CN105374996A - Method for treatment on high-voltage Ni-Co-Mn ternary positive electrode material by surface drying method - Google Patents
Method for treatment on high-voltage Ni-Co-Mn ternary positive electrode material by surface drying method Download PDFInfo
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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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- 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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Abstract
A method for treatment on a high-voltage Ni-Co-Mn ternary positive electrode material by a surface drying method comprises the following steps of firstly, sieving and dispersing a lithium salt, weighing and adding the lithium salt and a Ni-Co-Mn hydroxide into a blending mixer for mixing according to a mole ratio of (1.0-1.2):1, mixing the lithium salt and the Ni-Co-Mn hydroxide to obtain mixed raw powder; secondly, loading and compacting the mixed raw powder in a pot, carrying out sintering in a high-temperature air atmosphere, cooling until the tapping temperature is less than or equal to 80 DEG C, taking a powder body out, and carrying out weak breaking, dispersing and sieving on the powder body in a drying room to obtain a high-dispersion Ni-Co-Mn ternary material substrate; thirdly, weighing and adding the high-dispersion Ni-Co-Mn ternary material substrate and a cladding agent A into a grinding blending mixer for mixing according to a mole ratio of 1:(0.1-0.001), and allowing the high-dispersion Ni-Co-Mn ternary material substrate and the cladding agent to be in mixed contact, thereby obtaining a mixed material; loading the mixed material in the pot, cooling after sintering the mixed material in the high-temperature air atmosphere to a solid phase until the tapping temperature is less than or equal to 80 DEG C, taking the powder body out, and carrying out sieving to obtain the high-voltage Ni-Co-Mn ternary material. According to the method, the high-voltage Ni-Co-Mn ternary positive electrode material which has the characteristics of high capacity, high cycle, high temperature and favorable safety can be prepared.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly a kind of preparation method of high voltage nickel-cobalt-manganternary ternary anode material of surperficial dry process.
Background technology
Nickel cobalt manganese (NCM) ternary material, because it possesses, high power capacity, safety are good, cheap etc. to be obtained researcher and pays close attention to widely.For meeting the demand of high energy battery, researcher proposes many modification thinkings to high voltage nickel cobalt-manganese ternary material surface modifying.At present, it is coated that what ternary material cladding applications was maximum are mainly wet method, but its complex process, cost is high, poor process control, requires higher to coating equipment, and the capacity of wet treatment on ternary material has impact, in the industry cycle there is larger dispute in the improvement degree of high temperature and fail safe; Adopt simple and effective method for coating, solve the bottleneck that nickel-cobalt-manganese ternary material surface instability problem becomes lithium electric industry circle.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of method of high voltage nickel-cobalt-manganternary ternary anode material of surperficial dry process, high power capacity can be produced, high circulation, the high voltage nickel-cobalt-manganternary ternary anode material that high temperatures fail safe is good.
To achieve these goals, technical scheme of the present invention is:
A method for surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material, comprises the following steps:
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 70 ~ 200 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide in molar ratio (1.0 ~ 1.2): 1 weigh after add rotating speed and mix in 300-600n/min batch mixer, carry out fully mixing 1 ~ 2h, obtain mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, temperature be in 700 ~ 1000 DEG C of air atmospheres sinter 5 ~ 20h, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix;
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are by 1:(0.1 ~ 0.001) molar ratio takes and adds to grind in batch mixer and mix 2 ~ 8h, high dispersive nickel-cobalt-manganese ternary material matrix is contacted with covering A Homogeneous phase mixing, obtains mixed material.
Sintering: mixed material is filled crucible, at temperature 700 ~ 1000 DEG C, fires after 5 ~ 15h becomes solid phase and be cooled to tapping temperature≤80 DEG C in air atmosphere, takes out powder, crosses 300 mesh sieve process, obtains high voltage nickel cobalt-manganese ternary material.
The chemical expression of the nickel cobalt manganese hydroxide in described step 1 is: Ni
xco
ymn
z(OH)
2, wherein x+y+z=1.
In described step 2, covering A is nano-scale particle, is Divalent metal hydroxide and the auxiliary agent mixture by 1:0 ~ 0.5 molar ratio; Wherein auxiliary agent is one or more mixtures of metal oxide.
Described step 1, in step 2, air atmosphere is by upper and lower tonifying Qi mode, ensures uniform alumina reaction.
The present invention has the following advantages: one is manufacture dispersed ternary material matrix; Two is that on the basis of material height dispersion, carry out dry laminating coated, a kind of smooth coating layer is formed at substrate material surface, under the prerequisite of protective material surface characteristic, take into account the cyclicity of material, security performance, effectively reduces the residual lithium amount of nickel-cobalt-manganese ternary material surface and the adaptability to environment; Three is that technique is simple, and workable, lot stability is high, is applicable to large batch of large-scale production.
Its performance index: polymolecularity nickel-cobalt-manganese ternary material matrix, namely control current rate and number of times, make dispersed parameter D
n-D
s≤ 0.2 (D
n, D
sfor sample ultrasonic forward and backward center granularity in water, D
n-D
s=D
n50– D
s50).High voltage condition is: >=4.35V.
Embodiment
Embodiment one
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 70 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: it is 500n/min batch mixer that 1.05:1 adds rotating speed, fully mixes 1.5h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 8h in the firing furnace of 960 DEG C of air in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix.
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.03 takes, wherein covering A is: hydroxide cobalt and lanthana are that 1:0.1 mixes according to mol ratio, then adds in grinding batch mixer and mixes 3h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 940 DEG C of high temperature solid-state, fire 8h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains target product one.
Embodiment two
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 100 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: 1.08:1 adds the batch mixer that rotating speed is 600n/min, fully mixes 1h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 12h in the firing furnace of the air of 940 DEG C in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix.
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.03 takes, wherein covering A is: hydroxide cobalt and titanium oxide, in molar ratio for 1:0.15 mixes, then add in grinding batch mixer and mix 6h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 920 DEG C of high temperature solid-state, fire 12h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains target product two.
Embodiment three
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 150 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: 1.1:1 adds the batch mixer that rotating speed is 400n/min, fully mixes 2h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 15h in the firing furnace of the air of 910 DEG C in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix.
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.1 takes, wherein covering A is: hydroxide cobalt: zirconic mol ratio: 1:0.1, then adds in grinding batch mixer and mixes 5h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 880 DEG C of high temperature solid-state, burn till 15h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains target product three.
Comparison example
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 70 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: 1.08:1 adds the batch mixer that rotating speed is 600n/min, fully mixes 1h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 12h in the firing furnace of the air of 940 DEG C, be then cooled to tapping temperature≤80 DEG C in temperature, takes out powder, after carrying out weak broken, dispersion, crossing 300 mesh sieve process, obtains contrast product at drying room.
Sample test comparing result:
1. residual alkali number test: Li
2cO
3%, LiOH%, adopt ICP test;
2. electro-chemical test condition (3.0-4.6) V detains electrical testing, and 0.2C fills-puts-fills, 1C, the capability retention of 100 circle electric discharges.
Table 1: the residual lithium test comparison of embodiment sample
Conclusion: as can be seen from table one, compared with comparative sample, the residual lithium amount in surface of the target product after dry surface process obviously reduces, and is conducive to material at high temperature performance, the performance of security performance.
Table 2: embodiment button battery testing contrasts
Conclusion: as can be seen from table two, compared with comparative sample, the target product after dry surface process is under the prerequisite taking into account capacity performance, and cycle performance is greatly improved, 100 circle circulation volume conservation rates bring up to more than 93.8.% by 78.8%, can meet needed for high voltage circulation.
Claims (7)
1. a method for surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material, is characterized in that, comprise the following steps:
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 70 ~ 200 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide 1:(1.0 ~ 1.2 in molar ratio) weigh after add rotating speed and mix in 300-600n/min batch mixer, carry out fully mixing 1 ~ 2h, obtain mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, temperature be in 700 ~ 1000 DEG C of air atmospheres sinter 5 ~ 20h, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix;
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are by 1:(0.1 ~ 0.001) molar ratio takes and adds to grind in batch mixer and mix 2 ~ 8h, high dispersive nickel-cobalt-manganese ternary material matrix is contacted with covering A Homogeneous phase mixing, obtains mixed material;
Sintering: mixed material is filled crucible, at temperature 700 ~ 1000 DEG C, fires after 5-15h becomes solid phase and be cooled to tapping temperature≤80 DEG C in air atmosphere, takes out powder, crosses 300 mesh sieve process, obtains high voltage nickel cobalt-manganese ternary material.
2. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, is characterized in that, the chemical expression of the nickel cobalt manganese hydroxide in described step 1 is: Ni
xco
ymn
z(OH)
2, wherein x+y+z=1.
3. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterized in that, in described step 2, covering A is nano-scale particle, is Divalent metal hydroxide and the auxiliary agent mixture by 1:0 ~ 0.5 molar ratio; Wherein auxiliary agent is one or more mixtures of metal oxide.
4. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterized in that, described step 1, in step 2, air atmosphere is by upper and lower tonifying Qi mode, ensures uniform alumina reaction.
5. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, is characterized in that, comprise the following steps:
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 70 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: it is 500n/min batch mixer that 1.05:1 adds rotating speed, fully mixes 1.5h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 8h in the firing furnace of the air of 960 DEG C in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix;
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.03 takes, wherein covering A is: hydroxide cobalt and lanthana are that 1:0.1 mixes according to mol ratio, then adds in grinding batch mixer and mixes 3h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 940 DEG C of high temperature solid-state, burn till 8h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains high voltage nickel cobalt-manganese ternary material.
6. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, is characterized in that comprising the following steps:
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 100 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: 1.08:1 adds the batch mixer that rotating speed is 600n/min, fully mixes 1h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 12h in the firing furnace of the air of 940 DEG C in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix;
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.03 takes, wherein covering A is: hydroxide cobalt and titanium oxide, in molar ratio for 1:0.15 mixes, then add in grinding batch mixer and mix 6h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 920 DEG C of high temperature solid-state, burn till 12h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains high voltage nickel cobalt-manganese ternary material.
7. the method for a kind of surperficial dry process high voltage nickel-cobalt-manganternary ternary anode material according to claim 1, is characterized in that comprising the following steps:
Step 1, the preparation of polymolecularity nickel-cobalt-manganese ternary material matrix:
Batch mixing: lithium salts is carried out 200 orders and to sieve dispersion, except after Slag treatment with nickel cobalt manganese hydroxide be in molar ratio: 1.1:1 adds the batch mixer that rotating speed is 400n/min, fully mixes 2h, obtains mixing cornflour;
Sintering: mixing cornflour is filled crucible compacting, be sinter 15h in the firing furnace of the air of 910 DEG C in temperature, be then cooled to tapping temperature≤80 DEG C, take out powder, after carrying out weak broken, dispersion at drying room, crossing 300 mesh sieve process, namely secure satisfactory grades loose nickel-cobalt-manganese ternary material matrix;
Step 2, the coated process of dry surface:
Batch mixing: high dispersive nickel-cobalt-manganese ternary material matrix and covering A are in molar ratio for 1:0.1 takes, wherein covering A is: hydroxide cobalt: zirconic mol ratio: 1:0.1, then adds in grinding batch mixer and mixes 5h, make its Homogeneous phase mixing, contact, obtains mixed material;
Sintering: mixed material is filled crucible, and 880 DEG C of high temperature solid-state, burn till 15h in air atmosphere, be cooled to tapping temperature≤80 DEG C, takes out powder, crosses 300 mesh sieve process, obtains high voltage nickel cobalt-manganese ternary material.
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