CN109786695A - A kind of high magnification nickel-cobalt lithium manganate cathode material and preparation method thereof - Google Patents
A kind of high magnification nickel-cobalt lithium manganate cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high magnification nickel-cobalt lithium manganate cathode materials and preparation method thereof, comprising the following steps: (1) by water soluble organic substance is soluble in water prepare solution after, be added nickel cobalt manganese presoma, ultrasonic treatment, through being dried to obtain dried powder;(2) dried powder prepared by step (1) is mixed with lithium source, is pre-sintered in inert gas, obtains pre-sintered mass;(3) pre-sintered mass of step (2) preparation, it is broken through oversintering, grinding, prepare nickel-cobalt lithium manganate cathode material.The present invention is by the way that water soluble organic substance to be embedded into nickel cobalt manganese presoma, water soluble organic substance is set to be carbonized by pre-sintering, skeleton is thus formed in nickel cobalt manganese presoma, porous structure is finally formed in nickle cobalt lithium manganate in turn by high temperature sintering removal skeleton, the nickel-cobalt lithium manganate cathode material with porous structure is obtained, the discharge capability under high magnification is significantly improved.
Description
Technical field
The present invention relates to field of lithium ion battery more particularly to a kind of high magnification nickel-cobalt lithium manganate cathode material and its preparations
Method.
Background technique
Lithium ion battery is as a kind of efficient green energy resource, not only with energy density is high, self discharge is small, memoryless effect
Answer, but also have many advantages, such as to have extended cycle life, open-circuit voltage it is high, be widely used in 3C, electric tool, model plane and new energy vapour
The fields such as vehicle.Wherein field of power tools and aviation model field, usually 3C field battery more demanding to the high rate performance of battery
Several times or even dozens of times.Key component one of of the positive electrode as lithium ion battery, the direct shadow of the superiority and inferiority of high rate performance
Ring the height of lithium ion battery high rate performance.
It is mainstream high-multiplying-power battery institute currently on the market since lithium cobaltate cathode material electric conductivity and ion mobility are good
Lithium cobaltate cathode material, and LiFePO4 and LiMn2O4 by lithium ion mobility rate, energy density, high temperature performance and
Stability etc. influences, and restricts it in the application in high-multiplying-power battery field.Although cobalt acid lithium high rate capability is excellent, cost compared with
It is high;Nickle cobalt lithium manganate is due to similar to cobalt acid lithium structure, and energy density is high, high temperature performance is good and inexpensive, and by market blueness
It looks at.
There is cationic mixing in nickel-cobalt lithium manganate cathode material, hinder material internal lithium ion mobility, lead to nickel cobalt
The problems such as manganate cathode material for lithium voltage platform under the conditions of high power charging-discharging is low, Capacity fading is fast and stability is poor,
It is limited in the application in the fields such as electric tool, model plane.Therefore, it is really necessary to provide a kind of high performance nickle cobalt lithium manganate material
Material is to improve above-mentioned deficiency.
Summary of the invention
The object of the present invention is to provide a kind of high magnification nickel-cobalt lithium manganate cathode materials and preparation method thereof, by material
Inside introduces porous structure, and to solve, nickel-cobalt lithium manganate cathode material voltage platform under the conditions of high power charging-discharging is low, recycles and holds
The problems such as amount decaying is fast and stability is poor.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of high magnification nickel-cobalt lithium manganate cathode material preparation method, comprising the following steps:
(1) by water soluble organic substance is soluble in water solution is made after, be added nickel cobalt manganese presoma, ultrasonic treatment, then exist
80-200 DEG C of dry 2-10h, obtains dried powder;
(2) dried powder prepared by step (1) is mixed with lithium source, is pre-sintered 3- in 300-500 DEG C of inert gas
10h obtains pre-sintered mass;
(3) by step (2) resulting pre-sintered mass, 6-20h is sintered in 600-1000 DEG C of temperature, sintering gas is sky
Gas or oxygen, cooled to room temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material.
As a preferred technical solution, in the step (1) water soluble organic substance be glucose, sucrose, polyethylene glycol and
At least one of citric acid.
Water soluble organic substance accounts for the mass concentration of solution and is in solution in the step (1) as a preferred technical solution,
5-30%.
Nickel cobalt manganese presoma accounts for the 30-70% of solution quality in the step (1) as a preferred technical solution,.
Nickel cobalt manganese presoma is Ni in the step (1) as a preferred technical solution,xCoyMn1-x-y(OH)2, wherein 0 < x
< 0.6,0 < y < 1,0 < x+y < 1, median particle diameter (D50) are 1-7um, specific surface area 5-20m2/g。
Dried powder and lithium source molar ratio are 1:(1.0-1.15 in the step (2) as a preferred technical solution).
The lithium source in the step (2) is lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate as a preferred technical solution,
At least one of.
Inert gas is nitrogen or argon gas in the step (2) as a preferred technical solution,.
The heating rate being sintered in the step (3) as a preferred technical solution, is 1-20 DEG C/min.
The nickel cobalt manganese anode material being prepared by the above method, median particle diameter (D50) are 1-10um, specific surface area
For 0.4-4.0m2/g。
The invention has the following advantages:
(1) present invention is by water soluble organic substance formation solution soluble in water being added after nickel cobalt manganese presoma by super
Sound mixing is uniformly mixed water soluble organic substance with nickel cobalt manganese presoma, is successfully embedded in water soluble organic substance by drying steps
Into nickel cobalt manganese presoma, then so that water soluble organic substance is carbonized by pre-sintering, thus forms bone in nickel cobalt manganese presoma
Frame finally forms porous structure by high temperature sintering removal skeleton progress in nickle cobalt lithium manganate, obtains having porous structure
Nickel cobalt manganese anode material.Porous structure can significantly improve the specific surface area of nickel cobalt manganese anode material, to increase lithium-ion electric
Lithium ion and electron transfer diffusion rate are improved in the reactivity site of pond anode, increase capacity of lithium ion battery, improve it and put
Electric multiplying power improves its discharge capability under high power charging-discharging.
(2) water soluble organic substance that the present invention selects is common raw material, cheap and nontoxic, is easy to grasp
Make, and preparation process of the present invention is simple, it is easy to accomplish industrialized production.
(3) soft-package battery 1C/30C high rate performance made of the nickel-cobalt lithium manganate cathode material obtained through the invention is significant
It improves, discharging efficiency is 145.7mAh/g up to 30C discharge capacity after 90% or more, 1C charging for the first time, and 30C discharge capacity is 1C
87.0%, 30C electric discharge mean voltage be 3.29V.
Detailed description of the invention
Fig. 1 is the SEM scanning electron microscope (SEM) photograph of nickel-cobalt lithium manganate cathode material prepared by embodiment 1;
Fig. 2 is the discharge curve of full battery 30C made of the nickel-cobalt lithium manganate cathode material of the preparation of embodiment 1;
Fig. 3 is nickel-cobalt lithium manganate cathode material scanning electron microscope (SEM) photograph prepared by comparative example 1;
Fig. 4 is the discharge curve of full battery 30C made of the nickel-cobalt lithium manganate cathode material of the preparation of comparative example 1.
Specific embodiment
Below with reference to embodiment, the present invention will be further explained.Obviously, described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, comprising the following steps:
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) it is added to mass concentration and is
In 10% glucose solution, nickel cobalt manganese presoma additional amount accounts for the 15% of solution quality, and ultrasound simultaneously stirs 0.5h, then exists
Dry 5h, obtains dried powder at 150 DEG C;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.08 with lithium acetate,
It is sintered 450 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
The SEM shape appearance figure of nickel-cobalt lithium manganate cathode material obtained by the present embodiment, as shown in Figure 1, as can be seen from Figure 1: institute
Obtaining nickel-cobalt lithium manganate cathode material pattern is in agglomerated particle, has pore structure between agglomerated particle, and pore structure is obvious;
Nickel-cobalt lithium manganate cathode material obtained by the present embodiment prepares soft-package battery 1C/30C high rate performance, as a result such as 1 He of table
Shown in Fig. 2, it will thus be seen that full battery 0.2C capacity is 166.9mAh/g, and discharging efficiency is 30C after 92.1%, 1C charging for the first time
Discharge capacity is 146.7mAh/g, and 30C discharge capacity is that 87.9%, the 30C electric discharge mean voltage of 0.2C is 3.29V.
Comparative example 1
A kind of preparation method of nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) with lithium acetate press nickel cobalt manganese
Metal is mixed with lithium molar ratio 1:1.08, is sintered 450 DEG C of pre-burning 5h under a nitrogen;
(2) material after step (1) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Unlike the first embodiment: comparative example 1 is added without glucose, other techniques are same as Example 1.
The SEM shape appearance figure of nickel-cobalt lithium manganate cathode material obtained by this comparative example, as shown in figure 3, as can be seen from Figure 3:
Sample topography is in agglomerated particle, and compact-sized, without obvious pore structure in agglomerated particle;It is compared with Fig. 1 it is found that embodiment
1, by the insertion of dissolved organic matter, may significantly improve the internal structure of nickel-cobalt lithium manganate cathode material, be formed in the interior thereof more
Hole on framework improves its specific surface area.
Nickel-cobalt lithium manganate cathode material obtained by the present embodiment prepares soft-package battery 1C/30C high rate performance, as a result table 1 and Fig. 4
It is shown, it will thus be seen that full battery 0.2C capacity is 163.2mAh/g, and discharging efficiency is 30C electric discharge after 88.5%, 1C charging for the first time
Capacity is 134.8mAh/g, and 30C discharge capacity is that 82.6%, the 30C electric discharge mean voltage of 0.2C is 3.21V.
Embodiment 2
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) it is added to mass concentration and is
In 20% glucose solution, nickel cobalt manganese presoma additional amount accounts for the 15% of solution quality, and ultrasound simultaneously stirs 0.5h, then exists
Dry 8h, obtains dried powder at 80 DEG C;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.02 with lithium acetate,
It is sintered 300 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Nickel-cobalt lithium manganate cathode material obtained by the present embodiment prepares soft-package battery 1C/30C high rate performance, as a result 1 He of table
Shown in Fig. 2, it will thus be seen that full battery 0.2C capacity is 168.3mAh/g, and discharging efficiency is 30C after 91.8%, 1C charging for the first time
Discharge capacity is 146.6mAh/g, and 30C discharge capacity is that 87.1%, the 30C electric discharge mean voltage of 0.2C is 3.31V.
Embodiment 3
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) it is added to mass concentration and is
In 30% glucose solution, nickel cobalt manganese presoma additional amount accounts for the 15% of solution quality, and ultrasound simultaneously stirs 0.5h, then exists
Dry 5h, obtains dried powder at 120 DEG C;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.1 with lithium acetate,
It is sintered 300 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Nickel-cobalt lithium manganate cathode material obtained by the present embodiment prepares soft-package battery 1C/30C high rate performance, as a result 1 institute of table
Show, it will thus be seen that full battery 0.2C capacity is 167.5mAh/g, and discharging efficiency is 30C electric discharge appearance after 92.6%, 1C charging for the first time
Amount is 145.7mAh/g, and 30C discharge capacity is that 87.0%, the 30C electric discharge mean voltage of 0.2C is 3.29V.
Embodiment 4
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) it is added to mass concentration and is
In 10% polyethylene glycol (molecular weight 400) aqueous solution, nickel cobalt manganese presoma additional amount accounts for the 15% of solution quality, and ultrasound is simultaneously stirred
0.5h is mixed, then the dry 5h at 150 DEG C, obtains dried powder;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.08 with lithium acetate,
It is sintered 450 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Nickel-cobalt lithium manganate cathode material obtained by the present embodiment prepares soft-package battery 1C/30C high rate performance, as a result 1 institute of table
Show, it will thus be seen that full battery 0.2C capacity is 167.4mAh/g, and discharging efficiency is 30C electric discharge appearance after 92.4%, 1C charging for the first time
Amount is 145.2mAh/g, and 30C discharge capacity is that 86.7%, the 30C electric discharge mean voltage of 0.2C is 3.30V.
Embodiment 5
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni0.5Co0.2Mn0.3(OH)2(D50=4um, BET=12m2/ g) it is added to mass concentration and is
In 10% aqueous citric acid solution, nickel cobalt manganese presoma additional amount accounts for the 15% of solution quality, and ultrasound simultaneously stirs 0.5h, then exists
Dry 5h, obtains dried powder at 150 DEG C;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.08 with lithium carbonate,
It is sintered 300 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 880 DEG C of sintering 14h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Embodiment 6
A kind of preparation method of high magnification nickel-cobalt lithium manganate cathode material, includes the following steps.
(1) nickel cobalt manganese presoma Ni1/3Co1/3Mn1/3(OH)2(D50=3.5um, BET=12.4m2/ g) to be added to quality dense
Degree is in 10% aqueous citric acid solution, nickel cobalt manganese presoma additional amount accounts for the 60% of solution quality, and ultrasound simultaneously stirs 0.5h, so
The dry 2h at 200 DEG C afterwards, obtains dried powder;
(2) dried material of step (1) preparation is mixed by nickel cobalt manganese Metal with lithium molar ratio 1:1.12 with lithium carbonate,
It is sintered 300 DEG C of pre-burning 5h under a nitrogen;
(3) material after step (2) resulting pre-burning is sintered gas air, is naturally cooled to room with 980 DEG C of sintering 16h
Temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material sample.
Table 1 is embodiment 1-4 and the electrical property of the nickel-cobalt lithium manganate cathode material prepared of comparative example 1 and its full battery of production
It can table
Through the foregoing embodiment it is found that the present invention is passed through by the way that organic matter is added during preparing nickel cobalt manganese presoma
Crossing pre-sintering makes organic carbon, and skeleton is formed in nickel cobalt manganese presoma, finally removes organic matter by high temperature sintering, in turn
Porous structure is formed in nickle cobalt lithium manganate, obtains the nickel cobalt manganese anode material with porous structure.Preparation method of the invention
The specific surface area of nickel-cobalt lithium manganate cathode material can be significantly improved, to reduce lithium ion mobility path, improves it in height
The discharge capability of multiplying power.
Claims (10)
1. a kind of high magnification nickel-cobalt lithium manganate cathode material preparation method, it is characterised in that: the following steps are included:
(1) by water soluble organic substance is soluble in water solution is made after, be added nickel cobalt manganese presoma, ultrasonic treatment, then in 80-
200 DEG C of dry 2-10h, obtain dried powder;
(2) dried powder prepared by step (1) is mixed with lithium source, is pre-sintered 3-10h in 300-500 DEG C of inert gas,
Obtain pre-sintered mass;
(3) by step (2) resulting pre-sintered mass, be sintered 6-20h in 600-1000 DEG C of temperature, sintering gas be air or
Oxygen, cooled to room temperature, grinding is broken, prepares nickel-cobalt lithium manganate cathode material.
2. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(1) water soluble organic substance is at least one of glucose, sucrose, polyethylene glycol or citric acid in.
3. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(1) mass concentration that water soluble organic substance accounts for solution in solution in is 5-30%.
4. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(1) nickel cobalt manganese presoma accounts for the 30-70% of solution quality in.
5. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(1) nickel cobalt manganese presoma is Ni inxCoyMn1-x-y(OH)2, wherein 0 < x < 0.6,0 < y < 1,0 < x+y < 1, in nickel cobalt manganese presoma
Value partial size is 1-7um, specific surface area 5-20m2/g。
6. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(2) dried powder and lithium source molar ratio are 1:(1.0-1.15 in).
7. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(2) lithium source is at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate in.
8. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(2) inert gas is nitrogen or argon gas in.
9. high magnification nickel-cobalt lithium manganate cathode material preparation method according to claim 1, it is characterised in that: the step
(3) heating rate being sintered in is 1-20 DEG C/min.
10. a kind of nickel-cobalt lithium manganate cathode material being prepared by the claims 1-9 either method, it is characterised in that:
The median particle diameter 1-10um of the nickel-cobalt lithium manganate cathode material, specific surface area 0.4-4.0m2/g。
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