CN108172825A - Real inexpensive lithium cobaltate cathode material of a kind of high voltage and preparation method thereof - Google Patents
Real inexpensive lithium cobaltate cathode material of a kind of high voltage and preparation method thereof Download PDFInfo
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- CN108172825A CN108172825A CN201711280987.7A CN201711280987A CN108172825A CN 108172825 A CN108172825 A CN 108172825A CN 201711280987 A CN201711280987 A CN 201711280987A CN 108172825 A CN108172825 A CN 108172825A
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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
- H01M4/52—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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- 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
Abstract
The present invention is suitable for anode material of lithium battery field, real inexpensive lithium cobaltate cathode material of a kind of high voltage and preparation method thereof is provided, this method prepares the big grain size lithium cobaltate cathode material of additive A doping first, then the small particle nickel-cobalt-manganternary ternary anode material of additive B doping is prepared, then the different quality ratio of big grain size cobalt acid lithium and small particle nickel-cobalt-manganternary ternary anode material is mixed, the compacted density of material can fully be improved, reduce the cost of positive electrode, finally crushing is sintered with the covering C containing indium sulfide, obtain final finished product lithium cobaltate cathode material.By adulterating In3+It may insure structural stability of the cobalt acid lithium under high-voltage state, improve the cycle life and security performance of material.
Description
Technical field
The invention belongs to the real inexpensive cobalt acid lithiums of anode material of lithium battery technical field more particularly to a kind of high voltage
Positive electrode and preparation method thereof.
Background technology
In lithium ion anode material, cobalt acid lithium is due to having higher operating voltage and energy density, being easily-synthesized and can
Fast charging and discharging, therefore be widely used.In recent years, with electronic product miniaturise and multifunction, to battery
The energy density of output proposes higher requirement, and conventional cobalt acid lithium cannot be met the requirements.Ensureing safety and fitting
When cyclicity under the premise of, improve the energy (mainly volume energy density) of lithium electricity, be still over the next several years small-sized lithium it is electric
Energy density is improved in basic development direction, and there are two main paths nothing but, improve electrode material capacity or improve battery work
Voltage.If it will can't be better that both high voltage and high power capacity can be combined to that, in fact this is exactly current 3C
The mainstream of anode material of lithium battery development.Existing lithium ion battery operating voltage range substantially between 3.0V-4.3V, and with
Cobalt acid lithium can increase by 20% or so capacity, but cobalt acid lithium at this time when being charged to 4.5V for the lithium ion battery of positive electrode
Due to depth deintercalation Li+, with the bad phase transition process of invertibity, material structure is extremely unstable, and battery security cannot
Ensure, cycle performance also drastically declines therewith.In addition to this, it due to cobalt resource scarcity, causes cobalt acid lithium material price high, increases
The material cost of lithium ion battery is added.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of real inexpensive lithium cobaltate cathode materials of high voltage
And preparation method thereof, it is intended to solve existing cobalt acid lithium battery poor circulation, the technical issues of cost is higher.
On the one hand, the preparation method of the real inexpensive lithium cobaltate cathode material of the high voltage includes the following steps：
S1, lithium source, big grain size cobaltosic oxide and additive A are pressed into Li:Co:A=(1.02~1.07):1:(0.005~
0.01) molar ratio, which is added to together in high speed mixer, to be sufficiently mixed uniformly, then carries out high temperature sintering, the additive A
Including at least nanoscale In2O3, further include at least one of strontium phosphate, molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide；
S2, step S1 is sintered after material crush, the median particle diameter D50 of control sintered material is 15~25 during crushing
μm, sieving obtains big grain size lithium cobaltate cathode material；
S3, lithium source, the compound precursor of small particle nickel cobalt manganese and additive B are pressed into Li:Me:B=(1.002~1.007):1:
The molar ratio of (0.0002~0.0005), which is added to together in high speed mixer, to be sufficiently mixed uniformly, and wherein Me is Ni, Co, Mn
Then the sum of mole carries out high temperature sintering, the additive B is strontium phosphate, in molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide
One or more；
S4, step S3 is sintered after material crush, the median particle diameter D50 of control sintered material is 4~8 μ during crushing
M, sieving, obtains small particle nickel-cobalt-manganternary ternary anode material；
S5, by the big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material in mass ratio (2~
9)：1 is mixed, and is then added in high speed mixer and is sufficiently mixed uniformly together with covering C, the mixing after being coated
Mixed-powder after cladding is carried out high temperature sintering by powder, and the covering C includes at least indium sulfide In2S3, further include phosphoric acid
One or more of strontium, molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide；
S6, step S5 is sintered after material crush, the median particle diameter D50 of control sintered material is 14~23 during crushing
μm, sieving obtains final finished product lithium cobaltate cathode material.
Further, step S1, lithium source used in S3 is lithium carbonate.
Further, in step S1, sintering temperature is 1000~1200 DEG C, and the sintered heat insulating time is 8~15h, sintered
Air is blasted in journey, air mass flow is 0.2~1.2m3/h；In step S3, sintering temperature is 700~1100 DEG C, during sintered heat insulating
Between for 8~15h, air is blasted in sintering process, air mass flow is 0.2~1.2m3In/h, step S5, sintering temperature for 600~
1000 DEG C, the sintered heat insulating time is 4~10h, and air is blasted in sintering process, and air mass flow is 0.2~1.2m3/h。
Further, step S1, in S3, S5, the incorporation time of high speed mixer is 10~30min；Step S2, S4, S6
In, the method that is crushed using the method or high-speed rotational of air-flow crushing during crushing material.
Further, the median particle diameter D50 of the additive A, additive B and covering C<=7 μm.
Further, step S1, in S3, S5, the heating rate in sintering process is 2.0~8.0 DEG C/min.
Further, in step S5, the amount of covering C is big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganese ternary
The 0.5%~2% of positive electrode gross mass.
On the other hand, the real inexpensive lithium cobaltate cathode material of the high voltage is prepared by the above method, material
Specific surface area 0.15m2/ g~0.25m2/ g, compacted density>=4.1g/m2。
The beneficial effects of the invention are as follows：First, the present invention is improved by the way of appropriate In ions are mixed, due to
In3+With Co3+Valence state it is identical, the In of incorporation3+Occupy Co3+Position, in charging process, Co can occur for Co ions3+To Co4+'s
Transformation, and the contraction of adjoint volume, if charging voltage is excessively high, depth of charge is excessive, the volume contraction of material will be irreversible,
And electro-chemical activity is finally lost, and In3+The fixed price in charge and discharge process is electrochemicaUy inert, is not sent out in charge and discharge
The variation of raw valence state, thus the variation of volume does not occur yet, skeleton can be played the role of, stable crystal structure improves material
Cycle life and security performance；Secondly, we are mixed using bulky grain cobalt acid lithium and little particle nickel-cobalt-manganternary ternary anode material
Mode, so as to improve the compacted density of material, reduce finished product cobalt acid lithium cost.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The preparation method of the real inexpensive lithium cobaltate cathode material of high voltage provided by the invention includes the following steps：
S1, lithium source, big grain size cobaltosic oxide and additive A are pressed into Li:Co:A=(1.02~1.07):1:(0.005~
0.01) molar ratio, which is added to together in high speed mixer, to be sufficiently mixed uniformly, then carries out high temperature sintering, the additive A
Including at least nanoscale In2O3, further include at least one of strontium phosphate, molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide.It is described
Lithium source is lithium carbonate, and in sintering process, sintering temperature is 1000~1200 DEG C, and the sintered heat insulating time is 8~15h, sintering process
In blast air, air mass flow is 0.2~1.2m3/ h, the heating rate in sintering process is 2.0~8.0 DEG C/min, mixed at a high speed
The incorporation time of material machine is 10~30min.Additive A median particle diameter D50<=7 μm.
S2, step S1 is sintered after material crush, the median particle diameter D50 of control sintered material is 15~25 during crushing
μm, 325 mesh screens are crossed, obtain big grain size lithium cobaltate cathode material.
S3, lithium source, the compound precursor of small particle nickel cobalt manganese and additive B are pressed into Li:Me:B=(1.002~1.007):1:
The molar ratio of (0.0002~0.0005), which is added to together in high speed mixer, to be sufficiently mixed uniformly, and wherein Me is Ni, Co, Mn
Then the sum of mole carries out high temperature sintering, the additive B is strontium phosphate, in molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide
One or more.The lithium source is lithium carbonate, and in sintering process, sintering temperature is 700~1100 DEG C, and the sintered heat insulating time is
8~15h, air is blasted in sintering process, and air mass flow is 0.2~1.2m3/ h, the incorporation time of high speed mixer for 10~
30min, the heating rate in sintering process are 2.0~8.0 DEG C/min.Additive B median particle diameter D50<=7 μm.
S4, step S3 is sintered after material crush, the median particle diameter D50 of control sintered material is 4~8 μ during crushing
M crosses 325 mesh screens, obtains small particle nickel-cobalt-manganternary ternary anode material.
S5, by the big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material in mass ratio (2~
9)：1 is mixed, and is then added in high speed mixer and is sufficiently mixed uniformly together with covering C, the mixing after being coated
Mixed-powder after cladding is carried out high temperature sintering by powder, and the covering C includes at least indium sulfide In2S3, further include phosphoric acid
One or more of strontium, molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide.Heating rate in sintering process is 2.0~8.0
DEG C/min, sintering temperature is 600~1000 DEG C, and the sintered heat insulating time is 4~10h, and air, air mass flow are blasted in sintering process
For 0.2~1.2m3/ h, the incorporation time of high speed mixer is 10~30min.The median particle diameter D50 of covering C<=7 μm, packet
The amount for covering agent C is the 0.5%~2% of big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material gross mass.
S6, step S5 is sintered after material crush, the median particle diameter D50 of control sintered material is 14~23 during crushing
μm, sieving obtains final finished product lithium cobaltate cathode material.
In the above process, the method that is crushed using the method or high-speed rotational of air-flow crushing during crushing material.It finally obtains
Material specific surface area 0.15m2/ g~0.25m2/ g, compacted density>=4.1g/m2。
Below by specific embodiment, the present invention will be described.
Embodiment 1
(1) by lithium carbonate, big grain size cobaltosic oxide, additive A (nanometer In2O3And nanometer strontium phosphate) in molar ratio
Li:Co:A=1.025：0.993：0.007 weighs corresponding raw material, is then added in high speed mixer and is sufficiently mixed together
It is even, incorporation time 15min.Mixture is placed in batch-type furnace and is sintered, is passed through 0.5m3The air of/h flows, heating speed
Rate is 2 DEG C/min, and sintering temperature is 1100 DEG C, and furnace cooling after sintered heat insulating 12h obtains sintered material, to sinter
Material crushes, and crosses 325 mesh screens, obtains big grain size lithium cobaltate cathode material.
(2) by lithium carbonate, the compound precursor of small particle nickel cobalt manganese and nanoscale iridium Li in molar ratio:Me:B=
1.006：0.994：0.009 weighs corresponding raw material, is then added in high speed mixer and is sufficiently mixed uniformly, during mixing together
Between be 15min.Mixture is placed in batch-type furnace and is sintered, is passed through 0.4m3The air of/h flows, heating rate for 4 DEG C/
Min, sintering temperature are 900 DEG C, and furnace cooling after sintered heat insulating 5h obtains sintered material, sintered material is crushed,
325 mesh screens are crossed, obtain small particle nickel-cobalt-manganternary ternary anode material.
(3) by above-mentioned big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material in mass ratio 7：3 into
Row mixing, then with indium sulfide (In2S3) and covering (molybdenum oxide, cerium oxide, bismuth oxide) be added in high speed mixer together
It is sufficiently mixed uniformly, the amount of the mixed-powder after being coated, wherein covering is the 0.8% of total amount, by the mixing after cladding
Powder carries out second of high temperature sintering, and sintering temperature is 950 DEG C, and the sintered heat insulating time is 6h, and air is blasted in sintering process, empty
Throughput is 0.5m3/ h obtains material after double sintering.
(4) material after double sintering is crushed, cross 325 mesh screens, obtain final high voltage in fact it is low into
This finished product lithium cobaltate cathode material.
The finished product lithium cobaltate cathode material specific surface area 0.15m finally obtained2/ g~0.25m2/ g, compacted density>=
4.1g/m2, carry out full battery testing, chemical property：In 3~4.4V charge and discharge, discharge capacity reaches 180mAh/g for the first time, and 50
All circulation volume conservation rates reach more than 95%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the real inexpensive lithium cobaltate cathode material of high voltage, which is characterized in that the method includes
Following step：
S1, lithium source, big grain size cobaltosic oxide and additive A are pressed into Li:Co:A=(1.02~1.07):1:(0.005~
0.01) molar ratio, which is added to together in high speed mixer, to be sufficiently mixed uniformly, then carries out high temperature sintering, the additive A
Including at least nanoscale In2O3, further include at least one of strontium phosphate, molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide；
S2, step S1 is sintered after material crush, the median particle diameter D50 of control sintered material is 15~25 μm during crushing,
Sieving, obtains big grain size lithium cobaltate cathode material；
S3, lithium source, the compound precursor of small particle nickel cobalt manganese and additive B are pressed into Li:Me:B=(1.002~1.007):1:
The molar ratio of (0.0002~0.0005), which is added to together in high speed mixer, to be sufficiently mixed uniformly, and wherein Me is Ni, Co, Mn
Then the sum of mole carries out high temperature sintering, the additive B is strontium phosphate, in molybdenum oxide, cerium oxide, yttrium oxide, bismuth oxide
One or more；
S4, step S3 is sintered after material crush, the median particle diameter D50 of control sintered material is 4~8 μm during crushing, mistake
Sieve, obtains small particle nickel-cobalt-manganternary ternary anode material；
S5, by the big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material (2~9) in mass ratio：1 into
Then row mixing is added to covering C in high speed mixer and is sufficiently mixed uniformly together, the mixed-powder after being coated,
Mixed-powder after cladding is subjected to high temperature sintering, the covering C includes at least indium sulfide In2S3, further include strontium phosphate, oxygen
Change one or more of molybdenum, cerium oxide, yttrium oxide, bismuth oxide；
S6, step S5 is sintered after material crush, the median particle diameter D50 of control sintered material is 14~23 μm during crushing,
Sieving, obtains final finished product lithium cobaltate cathode material.
2. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as described in claim 1, which is characterized in that step
Lithium source used in rapid S1, S3 is lithium carbonate.
3. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 2, which is characterized in that step
In rapid S1, sintering temperature is 1000~1200 DEG C, and the sintered heat insulating time is 8~15h, and air, air stream are blasted in sintering process
It measures as 0.2~1.2m3/h；In step S3, sintering temperature be 700~1100 DEG C, the sintered heat insulating time be 8~15h, sintering process
In blast air, air mass flow is 0.2~1.2m3In/h, step S5, sintering temperature is 600~1000 DEG C, the sintered heat insulating time
For 4~10h, air is blasted in sintering process, air mass flow is 0.2~1.2m3/h。
4. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 3, which is characterized in that step
In rapid S1, S3, S5, the incorporation time of high speed mixer is 10~30min；Step S2, in S4, S6, gas is used during crushing material
Flow the method that the method crushed or high-speed rotational crush.
5. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 4, which is characterized in that institute
State the median particle diameter D50 of additive A, additive B and covering C<=7 μm.
6. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 5, which is characterized in that step
In rapid S1, S3, S5, the heating rate in sintering process is 2.0~8.0 DEG C/min.
7. the preparation method of the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 6, which is characterized in that step
In rapid S5, the amount of covering C is big grain size lithium cobaltate cathode material and small particle nickel-cobalt-manganternary ternary anode material gross mass
0.5%~2%.
A kind of 8. real inexpensive lithium cobaltate cathode material of high voltage, which is characterized in that the real low cost of the high voltage
Lithium cobaltate cathode material is prepared using the preparation method as described in claim any one of 1-7.
9. the real inexpensive lithium cobaltate cathode material of high voltage as claimed in claim 8, which is characterized in that the high voltage is high
The specific surface area 0.15m of the inexpensive lithium cobaltate cathode material of compacting2/ g~0.25m2/ g, compacted density>=4.1g/m2。
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| CN109273684A (en) * | 2018-09-07 | 2019-01-25 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN109638291A (en) * | 2018-12-27 | 2019-04-16 | 清远佳致新材料研究院有限公司 | A kind of anode sizing agent, preparation method and positive plate and lithium ion battery |
| CN109888250A (en) * | 2019-03-29 | 2019-06-14 | 荆门市格林美新材料有限公司 | A kind of room temperature carbon coating monocrystalline nickel-cobalt-manganternary ternary anode material and preparation method |
| CN110048111A (en) * | 2019-04-25 | 2019-07-23 | 柔电（武汉）科技有限公司 | Cell positive material, battery anode slice and lithium battery |
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| CN114561686A (en) * | 2022-02-28 | 2022-05-31 | 蜂巢能源科技股份有限公司 | Method for improving compaction density of cobalt-free positive electrode material, cobalt-free positive electrode material and lithium ion battery |
| CN115000369A (en) * | 2022-05-31 | 2022-09-02 | 上海瑞浦青创新能源有限公司 | Positive electrode material, positive electrode plate and lithium ion battery |
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