CN106654255A - Aluminum-doped and modified cathode material for high-capacity lithium ion batteries - Google Patents
Aluminum-doped and modified cathode material for high-capacity lithium ion batteries Download PDFInfo
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- CN106654255A CN106654255A CN201611175209.7A CN201611175209A CN106654255A CN 106654255 A CN106654255 A CN 106654255A CN 201611175209 A CN201611175209 A CN 201611175209A CN 106654255 A CN106654255 A CN 106654255A
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- 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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Abstract
The invention relates to an aluminum-doped and modified cathode material for high-capacity lithium ion batteries. The chemical general formula of the material is Li[Ni0.5Mn0.3Co0.2]1-xAlxO2, wherein x is equal to 0.03 to 0.12. By adopting a high-temperature solid-phase sintering method, a lithium source compound, a lithium battery cathode material precursor (NCM532) and an aluminum source compound are mixed, and ball milling is carried out in a ball grinding mill; pre-sintering at the temperature of 500 DEG C and high-temperature calcinations at the temperature of 850 DEG C are carried out in sequence on the obtained mixture, and then the cathode material is obtained. A synthetic method adopted in the invention is pollution-free to the environment, short in synthesis period, simple in technology and easy to operate, and the synthetic specimen material is high in uniformity and high in purity; a modified ternary stratified material provided by the invention is stable in structure and regular in morphology, and has good electrochemical performance; and the first discharge specific capacity under the test conditions of 0.2C multiplying power and 55 DEG C is not lower than 210 mAh/g.
Description
Technical field
The present invention relates to a kind of preparation of anode material for lithium ion battery with high power capacity of aluminum doping vario-property and study on the modification, category
In technical field of lithium ion.
Background technology
In recent years, with the proposition of green clean energy resource, lithium ion battery is increasingly subject to people's attention.Because it has
Higher specific capacity, higher charging/discharging voltage, environmentally safe and easy to carry and be widely used portable electronic
Equipment, small vehicles, military domain etc..
In numerous positive electrodes, LiCoO2Successful commercialization and it has been widely used, since LiCoO2Commercialization with
Come, due to its architectural study comparative maturity, high comprehensive performance, be widely used in portable digital product, military communication and set
Standby, small-sized electric vehicles etc., recently, there is good development prospect in big-and-middle-sized electric automobile.But, LiCoO2Itself
Also there are many shortcomings to govern its application in modern society, can not increasingly meet expectation of the people to lithium battery, a side
Face, expensive due to Co scarcity of resources, production cost more and more higher, and also Co toxicity is very big, to environment and human body all to making
Into injury；Second, although LiCoO2With good cycle performance and heat stability, but its capacity is very low, and actual capacity is only
50% of theoretical capacity or so can be given play to, it is impossible to meet pursuit of the people to height ratio capacity, therefore people actively find
One kind can replace LiCoO2Battery material.In recent years ternary material Li (Ni-Co-Mn) O2 had lithium nickelate, LiMn2O4, cobalt
, there is obvious trielement synergistic effect in the advantage of sour lithium three.Consider from capacity, cost, security standpoint, LiNi0.5Co0 2Mn0 3O2(NCM523) ternary material is undoubtedly most hopeful to substitute LiCoO2One of material.It has hypotoxicity, height ratio capacity, peace
The characteristics of good perfection.The theoretical specific capacity of ternary lithium battery is 277mAh/g, and the specific capacity that can be played in practical application is
180mAh/g, far above current LiCoO2(140mAh/g) paid close attention to, therefore greatly.
Although NCM523 has very high capacity advantage and energy density, in charge and discharge process, its crystal structure
Easily it is destroyed under high voltages, hinders the deintercalation of lithium ion so as to which capacity is substantially reduced, its cycle performance is deteriorated, high temperature
Lower this situation is more serious；Also, in material synthesis processes, easily there is cation mixing, hinder the transmission of lithium ion.
The content of the invention
Present invention aim to address existing high power capacity stratiform LiNi0.5Co0.2Mn0.3O2Positive electrode coulombic efficiency first
The problem of low, cycle performance and high rate performance difference, now provides a kind of height of element with electrochemical stability to layer structure
The method of modifying of capacity low-cost lithium ion battery anode, is adulterated using Al, forms Li [Ni0.5Co0.2Mn0.3]1-xAlx.O2
Positive electrode, improves its chemical property.
The present invention realizes that the technical scheme of above-mentioned purpose is as follows：
A kind of anode material for lithium-ion batteries of the high capacity low cost with a-NaFeO2 layer structures, is characterized in that：
The chemical general formula of the positive electrode is Li [Ni0.5Co0.2Mn0.3]1-xAlx.O2, wherein 0≤x≤0.12.
The preparation method of the above-mentioned layered lithium ion battery positive electrode with high capacity low cost, comprises the steps：
(1) stoichiometrically lithium salts, aluminium salt, 523 presomas are placed in into ball milling 2-5h in ball mill；
(2) mix powder obtained in (1) is placed in Muffle furnace and is calcined, programming rate is 3～8 DEG C/min,
After being warming up to 350～550 DEG C, in this temperature calcination 12～20 hours, intermediate product is obtained；
(3) after (2) intermediate product is cooled to room temperature, in grinding in ball grinder 2～5 hours, by the product pressure after grinding
It is again placed in Muffle furnace in fact, is calcined in oxygen-enriched atmosphere or air atmosphere, programming rate is 3～8 DEG C/min, is warming up to
750～950 DEG C, calcine 12～24 hours, be cooled to after room temperature and obtain described anode material for lithium-ion batteries Li
[Ni0.5Co0.2Mn0 3]1-xAlx.O2。
Further, the preparation side of the anode material for lithium-ion batteries of the described high capacity low cost with layer structure
Method, is characterized in that：The lithium salts, 523 presomas, the mol ratio of aluminium salt are 1.05: 1: x～1.15: 1.05: x+0.03, wherein
Cause damage to prevent lithium during high-temperature calcination from volatilizing, the amount excessive 5% of the material of lithium.
Further, the preparation side of the anode material for lithium-ion batteries of the described high capacity low cost with spinel structure
Method, is characterized in that：The lithium salts is one or more in lithium carbonate, lithium nitrate, Quilonorm (SKB), Lithium hydrate；The aluminium salt is
One or more in aluminium carbonate, aluminum nitrate and aluminium acetate；523 presoma is business-like one kind in the market.
Further, the preparation method of described high capacity low cost anode material for lithium-ion batteries, is characterized in that：Step
(3) in, the excess oxygen is that oxygen concentration is more than 21%.
Beneficial effects of the present invention：
(1) Li [Ni for being adulterated using Al and being formed0.5Co0.2Mn0 3]1-xAlx.O2Positive electrode granule is uniform, is stratiform knot
Structure, degree of crystallinity is high, and the stability of material is improved；(2) content of nickel is further reduced in the anode material for lithium-ion batteries of synthesis,
Cation mixing degree is reduced, and more reduces the pollution to environment；(3) present invention introduces doped chemical can effectively improve material
Circulation and high rate performance.
Description of the drawings
Fig. 1 is positive electrode Li [Ni0.5Mn0.3Co0.2]1-xAlxO2(x=0.015,0.03,0.06,0.12) is filled first
Discharge curve (55 DEG C of 2.5～4.6V, 0.2C, 25 DEG C of room temperature and high temperature).
Fig. 2 is positive electrode Li [Ni0 5Mn0 3Co0.2]1-xAlxO2Cyclic curve figure (x=0.03) (2.5～4.6V,
0.2C, room temperature).
Fig. 3 is positive electrode Li [Ni0.5Mn0.3Co0.2]1-xAlxO2(x=0.03) SEM figures.
Fig. 4 is positive electrode Li [Ni0.5Mn0.3Co0.2]1-xAlxO2The X-ray of (x=0.015,0.03,0.06,0.12) is spread out
Penetrate figure.
Specific embodiment
Technical scheme is described further with reference to embodiment.
Embodiment 1
(1) by presoma, lithium carbonate and aluminum nitrate in molar ratio for 0.985: 0.525: 0.015 (wherein in order to make up height
5%) a small amount of volatilization of lithium under warm environment, lithium carbonate excessively weighs raw material, after mix homogeneously, uses ball mill grinding 3h；
(2) mixture that step (1) is obtained is placed in Muffle furnace and is calcined, programming rate is 5 DEG C/min, is warming up to
500 DEG C, in this temperature calcination 12～20 hours, obtain intermediate product；
(3) grind 0.5 hour in mortar machine after intermediate product is cooled to room temperature, after the presoma compacting after grinding
In being placed in Muffle furnace, calcined under in excess oxygen or air atmosphere, programming rate is 5 DEG C/min, is warming up to 850
DEG C, calcine 12～24 hours, it is cooled to after room temperature and obtains described anode material for lithium-ion batteries Li
[Ni0.5Co0.2Mn0.3]1-xAlx.O2(x=0.015).
The positive electrode that embodiment 1 is obtained is assembled into into CR2032 types button cell carries out charge and discharge cycles test.Using
Coating method prepares electrode, and with METHYLPYRROLIDONE (NMP) as solvent, in mass ratio 80: 12: 8 positive pole material is weighed respectively
Material, acetylene black and poly- inclined tetrafluoroethene (PVDF), after ground and mixed is uniform, are coated on pretreated aluminium foil, are put into vacuum and do
In dry case, after being dried 2-4 days at 80 DEG C, with microtome positive plate is obtained.Simple metal lithium piece is made to electrode, polypropylene microporous
Film Celgard 2325 is barrier film, the mixed solution of LB315 [m (DMC): m (EMC): m (EC)=1: 1: 1] as electrolyte,
Full of (H in argon glove box2O content ＜ 1ppm) it is assembled into simulated battery.Entered with LAND battery test system button type batteries
Row constant current charge-discharge is tested；In 2.5～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 0.2C, room temperature (25 DEG C)
First discharge specific capacity is 194.1mAh/g, and first coulombic efficiency is 87.7%, and capability retention is after 50 charge and discharge cycles
90.3%；In 2.5～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 5C, room temperature first discharge specific capacity is
133.9mAh/g。
Embodiment 2
(1) by presoma, lithium carbonate and aluminum nitrate in molar ratio for 0.970: 0.525: 0.03 (wherein in order to make up high temperature
5%) a small amount of volatilization of lithium under environment, lithium carbonate excessively weighs raw material, after mix homogeneously, uses ball mill grinding 3h；
(2) mixture that step (1) is obtained is placed in Muffle furnace and is calcined, programming rate is 5 DEG C/min, is warming up to
500 DEG C, in this temperature calcination 12～20 hours, obtain intermediate product；
(3) grind 0.5 hour in mortar machine after intermediate product is cooled to room temperature, after the presoma compacting after grinding
In being placed in Muffle furnace, calcined under in excess oxygen or air atmosphere, programming rate is 5 DEG C/min, is warming up to 850
DEG C, calcine 12～24 hours, it is cooled to after room temperature and obtains described anode material for lithium-ion batteries Li
[Ni0.5Co0.2Mn0.3]1-xAlxO2(x=0.03).
The positive electrode that embodiment 2 is obtained is assembled into into CR2032 types button cell carries out charge and discharge cycles test.Using
Coating method prepares electrode, and with METHYLPYRROLIDONE (NMP) as solvent, in mass ratio 80: 12: 8 positive pole material is weighed respectively
Material, acetylene black and poly- inclined tetrafluoroethene (PVDF), after ground and mixed is uniform, are coated on pretreated aluminium foil, are put into vacuum and do
In dry case, after being dried 2-4 days at 80 DEG C, with microtome positive plate is obtained.Simple metal lithium piece is made to electrode, polypropylene microporous
Film Celgard 2325 is barrier film, the mixed solution of LB315 [m (DMC): m (EMC): m (EC)=1: 1: 1] as electrolyte,
Full of (H in argon glove box2O content ＜ 1ppm) it is assembled into simulated battery.Entered with LAND battery test system button type batteries
Row constant current charge-discharge is tested；In 2.5～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 0.2C, room temperature is put first
Electric specific capacity is 196.0mAh/g, and first coulombic efficiency is 91.1%, and capability retention can be higher than after 50 charge and discharge cycles
94.3%；In 2.6～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 0.2C, 55 DEG C of first discharge specific capacities are
199.5mAh/g, first coulombic efficiency is 89.6%.
Embodiment 3
(1) by presoma, lithium carbonate and aluminum nitrate in molar ratio for 0.940: 0.525: 0.06 (wherein in order to make up high temperature
5%) a small amount of volatilization of lithium under environment, lithium carbonate excessively weighs raw material, after mix homogeneously, uses ball mill grinding 3h；
(2) mixture that step (1) is obtained is placed in Muffle furnace and is calcined, programming rate is 5 DEG C/min, is warming up to
500 DEG C, in this temperature calcination 12～20 hours, obtain intermediate product；
(3) grind 0.5 hour in mortar machine after intermediate product is cooled to room temperature, after the presoma compacting after grinding
In being placed in Muffle furnace, calcined under in excess oxygen or air atmosphere, programming rate is 5 DEG C/min, is warming up to 850
DEG C, calcine 12～24 hours, it is cooled to after room temperature and obtains described anode material for lithium-ion batteries Li
[Ni0.5Co0.2Mn0.3]1-xAlx.O2(x=0.06).
The positive electrode that embodiment 3 is obtained is assembled into into CR2032 types button cell carries out charge and discharge cycles test.Using
Coating method prepares electrode, and with METHYLPYRROLIDONE (NMP) as solvent, in mass ratio 80: 12: 8 positive pole material is weighed respectively
Material, acetylene black and poly- inclined tetrafluoroethene (PVDF), after ground and mixed is uniform, are coated on pretreated aluminium foil, are put into vacuum and do
In dry case, after being dried 12-24 hours at 80 DEG C, with microtome positive plate is obtained.Simple metal lithium piece is made to electrode, polypropylene
Microporous membrane Celgard 2325 is barrier film, and the mixed solution of LB315 [m (DMC): m (EMC): m (EC)=1: 1: 1] is used as electrolysis
Liquid, full of (H in argon glove box2O content ＜ 1ppm) it is assembled into simulated battery.With LAND battery test systems button type electricity
Pond carries out constant current charge-discharge test；In 2.5～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 0.2C, room temperature is first
Secondary specific discharge capacity is 180.8mAh/g, and first coulombic efficiency is 85.6%, and capability retention can be high after 50 charge and discharge cycles
In 90.5%.
Embodiment 4
(1) by presoma, lithium carbonate and aluminum nitrate in molar ratio for 0.880: 0.525: 0.12 (wherein in order to make up high temperature
5%) a small amount of volatilization of lithium under environment, lithium carbonate excessively weighs raw material, after mix homogeneously, uses ball mill grinding 3h；
(2) mixture that step (1) is obtained is placed in Muffle furnace and is calcined, programming rate is 5 DEG C/min, is warming up to
500 DEG C, in this temperature calcination 12～20 hours, obtain intermediate product；
(3) grind 0.5 hour in mortar machine after intermediate product is cooled to room temperature, after the presoma compacting after grinding
In being placed in Muffle furnace, calcined under in excess oxygen or air atmosphere, programming rate is 5 DEG C/min, is warming up to 850
DEG C, calcine 12～24 hours, it is cooled to after room temperature and obtains described anode material for lithium-ion batteries Li [Ni0 5Co0.2Mn0.3]1-xAlx.O2(x=0.12).
The positive electrode that embodiment 4 is obtained is assembled into into CR2032 types button cell carries out charge and discharge cycles test.Using
Coating method prepares electrode, and with METHYLPYRROLIDONE (NMP) as solvent, in mass ratio 80: 12: 8 positive pole material is weighed respectively
Material, acetylene black and poly- inclined tetrafluoroethene (PVDF), after ground and mixed is uniform, are coated on pretreated aluminium foil, are put into vacuum and do
In dry case, 12-24 hours are dried at 80 DEG C, with microtome positive plate is obtained.Simple metal lithium piece is made to electrode, and polypropylene is micro-
Pore membrane Celgard 2325 be barrier film, the mixed solution of LB315 [m (DMC): m (EMC): m (EC)=1: 1: 1] as electrolyte,
Full of (H in argon glove box2O content ＜ 1ppm) it is assembled into simulated battery.With LAND battery test system button type batteries
Carry out constant current charge-discharge test；In 2.5～4.6V of test voltage, under the conditions of testing the discharge and recharge of electric current 0.2C, room temperature is first
Specific discharge capacity is 171.6mAh/g, and first coulombic efficiency is 81.2%, and capability retention can be higher than after 50 charge and discharge cycles
89.1%.
Claims (7)
1. a kind of anode material for lithium ion battery with high power capacity of aluminum doping vario-property, is characterized in that：The chemistry of the positive electrode leads to
Formula is Li [Ni0.5Co0.2Mn0.3]1-xAlx.O2, wherein 0≤x≤0.12.
2. a kind of anode material for lithium ion battery with high power capacity of aluminum doping vario-property, is characterized in that, using following processing step：
(1) stoichiometrically lithium salts, aluminium salt, 523 presomas are placed in into 2～5h of ball milling in ball mill；
(2) mix powder obtained in (1) is placed in Muffle furnace and is calcined, programming rate is 3～8 DEG C/min, is heated up
To after 350～550 DEG C, in this temperature calcination 12～20 hours, intermediate product is obtained；
(3) after (2) intermediate product is cooled to room temperature, in grinding in ball grinder 2～5 hours, the product after grinding is compacted again
It is secondary to be placed in Muffle furnace, to be calcined in oxygen-enriched atmosphere or air atmosphere, programming rate is 3～8 DEG C/min, is warming up to 750
～950 DEG C, calcine 12～24 hours, be cooled to after room temperature and obtain described anode material for lithium-ion batteries Li
[Ni0.5Co0.2Mn0.3]1-xAlx.O2。
3. there is as claimed in claim 2 the lithium ion cell positive of the element doping high capacity low cost of electrochemical stability
The preparation method of material, is characterized in that：The n (lithium salts): n (532 presoma): n (Al salt)=1.05: 1: x～1.10: 1.05
: the excess of x+0.03, wherein lithium be in order to prevent high-temperature calcination under lithium volatilization loss, the amount of the material of lithium excessive 3～7%.
4. there is as claimed in claim 2 the lithium ion cell positive of the element doping high capacity low cost of electrochemical stability
The preparation method of material, is characterized in that：The lithium salts is the one kind or many in lithium carbonate, lithium nitrate, Quilonorm (SKB), Lithium hydrate
Kind.
5. there is as claimed in claim 2 the lithium ion cell positive of the element doping high capacity low cost of electrochemical stability
The preparation method of material, is characterized in that：The aluminium salt is one or more in aluminium carbonate, aluminum nitrate and aluminium acetate.
6. the preparation method of anode material for lithium-ion batteries as claimed in claim 2, is characterized in that：523 presoma is
A kind of business-like persursor material.
7. the preparation method of high capacity low cost anode material for lithium-ion batteries as claimed in claim 2, is characterized in that：Step
(3) in, the excess oxygen is that oxygen concentration is more than 21%.
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| CN107959002A (en) * | 2017-10-11 | 2018-04-24 | 宁波维科新能源科技有限公司 | A kind of lithium ion battery |
| CN108011144A (en) * | 2017-10-31 | 2018-05-08 | 合肥国轩高科动力能源有限公司 | A kind of recovery processing technique of ternary cathode material of lithium ion battery |
| CN113161534A (en) * | 2021-04-15 | 2021-07-23 | 江南大学 | Co-doped modified lithium ion battery ternary cathode material and preparation method thereof |
| CN113264560A (en) * | 2021-05-17 | 2021-08-17 | 青海师范大学 | Double-coated NCM811 cathode material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107959002A (en) * | 2017-10-11 | 2018-04-24 | 宁波维科新能源科技有限公司 | A kind of lithium ion battery |
| CN108011144A (en) * | 2017-10-31 | 2018-05-08 | 合肥国轩高科动力能源有限公司 | A kind of recovery processing technique of ternary cathode material of lithium ion battery |
| CN113161534A (en) * | 2021-04-15 | 2021-07-23 | 江南大学 | Co-doped modified lithium ion battery ternary cathode material and preparation method thereof |
| CN113264560A (en) * | 2021-05-17 | 2021-08-17 | 青海师范大学 | Double-coated NCM811 cathode material and preparation method thereof |
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