CN109037654A - Nickel manganese anode material for lithium-ion batteries and preparation method thereof - Google Patents
Nickel manganese anode material for lithium-ion batteries and preparation method thereof Download PDFInfo
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- CN109037654A CN109037654A CN201810935387.8A CN201810935387A CN109037654A CN 109037654 A CN109037654 A CN 109037654A CN 201810935387 A CN201810935387 A CN 201810935387A CN 109037654 A CN109037654 A CN 109037654A
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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
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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
- 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
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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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- 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
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Abstract
The present invention provides a kind of nickel manganese anode material for lithium-ion batteries and preparation method thereof, and the preparation method comprises the following steps: (1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then heating reaction, it is cooling, and obtain mixed liquor；(2) divalent nickel source, bivalent manganese source and citric acid are added in mixed liquor in step (1), reaction is heated under lasting mixing condition and adds Li source compound after cooling and is mixed, then calcined；Wherein, the molar ratio of divalent nickel source, bivalent manganese source and Li source compound is 0.65-0.75:0.25-0.35:1.The charge-discharge performance and recycling performance for the nickel manganese anode material for lithium-ion batteries that the present invention obtains largely are promoted, compared with existing nickel manganese anode material for lithium-ion batteries, the density of nickel manganese anode material for lithium-ion batteries is smaller, and has preferable charge-discharge performance.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries, and in particular, to a kind of nickel manganese anode material for lithium-ion batteries and
Preparation method.
Background technique
It is with the continuous progress of science and technology and continuous improvement of people's living standards, also higher and higher for the demand of the energy,
And lithium ion battery is as a kind of energy storage device with excellent service performance, in portable device, computer and telecommunications
Communication aspects have a wide range of applications.And conventional lithium ion battery is after a number of uses, capacitance has apparent reduction,
Cause its charge-discharge performance that there can be apparent decline.And the positive plate of lithium ion electronics can then largely effect on its charge-discharge performance
Deng.
Therefore it provides a kind of can make lithium ion battery still have good charge-discharge performance after using repeatedly and follow
Ring service performance, and then the anode material for lithium-ion batteries and preparation method thereof prolonged its service life is urgent need to resolve of the present invention
The problem of.
Summary of the invention
It is an object of the invention to overcome the lithium ion battery advised in the prior art after a number of uses, capacitance is had
It is apparent to reduce, cause its charge-discharge performance that there can be apparent decline, so that providing a kind of can make lithium ion battery make
With still there is good charge-discharge performance after repeatedly and performance, and then the nickel manganese lithium ion prolonged its service life is recycled
Cell positive material and preparation method thereof.
To achieve the goals above, the present invention provides a kind of preparation method of nickel manganese anode material for lithium-ion batteries, institutes
State preparation method the following steps are included:
(1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then heating reaction, it is cooling, obtain mixed liquor；
(2) divalent nickel source, bivalent manganese source and citric acid are added in mixed liquor in step (1), adds under lasting mixing condition
Thermal response adds Li source compound and is mixed, then calcined after cooling；
Wherein, the molar ratio of divalent nickel source, bivalent manganese source and Li source compound is 0.65-0.75:0.25-0.35:1.
The present invention also provides a kind of nickel manganese lithium ion cell positive materials being prepared according to previously described preparation method
Material.
Through the above technical solutions, the charge-discharge performance and circulation of the nickel manganese anode material for lithium-ion batteries that the present invention obtains
Service performance is largely promoted, and compared with existing nickel manganese anode material for lithium-ion batteries, nickel manganese lithium ion battery is just
The density of pole material is smaller, and has preferable charge-discharge performance and performance is recycled.Inventor's supposition, divalent nickel source, two
Mixed liquor in valence manganese source and citric acid and step (1) heats together, nickel ion, manganese ion coordination can be sequestered in alpha-cyclodextrin
Surface, add lithium ion, then mix, calcine, the alpha-cyclodextrin at chelating center can be removed, improve the ratio of positive electrode
Surface area and permeability, to largely improve the charge-discharge performance of positive electrode and performance is recycled.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation method of nickel manganese anode material for lithium-ion batteries, the preparation method includes following
Cetyl trimethylammonium bromide and alpha-cyclodextrin: (1) being dispersed in water by step, then heating reaction, cooling, must mix
Liquid；(2) divalent nickel source, bivalent manganese source and citric acid are added in mixed liquor in step (1), is heated under lasting mixing condition
Reaction adds Li source compound and is mixed, then calcined after cooling；Wherein, divalent nickel source, bivalent manganese source and lithium
The molar ratio of source compound is 0.65-0.75:0.25-0.35:1.
Through the above technical solutions, the charge-discharge performance and circulation of the nickel manganese anode material for lithium-ion batteries that the present invention obtains
Service performance is largely promoted, and compared with existing nickel manganese anode material for lithium-ion batteries, nickel manganese lithium ion battery is just
The density of pole material is smaller, and has preferable charge-discharge performance and performance is recycled.Inventor's supposition, divalent nickel source, two
Mixed liquor in valence manganese source and citric acid and step (1) heats together, nickel ion, manganese ion coordination can be sequestered in alpha-cyclodextrin
Surface, add lithium ion, then mix, calcine, the alpha-cyclodextrin at chelating center can be removed, improve the ratio of positive electrode
Surface area and permeability, to largely improve the charge-discharge performance of positive electrode and performance is recycled.
In order to obtain with preferable charge-discharge performance and be recycled performance cell positive material, the present invention more
In preferred embodiment, in step (1), relative to the water of 20mL, the dosage of cetyl trimethylammonium bromide is 0.04-
0.08g, the dosage of alpha-cyclodextrin are 1.5-2.5g.In this way, inventor speculates, the surface coordination chelating nickel of alpha-cyclodextrin can be improved
Ion, manganese ion ability, to achieve the object of the present invention.
It for the reaction condition in step (1), can be adjusted in a wider range, there is preferable charge and discharge in order to obtain
Electrical property and the cell positive material that performance is recycled, it is preferable that the reaction condition in step (1) includes: that temperature is 120-
150℃。
It for the reaction condition in step (1), can be adjusted in a wider range, there is preferable charge and discharge in order to obtain
Electrical property and the cell positive material that performance is recycled, it is preferable that reaction time 8-9h.
Wherein, for the dosage of divalent nickel source, bivalent manganese source and Li source compound and citric acid, can in a wider range into
Row adjustment, as long as the molar ratio for meeting divalent nickel source, bivalent manganese source and Li source compound is 0.65-0.75:0.25-0.35:
1, the present invention can be achieved.In the more preferred embodiment of one kind of the invention, have better charge and discharge electrical in order to obtain
The cell positive material of performance can and be recycled, it is preferred that relative to the alpha-cyclodextrin of 2g, the dosage of divalent nickel source is
0.8-1.2mol, the dosage of citric acid are 0.08-0.1mol.
The present invention can be realized according to preparation method above, still, in a kind of more preferred embodiment of the invention
In, in order to obtain with better charge-discharge performance and the cell positive material that performance is recycled, it is preferred that in step (2)
It further include that water is added in the mixed system in step (2) so that divalent nickel source, bivalent manganese source and citric acid before heating reaction
The step of dissolution, wherein after dissolution, the concentration of bivalent nickel ion is 0.03-0.06mol/L in aqueous solution.
And for the heating condition in step (2), it can be adjusted in a wider range.Of the invention a kind of more preferred
Embodiment in, in order to obtain with better charge-discharge performance and be recycled performance cell positive material, step (2)
It is 80-95 DEG C that the condition of middle heating reaction, which includes: temperature,.
And for the heating condition in step (2), it can be adjusted in a wider range.Of the invention a kind of more preferred
Embodiment in, in order to obtain with better charge-discharge performance and be recycled performance cell positive material, step (2)
It is middle heating reaction condition include: the time be 3-8h.
For the condition of calcining, can be adjusted in a wider range.In a kind of more preferred embodiment of the invention
In, in order to obtain with better charge-discharge performance and the cell positive material that performance is recycled, calcination condition includes: temperature
It is 300-600 DEG C.
For the condition of calcining, can be adjusted in a wider range.In a kind of more preferred embodiment of the invention
In, in order to obtain with better charge-discharge performance and the cell positive material that performance is recycled, calcination condition includes: the time
For 1-4h.
For bivalent manganese source, those skilled in the art can be adjusted in a wider range, as long as the bivalent manganese source can
It is soluble in water.In a preferred embodiment of the invention, there is better charge-discharge performance in order to obtain and follow
The cell positive material of ring service performance, bivalent manganese source are manganese chloride and/or manganese nitrate.
For divalent nickel source, those skilled in the art can be adjusted in a wider range, as long as the divalent nickel source can
It is soluble in water.In a preferred embodiment of the invention, there is better charge-discharge performance in order to obtain and follow
The cell positive material of ring service performance, divalent nickel source are nickel nitrate and/or nickel chloride.
For Li source compound, those skilled in the art can be adjusted in a wider range, as long as the Li source compound
It can be soluble in water.In a preferred embodiment of the invention, there is better charge-discharge performance in order to obtain
With the cell positive material that performance is recycled, Li source compound is one of lithium acetate, lithium nitrate and lithium chloride or a variety of.
Wherein, temperature cooling in step (1), can be adjusted in a wider range, as long as temperature is lower than in step (2)
Heating temperature.
And for the cooling temperature in step (2), it can adjust, in embodiment later, be cooled in a wider range
Room temperature (25 DEG C).
In the above-mentioned technical solutions, for the selection of water, deionized water, distilled water, distilled water, ultrapure water etc. be can choose
Deng, can be achieved the present invention, details are not described herein.
And the selection for reaction vessel or heating equipment etc., as long as can be realized the above-mentioned technical conditions of the present invention,
The present invention can be achieved, the present invention is not required, and details are not described herein.
The present invention also provides a kind of nickel manganese lithium ion cell positive materials being prepared according to previously described preparation method
Material.
Through the above technical solutions, the charge-discharge performance and circulation of the nickel manganese anode material for lithium-ion batteries that the present invention obtains
Service performance is largely promoted, and compared with existing nickel manganese anode material for lithium-ion batteries, nickel manganese lithium ion battery is just
The density of pole material is smaller, and has preferable charge-discharge performance and performance is recycled.Inventor's supposition, divalent nickel source, two
Mixed liquor in valence manganese source and citric acid and step (1) heats together, nickel ion, manganese ion coordination can be sequestered in alpha-cyclodextrin
Surface, add lithium ion, then mix, calcine, the alpha-cyclodextrin at chelating center can be removed, improve the ratio of positive electrode
Surface area and permeability, to largely improve the charge-discharge performance of positive electrode and performance is recycled.
The present invention will be described in detail by way of examples below.
Embodiment 1
The preparation method of nickel manganese anode material for lithium-ion batteries, the preparation method comprises the following steps:
(1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then react 9h in 120 DEG C of heating, it is cooling,
Obtain mixed liquor；Wherein, relative to the water of 20mL, the dosage of cetyl trimethylammonium bromide is 0.04g, the dosage of alpha-cyclodextrin
For 1.5g；
(2) nickel nitrate, manganese nitrate and citric acid are added in mixed liquor in step (1), water is added to adjust ion concentration, aqueous solution
The concentration of middle bivalent nickel ion is 0.03mol/L；Wherein, relative to the alpha-cyclodextrin of 2g, the dosage of nickel nitrate is 0.8mol,
The dosage of citric acid is 0.08mol；
8h is reacted after cooling in 80 DEG C of heating under lasting mixing condition to add lithium nitrate and mixed, then in 300 DEG C
Calcine 4h；And the molar ratio of nickel nitrate, manganese nitrate and lithium nitrate is 0.65:0.35:1.
Embodiment 2
The preparation method of nickel manganese anode material for lithium-ion batteries, the preparation method comprises the following steps:
(1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then react 8h in 150 DEG C of heating, it is cooling,
Obtain mixed liquor；Wherein, relative to the water of 20mL, the dosage of cetyl trimethylammonium bromide is 0.08g, the dosage of alpha-cyclodextrin
For 2.5g；
(2) nickel nitrate, manganese nitrate and citric acid are added in mixed liquor in step (1), water is added to adjust ion concentration, aqueous solution
The concentration of middle bivalent nickel ion is 0.06mol/L；Wherein, relative to the alpha-cyclodextrin of 2g, the dosage of nickel nitrate is 1.2mol,
The dosage of citric acid is 0.1mol；
3h is reacted after cooling in 95 DEG C of heating under lasting mixing condition to add lithium nitrate and mixed, then in 600 DEG C
Calcine 1h；And the molar ratio of nickel nitrate, manganese nitrate and lithium nitrate is 0.75:0.25:1.
Embodiment 3
The preparation method of nickel manganese anode material for lithium-ion batteries, the preparation method comprises the following steps:
(1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then react 8.5h in 130 DEG C of heating, it is cold
But, mixed liquor is obtained；Wherein, relative to the water of 20mL, the dosage of cetyl trimethylammonium bromide is 0.06g, alpha-cyclodextrin
Dosage is 2g；
(2) nickel nitrate, manganese nitrate and citric acid are added in mixed liquor in step (1), water is added to adjust ion concentration, aqueous solution
The concentration of middle bivalent nickel ion is 0.045mol/L；Wherein, relative to the alpha-cyclodextrin of 2g, the dosage of nickel nitrate is 1mol, lemon
The dosage of lemon acid is 0.1mol；
5.5h is reacted after cooling in 88 DEG C of heating under lasting mixing condition to add lithium nitrate and mixed, then in 450
DEG C calcining 2.5h；And the molar ratio of nickel nitrate, manganese nitrate and lithium nitrate is 0.7:0.3:1.
Comparative example 1
Nickel nitrate, manganese nitrate and citric acid is soluble in water, and the concentration of bivalent nickel ion is 0.045mol/L in aqueous solution；And nitre
Sour nickel, manganese nitrate, lithium nitrate molar ratio be 0.7:0.3:1；Relative to the nickel nitrate of 1mol, the dosage of citric acid is
0.1mol；
5.5h is reacted after cooling in 88 DEG C of heating under lasting mixing condition to add lithium nitrate and mixed, then in 450
DEG C calcining 2.5h.
Test case
By anode material for lithium-ion batteries, electrically conductive graphite and Kynoar obtained in embodiment 1-3 and comparative example 1 according to 7:
Ball milling after the weight ratio mixing of 1:1, is made spheroidal graphite slurry；By cut-parts after spheroidal graphite slurry compression molding, based lithium-ion battery positive plate is made,
Again using the LIPF6 of 1mol/L as electrolyte, microporous polypropylene membrane (Celgard2400) is diaphragm, and metal lithium sheet is reference electrode,
CR2032 type button cell is made in material in the glove box full of hydrogen.Under the conditions of 25 DEG C, Wuhan Lan electricity company is utilized
Land-CT2001A battery test system button type battery carry out constant current charge-discharge test, test voltage range be 2.5V ~
4.6V.Its discharge capacity under the conditions of 0.5C is detected, after being then recycled 100 times, detects its discharge capacity, obtained knot
Fruit is as shown in table 1.
Table 1
| Number | Discharge capacity (mAh/g) | Discharge capacity (mAh/g) after 100 times |
| Embodiment 1 | 369 | 361 |
| Embodiment 2 | 376 | 368 |
| Embodiment 3 | 372 | 365 |
| Comparative example 1 | 282 | 225 |
The preferred embodiment of the present invention has been described above in detail, still, the tool during present invention is not limited to the embodiments described above
Body details within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, these letters
Monotropic type all belongs to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (8)
1. a kind of preparation method of nickel manganese anode material for lithium-ion batteries, which is characterized in that the preparation method includes following step
It is rapid:
(1) cetyl trimethylammonium bromide and alpha-cyclodextrin are dispersed in water, then heating reaction, it is cooling, obtain mixed liquor；
(2) divalent nickel source, bivalent manganese source and citric acid are added in mixed liquor in step (1), adds under lasting mixing condition
Thermal response adds Li source compound and is mixed, then calcined after cooling；
Wherein, the molar ratio of divalent nickel source, bivalent manganese source and Li source compound is 0.65-0.75:0.25-0.35:1.
2. preparation method according to claim 1, in which:
In step (1), relative to the water of 20mL, the dosage of cetyl trimethylammonium bromide is 0.04-0.08g, α-ring paste
The dosage of essence is 1.5-2.5g；
Reaction condition in step (1) includes: that temperature is 120-150 DEG C；And/or reaction time 8-9h.
3. preparation method according to claim 2, wherein relative to the alpha-cyclodextrin of 2g, the dosage of divalent nickel source is
0.8-1.2mol, the dosage of citric acid are 0.08-0.1mol.
4. preparation method according to claim 3, wherein further include in step (2) in step (2) before heating reaction
In mixed system in water is added so that the step of divalent nickel source, bivalent manganese source and lemon acid dissolution, wherein it is water-soluble after dissolution
The concentration of bivalent nickel ion is 0.03-0.06mol/L in liquid.
5. the preparation method according to claim 4, wherein it is 80- that the condition of heating reaction, which includes: temperature, in step (2)
95℃；And/or time 3-8h.
6. preparation method according to claim 1, wherein calcination condition includes: that temperature is 300-600 DEG C；And/or when
Between be 1-4h.
7. preparation method according to claim 1-6, wherein bivalent manganese source is manganese chloride and/or manganese nitrate；
And/or divalent nickel source is nickel nitrate and/or nickel chloride.
8. preparation method according to claim 1-6, wherein Li source compound is lithium acetate, lithium nitrate and chlorine
Change one of lithium or a variety of.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113845152A (en) * | 2021-08-30 | 2021-12-28 | 蜂巢能源科技有限公司 | Lithium nickel manganese oxide positive electrode material, preparation method thereof and lithium ion battery |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113845152A (en) * | 2021-08-30 | 2021-12-28 | 蜂巢能源科技有限公司 | Lithium nickel manganese oxide positive electrode material, preparation method thereof and lithium ion battery |
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Application publication date: 20181218 |