CN107565122A - A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material - Google Patents
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material Download PDFInfo
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- CN107565122A CN107565122A CN201710666346.9A CN201710666346A CN107565122A CN 107565122 A CN107565122 A CN 107565122A CN 201710666346 A CN201710666346 A CN 201710666346A CN 107565122 A CN107565122 A CN 107565122A
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Abstract
The invention belongs to technical field of lithium ion, specially a kind of preparation method of doping type nickel-cobalt lithium manganate cathode material.The chemical formula of the nickle cobalt lithium manganate is Li (NiaCobMn1‑a‑b)1‑xNbxO2, wherein 0≤x≤0.1,0.3≤a≤0.8,0.05≤b≤0.4.The concrete technology that it is prepared is as follows：By nickel cobalt manganese presoma, niobium source and lithium salts ball milling mixing according to a certain percentage, by pre-burning, secondary ball milling, in high-temperature atmosphere furnace the operation such as calcining obtain doping type nickel-cobalt lithium manganate cathode material.Preparation method flow involved in the present invention is simple, it is easy to accomplish industrialization, the doping type nickel-cobalt lithium manganate cathode material of gained have excellent cyclical stability, solve the capacity attenuation behavior of nickel-cobalt lithium manganate cathode material under high voltages under high voltages.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of system of doping type nickel-cobalt lithium manganate cathode material
Preparation Method.
Background technology
Lithium ion battery is widely used to the electronic products such as portable computer as a kind of important energy storage device.Traditional
Lithium ion battery mainly selects cobalt acid lithium as positive electrode, but because cobalt acid lithium is expensive, the more low reason of energy density,
Therefore there is an urgent need to find a kind of positive electrode of high-energy-density.Studying more positive electrode at present mainly has layer structure
Tertiary cathode material, lithium-rich manganese base material, LiMn2O4 and LiFePO4 etc., wherein, nickle cobalt lithium manganate tertiary cathode material
Because its high energy density receives the favor of people, particularly high Ni-based ternary material, its specific capacity can reach 200
mAh/g.The chemical formula of the nickle cobalt lithium manganate is Li (NiaCobMn1-a-b)1-xNbxO2, wherein 0≤x≤0.1,0.3≤a≤
0.8,0.05 ≤ b ≤ 0.4.But to face structural stability poor for nickel-cobalt lithium manganate cathode material, during high voltage cycle
The problems such as capacity rapid decay, thus limit its application in business.Be directed to that nickel-cobalt lithium manganate material faced asks
Topic, mainly has two kinds of methods to be improved, i.e. ion doping and Surface coating at present.Ion doping is as a kind of effective means
The structural stability of material of main part can be improved, particularly under high voltages, the doping of a small amount of inert ion can play stabilization
The purpose of nickel-cobalt lithium manganate material layer structure, thus the cyclical stability of such material under high voltages can be improved.Tradition
Ion doping realize that both approaches are cumbersome, expensive often through collosol and gel or the method for co-precipitation, because
This exploitation is a kind of simple to operate, and cheap doping method has very important significance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, to solve material
Under high voltages the problem of cyclical stability difference.
To achieve the above object, technical scheme is as follows：
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, comprises the following steps：
（1）By nickel cobalt manganese presoma, niobium source and the lithium salts ball milling mixing in planetary ball mill；
（2）The pre-burning in Muffle furnace by the mixture of gained；
（3）By the material after pre-burning, secondary ball milling mixes in planetary ball mill；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products.
As the preferred of above-mentioned technical proposal, step（1）In, described nickel cobalt manganese presoma, niobium source, the mol ratio of lithium salts
For 1.0: 0.002-0.1: 0.5-1.1.
As the preferred of above-mentioned technical proposal, step（1）In, the nickel cobalt manganese presoma is selected from Ni1/3Co1/3Mn1/3
(OH)2, Ni0.5Co0.2Mn0.3(OH)2, Ni0.6Co0.2Mn0.2(OH)2, Ni0.7Co0.15Mn0.15(OH)2, Ni0.8Co0.1Mn0.1
(OH)2, Ni1/3Co1/3Mn1/3CO3, Ni0.5Co0.2Mn0.3CO3, Ni0.6Co0.2Mn0.2CO3, Ni0.7Co0.15Mn0.15CO3,
Ni0.8Co0.1Mn0.1 CO3, in one or more.
As the preferred of above-mentioned technical proposal, step（1）In, the niobium source is selected from niobium oxide, niobium oxalate, niobic acid ammonium oxalic acid
One or more in salt hydrate.
As the preferred of above-mentioned technical proposal, step（1）In, the lithium salts is selected from lithium hydroxide, lithium carbonate, lithium nitrate,
One or more in lithium acetate.
As the preferred of above-mentioned technical proposal, step（1）In, the rotational speed of ball-mill is 80-200 r/min.
As the preferred of above-mentioned technical proposal, step（1）In, the Ball-milling Time is 1-6 hours.
As the preferred of above-mentioned technical proposal, step（2）In, the calcined temperature is 300-800 DEG C.
As the preferred of above-mentioned technical proposal, step（2）In, the burn-in time is 1-10 hours.
As the preferred of above-mentioned technical proposal, step（3）In, the rotational speed of ball-mill is 80-200 r/min.
As the preferred of above-mentioned technical proposal, step（3）In, the Ball-milling Time is 1-6 hours.
As the preferred of above-mentioned technical proposal, step（4）In, the calcining heat is 600-1000 DEG C.
As the preferred of above-mentioned technical proposal, step（4）In, the calcination time is 6-20 hours.
As the preferred of above-mentioned technical proposal, step（4）In, the sintering atmosphere is O2, Ar, H2, N2, one in air
Kind.
The nickel-cobalt lithium manganate cathode material of niobium doping prepared by the present invention, required device is simple, easy to operate, it is easy to accomplish
Industrialization.Because being doped with the Nb of electrochemicaUy inert in nickel-cobalt lithium manganate cathode material5+, nickle cobalt lithium manganate positive pole material can be improved
The body phase of material and the stability of surface texture, reduce the side reaction of electrode material and electrolyte interface.It is applied to lithium ion
During battery, the cycle performance under the performance of battery, particularly high voltage is significantly improved, extends the service life of battery.
Brief description of the drawings
Fig. 1 is the SEM figures of the resulting materials of embodiment 1.
Fig. 2 is the electrochemistry cycle performance figure of the resulting materials of embodiment 1.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only the part of the embodiment of the present invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art obtained under the premise of creative work is not made it is all its
His embodiment, belongs to the scope of protection of the invention.
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
Embodiment 1
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, comprises the following steps：
（1）By nickel cobalt manganese presoma Ni0.6Co0.2Mn0.2(OH)2, Nb2O5And Li2CO3The ball milling mixing in planetary ball mill.
Wherein Ni0.6Co0.2Mn0.2(OH)2, Nb2O5And Li2CO3Mol ratio be 1：0.005：0.54.Rotational speed of ball-mill is 150 r/min,
Ball-milling Time is 2 h；
（2）The pre-burning in Muffle furnace by the mixture of gained, sintering temperature are 600 DEG C, and sintering time is 7 h；
（3）By the material after pre-burning, ball milling mixing, rotational speed of ball-mill are 150 r/min in planetary ball mill, Ball-milling Time 2
h；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products, and sintering temperature is 870 DEG C, during sintering
Between be 15 h, sintering atmosphere O2, the chemical formula Li (Ni of products therefrom0.6Co0.2Mn0.2)0.99Nb0.01O2。
Embodiment 2
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, comprises the following steps：
（1）By nickel cobalt manganese presoma Ni0.8Co0.1Mn0.1(OH)2, Nb2O5And Li2CO3The ball milling mixing in planetary ball mill.
Wherein Ni0.8Co0.1Mn0.1(OH)2, Nb2O5And Li2CO3Mol ratio be 1：0.005：0.525.Rotational speed of ball-mill is 150 r/min,
Ball-milling Time is 2 h；
（2）The pre-burning in Muffle furnace by the mixture of gained, sintering temperature are 500 degree, and sintering time is 6 h；
（3）By the material after pre-burning, ball milling mixing, rotational speed of ball-mill are 150 r/min in planetary ball mill, Ball-milling Time 2
h；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products, and sintering temperature is 800 degree, during sintering
Between be 15 h, sintering atmosphere O2, the chemical formula Li (Ni of products therefrom0.8Co0.1Mn0.1)0.99Nb0.01O2。
Embodiment 3
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, comprises the following steps：
（1）By nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2, Nb2O5And Li2CO3The ball milling mixing in planetary ball mill.
Wherein Ni0.8Co0.1Mn0.1(OH)2, Nb2O5And Li2CO3Mol ratio be 1：0.005：0.55.Rotational speed of ball-mill is 150 r/min,
Ball-milling Time is 2 h；
（2）The pre-burning in Muffle furnace by the mixture of gained, sintering temperature are 600 degree, and sintering time is 7 h；
（3）By the material after pre-burning, ball milling mixing, rotational speed of ball-mill are 150 r/min in planetary ball mill, Ball-milling Time 2
h；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products, and sintering temperature is 900 degree, during sintering
Between be 12 h, sintering atmosphere O2, the chemical formula Li (Ni of products therefrom0.5Co0.2Mn0.3)0.99Nb0.01O2。
Embodiment 4
A kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, comprises the following steps：
（1）By nickel cobalt manganese presoma Ni0.33Co0.33Mn0.33(OH)2, Nb2O5And Li2CO3Ball milling mixes in planetary ball mill
Close.Wherein Ni0.8Co0.1Mn0.1(OH)2, Nb2O5And Li2CO3Mol ratio be 1：0.005：0.55.Rotational speed of ball-mill is 150 r/
Min, Ball-milling Time are 2 h；
（2）The pre-burning in Muffle furnace by the mixture of gained, sintering temperature are 600 degree, and sintering time is 7 h；
（3）By the material after pre-burning, ball milling mixing, rotational speed of ball-mill are 150 r/min in planetary ball mill, Ball-milling Time 2
h；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products, and sintering temperature is 950 degree, during sintering
Between be 15 h, sintering atmosphere is air, the chemical formula Li (Ni of products therefrom0.33Co0.33Mn0.33)0.99Nb0.01O2。
Tested below by the material obtained by embodiment, the effect of the embodiment of the present invention is illustrated.
ESEM（SEM）Test
The positive electrode of the gained of embodiment 1 is scanned Electronic Speculum（SEM）Test, tester model Hitachi S-4800
Field emission scanning electron microscope.
Understand that the gained nickel-cobalt lithium manganate cathode material of embodiment 1 is that primary particle accumulates form two by SEM test results
Secondary ball, the particle diameter of ball is ~ 8 um.
Chemical property is assessed
The positive electrode of the gained of embodiment 1 is formed into CR2016 type button cells, carries out chemical property assessment.Positive electrode,
Conductive agent and binding agent are according to weight ratio 8:1:1 ratio mixed slurry, then certain thickness is controlled to be coated on aluminum foil current collector
On.With 1.0 mol/L LiPF6/ EC+DEC (volume ratios 1:1) it is electrolyte, Li pieces are to electrode, U.S.'s production Cellgard-
2400 type polypropylene screens are barrier film, and button cell is assembled into the glove box full of argon gas.Then in Wuhan, gold promise electronics has
On the LandCT2001A type battery test systems of limit company production normal temperature is carried out to preparing material（25℃）Cycle life is tested.
Voltage range is 3.0-4.5V, and first five circle charge and discharge cycles of battery use current density 36mA/g（0.2C）Pre-activate, subsequently follow
Ring is with 180mA/g（1C）Current density discharge and recharge.
From electrochemical property test result, cycle performance is excellent under the products therefrom high voltage of embodiment 1.By 0.2C
After activation, the 1C of embodiment 1 discharge capacity is 177.6mAh/g, by 4.5 V, after 80 circle circulations, the electric discharge ratio of embodiment 1
Capacity is 163.9mAh/g.The capability retention of the doping type nickel-cobalt lithium manganate cathode material of the gained of embodiment 1 is 92.3%（In detail
See Fig. 2）.
The specific embodiment of the present invention is described in detail above, but it is only used as example, and the present invention is not intended to limit
In particular embodiments described above.To those skilled in the art, it is any to the practicality carry out equivalent modifications and replace
In generation, is also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and repair
Change, all should be contained within the scope of the invention.
Claims (10)
1. a kind of preparation method of doping type nickel-cobalt lithium manganate cathode material, it is characterised in that concretely comprise the following steps：
（1）By nickel cobalt manganese presoma, niobium source and the lithium salts ball milling mixing in planetary ball mill；
（2）The pre-burning in Muffle furnace by the mixture of gained；
（3）By the material after pre-burning, secondary ball milling mixes in planetary ball mill；
（4）The mixture of gained is calcined in high-temperature tubular atmosphere furnace and obtains final products.
2. preparation method according to claim 1, it is characterised in that step（1）Described in nickel cobalt manganese presoma, niobium
Source, the mol ratio of lithium salts are 1.0:（ 0.002-0.1）:（0.5-1.1）.
3. preparation method according to claim 1 or 2, it is characterised in that step（1）Described in nickel cobalt manganese presoma be selected from
Ni1/3Co1/3Mn1/3(OH)2, Ni0.5Co0.2Mn0.3(OH)2, Ni0.6Co0.2Mn0.2(OH)2, Ni0.7Co0.15Mn0.15(OH)2,
Ni0.8Co0.1Mn0.1(OH)2, Ni1/3Co1/3Mn1/3CO3, Ni0.5Co0.2Mn0.3CO3, Ni0.6Co0.2Mn0.2CO3,
Ni0.7Co0.15Mn0.15CO3, Ni0.8Co0.1Mn0.1 CO3, in one or more.
4. preparation method according to claim 3, it is characterised in that step（1）Described in niobium source be selected from niobium oxide, oxalic acid
Niobium, the one or more in niobic acid ammonium oxalic acid salt hydrate.
5. according to the preparation method described in claim 1,2 or 4, it is characterised in that step（1）Described in lithium salts be selected from hydroxide
Lithium, lithium carbonate, lithium nitrate, the one or more in lithium acetate.
6. preparation method according to claim 5, it is characterised in that step（1）Described in rotational speed of ball-mill be 80-200 r/
min；The Ball-milling Time is 1-6 hours.
7. according to the preparation method described in claim 1,2,4 or 6, it is characterised in that step（2）Described in calcined temperature be
300-800 DEG C, burn-in time is 1-10 hours.
8. preparation method according to claim 7, it is characterised in that step（3）Described in rotational speed of ball-mill be 80-200 r/
Min, Ball-milling Time are 1-6 hours.
9. according to the preparation method described in claim 1,2,4,6 or 8, it is characterised in that step（4）Described in calcining heat be
600-1000 DEG C, the calcination time is 6-20 hours.
10. preparation method according to claim 9, it is characterised in that step（4）Described in sintering atmosphere be O2、Ar、H2、
N2, one kind in air.
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| CN108346798A (en) * | 2018-03-23 | 2018-07-31 | 复旦大学 | The preparation method of doping type nickel-cobalt lithium manganate cathode material |
| CN108807975A (en) * | 2018-07-19 | 2018-11-13 | 力信（江苏）能源科技有限责任公司 | High voltage type nickel cobalt lithium manganate positive material for lithium ion battery and preparation method thereof |
| CN108899539A (en) * | 2018-06-28 | 2018-11-27 | 上海电力学院 | A kind of nickelic ternary lithium ion anode material and preparation method thereof |
| CN111584872A (en) * | 2020-05-20 | 2020-08-25 | 哈尔滨工业大学（威海） | Niobium-doped lithium ion battery positive electrode material and preparation method thereof |
| CN111785957A (en) * | 2020-06-10 | 2020-10-16 | 广东邦普循环科技有限公司 | Monocrystal-like ternary cathode material and preparation method and application thereof |
| CN112740442A (en) * | 2018-09-21 | 2021-04-30 | 株式会社田中化学研究所 | Positive electrode active material for secondary battery and method for producing same |
| CN113184923A (en) * | 2021-04-29 | 2021-07-30 | 昆山宝创新能源科技有限公司 | Preparation method of niobium modified lithium-rich manganese-based material, positive electrode material and lithium ion battery |
| CN114566625A (en) * | 2022-03-02 | 2022-05-31 | 重庆理英新能源科技有限公司 | Lithium-rich manganese-based positive electrode material with low pressure drop performance and preparation method and application thereof |
| CN116885177A (en) * | 2023-04-13 | 2023-10-13 | 华北电力大学 | Lithium ion battery and preparation method thereof |
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| CN108346798A (en) * | 2018-03-23 | 2018-07-31 | 复旦大学 | The preparation method of doping type nickel-cobalt lithium manganate cathode material |
| CN108899539A (en) * | 2018-06-28 | 2018-11-27 | 上海电力学院 | A kind of nickelic ternary lithium ion anode material and preparation method thereof |
| CN108807975A (en) * | 2018-07-19 | 2018-11-13 | 力信（江苏）能源科技有限责任公司 | High voltage type nickel cobalt lithium manganate positive material for lithium ion battery and preparation method thereof |
| EP3855541A4 (en) * | 2018-09-21 | 2022-11-02 | Tanaka Chemical Corporation | Positive electrode active material for secondary battery, and method for producing same |
| CN112740442A (en) * | 2018-09-21 | 2021-04-30 | 株式会社田中化学研究所 | Positive electrode active material for secondary battery and method for producing same |
| KR20210058959A (en) * | 2018-09-21 | 2021-05-24 | 가부시끼가이샤 다나까 가가꾸 겡뀨쇼 | Positive electrode active material for secondary battery and its manufacturing method |
| KR102648286B1 (en) * | 2018-09-21 | 2024-03-15 | 가부시끼가이샤 다나까 가가꾸 겡뀨쇼 | Cathode active material for secondary batteries and manufacturing method thereof |
| CN111584872A (en) * | 2020-05-20 | 2020-08-25 | 哈尔滨工业大学（威海） | Niobium-doped lithium ion battery positive electrode material and preparation method thereof |
| CN111785957A (en) * | 2020-06-10 | 2020-10-16 | 广东邦普循环科技有限公司 | Monocrystal-like ternary cathode material and preparation method and application thereof |
| CN113184923A (en) * | 2021-04-29 | 2021-07-30 | 昆山宝创新能源科技有限公司 | Preparation method of niobium modified lithium-rich manganese-based material, positive electrode material and lithium ion battery |
| CN114566625A (en) * | 2022-03-02 | 2022-05-31 | 重庆理英新能源科技有限公司 | Lithium-rich manganese-based positive electrode material with low pressure drop performance and preparation method and application thereof |
| CN114566625B (en) * | 2022-03-02 | 2023-06-20 | 重庆理英新能源科技有限公司 | Lithium-rich manganese-based positive electrode material with low pressure drop performance and preparation method and application thereof |
| CN116885177A (en) * | 2023-04-13 | 2023-10-13 | 华北电力大学 | Lithium ion battery and preparation method thereof |
| CN116885177B (en) * | 2023-04-13 | 2024-04-09 | 华北电力大学 | Lithium ion battery and preparation method thereof |
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Application publication date: 20180109 |