CN109411735A - A kind of positive electrode and preparation method thereof and lithium ion battery - Google Patents
A kind of positive electrode and preparation method thereof and lithium ion battery Download PDFInfo
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- CN109411735A CN109411735A CN201811450928.4A CN201811450928A CN109411735A CN 109411735 A CN109411735 A CN 109411735A CN 201811450928 A CN201811450928 A CN 201811450928A CN 109411735 A CN109411735 A CN 109411735A
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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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- 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
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- 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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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to field of batteries, a kind of positive electrode and preparation method thereof and lithium ion battery are disclosed.The preparation method of the positive electrode is the following steps are included: (1) mixes: carrying out lithium-rich manganese-based anode material and Organometallic framework material to be mixed to get mixture；The molecular formula of the lithium-rich manganese-based anode material is xLi2MnO3·(1‑x)LiMO2, at least one of M Ni, Co and Mn, 0 < x < 1；The quality of the Organometallic framework material accounts for the 1%~15% of lithium-rich manganese-based anode material quality；(2) it calcines: the mixture being calcined in air atmosphere, so that the Organometallic framework material oxygenolysis.Method provided by the invention can form continuous uniform clad on lithium-rich manganese-based anode material surface, active material in the clad will not only hinder the transmission of lithium ion, but also the side reaction occurred with the electrolyte in lithium ion battery can be greatly reduced, the lithium ion battery enabled to has extraordinary comprehensive electrochemical, especially cyclical stability.
Description
Technical field
The invention belongs to field of batteries, and in particular to a kind of positive electrode and preparation method thereof and lithium ion battery.
Background technique
In recent years, lithium ion battery (LIBs) is applied to all trades and professions, including 3C electronic product, various electronic
The vehicles (HEVs, PHEVs and EVs etc.) and energy-storage system (ESSs), this make high-energy density, fast charge, safety it is good,
The anode material for lithium-ion batteries such as LiCoO of low cost2, stratiform LiNi1-x-yCoxMnyO2With rich lithium material (1-xLiMO2·
xLi2MnO3, M Ni, Co or Mn) and obtain extensive research.Wherein, rich lithium material receives much attention, it has than other positive materials
Expect higher specific capacity (> 250mAh/g) and operating voltage, is most hopeful to break through the requirement of battery specific energy, and largely using honest and clean
The manganese element of valence compares LiCoO2With stratiform LiNi1-x-yCoxMnyO2With lower cost and better safety.But it is rich
Lithium material need to work to play the excellent properties of material under the high voltage higher than 4.5V (vs.Li+/Li), the lattice of material
There are also electrolyte and electrode material side reaction to make the stability of material by baptism for oxygen loss.
Surface cladding is a kind of effective ways for improving rich lithium material stability, has Al for coat rich lithium material2O3、
SiO2、TiO2Deng can effectively prevent material and electrolyte using surface coated method occurs side reaction, inhibits material lattice
Destroy, make material cyclical stability be improved significantly.Collosol and gel and co-precipitation have simple as common method for coating
Single easy feature, but that there are coatings is impure, reunites and the non-uniform problem of clad.And existing some novel sides
Method is capable of forming the clad of continuous densification such as chemical vapor deposition (CVD) and atomic layer deposition (ALD), but is formed by
Clad be usually it is non-porous and nonconducting, such clad is difficult that ion and electronics is allowed to pass through, and is unfavorable for the electricity of material
Chemical property.
CN108336316A discloses a kind of preparation method of lithium-rich anode material, this method comprises: (1) is by N, N- diformazan
Base formamide, dehydrated alcohol and deionized water mixing, add metal salt and 1,3,5- benzenetricarboxylic acids obtain mixed solution；(2)
Rich lithium material is added in mixed solution, is put into be stirred under vacuum in reaction kettle and react, obtain suspension；(3) by suspension from
The heart collects solid phase, washed, the dry lithium-rich anode material for obtaining metal organic framework compound cladding；(4) metal is organic
The lithium-rich anode material of framework compound cladding is sintered at 250~700 DEG C, obtains lithium-rich anode material.However, using
This method does not solve MOFs material in the surface coated technical problem of rich lithium material, covered effect be entirely MOFs material and
The effect of the mixing of rich lithium material in the solution, cladding not can guarantee.In addition, disclosed in the CN108336316A in method,
The rich lithium material of MOFs cladding is to be heat-treated in an inert atmosphere, due to containing organic ligand in MOFs material, therefore is being heat-treated
It being likely to generate carbon in the process, the metal of high-valence state in rich lithium material is caused to be reduced, the consistency of product is difficult to ensure, and
This method preparation process is more complex, is not suitable for large-scale production.
Summary of the invention
The purpose of the invention is to overcome the prior art to prepare positive material using the method for surface clad oxide
That there are coatings is impure for material, reunite and the non-uniform problem of clad or ion and electronics are difficult to by being formed by
The defect of clad, and provide a kind of new positive electrode and preparation method thereof and lithium ion battery.
Specifically, the present invention provides a kind of preparation methods of positive electrode, wherein method includes the following steps:
(1) it mixes: carrying out lithium-rich manganese-based anode material and Organometallic framework material to be mixed to get mixture；The richness
The molecular formula of lithium manganese-based anode material is xLi2MnO3·(1-x)LiMO2, at least one of M Ni, Co and Mn, 0 < x < 1；Institute
The quality for stating Organometallic framework material accounts for the 1%~15% of the lithium-rich manganese-based anode material quality；
(2) it calcines: the mixture is calcined in air atmosphere, so that Organometallic framework material oxidation point
Solution forms metal oxide.
The Organometallic framework material (MOFs) refers between organic bridging ligand and inorganic metal ion by from group
One kind that dress is formed has the crystalline material of periodic network structure.Preferably, the metal in the Organometallic framework material
Element is Al and/or Fe.The present inventor has found after further investigation, when the metal in Organometallic framework material
When element is Al and/or Fe, the corresponding lithium ion battery of resulting positive electrode has very excellent cyclical stability.It is more excellent
Selection of land, the Organometallic framework material are MIL-100 (Al) and/or MIL-101 (Fe).
Preferably, the mixed method is ball milling.
Preferably, the ball milling is using ethyl alcohol as grinding aid.
Preferably, in terms of by the total weight of the lithium-rich manganese-based anode material and Organometallic framework material for 1g, ethyl alcohol
Dosage is 100~2000 μ L.
Preferably, it is room temperature that the condition of the ball milling, which includes ball milling temperature, and Ball-milling Time is 5~120min.
Preferably, the mode and condition of the calcining be the mixture is warming up to 500 with 1~20 DEG C/min rate~
1000 DEG C, and at such a temperature maintain 1~for 24 hours.
The present invention also provides positive electrodes prepared by the above method.
In addition, the present invention also provides a kind of lithium ion batteries, wherein the positive electrode of the lithium ion battery is above-mentioned
Positive electrode.
The present inventor by further investigation after find, directly with specific lithium-rich manganese-based anode material with it is organic
Metallic framework material, only need to can be in lithium-rich manganese-based anode material through simple mechanical mixture and calcination processing as starting material
Surface forms the clad of continuous uniform, and the active material in the clad will not only hinder the transmission of lithium ion, but also
It can greatly reduce and side reaction occurs with the electrolyte in lithium ion battery, it is very good that the lithium ion battery enabled to has
Comprehensive electrochemical, especially cyclical stability.In addition, the preparation method that the present invention provides positive electrode is simple, it can be with
Extensive synthesis, great prospects for commercial application.
Detailed description of the invention
Fig. 1 a is the transmission electron microscope image of lithium-rich manganese-based anode material used by embodiment 1；
Fig. 1 b is the transmission electron microscope image for the positive electrode that embodiment 1 obtains；
Fig. 2 is lithium-rich manganese-based anode material used by embodiment 1 and the positive electrode finally obtained in current density
First circle charging and discharging curve figure when for 20mA/g；
Fig. 3 is lithium-rich manganese-based anode material used by embodiment 1 and the positive electrode finally obtained through the small electricity of first circle
Cycle performance figure after stream activation, in the case where current density is 200mA/g；
Fig. 4 be lithium-rich manganese-based anode material and the positive electrode finally obtained used by embodiment 1 0.2C,
Specific discharge capacity figure under 0.5C, 1C, 2C, 5C difference current density.
Specific embodiment
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to
Cross the conventional products of commercially available acquisition.
Embodiment 1
The embodiment is for illustrating positive electrode provided by the invention and preparation method thereof.
(1) it mixes: taking a ball grinder and several different size of zirconium pearls.1g lithium-rich manganese-based anode is added into ball grinder
Material (Li1.2Ni0.13Co0.13Mn0.54O2) and MIL-100 (Al), MIL-100 (Al) by lithium-rich manganese-based anode material quality
4.3% is added；Then 200 μ L of ethyl alcohol is instilled into the ball grinder, is resealed jar, at room temperature high-energy ball milling 30min, is obtained
Ball milling object.
(2) it calcines: by the ball milling object from scraping and being added in Muffle furnace in ball grinder, being heated with the rate of 5 DEG C/min
To 600 DEG C, 3h is then calcined at 600 DEG C, furnace cooling obtains positive electrode.
Wherein, the transmission electron microscope image of lithium-rich manganese-based anode material and the positive electrode finally obtained is respectively such as
Shown in Fig. 1 a and Fig. 1 b.It can be seen that lithium-rich manganese-based anode material with sharp-featured boundary from Fig. 1 a and Fig. 1 b, illustrate original
Material has good crystallinity, and there is the alumina-coated layer of one layer of continuous uniform on the positive electrode surface finally obtained, thick
Degree is in 20nm or so.Unformed aluminium oxide continuously coats on the surface of the material, can effectively inhibit the side reaction of material interface,
The SEI membrane component and structure of optimizing surface, thus the structural stability of protection materials.
Lithium-rich manganese-based anode material (rich lithium material) and the positive electrode finally obtained (rich lithium material after cladding) are in electricity
First circle charging and discharging curve when current density is 20mA/g is as shown in Figure 2.Figure it is seen that using method provided by the invention
The specific discharge capacity that lithium-rich manganese-based anode material can be improved, the discharge capacity of the positive electrode finally obtained first circle at 0.1C
For 279.1mAh/g, coulombic efficiency 83.7%.
Lithium-rich manganese-based anode material (rich lithium material) and the positive electrode finally obtained (rich lithium material after cladding) are through head
It encloses after low current activation, the cycle performance in the case where current density is 200mA/g is as shown in Figure 3.From figure 3, it can be seen that using
Method provided by the invention is significant to the cyclical stability for improving lithium-rich manganese-based anode material, and 0.1C (20mA/g) electric current is close
Reversible capacity still has 202.0mAh/g, capacity retention ratio 94.3% after degree 100 charge and discharge of lower circulation.
Lithium-rich manganese-based anode material (rich lithium material) and the positive electrode finally obtained (rich lithium material after cladding) exist
Specific discharge capacity under 0.2C, 0.5C, 1C, 2C, 5C difference current density is as shown in Figure 4.From fig. 4, it can be seen that using this hair
The method of bright offer can be improved the specific discharge capacity of lithium-rich manganese-based anode material, finally obtained positive electrode 0.2C,
Specific discharge capacity under 0.5C, 1C, 2C, 5C be respectively 252.2mAh/g, 223.5mAh/g, 198.5mAh/g, 177.5mAh/g,
149.7mAh/g also has good capacity under high current.
Embodiment 2
The embodiment is for illustrating positive electrode provided by the invention and preparation method thereof.
(1) it mixes: taking a ball grinder and several different size of zirconium pearls.1g lithium-rich manganese-based anode is added into ball grinder
Material (Li1.2Ni0.13Co0.13Mn0.54O2) and MIL-101 (Fe), MIL-101 (Fe) by lithium-rich manganese-based anode material quality
15% is added；Then 200 μ L of ethyl alcohol is instilled into the ball grinder, is resealed jar, at room temperature high-energy ball milling 30min, is obtained
Ball milling object.
(2) it calcines: by the ball milling object from scraping and being added in Muffle furnace in ball grinder, being heated with the rate of 10 DEG C/min
To 1000 DEG C, 1h is then calcined at 1000 DEG C, furnace cooling obtains positive electrode.
After tested, the discharge capacity of the positive electrode finally obtained first circle at 0.1C is 268.4mAh/g, coulombic efficiency
It is 80.0%.The cyclical stability of lithium-rich manganese-based anode material, 1C (200mA/g) can be improved using method provided by the invention
Reversible capacity still has 179.3mAh/g, capacity retention ratio 97.1% after recycling 100 charge and discharge under current density.
Embodiment 3
The embodiment is for illustrating positive electrode provided by the invention and preparation method thereof.
(1) it mixes: taking a ball grinder and several different size of zirconium pearls.1g lithium-rich manganese-based anode is added into ball grinder
Material (Li1.2Ni0.13Co0.13Mn0.54O2) and MIL-100 (Al), MIL-100 (Al) by lithium-rich manganese-based anode material quality
1% is added；Then 200 μ L of ethyl alcohol is instilled into the ball grinder, is resealed jar, at room temperature high-energy ball milling 30min, is obtained ball
Grind object.
(2) it calcines: by the ball milling object from scraping and being added in Muffle furnace in ball grinder, being heated with the rate of 1 DEG C/min
To 500 DEG C, 6h is then calcined at 500 DEG C, furnace cooling obtains positive electrode.
After tested, the discharge capacity of the positive electrode finally obtained first circle at 0.1C is 256.2mAh/g, coulombic efficiency
It is 80.5%.The cyclical stability of lithium-rich manganese-based anode material, 1C (200mA/g) can be improved using method provided by the invention
Reversible capacity still has 171.4mAh/g, capacity retention ratio 92.1% after recycling 100 charge and discharge under current density.
Embodiment 4
The embodiment is for illustrating positive electrode provided by the invention and preparation method thereof.
Positive electrode is prepared according to the method for embodiment 2, unlike, by MIL-100 (Fe) using identical weight part
ZIF-8 substance substitution, obtains positive electrode.
After tested, the discharge capacity of the positive electrode finally obtained first circle at 0.1C is 250mAh/g, and coulombic efficiency is
79%.Reversible capacity still has 150mAh/g, capacity retention ratio 92% after recycling 100 charge and discharge under 1C current density.
Comparative example 1 (positive electrode replaces with nickel cobalt aluminic acid lithium material)
The comparative example is for illustrating positive electrode of reference and preparation method thereof.
Positive electrode is prepared according to the method for embodiment 4, unlike, rich lithium material is used to the nickel cobalt of identical weight part
Aluminic acid lithium material (LiNi0.7Co0.2Al0.1O2) substitution, obtain reference positive electrode.
After tested, the discharge capacity of the reference positive electrode first circle at 0.1C finally obtained is 158mAh/g, coulomb effect
Rate is 80%.Reversible capacity is 127mAh/g after recycling 100 charge and discharge under 0.1C current density, and capacity retention ratio is
80.3%.
Comparative example 2 (CN108336316A embodiment 1)
(1) by n,N-Dimethylformamide, dehydrated alcohol and deionized water, 15:1:1 is mixed by volume, and 0.3g nitre is added
The 1,3,5- benzenetricarboxylic acid of sour aluminium and 0.17g obtain mixed solution；
(2) by 2g lithium-rich anode material (Li1.2Mn0.54Ni0.13Co0.13O2) to be added to mixing prepared by step (1) molten
In liquid, it is put into and is stirred under vacuum in reaction kettle, react 2h at 80 DEG C；
(3) suspension for obtaining reaction is centrifuged and washs three times, and vacuum drying obtains the lithium-rich anode material of MOFs cladding
Material；
(4) lithium-rich anode material of the MOFs cladding obtained step (3) obtains in a nitrogen atmosphere in 550 DEG C of sintering 2h
The lithium-rich anode material modified to MOFs.
After tested, the MOFs that finally obtains modified lithium-rich anode material discharge capacity of first circle at 0.5C is about
Reversible capacity is about 225mAh/g after recycling 100 charge and discharge under 270mAh/g, 0.5C current density, and capacity retention ratio is
83%.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. a kind of preparation method of positive electrode, which is characterized in that method includes the following steps:
(1) it mixes: carrying out lithium-rich manganese-based anode material and Organometallic framework material to be mixed to get mixture；The richness lithium manganese
The molecular formula of base anode material is xLi2MnO3·(1-x)LiMO2, at least one of M Ni, Co and Mn, 0 < x < 1；It is described to have
The quality of machine metallic framework material accounts for the 1%~15% of the lithium-rich manganese-based anode material quality；
(2) it calcines: the mixture being calcined in air atmosphere, so that the Organometallic framework material oxygenolysis shape
At metal oxide.
2. preparation method according to claim 1, which is characterized in that the metallic element in the Organometallic framework material
For Al and/or Fe.
3. preparation method according to claim 2, which is characterized in that the Organometallic framework material is MIL-100
(Al) and/or MIL-101 (Fe).
4. preparation method described in any one of -3 according to claim 1, which is characterized in that the mixed method is ball
Mill.
5. the preparation method according to claim 4, which is characterized in that the ball milling is using ethyl alcohol as grinding aid.
6. preparation method according to claim 5, which is characterized in that with the lithium-rich manganese-based anode material and organic metal
The total weight of framework material is 1g meter, and the dosage of ethyl alcohol is 100~2000 μ L.
7. the preparation method according to claim 4, which is characterized in that the condition of the ball milling includes that ball milling temperature is room
Temperature, Ball-milling Time are 5~120min.
8. preparation method described in any one of -3 according to claim 1, which is characterized in that the mode and condition of the calcining
For the mixture is warming up to 500~1000 DEG C with 1~20 DEG C/min rate, and at such a temperature maintain 1~for 24 hours.
9. the positive electrode that the method as described in any one of claim 1-8 is prepared.
10. a kind of lithium ion battery, which is characterized in that the positive electrode of the lithium ion battery be it is as claimed in claim 9 just
Pole material.
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Cited By (7)
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| CN110289405A (en) * | 2019-06-13 | 2019-09-27 | 浙江天能能源科技股份有限公司 | Nickelic tertiary cathode material of a kind of MOFs Derived Oxides cladding and preparation method thereof |
| CN110556526A (en) * | 2019-09-19 | 2019-12-10 | 宜宾锂宝新材料有限公司 | Coating method for improving cycle stability of lithium ion battery anode material |
| CN111048758A (en) * | 2019-12-17 | 2020-04-21 | 惠州亿纬锂能股份有限公司 | Positive electrode material with surface coated with porous oxide, preparation method and application thereof |
| CN111211290A (en) * | 2020-02-24 | 2020-05-29 | 福建翔丰华新能源材料有限公司 | High-performance quick-charging graphite lithium ion battery cathode and preparation method thereof |
| CN111430703A (en) * | 2020-03-18 | 2020-07-17 | 蜂巢能源科技有限公司 | Lithium-rich manganese-based positive electrode material for lithium ion battery, preparation method of lithium-rich manganese-based positive electrode material, positive plate, lithium ion battery and electric automobile |
| CN112614975A (en) * | 2020-12-16 | 2021-04-06 | 成都理工大学 | MOFs structure lithium ion battery negative electrode material MIL-53(Al-Fe) and preparation method thereof |
| CN114583120A (en) * | 2021-12-27 | 2022-06-03 | 武汉理工大学 | Method for designing and constructing gradient structure with metal ion component on surface of lithium-rich material |
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