CN105742596A - Preparation method for positive electrode material of lithium ion battery - Google Patents
Preparation method for positive electrode material of lithium ion battery Download PDFInfo
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- CN105742596A CN105742596A CN201610126716.5A CN201610126716A CN105742596A CN 105742596 A CN105742596 A CN 105742596A CN 201610126716 A CN201610126716 A CN 201610126716A CN 105742596 A CN105742596 A CN 105742596A
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- lithium
- positive electrode
- electrode material
- ion battery
- anode material
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
Abstract
The invention provides a preparation method for a positive electrode material of a lithium ion battery. A complexing agent is added to a lithium source solution firstly; the pH of the lithium source solution is adjusted to 5-7 to obtain lithium salt sol; a positive electrode material precursor is added to the lithium salt sol to be mixed to obtain paste; the solution is evaporated while stirring and heating to obtain dried gel; and the dried gel is calcined to obtain the positive electrode material of the lithium ion battery. According to the preparation method, the contact area between the lithium salt sol and the positive electrode material precursor is large, so that the uniform mixing between the lithium salt sol and the positive electrode material precursor can be facilitated; the rapid implementation of the reaction can be promoted in the high-temperature roasting process, so that the cost is saved; the prepared positive electrode material elements are uniform in distribution; and a more excellent electrochemical performance of the positive electrode material is realized.
Description
Technical field
The invention belongs to lithium ion battery material technical field, be specifically related to the preparation method of a kind of anode material for lithium-ion batteries.
Background technology
Lithium ion battery has specific energy height, stable circulation, voltage platform height, the low and eco-friendly feature of self-discharge rate, therefore has a wide range of applications in 3C consumer electronics and electrokinetic cell field.The beginning of this century, under the background of new energy field fast development, find the research emphasis direction that energy storage density is bigger, cycle life is longer, security performance more preferably lithium-ion battery system also becomes scientific research institutions and enterprise.High power capacity and High-Voltage Technology route become the main flow direction of current field of lithium ion battery development.The positive electrode that these two technology paths are used mainly includes high-tension LiNi0.5Mn1.5O4Material, and the layered cathode material of high power capacity such as ternary electrode Li (NixCoyMn1-x-y)O2(0 < x < 1,0 < y < 1), LiNixCo1-xO2(0≤x≤1), lithium-rich manganese-based electrode xLi2MnO3·(1-x)LiMO2(M=Ni,
Co, Mn, 0 < x < 1)), Li (NixCoyAl1-x-y)O2(0 < x < 1,0 < y < 1).
Common method for preparing anode material is by material precursor and Li2CO3Mechanical mixture, then process through high-temperature calcination, obtain finished-product material.But the method for mechanical mixture is relatively big to the destruction of presoma pattern, such as ternary material precursor uses coprecipitation to prepare, its pattern secondary spherical granule that generally crystal grain of submicron is reunited.Before not making finished product, its spherical structure is the loosest, if using machinery batch mixing, presoma pattern can be caused to crush, and ternary material finished product tap density is low, the shortcoming of poor processability.On the other hand, machinery mix grinding required time is long, and uneven phenomenon easily occurs in batch mixing, will also result in Li segregation in sintering process, the result that electrode material performance is low.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of lithium ion battery electrode material, be used for improving the chemical property of anode material for lithium-ion batteries.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The preparation method of a kind of anode material for lithium-ion batteries, comprises the following steps:
(1) in the solution of lithium source, chelating agent is added, the pH to 5-7 of regulation lithium source solution, obtain lithium salts colloidal sol；
(2) positive electrode material precursor is joined in lithium salts colloidal sol it is mixed into slurry, heating evaporation solution while stirring, obtain the gel being dried；
(3) dry gel is calcined, i.e. obtain anode material for lithium-ion batteries.
Scheme further, in the lithium source solution in described step (1), lithium source is at least one in lithium nitrate, lithium carbonate, Lithium hydrate.
Scheme further, the chelating agent in described step (1) is ammonia, and the addition of chelating agent is 1-1.5 times of lithium source mole.
Scheme further, the concentration of the lithium salts colloidal sol in described step (1) is 0.1-10mol/L.
Scheme further, the positive electrode material precursor in described step (2) is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Or NixCoyAl1-x-yO2Or NixCoyAl1-x-y(OH)2, wherein 0 < x < 1,0 < y < 1；Or be MnxM1-xO2Or NixCo1-xO2Or NixCo1-x(OH)2, wherein M=Ni, Co, Mn, 0 < x < 1.
Further scheme, the lithium salts colloidal sol in described step (2) is 0.98-1.2:1 with the mol ratio of positive electrode material precursor, described in the solid content that is mixed in slurry be 40-70wt%.
Further scheme, the calcining in described step (3) be in air or oxygen atmosphere, temperature be 800 ~ 950 DEG C of calcining 10-18h.
Positive electrode material precursor mentioned in the present invention is hydroxide or the oxide of corresponding positive electrode slaine.Lithium source solution is that lithium source is dissolved in water or acid the solution formed.
The invention has the beneficial effects as follows:
(1) present invention adds chelating agent ammonia and carrys out complexation lithium ion, makes system evenly；Regulate the pH to 5-7 of lithium salts sol system simultaneously, thus ensure that in lithium colloidal sol the lithium ion of complexation will not Precipitation, also ensure that the acidity of lithium colloidal sol will not corrode positive electrode material precursor；
(2) positive electrode material precursor being joined in lithium salts colloidal sol and be mixed into slurry, making solid content in this slurry is 40-70%, it is ensured that sol system is fully contacted with positive electrode material precursor, and shortens solvent evaporation time in next step dry run；
(3) method used in the present invention can allow positive electrode material precursor mix evenly with lithium source, and mixed process is conducive to keeping presoma pattern, improves chemical property and the processing characteristics of lithium ion anode material；
(4) present invention utilizes the feature that lithium salts colloidal sol is big with positive electrode material precursor contact area, it is beneficial to both uniformly mixing, high-temperature calcination process may advantageously facilitate quickly carrying out of reaction, saved cost, preparation positive electrode Elemental redistribution all with, have more excellent chemical property.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
The button battery first charge-discharge curve made by positive electrode that Fig. 1 is the embodiment of the present invention 1 and prepared by comparative example；
Fig. 2 is the embodiment of the present invention 1 and prepared by comparative example positive electrode multiplying power and circulation figure.
Specific implementation method
Below in conjunction with specific embodiment, the present invention is described in detail, but embodiments of the present invention are not limited to this.
Embodiment
1
(1), after lithium carbonate is added nitric acid dissolving, add chelating agent ammonia, the pH to 7 of regulation solution further, obtain the lithium salts colloidal sol that concentration is 2mol/L；
(2) by positive electrode material precursor Ni0.6Co0.2Mn0.2(OH)2Joining in lithium salts colloidal sol and be mixed into slurry, wherein lithium salts colloidal sol is 1.02:1 with the mol ratio of positive electrode material precursor, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the gel being dried；
(3) in atmosphere, by dry gel at 870 DEG C of temperature calcination 15h, anode material for lithium-ion batteries LiNi is i.e. obtained0.6Co0.2Mn0.2O2。
Comparative example: by Ni0.6Co0.2Mn0.2(OH)2Presoma and Li2CO3Powder body carries out machinery mix grinding according to mol ratio 1:0.51 ratio, then by it in atmosphere with 870 DEG C of temperature calcination 15h, i.e. obtains anode material for lithium-ion batteries.
With mass ratio as 0.8:0.1:0.1, positive electrode LiNi prepared by above-described embodiment 1 and comparative example0.6Co0.2Mn0.2O2Making lithium battery anode after uniformly mixing with conductive black and Kynoar respectively, its negative pole is metal lithium sheet, tests its charge-discharge performance the most respectively, the most as shown in Figure 1, 2.
Fig. 1 is first charge-discharge curve.Under 0.1C multiplying power, the discharge capacity first of the lithium battery that positive electrode prepared by the present invention is made has reached 180.5mAh/g, and the discharge capacity first of the lithium battery that comparative example positive electrode is made is 173.3mAh/g, the positive electrode that i.e. prepared by the present invention is compared the discharge capacity first of the positive electrode that more mechanical mix grinding method is made and is improve 4%.
Fig. 2 is multiplying power and the circulation figure of positive electrode.Under 2C multiplying power, the capability retention of positive electrode prepared by lithium sol method of the present invention is 89.2%, has promoted than the 87.0% of mechanical mix grinding method.After 1C charge and discharge circulates 100 times, the capability retention of positive electrode prepared by the present invention has reached 98%, is obviously improved than the 91.0% of mechanical mix grinding method.
Embodiment
2
(1), after lithium oxide lithium being added nitric acid dissolving, add chelating agent ammonia, the pH to 5 of regulation solution further, obtain the lithium salts colloidal sol that concentration is 10mol/L；
(2) by positive electrode material precursor Ni0.8Co0.15Al0.05(OH)2Joining and be mixed into slurry in lithium salts colloidal sol, lithium salts colloidal sol is 1.2:1 with the mol ratio of positive electrode material precursor, and the solid content in slurry is 70wt%, while stirring heating evaporation solution, obtains the gel being dried；
(3) in atmosphere, by dry gel at 950 DEG C of temperature calcination 10h, anode material for lithium-ion batteries LiNi is i.e. obtained0.8Co0.15Al0.05O2。
Scheme further, the positive electrode material precursor in described step (2) is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Or NixCoyAl1-x-yO2Or NixCoyAl1-x-y(OH)2, wherein 0 < x < 1,0 < y < 1；Or be MnxM1-xO2Or NixCo1-xO2, wherein M=Ni, Co, Mn, 0 < x < 1.
Embodiment
3
(1), after lithium nitrate being added to the water dissolving, add chelating agent ammonia, the pH to 6 of regulation solution further, obtain the lithium salts colloidal sol that concentration is 0.1mol/L；
(2) by positive electrode material precursor Mn0.7Ni0.2Co0.1(OH)2Joining and be mixed into slurry in lithium salts colloidal sol, lithium salts colloidal sol is 0.98:1 with the mol ratio of positive electrode material precursor, and the solid content in slurry is 40wt%, while stirring heating evaporation solution, obtains the gel being dried；
(3) in oxygen atmosphere, by dry gel at 800 DEG C of temperature calcination 18h, anode material for lithium-ion batteries 0.2Li is i.e. obtained2MnO3·0.8LiMn0.625Ni0.25Co0.125O2。
Above example is only the embodiment of part of the present invention.It should be noted that; embodiments of the present invention are not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify, be regarded as the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. the preparation method of an anode material for lithium-ion batteries, it is characterised in that: comprise the following steps:
(1) in the solution of lithium source, chelating agent is added, the pH to 5-7 of regulation lithium source solution, obtain lithium salts colloidal sol；
(2) positive electrode material precursor is joined in lithium salts colloidal sol it is mixed into slurry, heating evaporation solution while stirring, obtain the gel being dried；
(3) dry gel is calcined, i.e. obtain anode material for lithium-ion batteries.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterised in that: in the lithium source solution in described step (1), lithium source is at least one in lithium nitrate, lithium carbonate, Lithium hydrate.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterised in that: the chelating agent in described step (1) is ammonia, and the addition of chelating agent is 1-1.5 times of lithium source mole.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterised in that: the concentration of the lithium salts colloidal sol in described step (1) is 0.1-10mol/L.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterised in that: the positive electrode material precursor in described step (2) is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Or NixCoyAl1-x-yO2Or NixCoyAl1-x-y(OH)2, wherein 0 < x < 1,0 < y < 1；Or be MnxM1-xO2Or NixCo1-xO2Or NixCo1-x(OH)2, wherein M=Ni, Co, Mn, 0 < x < 1.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterized in that: the mol ratio of the lithium salts colloidal sol in described step (2) and positive electrode material precursor is 0.98-1.2:1, described in the solid content that is mixed in slurry be 40-70wt%.
Method for preparing anode material of lithium-ion battery the most according to claim 1, it is characterised in that: the calcining in described step (3) be in air or oxygen atmosphere, temperature be 800 ~ 950 DEG C calcining 10-18h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108736009A (en) * | 2018-05-29 | 2018-11-02 | 中伟新材料有限公司 | Cobalt nickel lithium manganate ternary material and preparation method thereof |
| CN108878821A (en) * | 2018-06-19 | 2018-11-23 | 合肥国轩高科动力能源有限公司 | A kind of nickelic tertiary cathode material and preparation method thereof of surface cladding lanthana |
| CN110790320A (en) * | 2019-10-25 | 2020-02-14 | 合肥国轩高科动力能源有限公司 | Core-shell structure precursor for lithium ion layered positive electrode material and preparation method thereof |
| CN113683125A (en) * | 2021-07-22 | 2021-11-23 | 宁夏汉尧石墨烯储能材料科技有限公司 | Method for preparing low-cobalt cathode material by sol-gel-solid phase sintering method |
| WO2022027981A1 (en) * | 2020-08-04 | 2022-02-10 | 厦门厦钨新能源材料股份有限公司 | Environment-friendly precursor and preparation method therefor, and composite oxide powder and preparation method therefor, and application |
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| CN102709543A (en) * | 2012-06-06 | 2012-10-03 | 株洲泰和高科技有限公司 | Rich-lithium ternary laminar lithium ion battery cathode material |
| CN102709568A (en) * | 2012-06-25 | 2012-10-03 | 天津工业大学 | Preparation method for nickel cobalt lithium manganate LiNixConMn1-x-yO2 of anode material of lithium ion battery |
| CN103413932A (en) * | 2013-08-19 | 2013-11-27 | 北大先行科技产业有限公司 | Modified single crystal type multielement anode material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102709543A (en) * | 2012-06-06 | 2012-10-03 | 株洲泰和高科技有限公司 | Rich-lithium ternary laminar lithium ion battery cathode material |
| CN102709568A (en) * | 2012-06-25 | 2012-10-03 | 天津工业大学 | Preparation method for nickel cobalt lithium manganate LiNixConMn1-x-yO2 of anode material of lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108736009A (en) * | 2018-05-29 | 2018-11-02 | 中伟新材料有限公司 | Cobalt nickel lithium manganate ternary material and preparation method thereof |
| CN108878821A (en) * | 2018-06-19 | 2018-11-23 | 合肥国轩高科动力能源有限公司 | A kind of nickelic tertiary cathode material and preparation method thereof of surface cladding lanthana |
| CN110790320A (en) * | 2019-10-25 | 2020-02-14 | 合肥国轩高科动力能源有限公司 | Core-shell structure precursor for lithium ion layered positive electrode material and preparation method thereof |
| CN110790320B (en) * | 2019-10-25 | 2022-03-11 | 合肥国轩高科动力能源有限公司 | Core-shell structure precursor for lithium ion layered positive electrode material and preparation method thereof |
| WO2022027981A1 (en) * | 2020-08-04 | 2022-02-10 | 厦门厦钨新能源材料股份有限公司 | Environment-friendly precursor and preparation method therefor, and composite oxide powder and preparation method therefor, and application |
| CN113683125A (en) * | 2021-07-22 | 2021-11-23 | 宁夏汉尧石墨烯储能材料科技有限公司 | Method for preparing low-cobalt cathode material by sol-gel-solid phase sintering method |
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