CN106159233B - A kind of surface modifying method of anode material for lithium-ion batteries - Google Patents

A kind of surface modifying method of anode material for lithium-ion batteries Download PDF

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CN106159233B
CN106159233B CN201610714472.2A CN201610714472A CN106159233B CN 106159233 B CN106159233 B CN 106159233B CN 201610714472 A CN201610714472 A CN 201610714472A CN 106159233 B CN106159233 B CN 106159233B
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lithium
anode material
ion batteries
coupling agent
surface modifying
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CN106159233A (en
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李新海
徐燕
王志兴
郭华军
胡启阳
彭文杰
潘伟
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Central South University
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Central South University
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/624—Electric conductive fillers
    • 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 surface modifying methods of anode material for lithium-ion batteries, comprising the following steps: (1) coupling agent is configured to the coupling agent solution that mass concentration is 0.05%~1%；(2) anode material for lithium-ion batteries and the coupling agent solution are mixed and stirred for uniformly, conducting polymer is then added and is uniformly mixed；(3) step (2) are uniformly mixed obtained solution to be spray-dried, i.e. the surface of completion anode material for lithium-ion batteries is modified.The uniformity of cladding substance not only may be implemented in method of modifying of the invention, the time of contact of positive electrode and water can also be reduced, the modification advantage of conducting polymer can be played to a greater extent, so that positive electrode possesses more excellent chemical property, the capacity retention ratio of material is significantly improved.

Description

A kind of surface modifying method of anode material for lithium-ion batteries
Technical field
The present invention relates to field of batteries more particularly to a kind of surface modifying methods of anode material for lithium-ion batteries.
Background technique
Lithium ion battery have energy density height, capacity height, voltage platform height, memory-less effect, source it is wide, it is nontoxic, follow The ring service life is long, the advantages that having a safety feature, and is widely used in communication tool and portable electronic device etc..
Currently, anode material for lithium-ion batteries mainly has cobalt acid lithium, LiMn2O4, lithium nickelate, nickle cobalt lithium manganate, LiFePO4 Deng.The chemical property of cobalt acid lithium material is more stable, excellent electric conductivity, good cycle, is earliest realization industrialization and business The positive electrode of change, but the lower (150mAh.g of its actual capacity-1), and be more toxic, it is expensive etc., make its application by To limitation；Layered lithium manganate, capacity is relatively high, but its structural stability is poor, and Jan-Telle effect is serious；It is sharp brilliant Stone LiMn2O4, structural stability is good, but capacity is low, and high temperature flowering structure stability is remarkably decreased；Lithium nickelate material capacity It is relatively high, but materials synthesis is difficult, and stability of material is poor, poor reproducibility；LiFePO 4 material capacity is relatively high, Excellent, the stable structure of material safety energy, but its poorly conductive, limit its application in big multiplying power electrical appliance；Nickel cobalt Lithium manganate material combines cobalt acid lithium, LiMn2O4, lithium nickelate material advantage, has good thermal stability, higher specific capacity And specific energy, abundance, it is at low cost the advantages that, but the voltage platform of the material is lower, and cycle performance reduces under high voltage. Therefore, in terms of current existing situation, lithium ion battery is in energy density, security performance, cycle life and high rate performance etc. Aspect still needs to improve, thus limits it in the application in lithium-ion-power cell field, needs to anode material for lithium-ion batteries It is modified.
Cladding is one of most common lithium ion anode material method of modifying, and the electricity of positive electrode not only can be improved in cladding Lotus diffusivity, while playing the role of protecting positive electrode, the stability of positive electrode in the electrolytic solution is improved, to improve Storage performance, high rate performance, security performance of material etc..Covering material common at present has oxide (such as: Al2O3、TiO2、 SiO2, MgO etc.), fluoride (MgF2、AlF3、(NH4)3AlF6Deng), phosphate (AlPO4、Co3(PO4)2Deng), oxide can be with Effective prevention positive electrode is reacted with electrolyte, is improved the corrosion resistance of material, is improved the cycle performance of material；Fluorination Object is able to suppress reacting for hydrofluoric acid and positive electrode in electrolyte, reduces the decaying of battery capacity in charge and discharge process.But It is that most oxides, fluoride, phosphate are all non-conductive, the clad of formation can prevent lithium ion in charge and discharge process Migration, reduce material conductivity, internal resistance increase, influence the high rate performance of material.It can not only be risen using conducting polymer To the effect of protection positive electrode, the migration of lithium ion can also be promoted, therefore be currently a kind of covering material haveing excellent performance, But polymer is easy to reunite in the synthesis process, and easily affected by environment, hardly possible realizes polymer in the uniform of modified material surface Cladding, so that the performance of material is inhibited.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of anode material for lithium-ion batteries Surface modifying method, this method may be implemented the method that conducting polymer uniformly coats, improves by the electrochemistry of positive electrode Performance.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of surface modifying method of anode material for lithium-ion batteries, comprising the following steps:
(1) coupling agent is configured to the coupling agent solution that mass concentration is 0.05%~1%；
(2) anode material for lithium-ion batteries and the coupling agent solution are mixed and stirred for uniformly, are then added conductive poly- Object is closed to be uniformly mixed；
(3) step (2) are uniformly mixed obtained solution to be spray-dried, that is, complete anode material for lithium-ion batteries Surface is modified.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that during the spray drying into Doses is controlled in 5~15mL/min；Air outlet temperature is controlled at 90~110 DEG C.Feed rate is excessive, is easy to cause equipment pipe And spray head blocking；Air outlet temperature is excessively high, and moisture loss is fast, and the polymer dispersion easily caused in solution is uneven；Air outlet Temperature is too low, and moisture evaporation is slow, and covering material can be fully dispersed under the action of air-flow, so that clad is more uniform, But cause to will cause material and moisture content time of contact too long, influence the performance of material；Therefore the present invention is suitable by selection Inlet amount and air outlet temperature, make that solution sufficiently evaporates and covering material is slowly deposited in positive electrode surface, guarantee cladding The uniformity of material.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that the conducting polymer and the lithium The mass ratio of ion battery positive electrode is (0.01~0.05): 1；Conducting polymer is very few, and the clad of formation is very few, can not It completely is covered in positive electrode surface, cannot sufficiently realize the protective effect to positive electrode；Conducting polymer covering amount is excessive, Material capacity can be seriously affected, because conducting polymer belongs to inert material in the voltage range of measurement, does not have electrochemistry Activity.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that the anode material for lithium-ion batteries Selected from any one of cobalt acid lithium, LiMn2O4, lithium nickelate, nickle cobalt lithium manganate and LiFePO4.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that the coupling agent is selected from silane coupled At least one of agent, titanate coupling agent, aluminate coupling agent.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that the conducting polymer is selected from polyphenyl Any one of amine, polythiophene, polypyrrole.
The surface modifying method of above-mentioned anode material for lithium-ion batteries, it is preferred that in the step (1), be additionally added vinegar Acid adjusts the pH value of coupling agent solution to 4.Acetic acid plays hydrolyzation catalysis in the use process of silane coupling agent and adjusts pH's Effect.Since there are lithium carbonate, the residual alkalis such as lithium hydroxide in positive electrode surface, so that the aobvious alkalinity of material surface, more if pH value is lower Remaining acid can destroy the surface of material, if pH higher, and cannot achieve the effect that it is modified, so pH value control is by final choice 4。
The principle of the surface modifying method of anode material for lithium-ion batteries of the invention will be as shown in Figure 1, will using coupling agent Conducting polymer is tentatively adsorbed on the surface of positive electrode, first with the chemical bond characteristics of coupling agent itself, makes it as intermediate Then in conjunction with polymer, polymer may be implemented in medium, the functional group of one end and the hydroxy combining on positive electrode surface, the other end Preliminary cladding on the surface of the material；But the liquid phase coating in solution can not achieve the cladding of metering ratio, therefore in liquid phase coating Under the premise of, secondary cladding is completed using spray seasoning, positive electrode surface treated with coupling agent has had coupling agent Functional group be dispersed in aerosol can when polymer molecule is under high temperature action, as temperature reduces and coupling agent chemistry The effect of key, makes polymer slowly be covered in material surface, to realize the uniformity of cladding.
The uniformity of cladding substance not only may be implemented in method of modifying of the invention, can also reduce positive electrode and water Time of contact can play the modification advantage of conducting polymer to a greater extent, so that positive electrode possesses more excellent electrification Performance is learned, the capacity retention ratio of material significantly improves.
Compared with the prior art, the advantages of the present invention are as follows:
(1) for the present invention on the basis of liquid phase coating, the method for recycling spray drying utilizes the steaming of moisture under high temperature Hair is realized and is uniformly present in around positive electrode after covering material forms fog, be then evenly affixed to positive electrode surface, to the greatest extent Possibly realize maximally utilizing for covering material.
(2) since sensitivity of the positive electrode to moisture is higher, using spraying method, liquid phase packet can be greatly shortened The time covered；Meanwhile during spray drying, moisture can evaporate rapidly；So that entirely coating process, positive material is reduced The time of contact of material and moisture, improve the chemical property of material.
(3) effect of the invention first with the chemical bond between group in coupling agent, by the very big material interface of performance difference Coupling is got up, to improve the performance of composite material and increase bond strength；Using coupling agent as connection conducting polymer with Medium between positive electrode can make polymer more firmly adhere to and be coated on positive electrode surface, while can be with Promote being uniformly distributed for conducting polymer, forms uniform clad.
Detailed description of the invention
Fig. 1 is the schematic diagram of the surface modifying method of anode material for lithium-ion batteries of the invention.
Fig. 2 is the flow chart of the surface modifying method of anode material for lithium-ion batteries of the invention.
Fig. 3 is the TEM figure of the modified anode material for lithium-ion batteries in 4 surface of the embodiment of the present invention.
Fig. 4 is the cyclic curve figure of the surface modification lithium-ion battery anode material of the embodiment of the present invention
Fig. 5 is the cyclic curve figure for the anode material for lithium-ion batteries (blank sample) that comparative example 1 of the present invention uses.
Fig. 6 is the cyclic curve figure of the surface modification lithium-ion battery anode material of comparative example 1 of the present invention.
Fig. 7 is the TEM figure of the modified anode material for lithium-ion batteries in the surface of comparative example 2 of the present invention.
Fig. 8 is the cyclic curve figure of the modified anode material for lithium-ion batteries in the surface of comparative example 2 of the present invention.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter 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 scope.
Except there is a special instruction, the various reagents used in the present invention, raw material be can commodity commercially or Person can the product as made from well known method.
Embodiment 1:
A kind of surface modifying method of anode material for lithium-ion batteries of the invention, flow chart is as shown in Fig. 2, specific packet Include following steps:
(1) Silane coupling agent KH550 is soluble in water, the pH value of vinegar acid-conditioning solution is added to 4, being made into mass concentration is 0.05% Silane coupling agent KH550 solution；
(2) the Silane coupling agent KH550 solution of anode material lithium nickle cobalt manganic acid of lithium ion battery and step (1) preparation is mixed Merging stirs evenly, and polypyrrole is then added and is uniformly mixed, and wherein the mass ratio of polypyrrole and nickle cobalt lithium manganate is 0.01:1；
(3) solution that step (2) are uniformly mixed is spray-dried, controlling charging rate in spray-drying process is 5mL/min, air outlet temperature are 90 DEG C, finally collect powder and dry 8h at 80 DEG C, complete the table of anode material for lithium-ion batteries Face is modified.
The modified anode material for lithium-ion batteries in the surface that step (3) are obtained carries out smear and battery assembly is tested, material Discharge capacity is 206.8mAh.g to material for the first time-1, first charge-discharge efficiency 86.2%, capacity retention ratio is after 1C is recycled 100 times 82.3%.
Embodiment 2:
A kind of surface modifying method of anode material for lithium-ion batteries of the invention, flow chart is as shown in Fig. 2, specific packet Include following steps:
(1) Silane coupling agent KH550 is soluble in water, the pH value of vinegar acid-conditioning solution is added to 4, being made into mass concentration is 0.05% Silane coupling agent KH550 solution；
(2) the Silane coupling agent KH550 solution of anode material lithium nickle cobalt manganic acid of lithium ion battery and step (1) preparation is mixed Merging stirs evenly, and polypyrrole is then added and is uniformly mixed, and wherein the mass ratio of polypyrrole and nickle cobalt lithium manganate is 0.02:1；
(3) solution that step (2) are uniformly mixed is spray-dried, controlling charging rate in spray-drying process is 10mL/min, air outlet temperature are 90 DEG C, finally collect powder and dry 8h at 80 DEG C, complete the table of anode material for lithium-ion batteries Face is modified.
The modified anode material for lithium-ion batteries in the surface that step (3) are obtained carries out smear and battery assembly is tested, material Discharge capacity is 207.1mAh.g to material for the first time-1, first charge-discharge efficiency 86.7%, capacity retention ratio is after 1C is recycled 100 times 84.5%.
Embodiment 3:
A kind of surface modifying method of anode material for lithium-ion batteries of the invention, flow chart is as shown in Fig. 2, specific packet Include following steps:
(1) Silane coupling agent KH550 is soluble in water, the pH value of vinegar acid-conditioning solution is added to 4, being made into mass concentration is 0.08% Silane coupling agent KH550 solution；
(2) anode material lithium nickle cobalt manganic acid of lithium ion battery is mixed simultaneously with Silane coupling agent KH550 prepared by step (1) It stirs evenly, polypyrrole is then added and is uniformly mixed, wherein the mass ratio of polypyrrole and anode material nickel cobalt manganic acid lithium is 0.02: 1；
(3) solution that step (2) are uniformly mixed is spray-dried, controlling charging rate in spray-drying process is 10mL/min, air outlet temperature are 100 DEG C, finally collect powder and dry 8h at 80 DEG C, complete anode material for lithium-ion batteries Surface is modified.
The TEM of the surface modification lithium-ion battery anode material of the present embodiment schemes as shown in figure 3, from figure 3, it can be seen that material Expect surface uniform fold layer of substance, and the thickness of clad is about 12-15nm, and be amorphous state, with polypyrrole It is amorphous consistent.
The surface modification lithium-ion battery anode material internal crystal framework of the present embodiment changes by Fourier, and determination is matrix Positive electrode, illustrate the method really on the surface of the material formed one layer of uniform polymer covering layer.
The modified anode material for lithium-ion batteries in the surface that step (3) are obtained carries out smear and battery assembly is tested, material Discharge capacity is 207.7mAh.g to material for the first time-1, first charge-discharge efficiency 87.1%, capacity retention ratio is after 1C is recycled 100 times 86.4%.
Embodiment 4:
A kind of surface modifying method of anode material for lithium-ion batteries of the invention, flow chart is as shown in Fig. 2, specific packet Include following steps:
(1) Silane coupling agent KH550 is soluble in water, the pH value of vinegar acid-conditioning solution is added to 4, being made into mass concentration is 0.08% Silane coupling agent KH550 solution；
(2) the Silane coupling agent KH550 solution of anode material lithium nickle cobalt manganic acid of lithium ion battery and step (1) preparation is mixed Merging stirs evenly, and polypyrrole is then added and is uniformly mixed, wherein the mass ratio of polypyrrole and anode material nickel cobalt manganic acid lithium is 0.03:1；
(3) solution that step (2) are uniformly mixed is spray-dried, controlling charging rate in spray-drying process is 10mL/min, air outlet temperature are 110 DEG C, finally collect powder and dry 8h at 80 DEG C, complete anode material for lithium-ion batteries Surface is modified, and cyclic curve figure is as shown in Figure 4.
The modified anode material for lithium-ion batteries in the surface that step (3) are obtained carries out smear and battery assembly is tested, material Discharge capacity is 207.6mAh.g to material for the first time-1, first charge-discharge efficiency 87.5%, capacity retention ratio is after 1C is recycled 100 times 87.7%.
Comparative example 1:
The anode material for lithium-ion batteries that this comparative example is selected is same as Example 4, and cyclic curve figure is as shown in Figure 5.
The method of modifying of the anode material for lithium-ion batteries of this comparative example: other not using coupling agent as intermediate medium Technical process it is same as Example 4, the cyclic curve figure for the surface modification lithium-ion battery anode material that this comparative example obtains As shown in Figure 6.
From Fig. 4~Fig. 6 it is found that at 25 DEG C of room temperature, 1C (160mA h under 2.8-4.6V-1) circulation 100 times after, do not appointed The capacity of the positive electrode of what modification has dropped 44mAh g-1, under the capacity of the modified anode material without coupling agent treatment 34mAh g has dropped-1, and the capacity for passing through the modified positive electrode of method of modifying of the invention only has dropped 23mAh g-1.By This is as it can be seen that the surface modifying method of anode material for lithium-ion batteries of the invention can improve the cycle performance of material really.
Comparative example 2:
The surface modifying method of the anode material for lithium-ion batteries of this comparative example and the difference of embodiment 4 are only that dry Mode is different, using vacuum drying.
The anode material for lithium-ion batteries TEM that the surface modifying method of the anode material for lithium-ion batteries of this comparative example obtains Figure is as shown in fig. 7, its cyclic curve figure is as shown in Figure 8.
As shown in Figure 7, the surface of anode material for lithium-ion batteries is modified using vacuum drying mode, also can One layer of clad is obtained on the surface of anode material for lithium-ion batteries, but the structure of the clad is lax and uneven Even.
As shown in Figure 8, the surface of anode material for lithium-ion batteries is modified using vacuum drying mode, is obtained Modification lithium-ion battery anode material 1C recycle 100 times after capacity decline 28mAh g-1。
It can be seen that the clad of material can not only be made compared to the mode of other dryings by the way of spray drying It is more uniform, and the chemical property of material can also be improved.
Embodiment 5:
A kind of surface modifying method of anode material for lithium-ion batteries of the invention, flow chart is as shown in Fig. 2, specific packet Include following steps:
(1) Silane coupling agent KH550 is soluble in water, the pH value of vinegar acid-conditioning solution is added to 4, being made into mass concentration is 0.1% Silane coupling agent KH550 solution；
(2) anode material lithium nickle cobalt manganic acid of lithium ion battery is mixed simultaneously with Silane coupling agent KH550 prepared by step (1) It stirs evenly, polypyrrole is then added and is uniformly mixed, wherein the mass ratio of polypyrrole and anode material nickel cobalt manganic acid lithium is 0.05: 1；
(3) solution that step (2) are uniformly mixed is spray-dried, controlling charging rate in spray-drying process is 15mL/min, air outlet temperature are 110 DEG C, finally collect powder and dry 8h at 80 DEG C, complete anode material for lithium-ion batteries Surface is modified.
The modified anode material for lithium-ion batteries in the surface that step (3) are obtained carries out smear and battery assembly is tested, material Discharge capacity is 206.9mAh.g to material for the first time-1, first charge-discharge efficiency 86.1%, capacity retention ratio is after 1C is recycled 100 times 85.9%.

Claims (6)

1. a kind of surface modifying method of anode material for lithium-ion batteries, which comprises the following steps:
(1) coupling agent is configured to the coupling agent solution that mass concentration is 0.05%~1%；
(2) it is mixed and stirred for anode material for lithium-ion batteries and the coupling agent solution uniformly, conducting polymer is then added It is uniformly mixed；
(3) step (2) are uniformly mixed obtained solution to be spray-dried, that is, complete the surface of anode material for lithium-ion batteries It is modified；Wherein, inlet amount is controlled in 5~15mL/min during the spray drying；Air outlet temperature is controlled 90~110 ℃。
2. the surface modifying method of anode material for lithium-ion batteries as described in claim 1, which is characterized in that described conductive poly- The mass ratio for closing object and the anode material for lithium-ion batteries is (0.01~0.05): 1.
3. the surface modifying method of anode material for lithium-ion batteries as described in claim 1, which is characterized in that the lithium ion Cell positive material is selected from any one of cobalt acid lithium, LiMn2O4, lithium nickelate, nickle cobalt lithium manganate and LiFePO4.
4. the surface modifying method of anode material for lithium-ion batteries as described in claim 1, which is characterized in that the coupling agent Selected from least one of silane coupling agent, titanate coupling agent, aluminate coupling agent.
5. the surface modifying method of anode material for lithium-ion batteries as described in claim 1, which is characterized in that described conductive poly- It closes object and is selected from any one of polyaniline, polythiophene, polypyrrole.
6. the surface modifying method of anode material for lithium-ion batteries as claimed in any one of claims 1 to 5, which is characterized in that In the step (1), it is additionally added acetic acid and adjusts the pH value of coupling agent solution to 4.
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