CN104241636A - Lithium ion battery manganese anode material with surface wrapped with LiAlO2 and preparation method thereof - Google Patents
Lithium ion battery manganese anode material with surface wrapped with LiAlO2 and preparation method thereof Download PDFInfo
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- CN104241636A CN104241636A CN201410558123.7A CN201410558123A CN104241636A CN 104241636 A CN104241636 A CN 104241636A CN 201410558123 A CN201410558123 A CN 201410558123A CN 104241636 A CN104241636 A CN 104241636A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a lithium ion battery manganese anode material with the surface wrapped with LiAlO2 and a preparation method of the lithium ion battery manganese anode material. The method comprises the following steps: 1, dissolving metallic nitrate to ethanol or the mixed solution of ethanol and water; 2, adding the anode material to the solution obtained in step 1, and agitating for 0.1 to 0.5 hours; 3, adjusting the pH of the solution to be 4 to 10 through ammonia solution, agitating for 3 to 5 hours, drying under a low temperature of 80 DEG C, or filtering and then drying under the temperature of 80 DEG C to obtain the material wrapped with a lithium-aluminum precursor; 4, thermally processing the material wrapped with the lithium-aluminum precursor under the temperature of 400 to 700 DEG C to obtain an anode material sample with surface wrapped with the LiAlO2. According to the surface wrapping preparation method of the lithium ion battery manganese anode material, the method is simple, the ethanol solution is used as a solvent for delaying the corrosion of acid to the manganese material, and meanwhile, the anode material is uniformly wrapped; the industrial production is easily carried out; the modified anode material can be greatly improved.
Description
Technical field
The invention belongs to field of lithium ion battery anode, relate to a kind of Surface coating LiAlO
2lithium ion battery manganese system positive electrode and preparation method thereof.
Technical background
Based on the lithium ion battery of " rocking chair " principle because of advantages such as its energy density is high, operating voltage is high, security performance is good, the storage time is long, operating temperature range is wide, environmental friendliness, be not only the main powering device of current portable type electronic product, also be used widely in fields such as power industry, space flight and aviation and weaponrys, become most important secondary chemical sources of electric energy.In current business-like anode material for lithium-ion batteries system, cobalt acid lithium is expensive and there is the significant problem such as resource and fail safe; LiFePO4 volume energy density is lower and consistency is poor; And a series of manganese cathode material is as LiMn2O4, nickel-cobalt-manganese ternary material, lithium-rich manganese base material etc., because its resources reserve is enriched, the advantage that fail safe is good and energy density is higher, has become the important directions that positive electrode further develops now.But the shortcoming of manganese-based anode material be its high-temperature behavior and cycle performance poor, thus limit the application of material.Correlative study shows, carries out to Mn-based material the cyclical stability that modification can significantly improve battery, thus expands the application of material, realizes the scale application of material.
For LiMn2O4, the main cause affecting its cycle performance has: Jahn-Teller effect during (1) deep discharge; (2) in cyclic process, the dissolving of divalence Mn ion causes the loss of active material, and easily in Carbon anode deposition, damages its structure; (3) during charging, the strong oxidizing property of tetravalent manganese ion causes electrolyte decomposition.For lithium-rich manganese base material, the main cause affecting its chemical property has: (1) high-tension activation causes initial coulomb efficiency lower; (2) undergo phase transition in cyclic process, structural stability is poor; (3) react serious with electrolyte under high voltages.At present, the method improving manganese-based anode material mainly comprises: (1), at the oxide coated passivation layer of material surface, reduces the direct contact between electrolyte and material, reduces the generation of side reaction; (2) doping vario-property process is carried out to material, improve the stability of material self frame structure; (3) high-voltage electrolyte adding additive is used.Wherein, carrying out Surface coating process to material is a kind of easy and effective method of modifying.
At present, the report about anode material for lithium-ion batteries coating modification method is a lot, and in all kinds of Surface coating material, the most commonly metal oxide is coated, especially Al
2o
3coated.This is due to Al
2o
3can react with HF, remove the acidic materials produced in electrolyte, greatly improve capability retention during material circulation.But in the alkaline solution method for coating adopted at present, due to Al (OH)
3settling rate is very fast, is difficult to ensure the uniformity of particle surface precipitation and coated particle is comparatively large, adopts acid coated solution that the stripping of manganese ion then can be caused to cause the decline of chemical property.
Therefore, need to research and develop a kind of good cycle, the preparation method of the manganese cathode material that capability retention is high.
Summary of the invention
The object of this invention is to provide a kind of Surface coating LiAlO
2lithium ion battery manganese system positive electrode and preparation method thereof, lay particular emphasis on the simplicity of method for coating.Because the autoprotolysis constant of ethanol and dielectric constant are all much smaller than water, cause H
+the degree of dissociation in ethanol reduces, thus solution acidity is declined.Therefore, by introducing ethanol as solvent, to slow down coated process middle acid substance to the corrosion of manganese based material, realize forming even coating layer on positive electrode surface, technique is simple, is applicable to suitability for industrialized production simultaneously.
For achieving the above object, the invention provides a kind of Surface coating LiAlO
2the preparation method of lithium ion manganese cathode material, the method comprises:
Step 1, by nitric acid dissolving metal salts in the mixed liquor of ethanol or ethanol and water; Described nitric acid slaine is aluminum nitrate and lithium nitrate;
Step 2, joins step 1 gained solution and stirs, mixing time 0.1-0.5 hour by manganese cathode material;
Step 3, adopts ammonia spirit, regulates the pH value of solution to 4-10, and after mixing time 3-5 hour, 80 DEG C of low temperature dryings or filter rear 80 DEG C of low temperature dryings, obtain the material that lithium aluminium presoma is coated;
Step 4, by material coated for lithium aluminium presoma, heat treatment at 400 DEG C of-700 DEG C of temperature, obtains Surface coating LiAlO
2positive electrode sample;
Wherein, the consumption of described nitric acid slaine is 0.5% ~ 5% of positive electrode quality.
Above-mentioned preparation method, wherein, in step 1, described ethanol and the mixed liquor of water refer to that the volume ratio of ethanol and water is 10:1 ~ 2:1.
Above-mentioned preparation method, wherein, the manganese cathode material described in step 2 is LiNi
xco
ymn
(1-x-y)o
2, Li
1+nni
xco
ymn
(1-x-y-n)o
2or Li
x1mn
2-y1m
y1o
4; Wherein, 0≤x≤1,0≤y≤1,0≤n≤1,0.8≤x1≤1.2,0.001≤y1≤0.3, M is one or more in Mg, Al, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, Zr.
Above-mentioned preparation method, wherein, the ammonia spirit concentration described in step 3 is 1M ~ 10M.
Above-mentioned preparation method, wherein, the stir speed (S.S.) that step 3 uses is 200r/min ~ 900r/min.
Above-mentioned preparation method, wherein, the weight ratio of the lithium aluminium presoma that the surface described in step 3 is coated and positive electrode is 0.5% ~ 8%.
Above-mentioned preparation method, wherein, the Surface coating LiAlO described in step 4
2the covering amount of material be 0.5% ~ 5%.
Present invention also offers a kind of Surface coating LiAlO obtained according to above-mentioned preparation method
2lithium ion battery manganese system positive electrode, the Surface coating of this positive electrode has LiAlO
2.
The Surface coating LiAlO that above-mentioned preparation method obtains
2lithium ion battery manganese system positive electrode, wherein, described Surface coating LiAlO
2the covering amount of material be 0.5% ~ 5%.
The present invention adopts ethanol as solvent by introducing, and to slow down the corrosion of acidic nitric aluminum solutions to LiMn2O4, adopts weak base ammoniacal liquor as precipitation reagent, by the regulation and control of pH value, reduces settling velocity from dynamics Controlling.Finally, be deposited in LiMn2O4 particle surface heterogeneous nucleation and form the coated presoma of uniform aluminium base hydroxide, obtained the modified lithium manganate material of excellent performance by follow-up heat treatment.
Technical scheme of the present invention has the following advantages:
Modification lithium-ion battery anode material after coated, adopts ethanol as solvent, weakens coated process middle acid substance to the corrosion of manganese based material, slow down the stripping of manganese ion, through ammoniacal liquor adjust ph, make coated material at particle surface nonhomogen-ous nucleation.The follow-up evaporation reflux that can pass through reclaims ethanol, and by the survivor ion in heat treatment removing material, make coating layer uniform fold.This method is simple, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 a is the Surface coating LiAlO of ESEM (SEM) figure, Fig. 1 b prepared by the embodiment of the present invention 1 of coated front LiMn2O4
2eSEM (SEM) figure (multiplication factor is 80,000 times) of LiMn2O4.
Fig. 2 is the Surface coating LiAlO prepared by the embodiment of the present invention 2
2eSEM (SEM) figure of LiMn2O4.
Fig. 3 is the embodiment of the present invention 1, the Surface coating LiAlO prepared by 2
2x-ray diffraction (XRD) figure of LiMn2O4.
Fig. 4 is the embodiment of the present invention 1, the Surface coating LiAlO prepared by 2
2the cycle performance curve (1C discharge and recharge, voltage range 3.2-4.35V) of LiMn2O4.
Fig. 5 is the Surface coating LiAlO prepared by the embodiment of the present invention 3
2the high rate performance (voltage range 3.2-4.35V) of LiMn2O4.
Fig. 6 is the Surface coating LiAlO prepared by the embodiment of the present invention 4
2eSEM (SEM) figure (multiplication factor is 80,000 times) of lithium-rich manganese base material.
Fig. 7 is the Surface coating LiAlO prepared by the embodiment of the present invention 4
2the cycle performance curve (0.1C discharge and recharge, voltage range 2.0-4.8V) of lithium-rich manganese base material.
specific implementation method
The present invention is described in detail below in conjunction with drawings and Examples.
Embodiment 1
Step 1, adds the Al (NO of 94.1g in 3.5L ethanol
3)
39H
2the LiNO of O and 17.3g
3, stir and treat that it dissolves; Step 2, by positive electrode LiMn
2o
4join step 1 gained solution to stir, mixing time 0.2 hour; Step 3, adopts 6M ammonia spirit, and regulate the pH value of solution to 5-6, mixing speed is 450r/min, keeps 80 DEG C of low temperature dryings after 3 hours, obtains the positive electrode of coated lithium aluminium presoma; Step 4, by the positive electrode of coated presoma, heat treated 4h at 500 DEG C of temperature, makes hydroxide change oxide into, finally obtains Surface coating LiAlO
2positive electrode sample.
By the LiMn that the present embodiment obtains
2o
4eSEM (SEM) figure of coated front and back as shown in Figure 1 b, contrast coated before ESEM (SEM) figure of LiMn2O4 (a), as can be seen from the figure there is obvious flakey coating layer in modified material surface to Fig. 1.
Embodiment 2
Step 1, adds the Al (NO of 78.4g in 3.5L ethanol
3)
39H
2the LiNO of O and 14.4g
3, stir and treat that it dissolves; Step 2, by positive electrode LiMn
2o
4join step 1 gained solution to stir, mixing time 0.2 hour; Step 3, adopts 10M ammonia spirit, and regulate the pH value of solution to 4-5, mixing speed is 400r/min, keeps 80 DEG C of low temperature dryings after 3 hours, obtains the positive electrode of coated lithium aluminium presoma; Step 4, by the positive electrode of coated presoma, heat treated 4h at 600 DEG C of temperature, makes hydroxide change oxide into, finally obtains Surface coating LiAlO
2positive electrode sample.
By the LiMn that the present embodiment obtains
2o
4as shown in Figure 2, as can be seen from the figure there is obvious class tile coating layer in modified material surface to ESEM (SEM) figure of coated front and back.
By the LiMn that the present embodiment obtains
2o
4as shown in Figure 3, coated front and back material crystalline structure does not change X-ray diffraction (XRD) figure of coated front and back as we can see from the figure.
As shown in Figure 4, in test process, first three circulation adopts the current density of 0.25C to the material circulation performance curve of coated front and back, and following cycle electric current is increased to 1C.Therefrom can find, the coated cycle performance that significantly can improve material.After not coated sample 150 times circulation, capacity reduces to 76 mAh/g, compares, decay 17.4% with 1C capacity first; After sample 300 circulations that flakey is coated, capacity keeps 84.8 mAh/g, decay 11%; After sample 450 circulations that tile is coated, still can keep the capacity of 85mAh/g, decay 6.5%.
Embodiment 3
Step 1, adds the Al (NO of 86.2g in 2.5L ethanol and 1L deionized water
3)
39H
2the LiNO of O and 15.9g
3, stir and treat that it dissolves; Step 2, by positive electrode LiMn
2o
4join step 1 gained solution to stir, mixing time 0.1 hour; Step 3, adopts 10M ammonia spirit, and regulate the pH value of solution to 7-8, mixing speed is 400r/min, keeps 3 hours, filters rear 80 DEG C of low temperature dryings, obtains the positive electrode of coated lithium aluminium presoma; Step 4, by the positive electrode of coated presoma, heat treated 1h at 700 DEG C of temperature, makes hydroxide change oxide into, finally obtains Surface coating LiAlO
2positive electrode sample.
The material high rate performance curve of coated front and back as shown in Figure 5.The discharge capacity of not coated sample when 1C, 5C and 10C is respectively 90.5,84.5 and 80.6 mAh/g; And LiAlO
2the discharge capacity of coated sample when 1C, 5C and 10C is respectively 92.2,88.5 and 81.6 mAh/g, when current density is increased to 15C, still has the capacity of 75 mAh/g, 81.3% when capability retention is 1C.
Embodiment 4
Step 1, adds the Al (NO of 78.4g in 3L ethanol
3)
39H
2the LiNO of O and 14.4g
3, stir and treat that it dissolves; Step 2, by positive electrode Li [Li
0.2mn
0.54ni
0.13co
0.13] O
2join step 1 gained solution to stir, mixing time 0.1 hour; Step 3, adopts 10M ammonia spirit, and regulate the pH value of solution to 9-10, mixing speed is 400r/min, keeps 80 DEG C of low temperature dryings after 4 hours, obtains the positive electrode of coated lithium aluminium presoma; Step 4, by the positive electrode of coated presoma, heat treated 2h at 600 DEG C of temperature, makes hydroxide change oxide into, finally obtains Surface coating LiAlO
2positive electrode sample.
Li [the Li obtained by the present embodiment
0.2mn
0.54ni
0.13co
0.13] O
2as shown in Figure 6, as can be seen from the figure there is obvious coated particle in modified material surface to ESEM (SEM) figure of coated front and back.
Material first charge-discharge curve after coated as shown in Figure 7, carries out discharge and recharge with the electric current of 0.1C, and as can be seen from the figure, the discharge capacity first of coated front material is 207mAh/g, and after circulating 40 weeks, capability retention is 87%; Coated LiAlO
2the discharge capacity of rear material stabilizes to 251mAh/g, and after circulating 40 weeks, capability retention reaches 98.9%.
Embodiment 5
Step 1, adds the Al (NO of 60.3g in 2L ethanol and 0.5L deionized water
3)
39H
2the LiNO of O and 11.1g
3, stir and treat that it dissolves; Step 2, by positive electrode LiMn
0.13ni
0.13co
0.13o
2join step 1 gained solution to stir, mixing time 0.5 hour; Step 3, adopts 10M ammonia spirit, and regulate the pH value of solution to 9-10, mixing speed is 550r/min, keeps 4 hours, filters rear 80 DEG C of low temperature dryings, obtains the positive electrode of coated lithium aluminium presoma; Step 4, by the positive electrode of coated presoma, heat treated 4h at 500 DEG C of temperature, makes hydroxide change oxide into, finally obtains Surface coating LiAlO
2positive electrode sample.
In technical scheme of the present invention, LiAlO
2evenly be coated on positive electrode surface, meanwhile, positive electrode does not change in coated front and back crystal grain structure, and the chemical property of coated rear material is significantly improved.This be due to and surface coated LiAlO
2material can be separated contact with the direct of electrolyte, slow down the erosion of HF in electrolyte, meanwhile, thin layer LiAlO
2lithium ion can be allowed to move into comparatively rapidly, battery performance is promoted.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong to the protection range of technical solution of the present invention.
Claims (9)
1. a Surface coating LiAlO
2the preparation method of lithium ion manganese cathode material, it is characterized in that, the method comprises:
Step 1, by nitric acid dissolving metal salts in the mixed liquor of ethanol or ethanol and water; Described nitric acid slaine is aluminum nitrate and lithium nitrate;
Step 2, joins step 1 gained solution and stirs, mixing time 0.1-0.5 hour by manganese cathode material;
Step 3, adopts ammonia spirit, regulates the pH value of solution to 4-10, and after mixing time 3-5 hour, 80 DEG C of low temperature dryings or filter rear 80 DEG C of low temperature dryings, obtain the material that lithium aluminium presoma is coated;
Step 4, by material coated for lithium aluminium presoma, heat treatment at 400 DEG C of-700 DEG C of temperature, obtains Surface coating LiAlO
2positive electrode sample;
Wherein, the consumption of described nitric acid slaine is 0.5% ~ 5% of positive electrode quality.
2. preparation method as claimed in claim 1, it is characterized in that, in step 1, described ethanol and the mixed liquor of water refer to that the volume ratio of ethanol and water is 10:1 ~ 2:1.
3. preparation method as claimed in claim 1, it is characterized in that, the manganese cathode material described in step 2 is LiNi
xco
ymn
(1-x-y)o
2, Li
1+nni
xco
ymn
(1-x-y-n)o
2or Li
x1mn
2-y1m
y1o
4; Wherein, 0≤x≤1,0≤y≤1,0≤n≤1,0.8≤x1≤1.2,0.001≤y1≤0.3, M is one or more in Mg, Al, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, Zr.
4. preparation method as claimed in claim 1, it is characterized in that, the ammonia spirit concentration described in step 3 is 1M ~ 10M.
5. described preparation method as claimed in claim 4, it is characterized in that, the stir speed (S.S.) that step 3 uses is 200r/min ~ 900r/min.
6. preparation method as claimed in claim 1, it is characterized in that, the weight ratio of the lithium aluminium presoma that the surface described in step 3 is coated and positive electrode is 0.5% ~ 8%.
7. preparation method as claimed in claim 1, is characterized in that, the Surface coating LiAlO described in step 4
2the covering amount of material be 0.5% ~ 5%.
8. the Surface coating LiAlO that obtains of the preparation method according to any one of claim 1-7
2lithium ion battery manganese system positive electrode, it is characterized in that, the Surface coating of this positive electrode has LiAlO
2.
9. the Surface coating LiAlO that obtains of preparation method as claimed in claim 8
2lithium ion battery manganese system positive electrode, it is characterized in that, described Surface coating LiAlO
2the covering amount of material be 0.5% ~ 5%.
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Cited By (12)
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| CN104766959A (en) * | 2015-03-24 | 2015-07-08 | 江苏乐能电池股份有限公司 | A preparing method of a Li(Ni<0.8>Co<0.1>Mn<0.1>)O2 ternary material |
| CN105185954A (en) * | 2015-06-17 | 2015-12-23 | 电子科技大学 | LiAlO2 coated LiNi1-xCoxO2 lithium-ion battery positive electrode material and preparation method thereof |
| CN105938899A (en) * | 2016-06-01 | 2016-09-14 | 中南大学 | Preparation method and application of cathode material of fast ion conductor coated modified lithium ion battery |
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| CN110071280A (en) * | 2019-05-14 | 2019-07-30 | 山东泰纳新材料科技有限公司 | A kind of solid electrolyte cladding silicon based anode material and preparation method thereof |
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| CN110581272A (en) * | 2019-09-30 | 2019-12-17 | 昆明云大新能源有限公司 | high-performance ternary cathode material for lithium ion battery and preparation method of ternary cathode material |
| CN111864188A (en) * | 2019-04-25 | 2020-10-30 | 比亚迪股份有限公司 | Lithium battery positive electrode material, preparation method thereof and all-solid-state lithium battery |
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