CN110342588A - A kind of ternary cathode material of lithium ion battery and preparation method thereof - Google Patents
A kind of ternary cathode material of lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of ternary cathode material of lithium ion battery, which is characterized in that in parts by weight, prepares and raw materials used includes: 21~42 parts of nickel salt；11~21 parts of manganese salt；11~21 parts of cobalt salt；60~150 parts of precipitating reagent；10~25 parts of lithium salts；20 parts and 12 parts of ethylene glycol of deionized water.The preparation method includes: step 1: nickel salt, manganese salt and cobalt salt are add to deionized water, stirring forms salting liquid, precipitating reagent and ethylene glycol are mixed, stirring forms precipitant solution, salting liquid and precipitant solution are mixed, stirring, is reacted 30 minutes in 160~200 DEG C of progress microwave hydrothermals, Deng taking out after cooling, fusiform presoma is obtained；Step 2: the resulting fusiform presoma of step 1 and lithium salts being mixed, are put into Muffle furnace at 800~900 DEG C heat preservation 12~for 24 hours, cooling obtains ternary cathode material of lithium ion battery.Pattern of the present invention is uniform, partial size is smaller, and energy density is high, and cycle performance is excellent and time-consuming short.
Description
Technical field
The present invention relates to a kind of ternary cathode material of lithium ion batteries and preparation method thereof.
Background technique
Lithium ion battery is a kind of secondary cell of clean and environmental protection.Its positive electrode directly determines battery performance, therein
Nickel-cobalt-manganternary ternary anode material is even more the anode material for lithium-ion batteries of a kind of high-energy density, low cost, can be widely used for electricity
The fields such as sub- device and electric car.
The main preparation process of nickel-cobalt-manganese ternary material has coprecipitation, spray drying process and hydro-thermal method etc. at present.It is coprecipitated
Shallow lake method only needs 100 DEG C of temperature below that can produce, but it is to pH value, and stirring rate etc. requires harsh, needs stringent
Control condition；Spray drying process high degree of automation, short preparation period, but the output capacity of its raw material investment is low；Hydro-thermal method behaviour
Make simple, easily obtained material, but it synthesizes time-consuming 18~24 hours, wastes a large amount of energy, and pattern partial size is all poor.
Patent CN105070903A prepares ternary material precursor using coprecipitation, although reducing the content of impurity, it is consumed
Shi Changda 15~30 hours, granular size was inhomogenous.Spray drying process is used in patent CN107464929A to be blended to obtain
Performance stable ternary material, however its particle size range is relatively large and size is uneven at 5~20 μm, first circle charging is held
Measure only 157mAhg-1。
Based on the above background.It is quickly being prepared there is an urgent need to develop one kind and have that preferable pattern, partial size is less than 5 μm and phase
It is higher to uniform, capacity (to be higher than 180mAhg-1) nickel-cobalt-manganternary ternary anode material.
Summary of the invention
It is taken a long time for the preparation of existing nickel-cobalt-manganese ternary material and microscopic appearance is different, partial size is relatively coarse, caused
The poor problem of cycle performance, that the purpose of the present invention is to provide patterns is uniform, partial size is smaller, and energy density is high, cycle performance
Excellent and time-consuming short lithium ion battery nickel-cobalt-manganese ternary positive electrode and preparation method thereof.
In order to achieve the above object, the present invention provides a kind of preparation method of ternary cathode material of lithium ion battery,
It is characterized in that, in parts by weight, prepares and raw materials used include:
The preparation method includes:
Step 1: nickel salt, manganese salt and cobalt salt being add to deionized water, stirring forms salting liquid, by precipitating reagent and second two
Alcohol mixing, stirring form precipitant solution, and salting liquid and precipitant solution are mixed, stirring, in 160~200 DEG C of progress microwaves
It hydro-thermal reaction 25~35 minutes, waits and takes out after cooling, obtain LiMn0.25Ni0.5Co0.25O2Fusiform presoma；
Step 2: by the resulting LiMn of step 10.25Ni0.5Co0.25O2Fusiform presoma and lithium salts mixing, be put into Muffle
In furnace at 800~900 DEG C heat preservation 12~for 24 hours, cooling obtain LiMn0.25Ni0.5Co0.25O2。
Preferably, the raw material for preparing includes:
Preferably, the nickel salt is that nickel sulfate hexahydrate closes object (NiSO4·6H2O), Nickel diacetate tetrahydrate (Ni
(CH3COO)2·4H2O), nickel chloride hexahydrate (NiCl2·6H2) and nickel nitrate hexahydrate (Ni (NO O3)2·6H2O) one
Kind is two or more.
Preferably, the manganese salt is manganese sulfate tetrahydrate (MnSO4·4H2O), manganese acetate tetrahydrate (Mn
(CH3COO)2·4H2O), manganese chloride tetrahydrate (MnCl2·4H2) and manganese nitrate tetrahydrate (Mn (NO O3)2·4H2O) one
Kind is two or more.
Preferably, the cobalt salt is cobaltous sulfate heptahydrate (CoSO4·7H2O), cobalt acetate tetrahydrate (Co
(CH3COO)2·4H2O), cobalt chloride hexahydrate (CoCl2·6H2) and Cobalt(II) nitrate hexahydrate (Co (NO O3)2·6H2O) one
Kind is two or more.
Preferably, the precipitating reagent is dimethyl carbonate (DMC), dimethyl oxalate (DMO) and urea (CO (NH2)2) in
One or more.
Preferably, the lithium salts is lithium hydroxide monohydrate (LiOHH2O), lithium carbonate (Li2CO3) and lithium acetate
(CH3One or more of COOLi).
Preferably, the reaction time in the step 1 is 25~35 minutes.
Preferably, lithium salts excessive 5~10% in the step 2.
Preferably, the molar ratio of Mn, Ni, Co for containing respectively in the manganese salt, nickel salt and cobalt salt are 1:2:1.
The present invention also provides lithium-ion electrics prepared by the preparation method of above-mentioned ternary cathode material of lithium ion battery
Pond tertiary cathode material.
Compared with prior art, the invention has the following advantages:
The present invention forms uniform thermal field using microwave and increases intergranular collision, and the process for having regulated and controled growth is allowed to
The uniform microwave-hydrothermal method of the pattern of generation material is prepared for 2~5 μm instead of the common hydro-thermal method of non-uniform resistance heat
Shuttle shape particle, and it is only 30 minutes or so time-consuming, it has saved the energy and has improved time efficiency.
Further, simple process of the invention, obtained LiMn under high temperature solid-state0.25Ni0.5Co0.25O2Pattern is uniform,
Surface covers one layer of small uniform particle, and about 2~5 μm of partial size, large specific surface area enables it to metric density height, cyclicity
It can be good.
The invention is simple and feasible, environmentally protective, the nickel-cobalt-manganese ternary material LiMn of preparation0.25Ni0.5Co0.25O2Its partial size is
2~5 μm, specific surface area is up to 1.60~1.67m2·g-1.There is 180~185mAhg under ordinary cycle-1It is higher initial
Discharge capacity, and in 1C (20mAg-1) under after 100 circle of circulation there are also 150~156mAhg-1High specific capacity and have
84% or more conservation rate.In 10C (discharge capacity 200mAg-1) under by 100 circulations there are also 99~105mAhg-1
Good high rate performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image of ternary cathode material of lithium ion battery.
Fig. 2 is the X-ray diffracting spectrum of ternary cathode material of lithium ion battery.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
For raw material used in various embodiments of the present invention in addition to following specified otherwises, other are purchased from Shanghai Chinese medicines group
Learn reagent Co., Ltd；
The preparation and test equipment used in this patent is as follows:
Microwave dissolver (WX-6000), reaction temperature are 160~200 DEG C, and the reaction time is 30 minutes.X-ray diffraction
(D/max-2200-PC), 10 °~80 ° of test condition, 4 ° per minute.Scanning electron microscope (SIGMA, ZEISS
microscope).Thermogravimetric/differential thermal analysis (TGA/SDTA851), 25 DEG C~1000 DEG C of test condition.Specific surface tests (ASAP
2020).Blue electricity (Wuhan LAND), when test, are kept for 25 DEG C of room temperature.
Embodiment 1
A kind of ternary cathode material of lithium ion battery, preparation raw material used in parts by weight, form and contain
It measures as follows:
Wherein, the nickel salt is that nickel sulfate hexahydrate closes object；
The manganese salt is manganese sulfate tetrahydrate；
The cobalt salt is cobaltous sulfate heptahydrate；
The precipitating reagent is dimethyl oxalate；
The lithium salts is lithium acetate；
Above-mentioned a kind of ternary cathode material of lithium ion battery and preparation method thereof, specifically comprises the following steps:
(1) preparation of presoma: nickel sulfate hexahydrate is closed into object, manganese sulfate tetrahydrate and cobaltous sulfate heptahydrate are in proportion
It is add to deionized water, is stirred continuously and directly forms transparent salting liquid.Dimethyl oxalate and ethylene glycol are mixed, constantly stirred
It mixes to form transparent clear precipitant solution.Later, salting liquid and precipitant solution are mixed, are stirred continuously to clarification uniformly,
The solution being stirred is added in microwave hydrothermal liner, microwave hydrothermal system is put into, keeps the temperature and carries out after being directly warming up to 180 DEG C
Microwave hydrothermal reacts 35 minutes, waits be cooled to 60 DEG C or less taking-ups later.In microwave hydrothermal reaction, form
LiMn0.25Ni0.5Co0.25O2Fusiform presoma；
(2)LiMn0.25Ni0.5Co0.25O2Synthesis: presoma obtained in step (1) and lithium acetate is uniform in proportion
Mixing, is put into Muffle furnace and is warming up at 900 DEG C with 5 DEG C/heating rate per minute and keep the temperature 20h, after be cooled to room temperature and take out
To LiMn0.25Ni0.5Co0.25O2。
Embodiment 2
A kind of ternary cathode material of lithium ion battery, preparation raw material used in parts by weight, form and contain
It measures as follows:
Wherein, the nickel salt is Nickel diacetate tetrahydrate；
The manganese salt is manganese acetate tetrahydrate；
The cobalt salt is cobalt acetate tetrahydrate；
The precipitating reagent is dimethyl carbonate；
The lithium salts is lithium hydroxide；
Above-mentioned a kind of ternary cathode material of lithium ion battery and preparation method thereof, specifically comprises the following steps:
(1) preparation of presoma: by Nickel diacetate tetrahydrate, manganese acetate tetrahydrate and cobalt acetate tetrahydrate are added by example
Enter into deionized water, is stirred continuously and directly forms transparent salting liquid.Dimethyl carbonate and ethylene glycol are mixed, are stirred continuously
Form transparent clear precipitant solution.Later, salting liquid and precipitant solution are mixed, is stirred continuously to clarification uniformly, it will
The solution being stirred is added in microwave hydrothermal liner, is put into microwave hydrothermal system, and heat preservation carries out micro- after being directly warming up to 190 DEG C
It wave hydro-thermal reaction 25 minutes, waits be cooled to 60 DEG C or less taking-ups later.In microwave hydrothermal reaction, form
LiMn0.25Ni0.5Co0.25O2Fusiform presoma；
(2)LiMn0.25Ni0.5Co0.25O2Synthesis: by presoma obtained in step (1) in proportion with lithium hydroxide one
Hydrate uniformly mixes, and is put into Muffle furnace and is warming up at 850 DEG C with 5 DEG C/heating rate per minute and keeps the temperature 12h, after be cooled to
Room temperature is taken out to obtain LiMn0.25Ni0.5Co0.25O2。
Embodiment 3
A kind of ternary cathode material of lithium ion battery, preparation raw material used in parts by weight, form and contain
It measures as follows:
Wherein, the nickel salt is nickel chloride hexahydrate；
The manganese salt is manganese chloride tetrahydrate；
The cobalt salt is cobalt chloride hexahydrate；
The precipitating reagent is urea；
The lithium salts is lithium carbonate；
Above-mentioned a kind of ternary cathode material of lithium ion battery and preparation method thereof, specifically comprises the following steps:
(1) preparation of presoma: by nickel chloride hexahydrate, manganese chloride tetrahydrate and cobalt chloride hexahydrate are in proportion
It is add to deionized water, is stirred continuously and directly forms transparent salting liquid.Urea and ethylene glycol are mixed, are stirred continuously to be formed
Transparent clear precipitant solution.Later, salting liquid and precipitant solution are mixed, is stirred continuously to clarification uniformly, will stirs
Good solution is added in microwave hydrothermal liner, is put into microwave hydrothermal system, and heat preservation carries out Microwave Water after being directly warming up to 200 DEG C
It thermal response 30 minutes, waits be cooled to 60 DEG C or less taking-ups later.In microwave hydrothermal reaction, form
LiMn0.25Ni0.5Co0.25O2Fusiform presoma；
(2)LiMn0.25Ni0.5Co0.25O2Synthesis: presoma obtained in step (1) is uniform with lithium carbonate in proportion
Mixing, is put into Muffle furnace and is warming up at 800 DEG C with 5 DEG C/heating rate per minute and keep the temperature 16h, after be cooled to room temperature and take out
To LiMn0.25Ni0.5Co0.25O2。
By the resulting LiMn of embodiment 30.25Ni0.5Co0.25O2Show material in generation by thermogravimetric and differential thermal analysis
When each stage the case where, also for we determined that the temperature range of materials synthesis；Pass through the material of SEM image display synthesis
Excellent spindle is kept, and covers one layer of subtle particle on presoma, it is clear that such spindle material covering
The pattern of layer of particles is more conducive to electrolyte permeability into electrode material, ensure that for electrode material and electrolyte bigger
Contact area (see Fig. 1)；It is seen to be pure by XRD analysis and there is no any impurity, and two pairs of peak splitting degrees are high, sample
The layer structure of product is good, wherein narrow and sharp peak shows that the crystallinity of material is very high (see Fig. 2)；Pass through EDS mapping
Elemental analysis proves that three elements are evenly distributed in the excellent layer structure of pattern；It is tested by CV cyclic voltammetry
The completed electrochemical reaction for also revealing material, explains the mechanism of the charge and discharge cycles of material；It is obtained under ordinary cycle
LiMn0.25Ni0.5Co0.25O2There is 180~185mAhg-1Higher discharge capacity, and at 1C circulation 100 circle after also
There is 150~156mAhg-1High specific capacity and have 84% or more conservation rate.There are also 99~105mAhg at 10C-1
Good high rate performance.
Above said content is only the basic explanation under present inventive concept, and is appointed made by technical solution according to the present invention
What equivalent transformation, is within the scope of protection of the invention.
Claims (9)
1. a kind of preparation method of ternary cathode material of lithium ion battery, which is characterized in that in parts by weight, prepare institute
Include with raw material:
The preparation method includes:
Step 1: nickel salt, manganese salt and cobalt salt being add to deionized water, stirring forms salting liquid, and precipitating reagent and ethylene glycol are mixed
It closes, stirring forms precipitant solution, salting liquid and precipitant solution is mixed, stirring, in 160~200 DEG C of progress microwave hydrothermals
Reaction 25~35 minutes, waits and takes out after cooling, obtain LiMn0.25Ni0.5Co0.25O2Fusiform presoma；
Step 2: by the resulting LiMn of step 10.25Ni0.5Co0.25O2Fusiform presoma and lithium salts mixing, be put into Muffle furnace
At 800~900 DEG C heat preservation 12~for 24 hours, cooling obtain LiMn0.25Ni0.5Co0.25O2。
2. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the preparation
Raw material includes:
3. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the nickel salt
For nickel sulfate hexahydrate close object, Nickel diacetate tetrahydrate, nickel chloride hexahydrate and nickel nitrate it is hexahydrated it is one or two kinds of with
On.
4. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the manganese salt
For manganese sulfate tetrahydrate, manganese acetate tetrahydrate, manganese chloride tetrahydrate and manganese nitrate tetrahydrate it is one or two kinds of with
On.
5. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the cobalt salt
For cobaltous sulfate heptahydrate, cobalt acetate tetrahydrate, cobalt chloride hexahydrate and Cobalt(II) nitrate hexahydrate it is one or two kinds of with
On.
6. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the precipitating
Agent is one or more of dimethyl carbonate, dimethyl oxalate and urea.
7. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the lithium salts
It is one or more of lithium hydroxide monohydrate, lithium carbonate and lithium acetate.
8. the preparation method of ternary cathode material of lithium ion battery as described in claim 1, which is characterized in that the step
Lithium salts excessive 5~10% in 2.
9. lithium ion prepared by the preparation method of ternary cathode material of lithium ion battery of any of claims 1-8
Battery tertiary cathode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110957488A (en) * | 2019-11-07 | 2020-04-03 | 太原科技大学 | Preparation method of peanut-like nickel cobalt lithium manganate positive electrode material |
| CN111816866A (en) * | 2020-07-17 | 2020-10-23 | 南京理工大学 | Method for preparing lithium-rich manganese-based positive electrode material by co-precipitation-hydrothermal combination |
| CN112777649A (en) * | 2021-01-15 | 2021-05-11 | 昆明理工大学 | Nickel-cobalt-manganese ternary precursor and preparation method and application thereof |
| CN112875766A (en) * | 2021-01-28 | 2021-06-01 | 山东宏匀纳米科技有限公司 | Method for preparing ternary cathode material by microwave heating solution method with carbon source added |
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| CN112875766A (en) * | 2021-01-28 | 2021-06-01 | 山东宏匀纳米科技有限公司 | Method for preparing ternary cathode material by microwave heating solution method with carbon source added |
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