CN104701528B - LiNi0.5Mn1.5O4The surface coating method of material - Google Patents
LiNi0.5Mn1.5O4The surface coating method of material Download PDFInfo
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- CN104701528B CN104701528B CN201310656754.8A CN201310656754A CN104701528B CN 104701528 B CN104701528 B CN 104701528B CN 201310656754 A CN201310656754 A CN 201310656754A CN 104701528 B CN104701528 B CN 104701528B
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Abstract
The present invention relates to a kind of LiNi0.5Mn1.5O4The surface coating method of material, including to lithium carbonate, nickel protoxide and manganese dioxide in the ball grinder for having mill ball ball milling, form surface coated slurry presoma, through drying, form surface coated LiNi0.5Mn1.5O4Material precursor is heat-treated the presoma, its main feature is that: ball grinder is corundum ball grinder；Mill ball is the mill ball that corundum ball or corundum ball are mixed with agate ball, nylon ball or polyurethane ball.The present invention uses corundum ball grinder and mill ball, to LiNi0.5Mn1.5O4The surface coating method of material carries out surface cladding; effectively reduce the dissolution of manganese element in the electrolytic solution; improve the cycle performance of material; meet the stable circulation of battery under high voltages; manufacture craft is simple, low energy consumption, environment protecting is good, facilitates material prepare with scale and industrialization promotion.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, more particularly to a kind of LiNi0.5Mn1.5O4Material
Surface coating method.
Background technique
Into 21st century, along with automobile bring global energy crisis and environmental pollution, national governments are all
Successively investment huge fund increases the development of new-energy automobile, and New-energy electric vehicle and hybrid vehicle become the favorite in epoch.
At present there are mainly three types of power battery of electric motor car: lead-acid battery, nickel-metal hydride battery and lithium dynamical battery.From the development trend in future
It sees, lithium-ion-power cell will become mainstream, have broad application prospects, correspondingly, lithium-ion-power cell critical material
Anode research and development must keep pace with the times requirement.
Requirement of the lithium-ion-power cell to positive electrode has preferable security performance first, in broad temperature model
It can be worked normally in enclosing, while energy density with higher, can adapt to lithium ion battery to positive electrode high power
The requirement of energy, and energy density depends primarily on the electricity such as the operating voltage and capacity of material itself and the tap density of material
Chemical and physical properties, the hot spot that anode material for lithium-ion batteries is studied in industry at present are concentrated mainly on olivine transition metal
Phosphate-based positive electrode (LiMPO4) and spinelle manganese cathode material on.
There is circulation using LiFePO 4 and lithium manganese phosphate as olivine transition metal phosphate system's positive electrode of representative
Service life is long, and safety is good, raw material sources extensively and lower-price characteristic, but at the same time there is also material electric conductivity compared with
It is low, the deficiency of the practical applications such as high rate performance difference.
For spinel manganese based material, usually using it is more be LiMn2O4 (LiMn2O4) material, but the material is deposited
It is exactly that charge-discharge performance is poor in inherent problem, capacity attenuation is quickly.It has been generally acknowledged that wherein the main reason for is Mn3+
Presence produce Jahn-Teller effect, distortion of lattice occurs in charge and discharge process for material, causes volume contraction or swollen
It is swollen.
For the above problem existing for lithium manganate material, manganese position in part is replaced using transition metal Ni, generates 5V spinelle
Phase oxidation nickel manganese lithium LiNi0.5Mn1.5O4Positive electrode can be improved the discharge platform voltage of battery, reach 4.7V or so, sufficiently
The generation for inhibiting Jahn-Teller effect effectively improves the cycle life of electrode.But due to the 5V spinelle anode
Contain a certain amount of manganese element in material, therefore inevitably there are a degree of during the charge and discharge cycles of material
Manganese is dissolved in the phenomenon that electrolyte, so that the cycle performance of material declines, it is difficult to realize the extensive industry of stable cycle performance
Change 5V spinel anode material.
Summary of the invention
The present invention is to solve technical problem present in well-known technique and provide one kind and be effectively reduced manganese element and be electrolysed
It is dissolved in liquid, promotes the cycle performance of material, meet manufactured battery stable circulation under high voltages, and manufacture craft letter
The LiNi single, low energy consumption, environment protecting is good0.5Mn1.5O4The surface coating method of material.
The present invention includes following technical solution:
The surface coating method of spinel anode material, including preparing the presoma of surface clad anode material and to surface
The presoma of clad anode material is heat-treated；The preparation of the presoma of surface clad anode material includes: according to molar ratio
Li:Ni:Mn=1.05:0.5:1.5 is placed in mill ball using lithium carbonate, nickel protoxide and manganese dioxide as mixing material
In ball grinder, using ethyl alcohol as ball-milling medium, the mill ball: mixing material: the weight ratio of ethyl alcohol is 3:1:1, carries out 1-20
The wet ball grinding of hour, forms surface coated anode sizing agent presoma；Surface coated anode sizing agent presoma is placed in 60-
It is 3-14 hours dry in 75 DEG C of drying boxes, after naturally cooling to room temperature, complete Spinel lithium nickel manganese oxide LiNi0.5Mn1.5O4
The surface of positive electrode material precursor coats process；The process being heat-treated to the presoma of surface clad anode material includes:
The presoma of surface clad anode material obtained is placed in high temperature Muffle furnace and first carries out 850-975 DEG C of progress 14-20 hours
Sintering heat treatment；Then the temperature in high temperature Muffle furnace is down to 625-585 DEG C in 3 hours, reburned at 625-585 DEG C
Knot 12-16 hours after naturally cooling to room temperature, that is, completes the surface coating method process of spinel anode material, its main feature is that:
The ball grinder is corundum ball grinder；The mill ball is the grinding that corundum ball is mixed with agate ball, nylon ball or polyurethane ball
Ball, corundum ball account for 38% or more of mill ball total weight.
The advantages and positive effects of the present invention are:
1, the present invention uses corundum ball grinder and the corundum ball as mill ball, or the mixed grinding ball including corundum ball
System, the 5V Spinel lithium nickel manganese oxide LiNi that will be generated in mixing process0.5Mn1.5O4Positive electrode carries out surface cladding,
The dissolution of manganese element in the electrolytic solution is significantly reduced, the cycle performance of material is improved, meets manufactured battery in height
Stablize circulation under voltage, and manufacture craft is simple, low energy consumption, environment protecting is good, facilitate material prepare with scale and
Industrialization promotion.
2, do not increase poisonous and harmful emission in production process of the present invention and meet environment protection requirement.
3, the LiNi prepared using the present invention0.5Mn1.5O4The surface coated positive electrode of material stone, cycle performance phase
Than in uncoated LiNi0.5Mn1.5O4Material, cycle performance, which has, to be obviously improved.
Specific embodiment
Further to disclose invention, features and effects of the invention, especially exemplified by following instance, detailed description are as follows.
The surface coating method of spinel anode material, including preparing the presoma of surface clad anode material and to surface
The presoma of clad anode material is heat-treated；The preparation of the presoma of surface clad anode material includes: according to molar ratio
Li:Ni:Mn=1.05:0.5:1.5 is placed in mill ball using lithium carbonate, nickel protoxide and manganese dioxide as mixing material
In ball grinder, using ethyl alcohol as ball-milling medium, 1-20 hours wet ball grindings is carried out, surface coated anode sizing agent forerunner is formed
Body；Surface coated anode sizing agent presoma is placed in drying 3-14 hours in 60-75 DEG C of drying box, naturally cools to room temperature
Afterwards, Spinel lithium nickel manganese oxide LiNi is completed0.5Mn1.5O4The surface of positive electrode material precursor coats process；Surface is coated
The process that the presoma of positive electrode is heat-treated includes: that the presoma of surface clad anode material obtained is placed in high temperature
The 850-975 DEG C of sintering heat treatment for carrying out 14-20 hours is first carried out in Muffle furnace；It then will be in high temperature Muffle furnace in 3 hours
Temperature be down to 625-585 DEG C, re-sinter 12-16 hours, after naturally cooling to room temperature at 625-585 DEG C, that is, it is brilliant to complete point
The surface coating method process of stone positive electrode, its main feature is that: the ball grinder used is corundum ball grinder；The mill ball packet of use
Include the mill ball that corundum ball or corundum ball are mixed with agate ball, nylon ball or polyurethane ball.
The corundum ball accounts for 38% or more of mill ball total weight.
Embodiment 1
According to molar ratio Li:Ni:Mn=1.05:0.5:1.5, by lithium carbonate (Li2CO3), nickel protoxide (NiO) and dioxy
Change manganese (MnO2) be placed in corundum ball grinder as mixing material, the mill ball in ball grinder is corundum ball, and ethyl alcohol is as ball milling
Medium；The corundum ball: mixing material: the weight ratio of ethyl alcohol is 3:1:1, carries out 2 hours wet ball grindings, forms surface packet
The anode sizing agent presoma covered；Surface coated anode sizing agent presoma is placed in drying 3 hours in 60 DEG C of drying boxes, it is naturally cold
But to after room temperature, 5V Spinel lithium nickel manganese oxide LiNi is formed0.5Mn1.5O4The surface of positive electrode material precursor coats process；
Positive electrode material precursor after surface is coated is placed in high temperature Muffle furnace, and 14 hours heat is carried out at 850 DEG C
Processing, then in 3 hours by the greenhouse cooling in high temperature Muffle furnace to 625 DEG C, it is 12 small to continue sintering at a temperature of 625 DEG C
When, room temperature is naturally cooled to, that is, completes 5V Spinel lithium nickel manganese oxide LiNi of the present invention0.5Mn1.5O4The surface of positive electrode
Cladding process.
Embodiment 2
According to molar ratio Li:Ni:Mn=1.05:0.5:1.5, by lithium carbonate (Li2CO3), nickel protoxide (NiO) and dioxy
Change manganese (MnO2) be placed in corundum ball grinder as mixing material, the mill ball in ball grinder is corundum ball and nylon ball, described
Corundum ball accounts for the 63% of mill ball total weight, and ethyl alcohol is as ball-milling medium；The mill ball: mixing material: the weight of ethyl alcohol
Than carrying out 6 hours wet ball grindings, forming surface coated anode sizing agent presoma for 3:1:1；By surface coated anode slurry
Material precursor is placed in drying 3 hours in 60 DEG C of drying boxes, after naturally cooling to room temperature, forms 5V Spinel lithium nickel manganese oxide
LiNi0.5Mn1.5O4The surface of positive electrode material precursor coats process；
Positive electrode material precursor after surface is coated is placed in high temperature Muffle furnace, and 14 hours heat is carried out at 850 DEG C
Processing, then in 3 hours by the greenhouse cooling in high temperature Muffle furnace to 625 DEG C, it is 12 small to continue sintering at a temperature of 625 DEG C
When, room temperature is naturally cooled to, that is, completes 5V Spinel lithium nickel manganese oxide LiNi of the present invention0.5Mn1.5O4The surface of positive electrode
Cladding process.
Embodiment 3
According to molar ratio Li:Ni:Mn=1.05:0.5:1.5, by lithium carbonate (Li2CO3), nickel protoxide (NiO) and dioxy
Change manganese (MnO2) be placed in corundum ball grinder as mixing material, the mill ball in ball grinder is corundum ball and polyurethane ball, institute
Corundum ball accounts for mill ball total weight 42% is stated, ethyl alcohol is as ball-milling medium；The mill ball: mixing material: the weight of ethyl alcohol
Amount carries out 12 hours wet ball grindings, forms surface coated anode sizing agent presoma than being 3:1:1；By it is surface coated just
Pole slurry presoma is placed in drying 3 hours in 60 DEG C of drying boxes, after naturally cooling to room temperature, forms 5V Spinel nickel manganese oxide
Lithium LiNi0.5Mn1.5O4The surface of positive electrode material precursor coats process；
Positive electrode material precursor after surface is coated is placed in high temperature Muffle furnace, and 14 hours heat is carried out at 850 DEG C
Processing, then in 3 hours by the greenhouse cooling in high temperature Muffle furnace to 625 DEG C, it is 12 small to continue sintering at a temperature of 625 DEG C
When, room temperature is naturally cooled to, that is, completes 5V Spinel lithium nickel manganese oxide LiNi of the present invention0.5Mn1.5O4The surface of positive electrode
Cladding process.
Comparative example 1
According to molar ratio Li:Ni:Mn=1.05:0.5:1.5, by lithium carbonate (Li2CO3), nickel protoxide (NiO) and dioxy
Change manganese (MnO2) be placed in agate jar as mixing material, the mill ball in ball grinder is agate ball, and ethyl alcohol is as ball milling
Medium；The mill ball: mixing material: the weight ratio of ethyl alcohol is 3:1:1, carries out 6 hours wet ball grindings, forms surface packet
The anode sizing agent presoma covered；Surface coated anode sizing agent presoma is placed in drying 3 hours in 60 DEG C of drying boxes, it is naturally cold
But to after room temperature, 5V Spinel lithium nickel manganese oxide LiNi is formed0.5Mn1.5O4The surface of positive electrode material precursor coats process；
Positive electrode material precursor after surface is coated is placed in high temperature Muffle furnace, and 14 hours heat is carried out at 850 DEG C
Processing, then in 3 hours by the greenhouse cooling in high temperature Muffle furnace to 625 DEG C, it is 12 small to continue sintering at a temperature of 625 DEG C
When, room temperature is naturally cooled to, i.e. the surface of completion 5V spinel anode material coats process.
Comparative example 2
According to molar ratio Li:Ni:Mn=1.05:0.5:1.5, by lithium carbonate (Li2CO3), nickel protoxide (NiO) and dioxy
Change manganese (MnO2) be placed in nylon ball grinder as mixing material, the mill ball in ball grinder is nylon, and ethyl alcohol is situated between as ball milling
Matter；The mill ball: mixing material: the weight ratio of ethyl alcohol is 3:1:1, carries out 6 hours wet ball grindings, forms surface cladding
Anode sizing agent presoma；Surface coated anode sizing agent presoma is placed in 60 DEG C of drying boxes to 3 hours dry, natural cooling
To after room temperature, 5V Spinel lithium nickel manganese oxide LiNi is formed0.5Mn1.5O4The surface of positive electrode material precursor coats process；
Positive electrode material precursor after surface is coated is placed in high temperature Muffle furnace, and 14 hours heat is carried out at 850 DEG C
Processing, then in 3 hours by the greenhouse cooling in high temperature Muffle furnace to 625 DEG C, it is 12 small to continue sintering at a temperature of 625 DEG C
When, room temperature is naturally cooled to, i.e. completion 5V spinelle LiNi0.5Mn1.5O4The surface of positive electrode coats process.
The test result contrast table of 1 embodiment of the present invention of table and comparative example
From the results shown in Table 1: LiNi is coated using 5V spinelle prepared by the present invention0.5Mn1.5O4Positive electrode,
Under the premise of guaranteed capacity performance is not lost, the cycle performance of material is effectively promoted.
Although the preferred embodiment of the present invention is described above, the invention is not limited to above-mentioned specific
Embodiment, the above mentioned embodiment is only schematical, is not restrictive, those skilled in the art
Under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, it can also make very
It is multi-form.Within these are all belonged to the scope of protection of the present invention.
Claims (1)
1.LiNi0.5Mn1.5O4The surface coating method of material, including preparing the presoma of surface clad anode material and to surface
The presoma of clad anode material is heat-treated；The preparation of the presoma of surface clad anode material includes: according to molar ratio
Li:Ni:Mn=1.05:0.5:1.5 is placed in mill ball using lithium carbonate, nickel protoxide and manganese dioxide as mixing material
In ball grinder, using ethyl alcohol as ball-milling medium, the mill ball: mixing material: the weight ratio of ethyl alcohol is 3:1:1, carries out 1-20
The wet ball grinding of hour, forms surface coated anode sizing agent presoma；Surface coated anode sizing agent presoma is placed in 60-
It is 3-14 hours dry in 75 DEG C of drying boxes, after naturally cooling to room temperature, complete Spinel lithium nickel manganese oxide LiNi0.5Mn1.5O4
The surface of positive electrode material precursor coats process；
The process being heat-treated to the presoma of surface clad anode material includes: by surface clad anode material obtained
Presoma is placed in high temperature Muffle furnace the first sintering heat treatment in 14-20 hours at 850-975 DEG C；It then will be high in 3 hours
Temperature in warm Muffle furnace is down to 625-585 DEG C, re-sinters at 625-585 DEG C 12-16 hours, after naturally cooling to room temperature,
Complete the surface coating method process of spinel anode material, it is characterised in that: the ball grinder is corundum ball grinder；It is described
Mill ball is the mill ball that corundum ball is mixed with agate ball, nylon ball or polyurethane ball, and corundum ball accounts for mill ball total weight
38% or more.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1801508A (en) * | 2005-01-06 | 2006-07-12 | 中南大学 | Method for preparing high voltage lithium ion battery anode material lithium nickel manganese oxide |
| CN102531071A (en) * | 2010-12-30 | 2012-07-04 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material LiNi0.5Mn1.5O4 |
| CN102760884A (en) * | 2012-07-20 | 2012-10-31 | 河南师范大学 | Cathode material for fast lithium ion conductor phase-modified lithium ion battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102263237A (en) * | 2010-11-19 | 2011-11-30 | 中信国安盟固利动力科技有限公司 | Preparation method for normal spinel-modified lithium manganate cathode material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1801508A (en) * | 2005-01-06 | 2006-07-12 | 中南大学 | Method for preparing high voltage lithium ion battery anode material lithium nickel manganese oxide |
| CN102531071A (en) * | 2010-12-30 | 2012-07-04 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material LiNi0.5Mn1.5O4 |
| CN102760884A (en) * | 2012-07-20 | 2012-10-31 | 河南师范大学 | Cathode material for fast lithium ion conductor phase-modified lithium ion battery and preparation method thereof |
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