CN106654251A - Modified lithium-rich manganese-based positive electrode material and preparation method thereof - Google Patents
Modified lithium-rich manganese-based positive electrode material and preparation method thereof Download PDFInfo
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- CN106654251A CN106654251A CN201611082270.7A CN201611082270A CN106654251A CN 106654251 A CN106654251 A CN 106654251A CN 201611082270 A CN201611082270 A CN 201611082270A CN 106654251 A CN106654251 A CN 106654251A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a modified lithium-rich manganese-based positive electrode material and a preparation method thereof, and belongs to the technical field of positive electrode materials for lithium-ion batteries. The preparation method comprises the steps of fully mixing a lithium-rich manganese-based precursor, a lithium salt and a doped metal compound, and then burning a mixture to prepare the modified lithium-rich manganese-based positive electrode material; and carrying out pretreatment of heat preservation on a lithium-rich manganese-based precursor at 300-650 DEG C for 2-6 hours before mixing. A pretreatment step of the precursor is added to an existing preparation technology of the lithium-rich manganese-based positive electrode material, a crystal structure of the precursor is more complete and an aluminum element is doped, so that the initial coulomb efficiency of the positive electrode material can be significantly improved and is improved by 15-20% in comparison with that of an un-pretreated material; and the rate capability is also greatly improved.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, and in particular to a kind of modified lithium-rich manganese-based anode material
And preparation method thereof.
Background technology
Energy problem is the key issue of a national sustainable development, and it is China to seek and develop alternative secondary energy sources
A current important state basic policy.Lithium ion battery is the nearly high-energy battery that during the last ten years fast development is got up, because it has height
The advantage such as voltage, high specific energy, good cycle, environmental pollution be little, has become at present a weight of various countries' New Energy Industry
Point direction.It is also the key point of performance of lithium ion battery and lithium ion anode material is the important component part of lithium ion battery.
In recent years low cost, the lithium-rich manganese-based anode material of high power capacity cause the extensive concern of people.Prepare at present
Although the lithium-rich manganese base material for going out possesses very high specific discharge capacity, but more problem is still faced in practical application.Such as head
Circle must carry out discharge and recharge under less current density, and what is brought therewith is the irreversible capacity of 30-120mAh/g；Poor
High rate performance, the specific discharge capacity under 1C multiplying powers is usually less than 200mAh/g；Higher capacity is gone for, is needed higher
Charge cutoff voltage, however bring be material structure change, cause the internal resistance of cell to become big, capacity attenuation is very fast, mainly
Because the special Mechanism of electrochemical behaviors of anhydrous of this material.
Solving the method for this problem of materials at present mainly has：Cladding, acid treatment, doping, pre- circulation, heat treatment etc..Such as
The patent document of the A of Publication No. CN 101562245 discloses one kind and utilizes MnO2Surface coating is carried out to lithium-rich anode material
Method, this method reduce the irreversible capacity loss first of material, improve cycle performance of the material under high magnification, but
It is that modified material discharging capacity is relatively low.The patent document of the A of Publication No. CN 102738458 using Al, Ce, Mn, Ru, Y,
The oxide or phosphate of the elements such as Ni, Co the method increases coulomb first as the clad of lithium-rich manganese-based anode material
Efficiency, cycle performance and high rate performance are improved, but this method of modifying puts down the discharge voltage of lithium-rich manganese-based anode material
Platform has declined, and the energy density for causing lithium-rich anode material has declined.The patent text of the A of Publication No. CN 102694164
The lithium-rich manganese-based anode material for disclosing a kind of surface nitrating or carbon is offered, although the method improves lithium-rich manganese-based anode material
Cycle performance, but this method does not solve the problems, such as that first coulombic efficiency is relatively low.The and for example patent of the A of CN 104681809
Document discloses a kind of method of modifying of lithium-rich manganese-based anode material, comprises the steps of：Prepare lithium-rich manganese-based anode material
Presoma, presoma, lithium carbonate and doping vario-property chloric metal-salt are sufficiently mixed uniformly, the compound after being well mixed is entered
Row high temperature sintering, obtains modified lithium-rich manganese-based anode material, and the method is by optimization slaine species and follow-up sintering system
Degree is expected to form LiAlO on positive electrode surface2、Li2ZrO3、Li2TiO3Deng lithium ion conductance clad, clad is effectively delaying
While solution electrolyte corrodes to active substances in cathode materials and suppresses SEI films to be formed, the deintercalation process for lithium ion is provided soon
Fast transmission channel, contributes to the raising of material circulation life-span and high rate performance.
The content of the invention
The invention provides a kind of preparation method of modified lithium-rich manganese-based anode material, the method increases positive electrode
Coulombic efficiency and high rate performance first.
A kind of preparation method of modified lithium-rich manganese-based anode material, including lithium-rich manganese-based presoma, lithium salts and doping is golden
Category compound carries out calcining and modified lithium-rich manganese-based anode material is obtained after being sufficiently mixed, it is characterised in that described before mixing
Lithium-rich manganese-based presoma first carries out 300～650 DEG C of insulations pretreatment of 2～6 hours.
Lithium-rich manganese-based presoma of the present invention is the general precursor powder in market.
Research finds that lithium-rich manganese-based presoma crystal structure after pretreatment is more complete, then doped metallic elements, energy
Enough coulombic efficiencies first for significantly mentioning positive electrode, reduce the migration of transition metal ions, and then reduce Lacking oxygen, alleviate
The structural rearrangement of positive electrode；The aluminium element of doping can suppress the Li under first circle high voltage2The effusion of O, improves the structure of material
It is stable, improve the transmission channel of Li, be conducive to improving coulomb effect and high rate performance first.
Preferably, the lithium salts is counted with the mol ratio of lithium-rich manganese-based presoma as 0.65～1 with lithium ion:1.It is more excellent
Choosing, the lithium salts is counted with the mol ratio of lithium-rich manganese-based presoma as 0.75 with lithium ion:1.
The present invention is sintered again the impurity that can realize element using the advanced row mixing of compound lithium salts, reduces first
Irreversible capacity, improves stability and high rate performance.Preferably, the lithium salts is the mixture of lithium carbonate and ruthenic acid lithium.
Based on lithium carbonate, appropriate RU ions can alleviate the obstruction of Mn ion pair lithium ion diffusion admittances to the lithium salts,
But ruthenic acid lithium should not be excessive, if Ru-O keys excessive after impurity can affect Li2MnO3Electro-chemical activity, so as to reduce
Capacity.Preferably, the lithium carbonate is 4～5.5 with the mol ratio of ruthenic acid lithium:1.More preferably, the lithium carbonate and ruthenic acid
The mol ratio of lithium is 4:1.
Preferably, the doping metals compound is AlF3、Al2O3、AlCl3In the mixture of one or more.More
For preferred, the doping metals compound is aluminum fluoride.
Preferably, the doping metals compound is 0.01～0.2 with the mol ratio of lithium-rich manganese-based presoma:1, more
It is preferred that, the doping metals compound is 0.1 with the mol ratio of lithium-rich manganese-based presoma:1.
Preferably, the pretreatment and calcining are carried out under air atmosphere, rate of air circulation is 10～15L/min.
Preferably, the calcining is, to 700～1000 DEG C, to be incubated 5～12h with the ramp of 2～10 DEG C/min.More
For preferred, the calcining is, to 750～850 DEG C, to be incubated 10～12h with the ramp of 5 DEG C/min.
Preferably, the pretreatment is to be incubated 3～6 hours to 400～600 DEG C with the ramp of 2～3 DEG C/min.
The present invention can improve the degree of crystallinity of material using pretreatment, make crystal structure more complete, while in mixed processes
Sample mix can be made evenly, doped chemical being dissolved in crystal structure evenly can be just made in sintering process.
After the preparation method of the present invention also terminates including calcining, product carries out being cooled to room temperature with the speed of 3 DEG C/min, mill
Broken sieving obtains final product the modified lithium-rich manganese-based anode material of the present invention.
Present invention also offers a kind of modified lithium-rich manganese-based anode material prepared by above-mentioned preparation method.The positive pole
The lithium-rich manganese base material that the coulombic efficiency first of material is more general rises 15～20 percentage points, can reach more than 92%,
Specific discharge capacity can reach 230mAh/g under 1C multiplying powers.
The beneficial effect that the present invention possesses：
(1) present invention increased the step to presoma pretreatment in the preparation technology of existing lithium-rich manganese-based anode material
Suddenly, make the crystal structure of presoma more complete, then the aluminium element that adulterates, the effect of coulomb first of positive electrode can be significantly improved
Rate.
(2) present invention introduces RU ions with lithium using compound lithium salts, alleviates the resistance of Mn ion pair lithium ion diffusion admittances
Hinder, be conducive to high rate performance to be lifted.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment one
By rich lithium manganese presoma NixCoyMnz(OH)2(x:y:Z=1:1:4) pre-processed in Muffle furnace, setting is protected
Temperature is 400 DEG C, and heating rate is 2 DEG C/min, and temperature retention time is 6h, and atmosphere is air, and air mass flow is 10L/min, is obtained
To pretreatment presoma；
By Li2CO3、Li2RuO3, step one process after rich lithium manganese presoma, alloy AlF3According to：0.55:0.1:1:
0.05 mol ratio is uniformly mixed, and the powder for obtaining is sintered in Muffle furnace, 750 DEG C of holding temperature, temperature retention time
12h, 5 DEG C/min of heating rate, atmosphere is air, and Ventilation Rate is 15L/min, and along with the furnace cooling after sintering, cooldown rate is 3
DEG C/min, and sinter is ground, sieve, obtain final product lithium-rich manganese-based anode material A.
Embodiment two
By rich lithium manganese presoma NixCoyMnz(OH)2(x:y:Z=1:1:4) pre-processed in Muffle furnace, setting is protected
Temperature is 600 DEG C, and heating rate is 3 DEG C/min, and temperature retention time is 3h, and atmosphere is air, and air mass flow is 15L/min, is obtained
To pretreatment presoma；
By Li2CO3、Li2RuO3, step one process after rich lithium manganese presoma, alloy AlF3According to：0.6:0.15:1:
0.1 mol ratio is uniformly mixed, and the powder for obtaining is sintered in Muffle furnace, 850 DEG C of holding temperature, temperature retention time
10h, 5 DEG C/min of heating rate, atmosphere is air, and Ventilation Rate is 15L/min, and along with the furnace cooling after sintering, cooldown rate is 3
DEG C/min, and sinter is ground, sieve, obtain final product lithium-rich manganese-based anode material B.
Comparative example one
By Li2CO3, not pretreated rich lithium manganese presoma NixCoyMnz(OH)2(x:y:Z=1:1:4), alloy
AlF3According to：0.6:0.15:1:0.1 mol ratio is uniformly mixed, and the powder for obtaining is sintered in Muffle furnace, insulation
850 DEG C of temperature, temperature retention time 10h, 5 DEG C/min of heating rate, atmosphere is air, and Ventilation Rate is 15L/min, with stove after sintering
Cooling, cooldown rate is 3 DEG C/min, and sinter is ground, and is sieved, and obtains final product lithium-rich manganese-based anode material C.
Detection example
Obtained three kinds of lithium-rich manganese-based anode materials are carried out into performance evaluation, as a result as shown in table 1.
Table 1
From upper table data, the 0.1C specific discharge capacities of the positive electrode that presoma is obtained after pretreatment substantially rise
Height, first circle irreversible capacity lowers, and so as to improve efficiency first, RU ions can alleviate Mn ion pair lithium ion diffusion admittances
Hinder, high rate performance is greatly improved.
Claims (10)
1. a kind of preparation method of modified lithium-rich manganese-based anode material, including by lithium-rich manganese-based presoma, lithium salts and doping metals
Compound carries out calcining and modified lithium-rich manganese-based anode material is obtained after being sufficiently mixed, it is characterised in that the richness before mixing
Lithium manganese base presoma first carries out 300～650 DEG C of insulations pretreatment of 2～6 hours.
2. the preparation method as described in right 1, it is characterised in that the lithium salts is rubbed in terms of lithium ion with lithium-rich manganese-based presoma
You are than being 0.65～1:1.
3. preparation method as claimed in claim 1 or 2, it is characterised in that the lithium salts is the mixing of lithium carbonate and ruthenic acid lithium
Thing.
4. preparation method as claimed in claim 3, it is characterised in that the lithium carbonate and the mol ratio of ruthenic acid lithium be 4～
5.5:1。
5. preparation method as claimed in claim 1, it is characterised in that the doping metals compound is AlF3、Al2O3、AlCl3
In the mixture of one or more.
6. the preparation method as described in claim 1 or 5, it is characterised in that the doping metals compound with it is lithium-rich manganese-based before
The mol ratio for driving body is 0.01～0.2:1.
7. preparation method as claimed in claim 1, it is characterised in that the pretreatment and calcining are entered under air atmosphere
OK, rate of air circulation is 10～15L/min.
8. preparation method as claimed in claim 7, it is characterised in that the calcining is with the ramp of 2～10 DEG C/min
To 700～1000 DEG C, 5～12h is incubated.
9. preparation method as claimed in claim 7, it is characterised in that the pretreatment is with the ramp of 2～3 DEG C/min
3～6 hours are incubated to 400～600 DEG C.
10. the modified lithium-rich manganese-based anode material that a kind of preparation method by described in any one of claim 1-9 is prepared.
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Cited By (7)
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| CN108400314A (en) * | 2018-05-08 | 2018-08-14 | 北京科技大学 | The method of modifying of high temperature induction yttrium fluoride grade doping lithium-rich manganese-based anode material |
| CN109411702A (en) * | 2017-08-15 | 2019-03-01 | 福建冠城瑞闽新能源科技有限公司 | A kind of preprocess method of lithium ion cell electrode |
| CN109671931A (en) * | 2018-12-13 | 2019-04-23 | 中国科学院宁波材料技术与工程研究所 | A kind of lithium ion anode composite material, preparation method and lithium ion battery |
| CN110797527A (en) * | 2019-10-23 | 2020-02-14 | 昆明理工大学 | Modified lithium-rich manganese-based oxide cathode material and preparation method thereof |
| CN113120972A (en) * | 2021-03-22 | 2021-07-16 | 安徽博石高科新材料股份有限公司 | Preparation method of lithium-rich manganese-based material |
| CN114883539A (en) * | 2022-03-31 | 2022-08-09 | 蜂巢能源科技股份有限公司 | Cobalt-free lithium-rich material, and preparation method and application thereof |
| CN116102069A (en) * | 2023-04-12 | 2023-05-12 | 天目湖先进储能技术研究院有限公司 | Preparation method and application of lithium-rich manganese-based material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109411702A (en) * | 2017-08-15 | 2019-03-01 | 福建冠城瑞闽新能源科技有限公司 | A kind of preprocess method of lithium ion cell electrode |
| CN108400314A (en) * | 2018-05-08 | 2018-08-14 | 北京科技大学 | The method of modifying of high temperature induction yttrium fluoride grade doping lithium-rich manganese-based anode material |
| CN108400314B (en) * | 2018-05-08 | 2021-06-18 | 北京科技大学 | Modification method for high-temperature induced yttrium fluoride gradient doped lithium-rich manganese-based positive electrode material |
| CN109671931A (en) * | 2018-12-13 | 2019-04-23 | 中国科学院宁波材料技术与工程研究所 | A kind of lithium ion anode composite material, preparation method and lithium ion battery |
| CN110797527A (en) * | 2019-10-23 | 2020-02-14 | 昆明理工大学 | Modified lithium-rich manganese-based oxide cathode material and preparation method thereof |
| CN113120972A (en) * | 2021-03-22 | 2021-07-16 | 安徽博石高科新材料股份有限公司 | Preparation method of lithium-rich manganese-based material |
| CN114883539A (en) * | 2022-03-31 | 2022-08-09 | 蜂巢能源科技股份有限公司 | Cobalt-free lithium-rich material, and preparation method and application thereof |
| CN114883539B (en) * | 2022-03-31 | 2024-01-30 | 蜂巢能源科技股份有限公司 | Cobalt-free lithium-rich material, preparation method and application thereof |
| CN116102069A (en) * | 2023-04-12 | 2023-05-12 | 天目湖先进储能技术研究院有限公司 | Preparation method and application of lithium-rich manganese-based material |
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