CN106058230A - Preparation method of aluminum-doped and surface-modified co-modified high-nickel positive electrode material - Google Patents
Preparation method of aluminum-doped and surface-modified co-modified high-nickel positive electrode material Download PDFInfo
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- CN106058230A CN106058230A CN201610658086.6A CN201610658086A CN106058230A CN 106058230 A CN106058230 A CN 106058230A CN 201610658086 A CN201610658086 A CN 201610658086A CN 106058230 A CN106058230 A CN 106058230A
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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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- 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 of an aluminum-doped and surface-modified co-modified high-nickel positive electrode material. The preparation method comprises the following steps: 1, adding a high-nickel positive electrode material precursor to aluminum salt sol, and mixing the precursor and the sol to obtain a slurry, and heating the slurry while stirring to evaporate a solution in order to obtain dry powder; and 2, mixing the dry powder with a lithium source, and calcining the obtained dry powder and lithium source mixture to obtain the aluminum-doped and surface-modified co-modified high-nickel positive electrode material. Aluminum doping and surface modification forms are realized through uniformly mixing the aluminum salt sol with the high-nickel positive electrode material precursor, mixing the obtained mixture with the lithium source and carrying out one-step high temperature roasting. The method has the advantages of simple process and no increase of extra sintering flow; and doping of the prepared modified material stabilizes the crystal structure, and oxide modification of the surface can obstruct contact of the material with an electrode, so the cycle stability is improved.
Description
Technical field
The invention belongs to lithium ion battery material technical field, be specifically related to the doping of a kind of aluminum and modify modification altogether with surface
The preparation method of nickelic positive electrode.
Background technology
Along with the fast development of power train in vehicle application lithium ion battery, exploration exploitation energy density is bigger, cyclic durability is longer,
Security performance more preferably lithium-ion battery system also becomes the research emphasis direction of scientific research institutions and enterprise.There is layer structure
High power capacity positive electrode Li (NixCoyMnzAl1-x-y-z)O2(0 < x < 1,0 < y < 1,0≤z < 1)) most there is DEVELOPMENT PROSPECT.
In its constituent of stratified material, each transition metal ions effect is different.It is generally believed that Al3+ and Mn4+
Effect is to reduce material cost, improve material safety and structural stability；The stratiform being possible not only to stabilizing material of Co3+
Structure, and circulation and the high rate performance of material can be improved；And the effect of Ni2+ is to improve the volume energy increasing material
Density.Therefore what current development in laboratory was more is then the system of Ni >=0.8, but nickel content relatively Gao Zechang can cause two to ask
Topic: first, in sintering process, the mixing of lithium nickel has a strong impact on the coulombic efficiency of lithium ion deintercalation；Secondly, the residual basicity of high nickel surface is relatively
Height, surface texture in cyclic process due to self phase transformation or and electrolyte react, destroyed more serious, therefore cycle performance
Difference.The main thought solving problems is then by surface modification, by introducing one layer of electro-chemical activity or burning
Thing inert material intercepts the Stability Analysis of Structures that positive electrode surface is certain with electrolyte contacts and guarantee.
Conventional doped chemical is Mn4+And Al3+.For ensureing that uniform doping all can be co-precipitated in the presoma stage,
But Al (OH)3Solubility product (p Ksp=32.34) much smaller than Ni (OH)2With Co (OH)2Solubility product (p Ksp ≈ 14), because of
The technology controlling and process of this homogeneous precipitation is the harshest, and cost puts into higher.Surface coating is mainly with metal-oxide (Al2O3,
ZnO, ZrO2Deng) double sintering forms after predecessor mixes with nickelic stratified material, i.e. original material is carried out two-step sintering, increase
Add technological process.Publication No. CN 103647073 A patent is coated with by two steps, reaches aluminium oxide and carbon is coated with altogether；Public
The number of opening be CN 104577128 A patent in by the way of simple aluminum nitrate and tertiary cathode material are by dropping ammonia
Cladding is realized after carrying out mixing low temperature calcination；Publication No. CN 104393277 A patent then by introducing, introduces high score
Sub-polyacrylamide is as dispersant and flocculant, it is achieved Al2O3Cladding；The patent of Publication No. CN 103296263 A is led to
Cross introducing Al in presoma coprecipitation process3+Realize the doping in later stage.
Positive electrode has all only been carried out in terms of single doping or modification by said method.Publication No. CN
After modified material is mixed by the patent of 1731605A and CN 104600282 A with finished-product material sinter, be prepared for containing
The positive electrode of the surface reforming layer of surface coating layer and diffusion thereof；Publication No. CN 103779556 A has applied for mixing
Miscellaneous type cobalt acid lithium is matrix, at its Surface coating Co3(PO4)2、AlPO4、Mn3(PO4)2、FePO4Etc. phosphatic doping and surface
The material that cladding is the most modified.
Nickelic positive electrode preparation process includes presoma preparation and mixes lithium and sinter two steps, but the material system of above-mentioned patent
During Bei, precursor doped can cause technology controlling and process complicated, and cost increases, the anode material doped or cladding of later stage finished product
Can additionally increase the technological process of a step sintering.The present invention directly introduces modified material between presoma and mixed lithium sinter, logical
Crossing a step sintering realization preparation doping and surface is modified and is total to modified material, do not increase extra sintering process, method is simple, easily
In large-scale production.
Summary of the invention
It is an object of the invention to provide the doping of a kind of aluminum and modify the preparation side being total to modified nickelic positive electrode with surface
Method, is used for improving the chemical property of the nickelic positive electrode of lithium ion battery.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The preparation method of altogether modified nickelic positive electrode is modified on the doping of a kind of aluminum and surface, it is characterised in that: include with
Lower step:
(1) nickelic positive electrode material precursor is mixed into slurry in joining aluminium salt colloidal sol, while stirring heating evaporation solution,
Obtain the powder body being dried；
(2) dry powder body mixing lithium source is calcined, i.e. obtain lithium ion battery aluminium doping and change altogether with surface modification
The nickelic positive electrode of property.
Further scheme, the aluminium salt colloidal sol in described step (1) is made up of aluminum nitrate, ammonia and nitric acid, and concentration is 0.1-
2mol/L。
Scheme further, the nickelic positive electrode material precursor in described step (1) is NixCo1-xO2Or NixCo1-x(OH)2,
Wherein 0.85≤x≤0.95.
Scheme further, the nickelic positive electrode material precursor in described step (1) and aluminium salt colloidal sol mol ratio are 1:
(0.01-0.08)。
Scheme further, the lithium source in described step (2) is LiOH.H2O, lithium source is 1-1.08 with the mol ratio of presoma:
1。
Further scheme, the calcining in described step (2) be in oxygen atmosphere, temperature be 700-780 DEG C of calcining 10-
18h。
Positive electrode material precursor mentioned in the present invention is hydroxide or the oxygen of corresponding positive electrode slaine
Compound.
The invention has the beneficial effects as follows:
(1) present invention uses the nickelic positive electrode material precursor of Al doping and modification, it is to avoid nickelic positive electrode material precursor is altogether
Precipitation synthesis phase introduces Al, simplifies preparation technology；Sol system can ensure that the mixing uniformity of raw material；
(2) do not increase extra sintering flow process, Al is modified two kinds of state of aggregations with doping and surface simultaneously and is incorporated into nickelic
Positive electrode surface, can improve the structural stability of material, improve chemical property.
Accompanying drawing explanation
Fig. 1 is the Al element XPS collection of illustrative plates of the embodiment of the present invention 1 powder body material.
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), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 1mol/L molten
Glue.By positive electrode material precursor Ni0.9Co0.1(OH)2Joining in aluminium salt colloidal sol and be mixed into slurry, wherein presoma is molten with aluminium salt
Glue mol ratio is 1:0.05, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder body being dried；
(2) LiOH is mixed according to 1.02:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 750 DEG C of temperature calcination
15h, i.e. obtains anode material for lithium-ion batteries Li1.02Ni0.857Co0.095Al0.048O2。
Comparative example: by Ni0.9Co0.1(OH)2Presoma and LiOH.H2O powder body carries out machinery according to mol ratio 1:1.02 ratio
Mix grinding, then by its in oxygen with 750 DEG C of temperature calcination 15h, i.e. obtain anode material for lithium-ion batteries.
Positive pole powder test XPS, analyzes Al2p collection of illustrative plates, the most as shown in Figure 1.It can be seen that Al2p occurs two after matching
Individual peak, includes the Al of Surface coating state2O3Peak and the Al being embedded into lattice3+Two types, illustrates a step high temperature in the present invention
Roasting process can realize modifying aluminum source with oxide on surface being present in nickelic positive electrode with two kinds of forms of surface doping.Separately
Outward, owing to using liquid phase method mixing, aluminum surface doping and modification can uniformly be present in nickelic positive electrode surface.
Embodiment 2
(1), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 2mol/L molten
Glue.By positive electrode material precursor Ni0.9Co0.1(OH)2Joining in aluminium salt colloidal sol and be mixed into slurry, wherein presoma is molten with aluminium salt
Glue mol ratio is 1:0.03, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder body being dried；
(2) LiOH is mixed according to 1.01:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 720 DEG C of temperature calcination
12h, i.e. obtains anode material for lithium-ion batteries Li1.01Ni0.873Co0.098Al0.029O2。
Embodiment 3
(1), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 0.5mol/L
Colloidal sol.By positive electrode material precursor Ni0.85Co0.15(OH)2Join in aluminium salt colloidal sol and be mixed into slurry, wherein presoma and aluminum
Salt sol mol ratio is 1:0.01, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder being dried
Body；
(2) LiOH is mixed according to 1.01:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 700 DEG C of temperature calcination
18h, i.e. obtains anode material for lithium-ion batteries Li1.01Ni0.841Co0.148Al0.01O2。
Embodiment 4
(1), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 2mol/L molten
Glue.By positive electrode material precursor Ni0.95Co0.05(OH)2Join in aluminium salt colloidal sol and be mixed into slurry, wherein presoma and aluminium salt
Colloidal sol mol ratio is 1:0.05, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder being dried
Body；
(2) LiOH is mixed according to 1.05:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 780 DEG C of temperature calcination
15h, i.e. obtains anode material for lithium-ion batteries Li1.05Ni0.922Co0.048Al0.048O2。
Embodiment 5
(1), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 2mol/L molten
Glue.By positive electrode material precursor Ni0.95Co0.05(OH)2Join in aluminium salt colloidal sol and be mixed into slurry, wherein presoma and aluminium salt
Colloidal sol mol ratio is 1:0.08, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder being dried
Body；
(2) LiOH is mixed according to 1.08:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 780 DEG C of temperature calcination
15h, i.e. obtains anode material for lithium-ion batteries Li1.08Ni0.879Co0.046Al0.074O2。
Embodiment 6
(1), with nine water aluminum nitrates as aluminium salt, after being first added in water dissolving, adding chelating agent ammonia further will
Al3+It is precipitated out completely, then adds the anti-molten precipitate of nitric acid, the pH to 5-7 of regulation solution, obtain the aluminium salt that concentration is 0.1mol/L
Colloidal sol.By positive electrode material precursor Ni0.85Co0.15O2Joining in aluminium salt colloidal sol and be mixed into slurry, wherein presoma is molten with aluminium salt
Glue mol ratio is 1:0.05, and the solid content in slurry is 60wt%, while stirring heating evaporation solution, obtains the powder body being dried；
(2) LiOH is mixed according to 1:1 ratio.H2After O, under oxygen atmosphere, by mixed powder at 780 DEG C of temperature calcination
10h, i.e. obtains anode material for lithium-ion batteries LiNi0.809Co0.142Al0.048O2。
Above example is only the embodiment of part of the present invention.It should be noted that, embodiments of the present invention are not by above-mentioned
The restriction of embodiment, 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 (6)
1. the preparation method being total to modified nickelic positive electrode is modified in an aluminum doping with surface, it is characterised in that: include following
Step:
(1) nickelic positive electrode material precursor is mixed into slurry in joining aluminium salt colloidal sol, while stirring heating evaporation solution, obtains
The powder body being dried；
(2) dry powder body mixing lithium source is calcined, i.e. obtain lithium ion battery aluminium doping and modify modification altogether with surface
Nickelic positive electrode.
The preparation method of the most modified nickelic positive electrode is modified on aluminum the most according to claim 1 doping and surface, and it is special
Levying and be: the aluminium salt colloidal sol in described step (1) is made up of aluminum nitrate, ammonia and nitric acid, concentration is 0.1-2mol/L.
The preparation method of the most modified nickelic positive electrode is modified on aluminum the most according to claim 1 doping and surface, and it is special
Levy and be: the nickelic positive electrode material precursor in described step (1) is NixCo1-xO2Or NixCo1-x(OH)2, wherein 0.85≤x
≤0.95。
The preparation method of the most modified nickelic positive electrode is modified on aluminum the most according to claim 1 doping and surface, and it is special
Levy and be: the nickelic positive electrode material precursor in described step (1) and aluminium salt colloidal sol mol ratio are 1:(0.01-0.08).
The preparation method of the most modified nickelic positive electrode is modified on aluminum the most according to claim 1 doping and surface, and it is special
Levy and be: the lithium source in described step (2) is LiOH.H2O, lithium source is 1-1.08:1 with the mol ratio of presoma.
The preparation method of the most modified nickelic positive electrode is modified on aluminum the most according to claim 1 doping and surface, and it is special
Levy and be: the calcining in described step (2) be in oxygen atmosphere, temperature be 700-780 DEG C calcining 10-18h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109920996A (en) * | 2019-03-19 | 2019-06-21 | 河南大学 | A kind of doping coats the anode material for lithium-ion batteries and preparation method thereof of double modification structures certainly in the process |
| WO2020063680A1 (en) | 2018-09-26 | 2020-04-02 | 宁德时代新能源科技股份有限公司 | Positive electrode active material and preparation method therefor, electrochemical cell, battery module, battery pack, and apparatus |
| CN112038608A (en) * | 2020-09-09 | 2020-12-04 | 昆明理工大学 | Method for synthesizing high-performance washing-free high-nickel lithium battery positive electrode material by one-step method |
| WO2021135923A1 (en) * | 2019-12-31 | 2021-07-08 | 深圳新宙邦科技股份有限公司 | Lithium ion battery |
| CN114122492A (en) * | 2020-08-31 | 2022-03-01 | 深圳新宙邦科技股份有限公司 | Lithium ion battery |
| US11539046B2 (en) | 2019-12-27 | 2022-12-27 | Industrial Technology Research Institute | Ion-conducting material, core-shell structure containing the same, electrode prepared with the core-shell structure and metal-ion battery employing the electrode |
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