CN102437323B - Anode material of lithium ion battery and preparation method thereof - Google Patents
Anode material of lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an anode material of a lithium ion battery and a preparation method thereof. The preparation method is characterized by adopting the following processing steps that: (1) lithium salt, manganese salt, nickel salt, cobalt salt and M salt are dissolved in deionized water in a stirring condition, a complexing agent is added into the deionized water, and the pH value is regulated; (2) a mixed solution obtained in the step (1) is evaporated at a constant temperature, and sol is obtained; (3) the sol is dried, and xerogel is obtained; (4) the xerogel is calcined, and a precursor is obtained; and (5) the precursor is ground after being cooled to a room temperature, the ground precursor is calcined, and the anode material Li[LiaMnbNicCodMe]O2 of the lithium ion battery is obtained after the ground precursor is cooled to a room temperature. The anode material of the lithium ion battery, which is synthesized by adopting the preparation method, has low cobalt content, so the pollution to the environment is decreased while the production cost is reduced; and the anode material synthesized after being compacted has the advantages of high specific capacity, good cycle performance, simple process, low cost, and the like.
Description
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries and preparation method thereof, belong to technical field of lithium ion.
Background technology
Along with the demand in the extensive use of portable mobile electronic product and the rise of pure EHV electric and hybrid vehicle and the energy storage such as wind energy, solar energy field, in the urgent need to developing the lithium ion battery of height ratio capacity, low production cost.In lithium ion battery, the performance of positive electrode and cost play decisive role again to the overall performance of lithium battery and price.Therefore, the anode material for lithium-ion batteries developing high-performance and low production cost becomes the key point improving performance of lithium ion battery.Present stage, commercial anode material for lithium-ion batteries mainly contained LiCoO
2, LiMn
2o
4, LiFePO
4, and LiCo
1/3mn
1/3ni
1/3o
2deng.Spinel-type LiMn
2o
4theoretical capacity is 148mAh/g, and actual discharge capacity is about about 120mAh/g, simultaneously in high temperature environments because Jahn-Teller distortion effect causes capacity attenuation very fast, constrains the development of this material to a certain extent.Stratiform LiCoO
2theoretical specific capacity is about 274mAh/g, and reality high-volume capacity can reach about 130 ~ 150mAh/g, and the price of Co is higher and have toxicity, and this material will progressively be substituted.Stratiform LiCo
1/3mn
1/3ni
1/3o
2theoretical specific capacity is about 278mAh/g, and reality high-volume capacity can reach 190 ~ 200mAh/g.LiFePO
4theoretical specific capacity is about 170mAh/g, and reality high-volume capacity can reach about 160mAh/g; But this material preparation condition is harsh and cryogenic property is bad, and theoretical capacity is not high, can room for promotion very limited.The lithium-rich anode material of high power capacity and stable circulation causes extensive concern in recent years, and lithium-rich anode material is Li mainly
2mnO
3with stratified material LiMO
2the solid solution that (M is Ni, Co, Fe or Cr) is formed, has α-NaFeO
2layer structure.
At present in existing report, the method for synthesis lithium-rich anode material is more with coprecipitation, but coprecipitation complex process in process of production, consume raw material more, should not as industrialization large-scale mass production.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of anode material for lithium-ion batteries and preparation method thereof, this anode material for lithium-ion batteries has height ratio capacity, good cycle.
According to technical scheme provided by the invention, described anode material for lithium-ion batteries, feature is: the chemical general formula of described positive electrode is Li [Li
amn
bni
cco
dm
e] O
2, wherein 0.05≤a≤0.25,0.4≤b≤0.8,0.03≤c, d, e≤0.15, and a+b+c+d+e=1, M are one or more in Al, Cr, Ti, Mg.
The present invention also protects a kind of preparation method of anode material for lithium-ion batteries, and feature is, adopts following processing step:
(1) lithium salts, manganese salt, nickel salt, cobalt salt and M salt are dissolved in deionized water under agitation, the total concentration of lithium salts, manganese salt, nickel salt, cobalt salt and M salt is 0.2 ~ 6mol/L, mixing speed is 90 ~ 180 revs/min, and mixing time is 10 ~ 60 minutes; Add the complexing agent aqueous solution that concentration is 0.5 ~ 3mol/L again, then low whipping speed be drip under the condition of 90 ~ 180 revs/min mass percentage concentration be 15 ~ 28% ammonia spirit adjust ph be 6 ~ 8; The mol ratio of described lithium salts, manganese salt, nickel salt, cobalt salt and M salt to be 1 ~ 1.25: 0.4 ~ 0.8: 0.03 ~ 0.15: 0.03 ~ 0.15: 0.03 ~ 0.15, M salt be in aluminium salt, chromic salts, titanium salt, magnesium salts one or more; The total amount of described manganese salt, nickel salt, cobalt salt and M salt and the mol ratio of complexing agent are 1: 0.9 ~ 1.2;
(2) under the condition of 50 ~ 90 DEG C, carry out evaporation at constant temperature 4 ~ 10 hours under the condition of the mixed solution low whipping speed 200 ~ 500 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 80 ~ 180 DEG C of conditions dry 4 ~ 12 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 1 ~ 5 DEG C/min, is warming up to 200 ~ 600 DEG C, calcines 2 ~ 20 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 0.5 ~ 2 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 3 ~ 8 DEG C/min, be warming up to 700 ~ 1100 DEG C, calcine 3 ~ 30 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
amn
bni
cco
dm
e] O
2.
Described lithium salts is one or more in lithium carbonate, lithium nitrate, lithium acetate, lithium hydroxide; Described manganese salt is one or more in manganese sulfate, manganese nitrate, manganese acetate; Described nickel salt is one or more in nickelous sulfate, nickel nitrate, nickel acetate; Described cobalt salt is one or more in cobaltous sulfate, cobalt nitrate, cobalt acetate; Described aluminium salt is one or more in aluminum sulfate, aluminum nitrate and lithium acetate; Described chromic salts is one or more in chromium sulfate, chromic nitrate and chromium acetate; Described titanium salt is one or more in titanium sulfate, Titanium Nitrate, acetic acid titanium; Described magnesium salts is one or more in magnesium nitrate, magnesium sulfate, magnesium acetate.
Described complexing agent aqueous solution is one or more the aqueous solution in citric acid, tartaric acid, ethylene glycol.
In step (5), described excess oxygen is that oxygen concentration is greater than 21%.
In preparation method of the present invention, pH value is adjusted to 7 for neutral, without acid and alkali corrosion, can increase duration of service, and need not wash; The content of the anode material for lithium-ion batteries cobalt of synthesis reduces further, more decrease the pollution to environment, and the positive electrode specific capacity be synthesized after overcompaction is high, good cycle, technique are simple and cost is low while reducing production cost.
Accompanying drawing explanation
Fig. 1 is positive electrode Li [Li
0.2mn
0.54ni
0.13co
0.08al
0.05] O
2xRD figure.
Fig. 2 is positive electrode Li [Li
0.2mn
0.54ni
0.13co
0.08al
0.05] O
2sEM figure.
Fig. 3 is positive electrode Li [Li
0.2mn
0.54ni
0.13co
0.08cr
0.05] O
2first charge-discharge curve (2.0 ~ 4.8V, 0.1C, room temperature).
The abscissa of Fig. 1 is sweep limits 2 θ (10 ~ 90 °), and ordinate is the intensity at peak.The times magnification of Fig. 2 is 50000 times.The abscissa of Fig. 3 is specific capacity, mAh/g, and ordinate is voltage, and unit is that in V, Fig. 3, curve A refers to charging curve, and curve B refers to discharge curve.
Embodiment
Below in conjunction with concrete drawings and Examples, the invention will be further described.
Embodiment one: a kind of preparation method of anode material for lithium-ion batteries, adopts following processing step:
(1) be 1.236: 0.54: 0.13: 0.08: 0.05 in molar ratio by lithium nitrate, manganese acetate, nickel nitrate, cobalt nitrate and aluminum nitrate (wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium nitrate excessive 3%) mixing, be dissolved under agitation in deionized water, the total concentration of lithium nitrate, manganese acetate, nickel nitrate, cobalt nitrate and aluminum nitrate is 0.2mol/L, mixing speed is 90 revs/min, and mixing time is 30 minutes; Add the aqueous citric acid solution that concentration is 0.5mol/L again, then low whipping speed be drip under the condition of 90 revs/min mass percentage concentration be 15% ammonia spirit adjust ph be 6; The total amount of described manganese acetate, nickel nitrate, cobalt nitrate and aluminum nitrate and the mol ratio of citric acid are 1: 0.9;
(2) under the condition of 50 DEG C, carry out evaporation at constant temperature 10 hours under the condition of the mixed solution low whipping speed 200 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 80 DEG C of conditions dry 12 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 1 DEG C/min, is warming up to 200 DEG C, calcines 20 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 0.5 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 3 DEG C/min, be warming up to 700 DEG C, calcine 30 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.54ni
0.13co
0.08al
0.05] O
2.
The positive electrode that embodiment one obtains is assembled into CR2032 type button cell and carries out charge and discharge cycles test.Coating method is adopted to prepare electrode, with METHYLPYRROLIDONE (NMP) for solvent, respectively take positive electrode, acetylene black and poly-inclined tetrafluoroethene (PVDF) at 80: 12: 8 in mass ratio, after ground and mixed is even, be coated on pretreated aluminium foil, put into vacuum drying chamber and obtain positive plate 80 DEG C of dryings.Pure metal lithium sheet makes negative pole, microporous polypropylene membrane Celgard 2325 is barrier film, the mixed solution of LB315 [m (DMC): m (EMC): m (EC)=1: 1: 1] as electrolyte, being full of (H in argon gas glove box
2o content < 1ppm) be assembled into simulated battery.Constant current cycle charge discharge electrical testing is carried out with LAND battery test system button type battery; Under the discharge and recharge condition of test voltage 2.0 ~ 4.8V, 0.1C, room temperature specific discharge capacity is 262.7mAh/g, and after 60 charge and discharge cycles, capability retention can higher than 92%.
Embodiment two: a kind of preparation method of anode material for lithium-ion batteries, adopts following processing step:
(1) be 1.248: 0.54: 0.13: 0.08: 0.05 in molar ratio by lithium hydroxide, manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate (wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium hydroxide excessive 4%) mixing, be dissolved under agitation in deionized water, the total concentration of lithium hydroxide, manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate is 1mol/L, mixing speed is 100 revs/min, and mixing time is 25 minutes; Add the aqueous citric acid solution that concentration is 1mol/L again, then low whipping speed be drip under the condition of 100 revs/min mass percentage concentration be 16% ammonia spirit adjust ph be 7; The total amount of described manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate and the mol ratio of citric acid are 1: 1;
(2) under the condition of 60 DEG C, carry out evaporation at constant temperature 8 hours under the condition of the mixed solution low whipping speed 300 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 90 DEG C of conditions dry 10 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 2 DEG C/min, is warming up to 300 DEG C, calcines 18 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 0.6 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 4 DEG C/min, be warming up to 800 DEG C, calcine 25 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.54ni
0.13co
0.08cr
0.05] O
2.
The positive electrode that embodiment two obtains is assembled into CR2032 type button cell and carries out charge and discharge cycles test.Constant current cycle charge discharge electrical testing is carried out with LAND battery test system button type battery; Under the discharge and recharge condition of test voltage 2.0 ~ 4.8V, 0.1C, room temperature specific discharge capacity is 274.9mAh/g, and after 60 charge and discharge cycles, capability retention can reach 91.5%.
Embodiment three: a kind of preparation method of anode material for lithium-ion batteries, adopts following processing step:
(1) be 1.242: 0.55: 0.1: 0.1: 0.05 in molar ratio by lithium acetate, manganese nitrate, nickel nitrate, cobalt nitrate and ferric nitrate (wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium salts excessive 3.5%) mixing, be dissolved under agitation in deionized water, the total concentration of lithium acetate, manganese nitrate, nickel nitrate, cobalt nitrate and ferric nitrate is 2mol/L, mixing speed is 110 revs/min, and mixing time is 20 minutes; Add the aqueous citric acid solution that concentration is 1.5mol/L again, then low whipping speed be drip under the condition of 110 revs/min mass percentage concentration be 17% ammonia spirit adjust ph be 6.5; The total amount of described manganese nitrate, nickel nitrate, cobalt nitrate and ferric nitrate and the mol ratio of citric acid are 1: 1.1;
(2) under the condition of 70 DEG C, carry out evaporation at constant temperature 6 hours under the condition of the mixed solution low whipping speed 400 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 100 DEG C of conditions dry 8 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 3 DEG C/min, is warming up to 400 DEG C, calcines 16 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 0.8 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 5 DEG C/min, be warming up to 900 DEG C, calcine 20 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.55ni
0.1co
0.1fe
0.05] O
2.
The positive electrode that embodiment three obtains is assembled into CR2032 type button cell and carries out charge and discharge cycles test.Constant current cycle charge discharge electrical testing is carried out with LAND battery test system button type battery; Under the discharge and recharge condition of test voltage 2.0 ~ 4.8V, 0.1C, room temperature specific discharge capacity is 231.9mAh/g, and after 60 charge and discharge cycles, capability retention can reach 96%.
Embodiment four: a kind of preparation method of anode material for lithium-ion batteries, adopts following processing step:
(1) be 1.2432: 0.54: 0.13: 0.03: 0.1 in molar ratio by lithium nitrate, manganese acetate, nickel nitrate, cobalt acetate and aluminum nitrate (wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium salts excessive 3.6%) mixing, be dissolved under agitation in deionized water, the total concentration of lithium nitrate, manganese acetate, nickel nitrate, cobalt acetate and aluminum nitrate is 3mol/L, mixing speed is 120 revs/min, and mixing time is 15 minutes; Add the aqueous citric acid solution that concentration is 2mol/L again, then low whipping speed be drip under the condition of 120 revs/min mass percentage concentration be 18% ammonia spirit adjust ph be 7.5; The total amount of described manganese acetate, nickel nitrate, cobalt acetate and aluminum nitrate and the mol ratio of citric acid are 1: 1;
(2) under the condition of 80 DEG C, carry out evaporation at constant temperature 5 hours under the condition of the mixed solution low whipping speed 450 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 120 DEG C of conditions dry 6 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 4 DEG C/min, is warming up to 500 DEG C, calcines 15 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 1 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 6 DEG C/min, be warming up to 1000 DEG C, calcine 15 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.54ni
0.13co
0.03al
0.1] O
2.
The positive electrode that embodiment four obtains is assembled into CR2032 type button cell and carries out charge and discharge cycles test.Constant current cycle charge discharge electrical testing is carried out with LAND battery test system button type battery; Under the discharge and recharge condition of test voltage 2.0 ~ 4.8V, 0.1C, room temperature specific discharge capacity is 248.6mAh/g, and after 60 charge and discharge cycles, capability retention can reach 92.3%.
Embodiment five: a kind of preparation method of anode material for lithium-ion batteries, adopts following processing step:
(1) be 1.2444: 0.54: 0.13: 0.08: 0.05 in molar ratio by lithium carbonate, manganese acetate, nickelous sulfate, cobaltous sulfate and magnesium sulfate (wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium salts excessive 3.7%) mixing, be dissolved under agitation in deionized water, the total concentration of lithium carbonate, manganese acetate, nickelous sulfate, cobaltous sulfate and magnesium sulfate is 6mol/L, mixing speed is 180 revs/min, and mixing time is 10 minutes; Add the aqueous citric acid solution that concentration is 3mol/L again, then low whipping speed be drip under the condition of 180 revs/min mass percentage concentration be 28% ammonia spirit adjust ph be 8; The total amount of described manganese acetate, nickelous sulfate, cobaltous sulfate and magnesium sulfate and the mol ratio of citric acid are 1: 1.2;
(2) under the condition of 90 DEG C, carry out evaporation at constant temperature 4 hours under the condition of the mixed solution low whipping speed 500 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 180 DEG C of conditions dry 4 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 5 DEG C/min, is warming up to 600 DEG C, calcines 2 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 2 hours, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 8 DEG C/min, be warming up to 1100 DEG C, calcine 3 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.54ni
0.13co
0.08mg
0.05] O
2.
The positive electrode that embodiment five obtains is assembled into CR2032 type button cell and carries out charge and discharge cycles test.Constant current cycle charge discharge electrical testing is carried out with LAND battery test system button type battery; Under the discharge and recharge condition of test voltage 2.0 ~ 4.8V, 0.1C, room temperature specific discharge capacity is 254.4mAh/g, and after 60 charge and discharge cycles, capability retention can reach 91.6%.
Claims (1)
1. a preparation method for anode material for lithium-ion batteries, is characterized in that adopting following steps:
(1) by lithium hydroxide, manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate be 1.248: 0.54: 0.13: 0.08: 0.05 mixing in molar ratio, wherein in order to prevent a small amount of volatilization of lithium under hot environment, lithium hydroxide excessive 4%; Be dissolved under agitation in deionized water, the total concentration of lithium hydroxide, manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate is 1mol/L, and mixing speed is 100 revs/min, and mixing time is 25 minutes; Add the aqueous citric acid solution that concentration is 1mol/L again, then low whipping speed be drip under the condition of 100 revs/min mass percentage concentration be 16% ammonia spirit adjust ph be 7; The total amount of described manganese acetate, nickel nitrate, cobalt nitrate and chromic nitrate and the mol ratio of citric acid are 1:1;
(2) under the condition of 60 DEG C, carry out evaporation at constant temperature 8 hours under the condition of the mixed solution low whipping speed 300 revs/min that step (1) obtains, obtain colloidal sol;
(3) colloidal sol is placed in air dry oven under 90 DEG C of conditions dry 10 hours, to evaporate expeling moisture, obtains xerogel;
(4) xerogel is placed in Muffle furnace to calcine, programming rate is 2 DEG C/min, is warming up to 300 DEG C, calcines 18 hours, obtains presoma;
(5) presoma is cooled to after room temperature grinding in ball grinder 0.6 hour, presoma compacting after grinding is placed in Muffle furnace, in excess oxygen or air atmosphere under calcine, programming rate is 4 DEG C/min, be warming up to 800 DEG C, calcine 25 hours, after being cooled to room temperature, namely obtain described anode material for lithium-ion batteries Li [Li
0.2mn
0.54ni
0.13co
0.08cr
0.05] O
2.
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| US11233239B2 (en) | 2020-03-27 | 2022-01-25 | Board Of Regents, The University Of Texas System | Low-cobalt and cobalt-free, high-energy cathode materials for lithium batteries |
| CN112174214A (en) * | 2020-08-17 | 2021-01-05 | 安徽绿沃循环能源科技有限公司 | Lithium battery LiMn2O4Preparation method of positive electrode material |
| CN112786876A (en) * | 2021-03-02 | 2021-05-11 | 昆明理工大学 | Preparation method of lithium-rich lithium battery cathode material with single crystal structure |
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| CN114180635A (en) * | 2021-10-28 | 2022-03-15 | 厦门理工学院 | Single-crystal lithium manganate positive electrode material, preparation method and application |
| CN114497533A (en) * | 2022-01-27 | 2022-05-13 | 西南石油大学 | In-situ spinel modified low-cobalt spherical lithium-rich manganese-based positive electrode material and preparation method thereof |
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