CN103000870B - Compounding method for LizNixCoyMn (1-x-y) O2 material - Google Patents
Compounding method for LizNixCoyMn (1-x-y) O2 material Download PDFInfo
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Abstract
The invention relates to a compounding method for a LizNixCoyMn (1-x-y) O2 material. The compounding method comprises the following steps of: 1, preparing compact small-grained spherical LizNixCoyMn (1-x-y) O2 powder; 2, preparing compact large-grained spherical LizNixCoyMn (1-x-y) O2 powder; and 3, compounding the two LizNixCoyMn (1-x-y) O2 materials. According to the compounding method provided by the invention, the two LizNixCoyMn (1-x-y) O2 powders with different size distributions and tap densities are compounded and mixed for optimizing the grain size distribution of the material; the large and small particles are tightly matched for solving the problem that the compaction density and energy density are low when a ternary material is independently utilized; and the mass density is higher than 600 mAh/cm＜3＞, specific surface area is smaller than 0.23g/m＜2＞, safety and cyclicity of the material are improved. Besides, the compounding method has a simple process and low cost, is very suitable for industrial operation, and has an extensive development prospect.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, more particularly to a kind of LiZNiXCoYMn1-X-YO2Material
Material preparation method.
Background technology
Cobalt acid lithium is due to energy density and the characteristics of high compacted density, being the main flow positive pole material of lithium ion battery all the time
Material, through the development of about 30 years, a few near limits of exploitation of cobalt acid lithium performance.In the present that high-energy-density new material is a dark horse
My god, the energy density of cobalt acid lithium is difficult to the demand for meeting current 3C Product energy density；In terms of compacted density, cobalt acid lithium tool
There is good electrode machining performance, morphology control has tended to perfect, and its compacted density has also reached the pole of itself at present
Limit, as a consequence it is hardly possible to have a space for being lifted once again, and cobalt acid lithium also to there is safety undesirable with overcharge resistance performance, and for
The dependency of rare cobalt resource, the defect such as cycle performance is relatively poor.The LiNiO for developing at present2With NCA and nickelic ternary
Although the energy density of material has different advantages compared with cobalt acid lithium, due to a series of reasons such as technique is immature so that
Cobalt acid lithium still occupies dominant position in field of lithium ion battery anode.
To solve poor cobalt acid lithium overcharge resistance performance, poor stability and causing material cost to the dependence of excessive noble metal cobalt
The problem of higher grade, people have developed the ternary material Li of hydroxide coprecipitation step preparationZNiXCoYMn1-X-YO2, the material
It is good with specific capacity height, good cycle, safety, the advantage such as cheap.But the short grained secondary agglomeration body of the material exists
Generation is easy to during roll-in broken, is kept not under high-pressure solid even if the primary particle of aggregate being done and also be difficult to greatly guarantee material
Rupture, breakage of particles necessarily causes active material not tight with the contact of binding agent conductive agent, and then causes polarization, makes electric polarity
Can be deteriorated, therefore the material is not suitable for being used alone.The ternary material and cobalt acid lithium mixing are made by majority battery manufacturers at present
With as once oarse-grained monocrystalline cobalt acid lithium provides support for ternary material, so ensure that blended anode material is good
Electrode machining performance, the compacted density of blended anode material is slightly less than the compacted density of cobalt acid lithium, a little higher than cobalt of energy density
Sour lithium, but still there is multiple sintering, complex process, high energy consumption, mixed powder matching in the blended anode material.
Jing retrieval discoveries, Application No. 200910110132.9, Publication No. CN101707252A, entitled " polycrystalline cobalt
The Chinese invention patent of Ni-Mn ternary positive electrode and preparation method thereof, secondary lithium battery ", is produced by high temperature fusion many
Different positive electrodes is grown to serve as an entirety, is combined with the advantage of mixing material, table by brilliant Co-Ni-Mn ternary positive electrode
Reveal good chemical property, compacted density can reach 3.9g/cm3More than, monolithic pole piece energy density is more than 570mAh/
cm3(pole piece energy density mAh/cm3=initial discharge capacity mAh/g X compacted densities g/cm3)；But this material does not still have
The safety for having the state of the art broken away from cobalt acid lithium multifuel combustion, material does not improve, although and cobalt acid lithium about 570mAh/cm3It is single
Potential energy metric density quite, but due to multiple sintering and mixes, and the use of more cobalt, weakens its technical advantage again.
The content of the invention
The present invention provides process is simple to solve technical problem present in known technology, and cost of manufacture is cheap, not only
Compacted density is high, and energy density is high, and monolithic pole piece energy density is more than 600mAh/cm3, while being especially suitable for scale metaplasia
The Li of productZNiXCoYMn1-X-YO2Material preparation method.
It is of the invention by solving the technical scheme that technical problem is adopted present in background technology to be：
Step 1：Prepare the spherical Li of fine and close little particleZNiXCoYMn1-X-YO2
(1) step prepares solution
The soluble nickel of stoichiometric proportion, cobalt, manganese salt are weighed, nickel cobalt manganese mixing salt solution is configured to, is designated as solution a；With
Sodium hydroxide or potassium hydroxide are precipitant, and ammonia or ammonium salt are chelating agent, according to ammonia alkali mol ratio 0.2-0.5 mixed precipitant
Solution and enveloping agent solution, are designated as solution b；
The course of reaction of step (2) two kinds of solution
In the reactor of the 40-70 DEG C of temperature that two kinds of solution cocurrents of a and b pump into inert atmosphere protection, with 300-400r/
Min rotating speeds are stirred, and pH value 11.7-13, isothermal reaction 24-35 hours obtain fine and close little particle type presoma NiXCoYMn1-X-Y
(OH)2Suspension；
Step (3) solid-liquid separation
By step (2) in obtained NiXCoYMn1-X-Y(OH)2Suspension carries out solid-liquid separation, obtains fine and close little particle type
NiXCoYMn1-X-Y(OH)2Filter cake, washing filter cake are dried to filter cake between 100-140 DEG C to the pH7-8 of cleaning mixture
Obtain NiXCoYMn1-X-Y(OH)2；
(4) step prepares the spherical Li of fine and close little particleZNiXCoYMn1-X-Y(OH)2
According to stoichiometric proportion 1:1-3 weighs the step Ni that (3) middle drying is obtainedXCoYMn1-X-Y(OH)2And Li2CO3,
After 300-500r/min mixes 15 minutes, then mixed 5 minutes with 700-1000r/min, form NiXCoYMn1-X-Y(OH)2With
Li2CO3Homogeneous mixture；By 350-470 DEG C of insulation 4-8 hour of homogeneous mixture, then temperature is adjusted to into 900-950 DEG C of insulation
15-18 hours, are cooled to room temperature, cross 200-400 mesh sieves, that is, complete the spherical Li of fine and close little particleZNiXCoYMn1-X-YO2Preparation
Process；In LiZNiXCoYMn1-X-YO2Middle Z >=1, X, Y, X+Y≤1；
Step 2：Prepare fine and close large granular spherical LiZNiXCoYMn1-X-YO2
(1) step prepares solution
The ammonia alkali molar ratio (1) of step in step 1 is changed to into 0.6-1, other conditions are (1) identical with step in step 1；
The course of reaction of step (2) two kinds of solution
By step in step 1, (2) speed of agitator is 100-250r/mim, and pH value 11.3-11.5, isothermal reaction 36-48 are little
When, other conditions are (2) identical with step in step 1；
Step (3) solid-liquid separation
It is (3) identical with step in step 1；
(4) step prepares fine and close large granular spherical LiZNiXCoYMn1-X-YO2
By the step of step 1 (4) in " 900-950 be incubated 15-18 hours " be changed to " 960-1000 DEG C of insulation 20-30 hour ",
Other conditions are (4) identical with step in step 1；Fine and close large granular spherical Li is completedZNiXCoYMn1-X-YO2Preparation process；
Step 3：To two kinds of LiZNiXCoYMn1-X-YO2Compounded
According to mass ratio 1-10:10, the spherical Li of fine and close little particle prepared by step 1ZNiXCoYMn1-X-YO2Make with step 2
Standby fine and close large granular spherical LiZNiXCoYMn1-X-YO2Insert in dry batch mixer, with the speed mixing 10- of 300-500r/min
20 minutes, that is, make LiZNiXCoYMn1-X-YO2Compounding positive electrode.
The present invention can also be adopted the following technical scheme that：
The LiZNiXCoYMn1-X-YO2Middle Z=1, X=1/3, Y=1/3.
In the step 1, the (1) described soluble nickel of step, cobalt, manganese salt are respectively nickel sulfate, cobaltous sulfate, manganese sulfate.
The present invention has the advantages and positive effects that：
1. the present invention is distributed the Li with tap density using by two kinds of different grain sizesZNiXCoYMn1-X-YO2Powder body compounding, machine
Tool mixes, and optimizes the particle size distribution of material, coordinates tight between size particles, is compacted close when solving ternary material exclusive use
Degree and the low problem of energy density, mass density reach 600mAh/cm3More than；The material specific surface area of the invention is less,
The security performance and cycle performance of material, and process is simple are improve on the premise of keeping material electrochemical activity, it is with low cost,
Industrialization operation is especially suitable for, with wide DEVELOPMENT PROSPECT.
2. the present invention is as a result of fine and close large granular spherical LiNi1/3Co1/3Mn1/3O2Support, material is making pole piece
Avoid spherical short grained broken during roll-in, improve the fillibility of powder body, it is to avoid material is contacted with binding agent, conductive agent
Untight problem, the material also have excellent fillibility and mobility, further improve the energy density of material；By
It is larger in the primary particle of material, more than 1 μm, so the material has preferable high rate performance and cycle performance simultaneously.
Description of the drawings
Fig. 1 is the Laser particle-size distribution figure that the embodiment of the present invention 1 prepares material；
Fig. 2 is the electron scanning micrograph (SEM) that the embodiment of the present invention 1 prepares material.
Specific embodiment
For the content of the invention, feature and effect of the present invention can be further appreciated that, following examples are hereby enumerated, and coordinates accompanying drawing
Describe in detail as follows：
Embodiment 1：
Step 1：Prepare the spherical LiNi of fine and close little particle1/3Co1/3Mn1/3O2
(1) step prepares solution
Stoichiometric proportion is weighed for 1:1:1 nickel sulfate, cobaltous sulfate, manganese sulfate, are configured to the mixing of nickel cobalt mn sulphate molten
Liquid, is designated as solution a；With sodium hydroxide as precipitant, ammonia is chelating agent, according to 0.37 ammonia alkali molar ratio mixed precipitant
Solution and enveloping agent solution, are designated as solution b；
The course of reaction of step (2) two kinds of solution
Two kinds of solution cocurrents of a and b have pumped into nitrogen atmosphere and have protected, and volume is 3m3Stainless steel cauldron in, it is warm at 50 DEG C
Under degree, stirred with 300r/mim rotating speeds, make pH value in reaction be maintained at 11.8 ± 0.05 or so using on-line pH value control system, perseverance
Temperature reaction 32 hours, obtains fine and close little particle type presoma Ni1/3Co1/3Mn1/3(OH)2Suspension；
Step (3) solid-liquid separation
By step (2) in obtained Ni1/3Co1/3Mn1/3(OH)2Suspension is inserted the closed pressure filtration of rustless steel and washs one
After body machine, apply 0.5Mpa pressure, to Ni1/3Co1/3Mn1/3(OH)2Suspension carries out solid-liquid separation, obtains fine and close little particle type
Ni1/3Co1/3Mn1/3(OH)2Filter cake, with 80 DEG C of deionized water wash filter cakes, until accurate pH test paper filtrates tested pH value is to 7-8
Till, filter cake is placed in air dry oven after drying in 15 hours is carried out at 120 DEG C, by Ni1/3Co1/3Mn1/3(OH)2Filter cake strikes
It is broken；
(4) step prepares the spherical LiNi of fine and close little particle1/3Co1/3Mn1/3O2
According to stoichiometric proportion 1:1.04 weigh step (3) in the Ni that breaks into pieces1/3Co1/3Mn1/3(OH)2And Li2CO3, by institute
State bi-material and insert high speed mixer, first with the mixed on low speed 15 minutes of 400r/min, then with 5 points of 700r/min mixed at high speed
Clock, forms Ni1/3Co1/3Mn1/3(OH)2And Li2CO3Homogeneous mixture；Homogeneous mixture is inserted in push-plate type kiln,
450 DEG C are incubated 4 hours, then temperature is adjusted to 950 DEG C of insulations 15 hours, are cooled to room temperature with furnace temperature, cross 300 mesh sieves, that is, complete
The spherical LiNi of fine and close little particle1/3Co1/3Mn1/3O2Preparation process；Jing is tested, the particle size distribution of the material between 2-8 μm,
Primary particle particle diameter is more than 1 μm, tap density 2.46g/cm3, compacted density 3.45g/cm3。
Step 2：Prepare fine and close large granular spherical LiNi1/3Co1/3Mn1/3O2
(1) step prepares solution
Ammonia alkali molar ratio is changed to into 0.65, other conditions are (1) identical with step in step 1；
The course of reaction of step (2) two kinds of solution
Speed of agitator is 200r/mim, and pH value 11.4 ± 0.05, isothermal reaction 40 hours are walked in other conditions and step 1
It is rapid (2) identical；
Step (3) solid-liquid separation
It is (3) identical with step in step 1；
(4) step prepares fine and close large granular spherical LiNi1/3Co1/3Mn1/3O2
By the step of step 1 (4) in " 950 DEG C be incubated 15 hours " be changed to " 1000 DEG C are incubated 20 hours ", other conditions and step
In rapid 1, step is (4) identical；Form fine and close large granular spherical LiNi1/3Co1/3Mn1/3O2Material, it is identical with step 1,300 mesh sieves are crossed,
Dense spherical bulky grain LiNi is completed1/3Co1/3Mn1/3O2Preparation process；Jing is tested, and the particle size distribution of the material is in 7-26 μ
Between m, primary particle particle diameter is more than 1 μm, tap density 2.88g/cm3, compacted density 3.64g/cm3。
Step 3：To two kinds of LiNi1/3Co1/3Mn1/3O2Compounded
According to mass ratio 1:5, the spherical LiNi of fine and close little particle prepared by step 11/3Co1/3Mn1/3O2Prepare with step 2
Fine and close large granular spherical LiNi1/3Co1/3Mn1/3O2, insert in dry batch mixer, mixed 15 minutes with the speed of 400r/min,
LiNi of the present invention is made1/3Co1/3Mn1/3O2Compounding positive electrode；Jing tests the material particle size and is distributed between 4-23 μm, shakes
Real density 2.94g/cm3, compacted density 3.85g/cm3, monolithic pole piece energy density 613mAh/cm under 0.5C3；Jing BET methods are surveyed
It is fixed, specific surface area 0.25m2/g。
Embodiment 2：
It is 1 in mass ratio:10, the spherical LiNi of fine and close little particle prepared by step 1 in embodiment 11/3Co1/3Mn1/3O2With
Fine and close large granular spherical LiNi prepared by step 21/3Co1/3Mn1/3O2Insert in dry batch mixer, it is mixed with the speed of 400r/min
Close 15 minutes, that is, make the compounding positive electrode LiNi of the present invention1/3Co1/3Mn1/3O2；The material particle size be distributed in 7-26 μm it
Between, tap density 2.96g/cm3, compacted density 3.79g/cm3, monolithic pole piece energy density 605mAh/cm under 0.5C3.By few
The compounding mixing of amount, the compacted density of the positive electrode are compared homogenous material with tap density and are improved, and energy density is better than
LiNi prepared by single lithium cobaltate cathode material and other methods1/3Co1/3Mn1/3O2Positive electrode.
Embodiment 3：
It is 3 in mass ratio:10, the spherical LiNi of fine and close little particle prepared by step 1 in embodiment 11/3Co1/3Mn1/3O2With
Fine and close large granular spherical LiNi prepared by step 21/3Co1/3Mn1/3O2Insert in dry batch mixer, it is mixed with the speed of 400r/min
Close 15 minutes, that is, make the compounding positive electrode LiNi of the present invention1/3Co1/3Mn1/3O2；The material particle size is distributed in 4-21 microns
Between, tap density 2.83g/cm3, compacted density 3.67g/cm3, monolithic pole piece energy density 591mAh/cm under 0.5C3.Pass through
Compounding mixing, the compacted density of the positive electrode are compared homogenous material and are increased, and energy density is higher than single cobalt acid lithium just
LiNi prepared by pole material and other methods1/3Co1/3Mn1/3O2Positive electrode.
Embodiment 4：
It is 1 in mass ratio:1, the spherical LiNi of fine and close little particle prepared by step 1 in embodiment 11/3Co1/3Mn1/3O2With
Fine and close large granular spherical LiNi prepared by step 21/3Co1/3Mn1/3O2Insert in dry batch mixer, it is mixed with the speed of 400r/min
Close 15 minutes, that is, make the compounding positive electrode LiNi of the present invention1/3Co1/3Mn1/3O2；The material particle size be distributed in 5-18 μm it
Between, tap density 2.73g/cm3, compacted density 3.55g/cm3, monolithic pole piece energy density 578mAh/cm under 0.5C3.By multiple
With mixing, due to little particle type LiNi1/3Co1/3Mn1/3O2Mixed proportion is more, and the compacted density of the positive electrode is compared single
Bulky grain section bar material LiNi1/3Co1/3Mn1/3O2Decrease, but energy density and single lithium cobaltate cathode material be still suitable,
Still there are during exclusive use cost and security advantages.
Comparative example：
Domestic commercially available monocrystalline cobalt acid lithium, Granularity Distribution between 8-32 μm, tap density 2.97g/cm3, compacting
Density 4.05g/cm3, monolithic pole piece energy density 535mAh/cm under 0.5C3, specific surface area 0.23g/m2, the material energy densities
Do not surmount the energy density of the compounding positive electrode of the present invention, and compare complex material of the invention, price is higher, and
It is not suitable for electrokinetic cell field.
By the comparison of embodiment of the present invention 1-4 and known comparative example data, and combine Fig. 1 and Fig. 2, it can be seen that
The optimization of material particle size distribution of material prepared by the present invention, coordinates tight between size particles, to solve ternary material individually make
The low problem of used time compacted density and energy density, mass density reach 600mAh/cm3More than；The material of the invention compares table
Area is less, and the security performance and cycle performance of material, and technique letter are improve on the premise of material electrochemical activity is kept
It is single, it is with low cost, it is especially suitable for industrialization operation.
Although being described to the preferred embodiments of the present invention above in conjunction with accompanying drawing, the invention is not limited in
The specific embodiment stated, above-mentioned specific embodiment are only schematic, be not it is restricted, this area it is common
Technical staff in the case of without departing from present inventive concept and scope of the claimed protection, may be used also under the enlightenment of the present invention
To make many forms.These are belonged within protection scope of the present invention.
Claims (3)
1.LiZNiXCoYMn1-X-YO2Material preparation method, it is characterised in that：Including following preparation process：
Step 1：Prepare the spherical Li of fine and close little particleZNiXCoYMn1-X-YO2
(1) step prepares solution
The soluble nickel of stoichiometric proportion, cobalt, manganese salt are weighed, nickel cobalt manganese mixing salt solution is configured to, is designated as solution a；With hydrogen-oxygen
It is precipitant to change sodium or potassium hydroxide, and ammonia or ammonium salt are chelating agent, according to ammonia alkali mol ratio 0.2-0.5 mixed precipitation agent solution
And enveloping agent solution, it is designated as solution b；
The course of reaction of step (2) two kinds of solution
In the reactor of the 40-70 DEG C of temperature that two kinds of solution cocurrents of a and b pump into inert atmosphere protection, with 300-400r/min
Rotating speed is stirred, and pH value 11.7-13, isothermal reaction 24-35 hours obtain fine and close little particle type presoma NiXCoYMn1-X-Y(OH)2
Suspension；
Step (3) solid-liquid separation
By step (2) in obtained NiXCoYMn1-X-Y(OH)2Suspension carries out solid-liquid separation, obtains fine and close little particle type
NiXCoYMn1-X-Y(OH)2Filter cake, washing filter cake are dried to filter cake between 100-140 DEG C to the pH7-8 of cleaning mixture
Obtain NiXCoYMn1-X-Y(OH)2；
(4) step prepares the spherical Li of fine and close little particleZNiXCoYMn1-X-Y(OH)2
According to stoichiometric proportion 1:1-3 weighs the step Ni that (3) middle drying is obtainedXCoYMn1-X-Y(OH)2And Li2CO3, 300-
After 500r/min mixes 15 minutes, then mixed 5 minutes with 700-1000r/min, form NiXCoYMn1-X-Y(OH)2And Li2CO3's
Homogeneous mixture；By 350-470 DEG C of homogeneous mixture insulation 4-8 hours, then that temperature is adjusted to 900-950 DEG C of insulation 15-18 is little
When, room temperature is cooled to, 200-400 mesh sieves is crossed, that is, is completed the spherical Li of fine and close little particleZNiXCoYMn1-X-YO2Preparation process；
LiZNiXCoYMn1-X-YO2Middle Z >=1, X, Y, X+Y≤1；
Step 2：Prepare fine and close large granular spherical LiZNiXCoYMn1-X-YO2
(1) step prepares solution
The ammonia alkali molar ratio (1) of step in step 1 is changed to into 0.6-1, other conditions are (1) identical with step in step 1；
The course of reaction of step (2) two kinds of solution
By step in step 1 (2) speed of agitator be 100-250r/mim, pH value 11.3-11.5, isothermal reaction 36-48 hours, its
Its condition is (2) identical with step in step 1；
Step (3) solid-liquid separation
It is (3) identical with step in step 1；
(4) step prepares fine and close large granular spherical LiZNiXCoYMn1-X-YO2
By the step of step 1 (4) in " 900-950 be incubated 15-18 hours " be changed to " 960-1000 DEG C of insulation 20-30 hour ", other
Condition is (4) identical with step in step 1；Fine and close large granular spherical Li is completedZNiXCoYMn1-X-YO2Preparation process；
Step 3：To two kinds of LiZNiXCoYMn1-X-YO2Compounded
According to mass ratio 1-10:10, the spherical Li of fine and close little particle prepared by step 1ZNiXCoYMn1-X-YO2With step 2 preparation
Fine and close large granular spherical LiZNiXCoYMn1-X-YO2Insert in dry batch mixer, with 10-20 point of the speed mixing of 300-500r/min
Clock, that is, make LiZNiXCoYMn1-X-YO2Compounding positive electrode.
2. Li according to claim 1ZNiXCoYMn1-X-YO2Material preparation method, it is characterised in that：It is described
LiZNiXCoYMn1-X-YO2Middle Z=1, X=1/3, Y=1/3.
3. Li according to claim 1ZNiXCoYMn1-X-YO2Material preparation method, it is characterised in that：Step in the step 1
(1) described soluble nickel, cobalt, manganese salt are respectively nickel sulfate, cobaltous sulfate, manganese sulfate.
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| CN103904310A (en) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | Preparation method for mixed nickel-cobalt-lithium manganate material |
| CN103811746B (en) * | 2014-02-20 | 2017-02-15 | 新乡锦润科技有限公司 | Method for preparing nano ternary composite lithium ion anode material by utilizing microemulsion |
| CN103979611A (en) * | 2014-05-12 | 2014-08-13 | 南京工业大学 | High-tap-density nickel cobalt lithium manganate layered cathode material prepared by improved coprecipitation method and preparing method thereof |
| CN105489881A (en) * | 2016-01-12 | 2016-04-13 | 哈尔滨工业大学 | Method for improving tap density of ternary nickel-cobalt-manganese cathode material for lithium-ion battery |
| CN106159244A (en) * | 2016-09-27 | 2016-11-23 | 宁德时代新能源科技股份有限公司 | Lithium battery cathode material, preparation method thereof and lithium ion battery for power |
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| CN109888242A (en) * | 2019-03-12 | 2019-06-14 | 四川纳创时代新能源科技有限公司 | A kind of high-tap density cobalt nickel lithium manganate ternary material and preparation method thereof |
| CN110010889B (en) * | 2019-04-17 | 2021-09-07 | 贵州容百锂电材料有限公司 | High-compaction high-stability high-nickel cathode material, preparation method thereof and lithium ion battery |
| CN113921782A (en) * | 2021-09-26 | 2022-01-11 | 宁波容百新能源科技股份有限公司 | Ultrahigh nickel ternary cathode material with high compaction and high energy density |
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| CN101707252A (en) * | 2009-11-09 | 2010-05-12 | 深圳市振华新材料股份有限公司 | Polycrystal Co-Ni-Mn ternary anode material and preparation method thereof as well as secondary lithium-ion battery |
| CN101789523A (en) * | 2009-01-28 | 2010-07-28 | 三洋电机株式会社 | Nonaqueous electrolyte secondary battery |
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| CN101789523A (en) * | 2009-01-28 | 2010-07-28 | 三洋电机株式会社 | Nonaqueous electrolyte secondary battery |
| CN101707252A (en) * | 2009-11-09 | 2010-05-12 | 深圳市振华新材料股份有限公司 | Polycrystal Co-Ni-Mn ternary anode material and preparation method thereof as well as secondary lithium-ion battery |
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