Stable circulation performance decays.
Preferably, the lithium manganese phosphate is amorphous state.The porous state of amorphous state is conducive to carry out reversible electricity
Chemical reaction.
Application of the lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material in lithium ion battery is prepared.
The preparation method of the lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, concretely comprises the following steps：
1）It is 1.1-1.5 that immunomodulator compounds, Li source compound, manganese source compound, P source compound, which will be complexed, according to molar ratio:
1.05:1:1, preparation solution soluble in water, and be 3.7-4.2 with adjusting pH value successively；
2）By a certain amount of solid powder nickle cobalt lithium manganate LiNixCoyMnzO2It is added to step 1）In solution obtained,
Solid content is 25%-30% in order to control；
3）By step 2）Obtained solution stirs evaporation solution to sticky at 80-90 DEG C, and it is small to be stored at room temperature ageing 2-4
When, by product be placed in 90 DEG C of baking ovens dry 3-6 it is small when；Sample comminution crosses 400 mesh screens；
4）By step 3）Obtained solid powder is put into tube furnace and is heated up with 1-5 DEG C/min heating rates, is warming up to 350-
Under 550 DEG C of air atmospheres, when roasting 3- 4 is small, room temperature is naturally cooling to, the nickle cobalt lithium manganate anode of lithium manganese phosphate cladding is made
Material.
Preferably, step 2）In, the mass fraction control of lithium manganese phosphate is 0.5%-1.5%.
Preferably, the complexing immunomodulator compounds are at least one of citric acid, ascorbic acid, tartaric acid.Complexing agent exists
It generates and chemical reaction rate is controlled in the reaction process of lithium manganese phosphate, and then promote to realize the uniform cladding to nickle cobalt lithium manganate,
The modified effect of the present invention has been significantly greatly increased in the use of complexing agent.And citric acid, ascorbic acid, tartaric acid is as complexing agent, into
This low and chemical reaction rate control to generating lithium manganese phosphate is just right.
Preferably, the Li source compound is at least one of lithium hydroxide, lithium acetate, lithium nitrate；It is described
Manganese source compound is at least one of manganese acetate, manganese citrate；Phosphorus source compound is ammonium dihydrogen phosphate, phosphoric acid hydrogen two
At least one of ammonium, phosphoric acid.
LiMnPO4As its stable structure of transition metal phosphate lithium salts, cheap environmental protection has higher voltage（4.1V),
It can promote the conduction of nickle cobalt lithium manganate surface lithium ion as covering material, be conducive to improve high rate performance.LiMnPO4In
PO4 3-The dissolving of electrode material in the electrolytic solution can effectively be inhibited, prevent corruption of the hydrofluoric acid in electrolyte to surface of active material
Erosion improves security performance and cyclical stability.Therefore, nickle cobalt lithium manganate is coated using lithium manganese phosphate, nickle cobalt lithium manganate can be improved
Cyclical stability and high rate performance.And this method is easily operated, it is easy to spread.
Beneficial effects of the present invention are：
The surface coated lithium manganese phosphate of nickel-cobalt lithium manganate cathode material prepared by the present invention is amorphous state, to the electricity of material
Chemical property is favourable, while lithium manganese phosphate can prevent corrosion of the hydrofluoric acid to nickle cobalt lithium manganate surface in electrolyte, significantly carry
The cyclical stability of high nickle cobalt lithium manganate, especially high voltage（4.4V）Lower cyclical stability；
Lithium manganese phosphate has higher voltage as positive electrode in itself（4.1V）, nickle cobalt lithium manganate material can be promoted after cladding
Expect surface lithium ion conduction, improve its high rate performance.
The present invention has actual application prospect in power battery and high-energy density type field of batteries.Present invention improves nickel
The cyclical stability and high rate performance of cobalt manganic acid lithium, preparation process is simple, and time-consuming short, and low energy consumption, of low cost, environment friend
It is good, it is easy to industrialized production.
Description of the drawings
It in order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
To obtain other attached drawings according to these attached drawings.
Fig. 1 coats the scanning electron microscope (SEM) photograph of nickel-cobalt lithium manganate material, enlargement ratio for the lithium manganese phosphate prepared by the present invention
2000 times.
Fig. 2 coats the scanning electron microscope (SEM) photograph of nickel-cobalt lithium manganate material, enlargement ratio for the lithium manganese phosphate prepared by the present invention
5000 times.
Fig. 3 is the X-ray diffraction spectrogram before and after lithium manganese phosphate cladding nickle cobalt lithium manganate prepared by the present invention；
Fig. 4 is that lithium manganese phosphate cladding nickle cobalt lithium manganate prepared by the present invention is front and rear under 1C multiplying powers, the electric discharge of 3.0V-4.4V
Specific capacity stable circulation performance figure.
Fig. 5 is that lithium manganese phosphate cladding nickle cobalt lithium manganate prepared by the present invention is front and rear under 0.2C-8C multiplying powers, 3.0V-4.3V
Discharge-rate performance map.
Specific embodiment
Embodiment 1
By 0.1844 g C6H8O7·H2O、0.0351 g LiOH·H2O、0.1955 g Mn(CH3COO)2·4H2O and
0.0917 g NH4H2PO4(complexing agent：Li:Mn:P=1.1:1.05:1:1) it is dissolved in successively in 60ml deionized waters, use is dense
It is 4.2 that nitric acid or concentrated ammonia liquor, which adjust pH value of solution, by 25g LiNi0.5Mn0.3Co0.2O2Powder infusion is in above-mentioned solution, phosphoric acid
The mass fraction control of manganese lithium is 0.5%；Solution magnetic agitation at 90 DEG C evaporates solution to sticky, and it is small to be stored at room temperature ageing 2
When, be subsequently placed in 90 DEG C of baking ovens dry 3 it is small when, crushed 400 mesh screens；The 450 DEG C of roastings 4 in air atmosphere of gained sample
Hour, the nickel-cobalt lithium manganate cathode material that lithium manganese phosphate coats finally is made in cooled to room temperature.
Embodiment 2：
By 0.7538 g C6H8O7·H2O、0.2563 g Li(CH3COO)2·2H2O、0.5864 g Mn(CH3COO)2·
4H2O and 0.3160 g (NH4)2HPO4(complexing agent：Li:Mn:P=1.5:1.05:1:1) 60ml deionized waters are dissolved in successively
In, concentrated nitric acid or concentrated ammonia liquor is used to adjust pH value of solution as 3.7, by 25g LiNi0.5Mn0.3Co0.2O2Powder infusion is in above-mentioned molten
In liquid, the mass fraction control of lithium manganese phosphate is 1.5%；Solution magnetic agitation at 90 DEG C evaporates solution to sticky, and room temperature is quiet
Put ageing 2 it is small when, be subsequently placed in 90 DEG C of baking ovens dry 6 it is small when, crushed 400 mesh screens；Gained sample is in air atmosphere
When 550 DEG C of roastings 4 are small, the nickel-cobalt lithium manganate cathode material that lithium manganese phosphate coats finally is made in cooled to room temperature.
Embodiment 3：
By 0.4355g C6H8O7·H2O、0.0703gLiOH·H2O、0.3910gMn(CH3COO)2·4H2O and 0.1834g
NH4H2PO4(complexing agent：Li:Mn:P=1.3:1.05:1:1) it is dissolved in successively in 75ml deionized waters, using concentrated nitric acid or dense
It is 4.2 that ammonium hydroxide, which adjusts pH value of solution, by 25g LiNi0.5Mn0.3Co0.2O2Powder infusion is in above-mentioned solution, the quality of lithium manganese phosphate
Fractional domination is 1.0%；Solution magnetic agitation at 85 DEG C evaporates solution to sticky, be stored at room temperature ageing 4 it is small when, then put
When drying 6 is small in 90 DEG C of baking ovens, 400 mesh screens are crushed；Gained sample is natural when 450 DEG C of roastings 4 are small in air atmosphere
It is cooled to room temperature, the nickel-cobalt lithium manganate cathode material of lithium manganese phosphate cladding is finally made.
Embodiment 4：
By 0.1844g C6H8O7·H2O、0.0351gLiOH·H2O、0.1955gMn(CH3COO)2·4H2O and 0.0917g
NH4H2PO4(complexing agent：Li:Mn:P=1.1:1.05:1:1) it is dissolved in successively in 75ml deionized waters, using concentrated nitric acid or dense
It is 4.0 that ammonium hydroxide, which adjusts pH value of solution, by 25g LiNi0.3Mn0.4Co0.3O2Powder infusion is in above-mentioned solution, the quality of lithium manganese phosphate
Fractional domination is 0.5wt%；Solution magnetic agitation at 85 DEG C evaporates solution to sticky, be stored at room temperature ageing 4 it is small when, then
Be placed in 90 DEG C of baking ovens dry 6 it is small when, crushed 400 mesh screens；Gained sample in air atmosphere 350 DEG C roasting 4 it is small when, from
It is so cooled to room temperature, the nickel-cobalt lithium manganate cathode material of lithium manganese phosphate cladding is finally made.
As shown in Figure 1, the scanning electron microscope (SEM) photograph of the lithium manganese phosphate cladding nickel-cobalt lithium manganate material prepared by the embodiment of the present invention 1
Piece, 2000 times of enlargement ratio.
As shown in Fig. 2, the scanning electron microscope (SEM) photograph of the lithium manganese phosphate cladding nickel-cobalt lithium manganate material prepared by the embodiment of the present invention 1
Piece, 5000 times of enlargement ratio, nickel cobalt manganese lithium surface can substantially observe the lithium manganese phosphate of amorphous state.
As shown in figure 3, the X-ray diffraction of the lithium manganese phosphate cladding nickel-cobalt lithium manganate material prepared by the embodiment of the present invention 1
Spectrogram shows that lithium manganese phosphate is amorphous state.
As shown in figure 4, the lithium manganese phosphate cladding LiNi prepared by embodiment 10.5Mn0.3Co0.2O2As positive electrode, lithium
For negative material, button cell is assembled, cycle charge discharge coats manganese phosphate after 100 weeks under voltage window 3.0-4.4 V, 1C multiplying powers
Material capacity conservation rate after lithium is increased to 92.6% by 80.1%, high voltage（4.4V）Lower cycle performance is obviously improved.
As shown in figure 5, the lithium manganese phosphate cladding LiNi prepared by embodiment 10.5Mn0.3Co0.2O2As positive electrode, lithium
For negative material, button cell is assembled, under voltage window 3.0-4.4 V, big multiplying power（5C, 8C）Discharge performance is obviously improved.
Claims (4)
1. a kind of lithium manganese phosphate coats nickel-cobalt lithium manganate cathode material, including nickle cobalt lithium manganate and the nickle cobalt lithium manganate is coated on
The lithium manganese phosphate of the amorphous state on surface, the chemical formula of the nickle cobalt lithium manganate is LiNixCoyMnzO2, wherein x+y+z=1,
0.25≤x≤0.6,0.1≤y≤0.4,0.2≤z≤0.5；The mass fraction of the lithium manganese phosphate is 0.5%-1.5%；
The preparation method of the lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material, concretely comprises the following steps：
1）It is 1.1-1.5 that immunomodulator compounds, Li source compound, manganese source compound, P source compound, which will be complexed, according to molar ratio:
1.05:1:1, preparation solution soluble in water, and be 3.7-4.2 with adjusting pH value successively；
2）By a certain amount of solid powder nickle cobalt lithium manganate LiNixCoyMnzO2It is added to step 1）In solution obtained, admittedly contain
Amount control is 25%-30%；
3）By step 2）Obtained solution stirs evaporation solution to sticky at 80-90 DEG C, be stored at room temperature ageing 2-4 it is small when, will
Product be placed in 90 DEG C of baking ovens dry 3-6 it is small when；Sample comminution crosses 400 mesh screens；
4）By step 3）Obtained solid powder is put into tube furnace and is heated up with 1-5 DEG C/min heating rates, is warming up to 350-550
Under DEG C air atmosphere, when roasting 3- 4 is small, room temperature is naturally cooling to, the nickle cobalt lithium manganate anode material of lithium manganese phosphate cladding is made
Material.
2. lithium manganese phosphate as described in claim 1 coats nickel-cobalt lithium manganate cathode material, it is characterised in that：The complexing agent chemical combination
Object is at least one of citric acid, ascorbic acid, tartaric acid.
3. the preparation method of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material as claimed in claim 1 or 2, it is characterised in that：
The Li source compound is at least one of lithium hydroxide, lithium acetate, lithium nitrate；The manganese source compound is manganese acetate, lemon
At least one of lemon acid manganese；Phosphorus source compound is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, phosphoric acid.
4. a kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material answering in lithium ion battery is prepared described in claim 1
With.
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| CN201510365733.XA CN105161705B (en) | 2015-06-29 | 2015-06-29 | A kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material and preparation method thereof |
| PCT/CN2016/084413 WO2017000741A1 (en) | 2015-06-29 | 2016-06-01 | Lithium manganese phosphate-coated lithium nickel cobalt manganese oxide cathode material and preparation method thereof |
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| CN201510365733.XA CN105161705B (en) | 2015-06-29 | 2015-06-29 | A kind of lithium manganese phosphate cladding nickel-cobalt lithium manganate cathode material and preparation method thereof |
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| CN105552360B (en) * | 2016-03-03 | 2018-05-15 | 四川浩普瑞新能源材料股份有限公司 | A kind of nickel-cobalt lithium manganate cathode material of modification and preparation method thereof |
| CN106058221B (en) * | 2016-08-12 | 2019-03-29 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of the compound manganese salt cladding lithium-rich manganese-based anode material of phosphate radical polyanion |
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