CN108376784A - Improve the method for tertiary cathode material hygroscopicity and pulp gel phenomenon - Google Patents
Improve the method for tertiary cathode material hygroscopicity and pulp gel phenomenon Download PDFInfo
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- CN108376784A CN108376784A CN201810190736.8A CN201810190736A CN108376784A CN 108376784 A CN108376784 A CN 108376784A CN 201810190736 A CN201810190736 A CN 201810190736A CN 108376784 A CN108376784 A CN 108376784A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of methods improving tertiary cathode material hygroscopicity and pulp gel phenomenon, include the following steps：A certain amount of silane coupler solution is taken, tertiary cathode material is added thereto, is sufficiently stirred, is then dried；It is mixed and made into slurry in proportion by binder, conductive additive and through treated tertiary cathode material, is coated on positive substrate, drying；It takes a certain amount of silane coupler solution to be coated to tertiary cathode piece surface again, finally obtains complete tertiary cathode piece.One layer of silane coupling agent that the present invention is coated in tertiary cathode material and pole piece; the trace water that substrate surface is adsorbed can be fallen with effecting reaction; and it is formed on its surface the hydrophobic protective layer of one layer of resistance to HF corrosion, to improve the air storage performance and chemical property of positive plate.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of improvement tertiary cathode material hygroscopicity and pulp gel
The method of phenomenon.
Background technology
Current commercialized lithium ion battery mainly uses LiCoO at present2As positive electrode, but LiCoO2There are safety
Property and overcharge resistance performance problem, Co belong to scarce resource, expensive, and metallic cobalt is easy to pollute the environment.And LiNiO2
Stability it is poor, easily cause safety problem, need to be synthesized under oxygen atmosphere, and be easy to happen cationic mixing and generate it is non-
Stoichiometric ratio structural compounds.LiMn2O4The dissolving Jahn- of crystal transfer and manganese ion is easy to happen in cyclic process
Teller effects, cause battery capacity to decay.
Tertiary cathode material nickel, cobalt and manganese oxide system combines LiCoO2Good cycle performance, LiNiO2Fabrication of High Specific Capacitance
Amount and LiMnO2High security and the features such as low cost, but its poor cyclical stability, thermal stability and storge quality
Significantly limit its application.These disadvantages are the essential attribute of tertiary cathode material mostly, larger to overcome them to bring
Challenge.The water in air is easily adsorbed due to tertiary cathode material, generates the water of trace on surface, this can lead to tertiary cathode
The chemical property of material is not high.First, it is thick to cooperatively form comparison with the carbon dioxide in air for this partial moisture
Lithium carbonate film layer, this film layer can cause coated active material can not participate in carry out charge and discharge process, lead to material
Specific capacity reduces, and gas can be generated in charge and discharge process, cause battery bulge flatulence.Secondly, positive electrode surface alkali is made after water suction
Degree increases, and can occur gelatin phenomenon in pulping process, influences the progress of subsequent coated technique, and then influence the performance of battery.
The water of certain trace can be with the salt (LiPF in electrolyte6) react, cause electrolyte to be destroyed, reaction can also be formed
HF corrodes tertiary cathode material, and it is rapid that this results in the cycle performance of material to decay.
In recent years, researchers have attempted a variety of methods, it is intended to which get both advantage of both height ratio capacity and high stability.
Common method has doping, coats and be prepared into the material of special construction, however these work are to material electrochemical performance
Improvement degree is unsatisfactory.
Invention content
In order to solve the deficiencies in the prior art, it is an object of the present invention to provide a kind of improvement tertiary cathode material moisture absorptions
The method of property and pulp gel phenomenon, makes one layer of silane coupling agent of positive electrode surface uniform fold, the layer is not by this method
The transmission of lithium ion can be had an impact, the performance of tertiary cathode can be improved instead.
Improving the method for tertiary cathode material hygroscopicity and pulp gel phenomenon the present invention provides a kind of, including walks as follows
Suddenly：
S1：Silane coupling agent is distributed to volatile organic solvent, obtains certain density silane coupler solution；Institute
The chemical expression for stating silane coupling agent is YSiX3, wherein Y is non-hydrolytic group；X is hydrolysising group；
S2：Tertiary cathode material is added to the part silane coupling agent by the silane coupler solution for taking a certain amount of S1
It in solution, is sufficiently stirred, is then dried；
S3：By binder, conductive additive and treated that tertiary cathode material mixes in proportion through S2, prepares
It at slurry, is coated on positive substrate, drying is prepared into tertiary cathode piece；
S4：It takes the silane coupler solution of a certain amount of S1 to be coated to the tertiary cathode piece surface of S3 preparations again, waits for solvent
After evaporating, complete tertiary cathode piece is finally obtained.
Preferably, the chemical expression YSiX of the silane coupling agent3In, Y is selected from vinyl, amino, epoxy group, methyl
Any one in acryloxy, sulfydryl, urea groups；X is selected from halogen, methoxyl group, ethyoxyl, methoxy ethoxy, acetyl oxygen
Any one in base.
It is highly preferred that a concentration of 1~10% of silane coupler solution obtained by S1.
Preferably, in S1, the one kind or more of the organic solvent in methanol, ethyl alcohol, acetone, DMF, NMP, chloroform
Kind.
Preferably, in S2, the chemical expression of the tertiary cathode material is LiNixCoyAzO2, wherein A is element M n
Or element al, the value that the value that the value of x is 0.5~0.9, y is 0.05~0.2, z is 0.05~0.3, and x+y+z=1.
It is highly preferred that the tertiary cathode material is LiNi0.5Co0.2Mn0.3O2、LiNi0.6Co0.2Mn0.2O2、
LiNi0.8Co0.1Mn0.1O2、LiNi0.9Co0.05Mn0.05O2、LiNi0.8Co0.1Al0.1O2、LiNi0.8Co0.15Al0.05O2、
LiNi0.9Co0.05Al0.05O2At least one of.
Preferably, in S2, the matter of contained silane coupling agent and the tertiary cathode material in the silane coupler solution
Amount is than being 1:35~1000.
Preferably, in S3, coating thickness is 200~250 μm.
Preferably, in S4, the painting method is blade coating, spin coating or spraying.
Compared with prior art, the beneficial effects of the present invention are：
One layer of silane coupling agent that the present invention is coated in tertiary cathode material and pole piece, can fall substrate with effecting reaction
The trace water that surface is adsorbed, and it is formed on its surface the hydrophobic protective layer of one layer of resistance to HF corrosion, to improve positive plate
Air storage performance and chemical property (height ratio capacity and cyclical stability etc.).Improvement tertiary cathode material provided by the invention
Expect the method for hygroscopicity and pulp gel phenomenon, it is easy to operate, effectively increase the chemical property of tertiary cathode.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is ternary material surface cladding silane coupling agent mechanism schematic diagram；
Fig. 2 is the cyclic curve of the silane coupled agent dispersing liquid of different content in the embodiment of the present invention 1.
Specific implementation mode
In order to enable those skilled in the art to more fully understand, technical scheme of the present invention is practiced, with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
Unless otherwise defined, the hereinafter used all technical terms for being and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.Unless otherwise specified, it the various raw materials used in the following embodiment of the present invention, reagent, instrument and sets
It is standby to be commercially available by market or be prepared by existing method.
The present invention is by one layer of silane coupling agent of positive electrode surface uniform fold, first by certain density silane idol
Join agent solution and tertiary cathode material mixing, obtains silane coupler modified tertiary cathode material, use the tertiary cathode material
Tertiary cathode piece is made, certain density silane coupler solution is then coated to tertiary cathode piece surface again, passes through method
It can be effectively improved tertiary cathode material hygroscopicity and pulp gel phenomenon, and the transmission of lithium ion will not only be had an impact,
The performance of tertiary cathode can be improved instead.
It should be noted that silane coupling agent (the YSiX that the above method uses3) have there are two types of different chemical property groups,
One is non-hydrolytic group (Y group), another kind is hydrolysising group (X group).X group can hydrolyze, this hydrolytic process can be with
The trace water of tertiary cathode material adsorption and the existing minimal amount of moisture in electrolyte are consumed, to prevent liquid
The decomposition of middle lithium salts keeps the stabilization of electrolyte, improves battery performance.And silane coupling agent can form one on tertiary cathode surface
The hydrophobic layer of layer, prevents tertiary cathode from further adsorbing water.Silane coupling agent can form one layer of resistance to HF on tertiary cathode material surface
The protective layer of corrosion prevents corrosion of the HF to tertiary cathode material, to improve the performance of battery.Specific reaction is as shown in Figure 1.
Just technical scheme of the present invention is described in detail with specific example below.
Embodiment 1
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
A certain amount of silane coupling agent is added into ethyl alcohol, is carrying out ultrasonic disperse under an inert atmosphere, is obtaining a concentration of
1% silane coupler solution；The chemical expression of the silane coupling agent is YSiX3, wherein Y is vinyl；X is methoxy
Base；
By the tertiary cathode material LiNi of 970mg0.6Co0.2Mn0.2O2The above-mentioned silane for being added to the silane coupling agent containing 1g is even
Join in agent solution, is sufficiently stirred, is then dried；
The treated tertiary cathode material LiNi of 80mg are taken again0.8Co0.1Mn0.1O2It is conductive with 10mg PVDF and 10mg
Carbon black is uniformly mixed, and is prepared into slurry, and be coated on aluminium foil with 200 μm of height faces of scraper, and dry and form tertiary cathode
Piece；
The silane coupler solution for taking 5ml a concentration of 3% again is coated in above-mentioned tertiary cathode with 250 μm of height faces of scraper
Piece surface, and 4h is dried under the conditions of 60 DEG C, finally obtain complete tertiary cathode piece.
Embodiment 2
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process and embodiment 1 are identical,
It the difference is that only, a concentration of the 2% of silane coupling agent used.
Embodiment 3
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process and embodiment 1 are identical,
It the difference is that only, a concentration of the 3% of silane coupling agent used.
Embodiment 4
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process and embodiment 1 are identical,
It the difference is that only, a concentration of the 5% of silane coupling agent used.
Embodiment 5
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
A certain amount of silane coupling agent is added into ethyl alcohol, is carrying out ultrasonic disperse under an inert atmosphere, is obtaining a concentration of
1% silane coupler solution；The chemical expression of the silane coupling agent is YSiX3, wherein Y is vinyl；X is methoxy
Base；
By the tertiary cathode material LiNi of 990mg0.6Co0.2Mn0.2O2The above-mentioned silane for being added to the silane coupling agent containing 1g is even
Join in agent solution, is sufficiently stirred, is then dried；
The treated tertiary cathode material LiNi of 80mg are taken again0.8Co0.1Mn0.1O2It is conductive with 10mg PVDF and 10mg
Carbon black is uniformly mixed, and is prepared into slurry, and be coated on aluminium foil with 200 μm of height faces of scraper, and dry and form tertiary cathode
Piece；
The tertiary cathode piece being prepared into is cut into the disk of a diameter of 7cm, and is fixed on the estrade of spin coating instrument, to turn
Fast 500r/min starts spin coating instrument；1% silane coupler solution that 1 milliliter is drawn by liquid-transfering gun, slowly drips to positive disk
Center, pole piece is dried under the conditions of 60 DEG C after spin coating, finally obtains complete tertiary cathode piece.
Embodiment 6
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
A certain amount of silane coupling agent is added into ethyl alcohol, is carrying out ultrasonic disperse under an inert atmosphere, is obtaining a concentration of
5% silane coupler solution；The chemical expression of the silane coupling agent is YSiX3, wherein Y is vinyl；X is methoxy
Base；
By the tertiary cathode material LiNi of 950mg0.8Co0.15Mn0.05O2It is added to the above-mentioned silane of the silane coupling agent containing 1g
It in coupling agent solution, is sufficiently stirred, is then dried；
The treated tertiary cathode material LiNi of 80mg are taken again0.8Co0.1Mn0.1O2It is conductive with 10mg PVDF and 10mg
Carbon black is uniformly mixed, and is prepared into slurry, and be coated on aluminium foil with 200 μm of height faces of scraper, and dry and form tertiary cathode
Piece；
It takes coupling agent solution 20ml to be fitted into flush coater, against the positive plate that the length of side is 10cm, is sprayed with given pace
It applies, is finished until dispersion liquid sprays, pole piece is dried under the conditions of 60 DEG C after spraying, finally obtains complete ternary
Positive plate.
Comparative example 1
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
Take 80mg tertiary cathode materials LiNi0.8Co0.1Mn0.1O2It is uniformly mixed with 10mg PVDF and 10mg conductive blacks,
It is prepared into slurry, and is coated on aluminium foil with 200 μm of height faces of scraper, and 4h is dried under the conditions of 60 DEG C.
Comparative example 2
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
By the tertiary cathode material LiNi of 970mg0.6Co0.2Mn0.2O21% silane for being added to the silane coupling agent containing 1g is even
Join in agent solution, is sufficiently stirred, is then dried；
The treated tertiary cathode material LiNi of 80mg are taken again0.8Co0.1Mn0.1O2It is conductive with 10mg PVDF and 10mg
Carbon black is uniformly mixed, and is prepared into slurry, and be coated on aluminium foil with 200 μm of height faces of scraper, and dried under the conditions of 60 DEG C
4h finally obtains complete tertiary cathode piece.
Comparative example 3
A method of improving tertiary cathode material hygroscopicity and pulp gel phenomenon, detailed process are as follows：
Take 80mg tertiary cathode materials LiNi0.8Co0.1Mn0.1O2It is uniformly mixed with 10mg PVDF and 10mg conductive blacks,
It is prepared into slurry, and is coated on aluminium foil with 200 μm of height faces of scraper, and dries and forms tertiary cathode piece；5ml concentration is taken again
For 1% silane coupler solution, it is coated in above-mentioned tertiary cathode piece surface with 250 μm of height faces of scraper, and in 60 DEG C of conditions
Lower drying 4h finally obtains complete tertiary cathode piece.
The method that 1~embodiment of embodiment 6 provides can significantly improve tertiary cathode material hygroscopicity and pulp gel is existing
As, obtained tertiary cathode piece all has good air storage performance and chemical property, below we combine comparison
Example 1-3, is specifically described the effect of the present invention.
Embodiment 1-2 and 1 providing method of comparative example the tertiary cathode piece being prepared are struck out respectively a diameter of
The pole piece of 12mm.It is assembled into button cell after above-mentioned pole piece is placed 7 days in air, in the voltage range of 2.8V-4.3V
Charge-discharge test is carried out with the current density of 1C.
The cyclic curve of the tertiary cathode piece that embodiment 1-2 and 1 providing method of comparative example are prepared as shown in Fig. 2,
As seen from Figure 2, the tertiary cathode for comparing and being not added with silane coupling agent adds the cell decay speed of silane coupling agent
It decreases, and the conservation rate of circulation volume increases, so tertiary cathode can be improved by adding silane coupling agent
Cyclical stability, this just because of silane coupling agent by ternary material trace water absorb and surface formed protection
Layer.
It the coulombic efficiency for the first time for the tertiary cathode piece that embodiment 1-2 and 1 providing method of comparative example are prepared and follows
Environmentally friendly holdup is as shown in table 1 below.
The Electrochemical results of 1 embodiment 1-2 of table and the tertiary cathode piece of comparative example 1
As can be seen from Table 1, pole piece is exposed in air after 7 days, ternary can be greatly improved just in silane coupling agent
The coulombic efficiency for the first time (coulombic efficiency for improving about 10%) of pole, and improve 10 on 200 cycle conservation rates
~15%, these are all strong to demonstrate silane coupling agent can promote the cyclical stability and air of tertiary cathode material very well
Stability keeps relatively high specific capacity.
Further, we also carry out the tertiary cathode piece that embodiment 1 and comparative example 2-3 providing methods are prepared
Electro-chemical test；Specific electro-chemical test condition is identical with the above process.
The Electrochemical results of the tertiary cathode piece of 2 embodiment 1 of table and comparative example 2-3
| Coulombic efficiency (%) for the first time | Recycle conservation rate (%, 200 times) | Discharge capacity (0.1C, mA h/g) for the first time | |
| Embodiment 1 | 85.64 | 75.79 | 176.29 |
| Comparative example 2 | 78.23 | 70.67 | 179.5 |
| Comparative example 3 | 79.54 | 68.55 | 180.25 |
As can be seen from Table 2, a step processing (comparative example 2 and comparative example 3) is carried out to tertiary cathode, can not all changed well
The cyclical stability of kind tertiary cathode and for the first time coulombic efficiency, so carrying out tertiary cathode as at two steps in embodiment 1
Reason is necessary.
Obviously, those skilled in the art can carry out this 11 invention various modification and variations without departing from the present invention's
Spirit and scope.In this way, if these modifications and changes of the present invention belongs to the model of the claims in the present invention and its equivalent technologies
Within enclosing, then the present invention is also intended to include these modifications and variations.Embodiment described above is only to absolutely prove this hair
The bright and preferred embodiment lifted, protection domain are without being limited thereto.Those skilled in the art are on the basis of the present invention
Made by equivalent substitute or transformation, within protection scope of the present invention, protection scope of the present invention is with claims
It is accurate.
Claims (9)
1. a kind of method improving tertiary cathode material hygroscopicity and pulp gel phenomenon, which is characterized in that include the following steps：
S1：Silane coupling agent is distributed to volatile organic solvent, obtains certain density silane coupler solution；The silicon
The chemical expression of alkane coupling agent is YSiX3, wherein Y is non-hydrolytic group；X is hydrolysising group；
S2：Tertiary cathode material is added to the part silane coupler solution by the silane coupler solution for taking a certain amount of S1
In, it is sufficiently stirred, is then dried；
S3：By binder, conductive additive and treated that tertiary cathode material mixes in proportion through S2, and preparation is slurried
Material, is coated on positive substrate, and drying is prepared into tertiary cathode piece；
S4：It takes the silane coupler solution of a certain amount of S1 to be coated to the tertiary cathode piece surface of S3 preparations again, waits for evaporation of the solvent
After, finally obtain complete tertiary cathode piece.
2. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In the chemical expression YSiX of the silane coupling agent3In, Y be selected from vinyl, amino, epoxy group, methacryloxy,
Any one in sulfydryl, urea groups；X is any one in halogen, methoxyl group, ethyoxyl, methoxy ethoxy, acetoxyl group
Kind.
3. the method according to claim 2 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In a concentration of 1~10% of silane coupler solution obtained by S1.
4. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In in S1, the organic solvent is one or more in methanol, ethyl alcohol, acetone, DMF, NMP, chloroform.
5. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In in S2, the chemical expression of the tertiary cathode material is LiNixCoyAzO2, wherein A be element M n or element al, x's
The value that the value that value is 0.5~0.9, y is 0.05~0.2, z is 0.05~0.3, and x+y+z=1.
6. the method according to claim 5 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In the tertiary cathode material is LiNi0.5Co0.2Mn0.3O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.8Co0.1Mn0.1O2、
LiNi0.9Co0.05Mn0.05O2、LiNi0.8Co0.1Al0.1O2、LiNi0.8Co0.15Al0.05O2、LiNi0.9Co0.05Al0.05O2In extremely
Few one kind.
7. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In in S2, the mass ratio of contained silane coupling agent and the tertiary cathode material is 1 in the silane coupler solution:35~
1000。
8. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In in S3, coating thickness is 200~250 μm.
9. the method according to claim 1 for improving tertiary cathode material hygroscopicity and pulp gel phenomenon, feature exist
In in S4, the painting method is blade coating, spin coating or spraying.
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| CN111600002A (en) * | 2020-05-30 | 2020-08-28 | 海宏(唐河)新能源科技有限公司 | Preparation method of aluminum triethoxide coated nickel cobalt lithium manganate modified material |
| CN112467121A (en) * | 2020-12-03 | 2021-03-09 | 珠海冠宇电池股份有限公司 | Positive plate and preparation method and application thereof |
| CN112687878A (en) * | 2020-12-25 | 2021-04-20 | 东莞新能源科技有限公司 | Electrochemical device and electronic device |
| CN114447302A (en) * | 2022-01-27 | 2022-05-06 | 中国科学院电工研究所 | Layered oxide/conductive agent composite material and preparation method and application thereof |
| CN114824222A (en) * | 2022-05-07 | 2022-07-29 | 浙江南都电源动力股份有限公司 | Method for coating anode material by using organic silicon coupling agent |
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| CN108376784B (en) | 2020-12-04 |
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