CN103730636B - Prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method - Google Patents

Prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method Download PDF

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Publication number
CN103730636B
CN103730636B CN201310715365.8A CN201310715365A CN103730636B CN 103730636 B CN103730636 B CN 103730636B CN 201310715365 A CN201310715365 A CN 201310715365A CN 103730636 B CN103730636 B CN 103730636B
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lini
vacuum
metal
high potential
positive plate
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CN103730636A (en
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梁兴华
黄美红
吴汉杰
刘于斯
史琳
曾帅波
叶超超
刘天骄
华晓鸣
宋清清
刘浩
刘大玉
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Guangxi University of Science and Technology
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Guangxi University of Science and Technology
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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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • H01M4/0423—Physical vapour deposition
    • H01M4/0426—Sputtering
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/626—Metals
    • 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
    • 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 provides one and prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method, comprise the steps: steps A: by nickel ion doped, binding agent, conductive agent, ratio by amount of substance: 50-90:30-10:20-5 mixes, stir in vacuum, mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, coating thickness 10-200 micron, then after vacuum drying pole piece roll extrusion to 5-150 micron thickness; Step B: metal is heated to fusing point in vacuum casting furnace, pours in target mould after insulation, then is cooled to room temperature after metal melts completely; Step C: plasma direct-current sputtering metal-coated membrane, is cooled to room temperature subsequently, takes out, make high potential LiNi after cleaning 0.5mn 1.5o 4battery anode slice.After adopting the method, the multiplying power property of battery can be significantly improved, more than 2-10C high power charging-discharging can be realized, thus improve the power of battery.

Description

Prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method
Technical field
The present invention relates to a kind of based lithium-ion battery positive plate method, particularly relate to a kind of metal plasma direct current sputtering and prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method.
Background technology
High potential positive electrode LiNi 0.5mn 1.5o 4(nickel ion doped) has higher capacity (about 146mAh/g), high cycle life (higher than 2500 times) and high voltage (about 4.7V) discharge platform, not only can meet the personal electric consumer goods and electric automobile to the demand of power supply of new generation, and can the higher negative material of compatible operations voltage (as 1.55VLi 4ti 5o 12), thus improve the security performance of battery, become one of positive electrode that advanced lithium ion battery of future generation attracts most attention.When this positive electrode is prepared into battery pole piece, the general carbon black that adopts is as conductive agent.Plasma sputtering metal is used to the preparation of various function film, is a kind of novel coating technique.
The method improving electrodes of lithium-ion batteries conductivity mainly has doping again, adds the modes such as conductive additive, as conductive doped carbon black, adds the method such as conductive metal powder, silk.Can conductive network be built, the route of metastasis of lithium ion be got a promotion, thus improves its diffusion coefficient, increase conductivity.Though conventional method can improve electric conductivity, battery in use positive electrode due to electrochemical reaction be easy to dissolve in the electrolytic solution, namely prior art not can solve positive electrode dissolve problem.Therefore, the positive electrode LiNi of present invention process method process is not adopted 0.5mn 1.5o 4(nickel ion doped) cycle life is poor, and particularly under high magnification condition, cycle performance is poorer.
Summary of the invention
In order to solve above technical problem, the invention provides one and preparing high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method, comprises the steps:
Steps A: by nickel ion doped, binding agent, conductive agent, ratio by amount of substance: 50-90:30-10:20-5 mixes, stir in vacuum, mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, coating thickness 10-200 micron, then after vacuum drying pole piece roll extrusion to 5-150 micron thickness;
Step B: metal is heated to fusing point in vacuum casting furnace, pours in target mould after insulation, then is cooled to room temperature after metal melts completely;
Step C: the metal targets prepared and electrode slice are put into plasma sputtering instrument vacuum specimen chamber, plasma direct-current sputtering metal-coated membrane, is cooled to room temperature subsequently, takes out, make high potential LiNi after cleaning 0.5mn 1.5o 4battery anode slice.
The present invention adopts above technical scheme, its advantage is, the first step adopts the conventional conductive black that adds to prepare battery pole piece, second step adopts plasma direct-current sputtering technology by conducting metal target metal-coated membrane on battery electrode, be different from conventional mixing and doping technology, the netted half coated with conductive metal film of the continuous plating of electrode surface can be realized.In the existence of electrode interior due to carbon black conductive agent, " point-line " conductive network can be built, at electrode surface due to the high conductivity of metal film, " face-face " can be built and conduct electricity system, significantly can improve the conductivity of conventional batteries pole piece.Meanwhile, electrode surface metal film can completely cut off or reduce the contact area of electrode material and electrolyte, in discharge and recharge use procedure, can reduce electrolyte to high potential LiNi 0.5mn 1.5o 4the corrosivity of electrode, reduces electrode material dissolving in the electrolytic solution, significantly improves the useful life of battery.
Preferably, described conductive agent adopts one or more in carbon black, active carbon, carbon nano-tube, electrically conductive graphite, and described binding agent adopts one or more in PVDF, PTFE, carboxylic styrene butadiene latex.
Preferably, in described steps A, stir 12 hours in vacuum, stirred vessel vacuum degree 10 -5pa.
Preferably, in described steps A, the temperature of oven dry is 80 DEG C, drying time 18 hours.
Preferably, in described step B, metal adopts one or more in Al, Cu, Ni, Cr, Co, Zn, Fe, Mn, Ag, Au.
Preferably, in described step B, the fusing point of metal is 700-1650 DEG C, vacuum degree 10 -5pa, temperature retention time is 1 hour, and cooldown rate is 20 DEG C/min.
Preferably, in described step C, the condition in plasma sputtering instrument vacuum specimen chamber is: be evacuated to 5X10 -2mbar, passes into high-purity argon gas (99.99%) clean vacuum chambers, then is evacuated to 5X10 -2mbar.Regulation voltage to 1600-3000V, electric current 10-50mA.
Preferably, in described step C, the time of plasma direct-current sputtering metal-coated membrane is 0.85 hour.
The invention has the beneficial effects as follows: the present invention adopts two-step method to prepare high potential LiNi 0.5mn 1.5o 4(nickel ion doped) based lithium-ion battery positive plate.
After adopting the method, because positive electrode improves the tolerance of electrolyte, the multiplying power property of battery can be significantly improved, more than 5-10C high power charging-discharging can be realized, thus improve the power of battery.
Accompanying drawing explanation
Fig. 1 is cycle performance curve under pole piece battery 2C multiplying power in embodiment 1.
Fig. 2 is cycle performance curve under pole piece battery 2C multiplying power in embodiment 2.
Fig. 3 is cycle performance curve under pole piece battery 2C multiplying power in embodiment 3.
Fig. 4 is cycle performance curve under pole piece battery 5C multiplying power in embodiment 1.
Fig. 5 is cycle performance curve under pole piece battery 5C multiplying power in embodiment 2.
Fig. 6 is cycle performance curve under pole piece battery 5C multiplying power in embodiment 3.
Fig. 7 is cycle performance curve under pole piece battery 10C multiplying power in embodiment 1.
Fig. 8 is cycle performance curve under pole piece battery 10C multiplying power in embodiment 2.
Fig. 9 is cycle performance curve under pole piece battery 10C multiplying power in embodiment 3.
Figure 10 is that the electrode slice section S EM of coated metal film in the present invention schemes.
Embodiment
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
Embodiment 1:
A. by nickel ion doped: PVDF: the ratio 5:3:2 that carbon black presses amount of substance mixes, and mixing high-speed mixing equipment stirs 12 hours in a vacuum, stirred vessel vacuum degree 10-5Pa.Mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, and coating thickness 10-200 micron, then 80 DEG C of vacuum dryings 18 hours.After drying, pole piece roll extrusion is to 5-150 micron thickness, and cutting becomes assembled battery required size.
B. metal A l is heated in vacuum casting furnace fusing point 700 DEG C, vacuum degree 10 -5pa, is incubated 1 hour, pours in target mould, be cooled to room temperature with 20 DEG C/min speed after metal melts completely.
C. the metal targets prepared and electrode slice are put into plasma sputtering instrument vacuum specimen chamber, be evacuated to 5X10 -2mbar, passes into high-purity argon gas (99.99%) clean vacuum chambers, then is evacuated to 5X10 -2mbar.Regulation voltage is to 1600V, and electric current 10mA, plasma direct-current sputtering metal-coated membrane 0.85 hour, is cooled to room temperature subsequently, takes out after high-purity argon gas (99.99%) clean vacuum chambers, makes the high potential LiNi that conductivity is high, electrolyte resistance corrodes 0.5mn 1.5o 4battery anode slice.
Embodiment 2:
A. by nickel ion doped: PTFE: active carbon is 90:10:5 mixing by the ratio of amount of substance, and mixing high-speed mixing equipment stirs 12 hours in a vacuum, stirred vessel vacuum degree 10 -5pa.Mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, and coating thickness 10-200 micron, then 80 DEG C of vacuum dryings 18 hours.After drying, pole piece roll extrusion is to 5-150 micron thickness, and cutting becomes assembled battery required size.
B. Ni metal is heated in vacuum casting furnace fusing point 1150 DEG C, vacuum degree 10 -5pa, is incubated 1 hour, pours in target mould, be cooled to room temperature with 20 DEG C/min speed after metal melts completely.
C. the metal targets prepared and electrode slice are put into plasma sputtering instrument vacuum specimen chamber, be evacuated to 5X10 -2mbar, passes into high-purity argon gas (99.99%) clean vacuum chambers, then is evacuated to 5X10 -2mbar.Regulation voltage is to 3000V, and electric current 50mA, plasma direct-current sputtering metal-coated membrane 0.85 hour, is cooled to room temperature subsequently, takes out after high-purity argon gas (99.99%) clean vacuum chambers, makes the high potential LiNi that conductivity is high, electrolyte resistance corrodes 0.5mn 1.5o 4battery anode slice.
Embodiment 3
A. nickel ion doped, carboxylic styrene butadiene latex and electrically conductive graphite are pressed amount of substance than being 70:20:15 mixing, mixing high-speed mixing equipment stirs 12 hours in a vacuum, stirred vessel vacuum degree 10 -5pa.Mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, and coating thickness 10-200 micron, then 80 DEG C of vacuum dryings 18 hours.After drying, pole piece roll extrusion is to 5-150 micron thickness, and cutting becomes assembled battery required size.
B. W metal and Cr are heated to the above 20-50 DEG C of melting point metal with mass ratio 1:1 ratio, vacuum degree 10 in vacuum casting furnace -5pa, is incubated 1 hour, pours in target mould, be cooled to room temperature with 20 DEG C/min speed after metal melts completely.
C. the metal targets prepared and electrode slice are put into plasma sputtering instrument vacuum specimen chamber, be evacuated to 5X10 -2mbar, passes into high-purity argon gas (99.99%) clean vacuum chambers, then is evacuated to 5X10 -2mbar.Regulation voltage is to 2000V, and electric current 30mA, plasma direct-current sputtering metal-coated membrane 0.85 hour, is cooled to room temperature subsequently, takes out after high-purity argon gas (99.99%) clean vacuum chambers, makes the high potential LiNi that conductivity is high, electrolyte resistance corrodes 0.5mn 1.5o 4battery anode slice.
From Fig. 1 to 9, the battery that pole piece of the present invention and lithium form, than the battery that undressed nickel ion doped pole piece and lithium form, has the following advantages:
1. under identical multiplying power condition, cycle performance improves, and after 20 circulations, capability retention is high.
2. under high magnification 2-10C condition, particularly 10C cycle performance of battery is good, and capacity still can keep 92mAh/g.
3. the positive plate prepared by forms LiNi in inside 0.5mn 1.5o 4" line-line " the type conductive network be made up of conductive agent (in carbon black, active carbon, carbon nano-tube, electrically conductive graphite one or more) between particle, the thermal interface that " face-face " contact is formed at pole piece conductive metal film (in Al, Cu, Ni, Cr, Co, Zn, Fe, Mn, Ag, Au one or more), strengthen lithium ion on a large scale to deviate from and embedding path, and then significantly improve the conductivity of lithium ion cell electrode.Meanwhile, electrode surface metal film can completely cut off or reduce the contact area of electrode material and electrolyte, in discharge and recharge use procedure, can reduce electrolyte to high potential LiNi 0.5mn 1.5o 4the corrosivity of electrode, reduces electrode material dissolving in the electrolytic solution, significantly improves the useful life of battery.The first step of this method adopts conductive agent, LiNi 0.5mn 1.5o 4anode electrode prepared by positive electrode and binding agent, and second step adopts Conventional plasma direct current sputtering technology by conducting metal target metal-coated membrane on battery electrode, and as shown in Figure 10, final preparation conductivity is high, the battery anode slice of electrolyte resistance corrosion.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.

Claims (6)

1. prepare high potential LiNi for one kind 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, comprises the steps:
Steps A: ratio nickel ion doped, binding agent, conductive agent being pressed amount of substance: 50-90:30-10:20-5 mixes, stir in vacuum, mixed slurry double spread is on the aluminium film of 0.15-0.45 micron thickness, coating thickness 10-200 micron, then after vacuum drying pole piece roll extrusion to 5-150 micron thickness;
Step B: metal is heated to fusing point in vacuum casting furnace, pours in target mould after insulation, then is cooled to room temperature after metal melts completely;
Step C: the metal targets prepared and electrode slice are put into plasma sputtering instrument vacuum specimen chamber, plasma direct-current sputtering metal-coated membrane, is cooled to room temperature subsequently, takes out, make high potential LiNi after cleaning 0.5mn 1.5o 4battery anode slice;
In described step B, the fusing point of metal is 700-1650 DEG C, vacuum degree 10 -5pa, temperature retention time is 1 hour, and cooldown rate is 20 DEG C/min;
In described step C, the condition in plasma sputtering instrument vacuum specimen chamber is: be evacuated to 5X10 -2mbar, passes into high-purity argon gas clean vacuum chambers, then is evacuated to 5X10 -2mbar, regulation voltage to 1600-3000V, electric current 10-50mA.
2. prepare high potential LiNi as claimed in claim 1 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, described conductive agent adopts one or more in carbon black, active carbon, carbon nano-tube, electrically conductive graphite, and described binding agent adopts one or more in PVDF, PTFE, carboxylic styrene butadiene latex.
3. prepare high potential LiNi as claimed in claim 1 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, in described steps A, stirs 12 hours, stirred vessel vacuum degree 10 in vacuum -5pa.
4. prepare high potential LiNi as claimed in claim 1 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, in described steps A, the temperature of oven dry is 80 DEG C, drying time 18 hours.
5. prepare high potential LiNi as claimed in claim 1 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, in described step B, metal adopts one or more in Al, Cu, Ni, Cr, Co, Zn, Fe, Mn, Ag, Au.
6. prepare high potential LiNi as claimed in claim 1 0.5mn 1.5o 4based lithium-ion battery positive plate method, is characterized in that, in described step C, the time of plasma direct-current sputtering metal-coated membrane is 0.85 hour.
CN201310715365.8A 2013-12-20 2013-12-20 Prepare high potential LiNi 0.5mn 1.5o 4based lithium-ion battery positive plate method Expired - Fee Related CN103730636B (en)

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CN104795542A (en) * 2015-01-06 2015-07-22 宁波南车新能源科技有限公司 A plasma injection preparing method of a nanometer lithium ion composite anode
CN105161684B (en) * 2015-08-31 2018-11-13 无锡市嘉邦电力管道厂 A kind of lithium battery anode slurry and preparation method thereof
CN112615006A (en) * 2020-12-17 2021-04-06 广西科技大学 Preparation method of high-performance composite binder for energy storage charging system battery

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CN102185134A (en) * 2011-04-15 2011-09-14 福建师范大学 Method for preparing lithium cobalt oxide anode of silicon-based film lithium ion battery by using high temperature immobile phase-surface deposition method
CN102299316A (en) * 2011-09-08 2011-12-28 浙江吉能电池科技有限公司 Layered oxide lithium ion battery anode and preparation method thereof
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