CN106784739A - A kind of cobalt acid lithium material and preparation method thereof, positive electrode - Google Patents
A kind of cobalt acid lithium material and preparation method thereof, positive electrode Download PDFInfo
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Abstract
The invention provides a kind of cobalt acid lithium material and preparation method thereof, positive electrode.A kind of cobalt acid lithium material, mainly by the cobalt acid lithium particle doped with element M and is coated on the coating on its surface and constitutes；The molecular formula of the cobalt acid lithium particle is LiaCo1‑bMbO2, wherein, 0.95≤a≤1.15,0.003≤b≤0.01, M is at least one or more of in Mg, Al, Ti, Zr, Ni, Mn, Cr, Mo, W and rare earth element；The coating is selected from ZnO or SnO2Or both mixing, weight is 0.5~5wt% of the cobalt acid lithium particle, preferably preferably 1~5wt%, preferably 2~5wt%, 2~4wt%.Forthright again and cycle performance is poor under described cobalt acid lithium material solves the problems, such as current material high pressure.
Description
Technical field
The present invention relates to chemical field, more particularly, to a kind of cobalt acid lithium material and preparation method thereof, positive electrode.
Background technology
Lithium ion battery has that operating voltage is high, specific energy big, long lifespan, lightweight, memory-less effect, environmental protection etc.
Feature, in having been widely used for the power supply of all kinds equipment, in electric automobile, large-scale energy storage device, electric tool, number
The fields such as equipment play an important roll.
Positive electrode is the important component of lithium ion battery, be influence performance of lithium ion battery most important factor it
One, the positive electrode for researching and developing higher performance is the effective way and key point for improving lithium battery performance at present.Cobalt acid
Lithium, LiMn2O4, LiFePO4, ternary etc. are conventional commercialization positive electrodes, and stratiform cobalt acid lithium is due to its high voltage, electric discharge
The advantages of voltage stabilization, specific energy high, be most widely used positive electrode.
As the continuous expansion of range of application, the requirement to lithium ion battery are constantly updated and refined, it is right also just to expedite the emergence of out
The demand of different functionalities positive electrode.Such as in car mould, model plane, electronic cigarette, power driven vehicle, the extremely cold area automobile for rising
The fields such as startup power supply, charging quickly source, lithium ion battery is as the power supply of these equipment, it is necessary to often carry out lasting high current
Discharge to meet the demand of equipment.Therefore, it is very high to the requirement of the high rate performance of lithium battery, also with regard to an urgent demand positive electrode times
Rate performance is constantly improve, multiplying power property when particularly blanking voltage is higher than 4.2V.
Cobalt acid lithium is used as the maximum positive electrode of current usage amount, and production technology is extremely ripe.When the change of its particle diameter is big, times
Rate discharge performance is poor, when particle diameter becomes hour, is contacted between particle and particle closely, and lithium ion hinders in particle internal migration
Power is small, and battery impedance is small, therefore rate charge-discharge excellent performance.But, cobalt acid lithium haves the shortcomings that certain：On the one hand, due to solid
Some chemical property limitations, cobalt acid lithium can undergo phase transition the phenomenon for destruction occur when blanking voltage is higher than 4.35V, cause high pressure
Under multiplying power discharging property reduction；On the other hand, the particle diameter of conventional cobalt acid lithium is small, and specific surface area is larger, the contact with electrolyte
Area is big, and side reaction easily occurs between electrolyte, causes the cycle performance of battery to decline.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of cobalt acid lithium material, and described cobalt acid lithium material solves current material
The problem of forthright again and cycle performance difference under high pressure.
The second object of the present invention is the preparation method for providing above-mentioned cobalt acid lithium material, described preparation method flow letter
Single, the adjustment to current material manufacture craft is small, is more easy to promote.
The third object of the present invention is to provide a kind of positive electrode, and the positive electrode is compared to current material in high pressure work
There is significant advantage under condition.
In order to solve the above technical problems, the invention provides following technical scheme：
A kind of cobalt acid lithium material, mainly by the cobalt acid lithium particle doped with element M and is coated on the coating on its surface
Composition；
The molecular formula of the cobalt acid lithium particle is LiaCo1-bMbO2, wherein, 0.95≤a≤1.15,0.003≤b≤0.01,
M is at least one or more of in Mg, Al, Ti, Zr, Ni, Mn, Cr, Mo, W and rare earth element；
The coating is selected from ZnO or SnO2Or both mixing, weight be the cobalt acid lithium particle 0.5~
5wt%, preferably 1~5wt%, preferably 2~5wt%, preferably 2~4wt%.
The present invention solves under cobalt acid lithium material high pressure (especially more than 4.35V) cycle performance and again forthright difference in terms of two
Problem, i.e., on the one hand mix particular type, the miscellaneous element M of special ratios, the cobalt element in making it with cobalt acid lithium forms M-O
Key, so as to stablize the structure of cobalt acid lithium, suppresses phase transformation of the cobalt acid lithium during high-voltage discharge, improves cycle performance and multiplying power
Property；On the other hand in one layer of barrier of outwardly cladding --- the ZnO/SnO of cobalt acid lithium2, suppress the dissolution of cobalt under high pressure, so that
Improve cycle of higher pressure performance, in addition, coating can also to a certain extent reduce the side reaction between cobalt acid lithium and electrolyte,
Effectively improve the forthright again of cobalt acid lithium, security and cycle performance.
Reversible discharge specific capacity of the cobalt acid lithium material between 3.0~4.45V is higher than 192mAh/g after being improved more than
(0.5C), the big multiplying power discharging efficiency of 0.5C/20C has exceeded 97%, 1.0C/1.0C charge and discharge cycles more than 500 times, and capacity keeps
Rate can reach more than 96%
Above material can also be improved further, to reach more technique effects：
Preferably, the M is at least one or more of, at least one preferably in Mg, Al, Ti in Mg, Al, Ti, Zr
Or it is various, more preferably the mol ratio of Mg, Al, Ti is 2:2:1~2.
Mainly consider the stability of M-Co keys during from doped chemical, and doping element and cobalt acid lithium electric conductivity phase
The factors such as capacitive, secondary consideration cost, technology difficulty, coordinate factors above, at least one or many preferably in Mg, Al, Ti, Zr
Kind (for example, Mg or Al or Ti or Zr or Mg and Al equimolars ratio composition, or Ti and Al equimolars are than composition, or
Person Ti is with Zr equimolars than composition), preferably at least one or more of in Mg, Al, Ti, the mol ratio of more preferably Mg, Al, Ti is
2:2:1~2.
Or, it is preferable that the M is at least one or more of (for example, Ni or Mn or Cr in Ni, Mn, Cr, Mo
Or Mo, or Ni and Mn equimolars ratio composition, or Cr and Mo equimolars ratio composition), preferably in Ni, Mn, Cr at least one
Plant or various, more preferably the mol ratio of Ni, Mn, Cr is 1:1~2:1.
Preferably, the particle diameter of the cobalt acid lithium material is 3-8 μm；
The particle diameter of cobalt acid lithium is smaller, and it is higher with the side reaction degree of electrolyte, but electric conductivity is preferably, considers two
Person, preferable particle size is 3-8 μm.
Preferably, specific surface area is 0.1~0.5m2/g。
Preferably, 1.05≤a≤1.15,0.003≤b≤0.008.
Preferably, the coating is ZnO and SnO2With 1:The mol ratio composition of 1-3.
ZnO and SnO2With 1:Electric conductivity is greatly improved after the mol ratio composition of 1-3.
Cobalt acid lithium material mentioned above can use following preparation method：
According to the proportioning of molecular formula, lithium source, cobalt source, element M source are mixed, is granulated, then coated described in Surface coating
Thing, sinter afterwards, broken, sieving, except iron, obtain final product.
Preferably, also include after the granulation and before the cladding：The particle for obtaining will be granulated 200~500
It is heat-treated 0.5~3 hour at DEG C.
After so processing, the sphericity of spherical lithium cobalt granular precursor can be strengthened, improve hardness, reduce the cladding stage
Destroyed rate, while reducing the moisture of cobalt acid lithium presoma, sintering stage afterwards is preferably crystallized shaping.
Preferably, the method for the mixing is mixing wet grinding：Ground under conditions of solid content is 10~40wt%
0.1~0.5 μm is reached to slurry granularity.
The wet milling process makes doped chemical evenly, reduces material specific surface area, improves cobalt acid lithium crystalline structure.
Preferably, the surfactant that weight is 0.02~0.5wt% of thing to be ground is added in the process of lapping；
Preferably, the surfactant be selected from ammonium polymethacrylate, stearmide, HMDS, KD-1,
One or more in dodecyl sodium sulfate, preferably stearmide.
Adding surfactant helps to strengthen the mixing uniformity of miscellaneous element and cobalt element, improves grinding efficiency, while
Prevent from being sanded disposed slurry because the sinking lamination under Action of Gravity Field occurs.
Preferably, between 2~7 μm, moisture is preferably within 0.5wt% the granular size for obtaining that granulates；
Particle diameter, water content control can be obtained into more preferable cobalt acid lithium crystalline structure within the above range.
Preferably, the cladding is dry type cladding.
Dry type cladding is simple to operate, but being evenly coated property does not have wet method to coat height, is selected regarding concrete condition in actual production
Select.
Preferably, it is described to be sintered to：600~1000 DEG C sinter 3~15 hours, and throughput is 2~20m3/h。
As described above, cobalt acid lithium material provided by the present invention is answered mainly for the preparation of the positive pole of lithium battery in industry
In, in addition to matrix material, other auxiliary materials can also be added except using above-mentioned cobalt acid lithium material, do not enumerated herein.
To sum up, compared with prior art, invention achieves following technique effect：
(1) in cobalt acid lithium Surface coating composition, and doped chemical is combined, substantially increases cobalt acid lithium material under high pressure
High rate performance, cycle performance and security performance.
(2) parameter such as specific surface area, particle diameter of adjustment material improves the sphericity of material, so as to improve its electric conductivity.
(3) by improveing the process conditions such as grinding, granulation, sintering of cobalt acid lithium material, uniform doping, crystalline form knot are improved
Structure etc., so as to improve to essence the electric conductivity and processing characteristics of material on molecular structure, expands range of application.
Brief description of the drawings
The microscope figure of the cobalt acid lithium material that Fig. 1 is provided by the embodiment of the present invention 1.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with specific embodiment, but ability
Field technique personnel will be understood that, following described embodiment is a part of embodiment of the invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument
Unreceipted production firm person, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
Cobalt acid lithium material is made, chemical formula is Li0.95Co0.99Mg0.01O2
(1) battery-grade cobaltosic oxide, LITHIUM BATTERY lithium nitrate and doped chemical MgO are entered according to default stoichiometric proportion
Row dispensing, then carries out sand milling refinement in sand mill, and raw material is sanded and to add the scope of a certain amount of pure water, solid content to be
10wt%, will add the stearmide of 0.02wt% (compared with material quality summation is sanded), by certain in sand grinding process
Sand milling time, the granularity of disposed slurry to be sanded reaches 0.1~0.5 μm, stops being sanded, and releases and slurry to the bucket with stirring is sanded
(opening stirring, slurry each several part is in a uniform state) is placed in son, pending next step treatment.
(2) slurry that step (1) is obtained is carried out into mist projection granulating, prepares spherical small particle cobalt acid lithium presoma, particle
Between 2~7 μm, moisture is within 0.5wt% for size.
(3) dry type cladding：The particle that step (2) is obtained is transferred in coating equipment (double planetary mixer is high mixed
Machine), and a certain amount of cladding material (nano-ZnO) is added, the cladding time is 60min, and covering amount is 0.5wt%, it is ensured that cladding
Thing is evenly coated at spherical lithium cobalt presoma surface.
(4) sinter：Cobalt acid lithium presoma after cladding is placed on carries out high temperature sintering on pushed bat kiln, the cobalt acid of generation semi-finished product
Lithium.Maximum sintering temperature：700~850 DEG C, main warm area sintering time：15 hours, oxygen is passed through, throughput control range is
2m3/h。
(5) crush, crush, screening out iron excessively.
Material characterization：The microstructure of final resulting materials (amplifies 5000 times) as shown in Figure 1.
Embodiment 2
Cobalt acid lithium material is made, chemical formula is LiaCo1-bMbO2
It is that cobalt acid lithium presoma is heat-treated before coating with the difference of embodiment 1, technique is as follows.
(1) battery-grade cobaltosic oxide, LITHIUM BATTERY lithium nitrate and doped chemical MgO are entered according to default stoichiometric proportion
Row dispensing, then carries out sand milling refinement in sand mill, and raw material is sanded and to add the scope of a certain amount of pure water, solid content to be
10wt%, will add the stearmide of 0.02wt% (compared with material quality summation is sanded), by certain in sand grinding process
Sand milling time, the granularity of disposed slurry to be sanded reaches 0.1~0.5 μm, stops being sanded, and releases and slurry to the bucket with stirring is sanded
(opening stirring, slurry each several part is in a uniform state) is placed in son, pending next step treatment.
(2) slurry that step (1) is obtained is carried out into mist projection granulating, prepares spherical small particle cobalt acid lithium presoma, particle
Between 2~7 μm, moisture is within 0.5wt% for size.
(3) it is heat-treated：The particle that step (2) is obtained is heat-treated 3 hours at 200~250 DEG C.
(3) dry type cladding：The particle that step (2) is obtained is transferred in coating equipment (double planetary mixer is high mixed
Machine), and a certain amount of cladding material (nano-ZnO) is added, the cladding time is 60min, and covering amount is 0.5wt%, it is ensured that cladding
Thing is evenly coated at spherical lithium cobalt presoma surface.
(4) sinter：Cobalt acid lithium presoma after cladding is placed on carries out high temperature sintering on pushed bat kiln, the cobalt acid of generation semi-finished product
Lithium.Maximum sintering temperature：600~650 DEG C, main warm area sintering time：15 hours, oxygen is passed through, throughput control range is
2m3/h。
(5) crush, crush, screening out iron excessively.
Embodiment 3-7
From embodiment 1 differ only in doped chemical and ratio is different, the molecular formula of cobalt acid lithium particle is respectively
Li1.15Co0.997Al0.003O2, Li1.05Co0.997Mg0.001Al0.001Ti0.001O2, Li1.1Co0.99Mg0.004Al0.004Ti0.002O2,
Li1.05Co0.992Ni0.002Mn0.004Cr0.002O2, Li1.05Co0.991Ni0.003Mn0.003Cr0.003O2, remaining formula and technique are identical.
Embodiment 8-10
The type for differing only in coating from embodiment 1 is different, but covering amount and other condition all sames, respectively
SnO2, ZnO：SnO2=1:1 (mol ratio), ZnO：SnO2=1:3 (mol ratios).
Embodiment 11-14
The addition for differing only in coating from embodiment 1 is different, respectively 5wt%, 1wt%, 2wt%,
4wt%.
Embodiment 15
The condition for differing only in step (3) heat treatment from embodiment 2 is different, is：It is heat-treated 0.5 hour at 500 DEG C.
Embodiment 16
Solid content when differing only in step (1) wet grinding from embodiment 2 is different, is 40wt%.
Embodiment 17
Amount from the surfactant added when differing only in step (1) wet grinding of embodiment 2 is different, is
0.5wt%.
Embodiment 18-19
Type from the surfactant added when differing only in step (1) wet grinding of embodiment 2 is different, is six
Methyl disilazane, KD-1.
Embodiment 20
The condition for differing only in last sintering from embodiment 2 is different, is 850~1000 DEG C and sinters 3 hours, blowing air
It is 20m to measure3/h。
The chemical property of all of above embodiment resulting materials is characterized, as a result such as table 1.
Table 1
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
Pipe has been described in detail with reference to foregoing embodiments to the present invention, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a kind of cobalt acid lithium material, it is characterised in that main by the cobalt acid lithium particle doped with element M and to be coated on its surface
Coating composition；
The molecular formula of the cobalt acid lithium particle is LiaCo1-bMbO2, wherein, 0.95≤a≤1.15,0.003≤b≤0.01, M is
It is at least one or more of in Mg, Al, Ti, Zr, Ni, Mn, Cr, Mo, W and rare earth element；
The coating is selected from ZnO or SnO2Or both mixing, weight is 0.5~5wt% of the cobalt acid lithium particle,
It is preferred that 1~5wt%, preferably 2~5wt%, preferably 2~4wt%.
2. cobalt acid lithium material according to claim 1, it is characterised in that the M is at least one in Mg, Al, Ti, Zr
Or it is various, preferably at least one or more of in Mg, Al, Ti, more preferably the mol ratio of Mg, Al, Ti is 2:2:1~2.
3. cobalt acid lithium material according to claim 1, it is characterised in that the M is at least one in Ni, Mn, Cr, Mo
Or it is various, preferably at least one or more of in Ni, Mn, Cr, more preferably the mol ratio of Ni, Mn, Cr is 1:1~2:1.
4. the cobalt acid lithium material according to claim any one of 1-3, it is characterised in that the particle diameter of the cobalt acid lithium material is
3-8μm；
Preferably, specific surface area is 0.1~0.5m2/g。
5. the cobalt acid lithium material according to claim any one of 1-3, it is characterised in that 1.05≤a≤1.15,0.003≤b
≤0.008。
6. the cobalt acid lithium material according to claim any one of 1-3, it is characterised in that the coating is ZnO and SnO2With
1:The mol ratio composition of 1-3.
7. the preparation method of the cobalt acid lithium material described in any one of claim 1-6, it is characterised in that comprise the following steps：
According to the proportioning of molecular formula, lithium source, cobalt source, element M source are mixed, is granulated, then in coating described in Surface coating, it
Sinter afterwards, broken, sieving, except iron, obtain final product；
Preferably, also include after the granulation and before the cladding：The particle that granulation is obtained is at 200~500 DEG C
Heat treatment 0.5~3 hour.
8. the preparation method of cobalt acid lithium material according to claim 7, it is characterised in that the method for the mixing is mixing
Wet grinding：Slurry granularity is ground under conditions of solid content is 10~40wt% reach 0.1~0.5 μm；
Preferably, the surfactant that weight is 0.02~0.5wt% of thing to be ground is added in the process of lapping；
Preferably, the surfactant is selected from ammonium polymethacrylate, stearmide, HMDS, KD-1,12
One or more in sodium alkyl sulfonate, preferably stearmide.
Preferably, between 2~7 μm, moisture is preferably within 0.5wt% the granular size for obtaining that granulates；
Preferably, the cladding is dry type cladding.
9. the preparation method of the cobalt acid lithium material according to claim 7 or 8, it is characterised in that described to be sintered to：600~
1000 DEG C sinter 3~15 hours, and throughput is 2~20m3/h。
10. a kind of positive electrode, it is characterised in that including at least the cobalt acid lithium material described in claim any one of 1-6.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110137443A (en) * | 2019-03-18 | 2019-08-16 | 宁德新能源科技有限公司 | Positive electrode and electrochemical appliance comprising the positive electrode |
| CN110336006A (en) * | 2019-07-04 | 2019-10-15 | 中国科学院青岛生物能源与过程研究所 | A kind of high structural stability lithium cobaltate cathode material and preparation method thereof |
| CN111342005A (en) * | 2020-03-12 | 2020-06-26 | 江西省倍特力新能源有限责任公司 | Preparation method of lithium ion battery of electronic cigarette |
| EP3686159A1 (en) * | 2019-01-16 | 2020-07-29 | Ningde Amperex Technology Limited | Precursor of lithium cobalt oxide and preparation method thereof and composite of lithium cobalt oxide prepared from the precursor of lithium cobalt oxide |
| CN111960467A (en) * | 2020-08-27 | 2020-11-20 | 长沙矿冶研究院有限责任公司 | Preparation process of multi-element material |
| CN113113580A (en) * | 2021-03-12 | 2021-07-13 | 江门市力源电子有限公司 | Special high-rate high-capacity high-platform lithium ion battery for electronic cigarette |
| CN114068939A (en) * | 2022-01-17 | 2022-02-18 | 英德市科恒新能源科技有限公司 | Lithium cobaltate positive electrode material, preparation method thereof and lithium ion battery |
| CN114725367A (en) * | 2022-04-22 | 2022-07-08 | 格林美（无锡）能源材料有限公司 | Lithium cobaltate positive electrode material and preparation method and application thereof |
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| CN113113580A (en) * | 2021-03-12 | 2021-07-13 | 江门市力源电子有限公司 | Special high-rate high-capacity high-platform lithium ion battery for electronic cigarette |
| CN113113580B (en) * | 2021-03-12 | 2022-06-07 | 江门市力源电子有限公司 | Special high-rate high-capacity high-platform lithium ion battery for electronic cigarette |
| CN114068939A (en) * | 2022-01-17 | 2022-02-18 | 英德市科恒新能源科技有限公司 | Lithium cobaltate positive electrode material, preparation method thereof and lithium ion battery |
| CN114725367A (en) * | 2022-04-22 | 2022-07-08 | 格林美（无锡）能源材料有限公司 | Lithium cobaltate positive electrode material and preparation method and application thereof |
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