CN108039454A - A kind of preparation method of lithium anode, lithium anode and lithium battery - Google Patents
A kind of preparation method of lithium anode, lithium anode and lithium battery Download PDFInfo
- Publication number
- CN108039454A CN108039454A CN201711341704.5A CN201711341704A CN108039454A CN 108039454 A CN108039454 A CN 108039454A CN 201711341704 A CN201711341704 A CN 201711341704A CN 108039454 A CN108039454 A CN 108039454A
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- lithium
- anode
- preparation
- metal
- fluorocarbons
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
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- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a kind of preparation method of lithium anode, lithium anode and lithium battery.The preparation method includes：Step 1, positive plate slurry is prepared by positive active material of fluorocarbons, by the coating of positive plate slurry on a current collector, punching prepares fluorocarbons pole piece；Step 2, button cell is assembled with metal lithium sheet, fluorocarbons pole piece and lithium ion electrical conductance solution, wherein, metal lithium sheet, fluorocarbons pole piece directly contact；Step 3, a period of time is stood, dismantles button cell, takes out metal lithium sheet, its surface has lithium metal protective layer.The present invention introduces lithium fluoride in metallic lithium surface by way of reaction in-situ, so that stable metal lithium be made, is not required to add any additional technique, and method is simple and practicable, and commercial viability is strong, great industrial applications value and potentiality.Lithium anode prepared by the present invention is respectively provided with splendid cycle performance in all kinds of lithium batteries, has a good application prospect in the lithium secondary battery and universality.
Description
Technical field
The invention belongs to field of chemical power source, falls within technical field of energy material.More particularly to a kind of stable metal lithium
The preparation and application of anode.
Background technology
As the continuous innovation of electronic communication and development, secondary cell are increasingly subject to the concern of people.Lithium-ion electric
Pond is by advantages such as specific capacity height, good cycling stabilities, it is considered to be the most secondary cell of development potentiality and prospect.With people
To energy density requirement continuous improvement, lithium ion battery be difficult meet it is increasing than energy the needs of, exploitation
High power capacity anode be develop 400Wh/kg lithium batteries important prerequisite, the lithium anode then with height ratio capacity inherent advantage
Attract much attention.
The ratio energy of lithium ion battery is up to 250Wh/kg at present, but if we replace the anode of lithium ion battery
For lithium metal, then we are obtained with the ratio energy of 440Wh/kg even more highs, and as Li-S and Li- air cells ratio energy
Amount can then reach the ratio energy of 650Wh/kg and 950Wh/kg.The theoretical specific capacity of lithium metal is 3860mAh/g, electrochemical potential
It is a kind of ideal lithium cell cathode material for -3.04V (vs standard hydrogen electrodes).
Lithium metal has very tempting application prospect in terms of high-efficiency energy-storage, but since lithium is during discharge and recharge, by
It is uneven in concave-convex surface, cause surface potential skewness, cause the nonuniform deposition of lithium.The nonuniform deposition process causes lithium
It is too fast in some site depositions, produce the crystallization as branch, i.e. Li dendrite.When dendrite develops to a certain extent, a side
Face can fracture, fractureing partly because having completely cut off electrical contact with electrode and can not continue to participate in electrode reaction, referred to as " extremely
Lithium ", on the other hand more seriously, dendrite may pass through membrane, by positive electrode and negative electrode connection so as to short circuit, produce high current and
Thermal runaway, makes batteries caught fire, or even explodes.The growth of cathode of lithium Li dendrite in battery charge and discharge process restricts lithium metal
Application in commodity electrochemical cell.
Therefore, there is an urgent need for a kind of preparation process of stable metal cathode of lithium is developed, to adapt to lithium metal in commodity electrochemical cell
In application.
The content of the invention
Pole piece concave-convex surface inequality, surface potential skewness present invention aim to address conventional lithium battery cause
Cathode of lithium in battery charge and discharge process Li dendrite phenomenon, metal lithium sheet surface formed layer protective layer, formed stablize gold
Belong to cathode of lithium, which is not likely to produce dendrite in charge and discharge process, avoids security risk, and have excellent cyclicity
Energy.
In order to achieve the above object, the present invention provides a kind of preparation method of lithium anode, comprising：
Step 1, positive plate slurry is prepared by positive active material of fluorocarbons, positive plate slurry is coated on collector
On, punching prepares fluorocarbons pole piece；
Step 2, button cell is assembled with metal lithium sheet, fluorocarbons pole piece and lithium ion electrical conductance solution, wherein, lithium metal
Piece, fluorocarbons pole piece directly contact；
Step 3, a period of time is stood, dismantles button cell, takes out metal lithium sheet, which is the processing of perfluorinated carbon
Metal lithium sheet afterwards, its surface have lithium metal protective layer, can serve as stable metal cathode of lithium.Wherein, lithium metal and fluorocarbons
After contact, following spontaneous reaction occurs：
xLi+CFx→xLiF+C
Generate lithium fluoride protective layer.
It is preferred that the positive plate slurry also includes conductive agent, conductive agent selection conductive black.
It is preferred that the collector selection copper foil or aluminium foil.
It is preferred that in step 2, the lithium ion electrical conductance solution is lithium-ion battery electrolytes.
It is preferred that in step 2, lithium ion electrical conductance solution selection 1.2M LiPF6Solution, solvent are ethylene
The mixed liquor of enester EC and methyl ethyl ester EMC, wherein, EC:EMC=3:7, with volume basis.
It is preferred that in step 3, when time of repose is 0.01-48 small；More preferably, when time of repose is 0.01-24 small.
Present invention also offers a kind of lithium anode according to made from above-mentioned preparation method, lithium anode surface tool
There is lithium metal protective layer, it is preferred that the protective layer is lithium fluoride protective layer.
Present invention also offers a kind of lithium battery, which contains：Membrane, organic electrolyte, anode pole piece and according to
Lithium anode pole piece made from above-mentioned preparation method.It is preferred that the active material selection ferric phosphate of the anode pole piece
Any one in lithium, sulphur carbon material, lithium titanate material.The operating temperature of the lithium ion is mainly -30~50 DEG C.
Battery not is assembled into having the structure means of protective layer lithium metal in the present invention, but directly uses lithium metal and fluorine
Change carbon contact, one layer of lithium fluoride protective layer is formed on metal lithium sheet surface, so as to avoid lithium metal battery in discharge and recharge
The generation of Li dendrite in journey.For convenience of the separation after subsequent operation, and fluorocarbons reaction, fluorocarbons is coated on collector
On, then be allowed to contact with lithium metal；To ensure that contact is good, lithium ion electrical conductance solution also added wherein.Reaction is completed
Afterwards, it is necessary to throw off fluorocarbons, the lithium anode of stabilization with protective layer is obtained.
The present invention is not required to add any additional technique, it is only necessary to fluorocarbons is directly being contacted with lithium metal, is passing through fluorocarbons
The lithium anode is prepared with lithium metal reaction in-situ preparation lithium fluoride protective layer, method is simple and practicable, and lithium and fluorine
Changing the degree of carbon reaction can control by time of contact, and highly practical, the lithium anode being prepared has excellent
Cycle performance, can be used as long-life, high-specific energy battery to be applied, have great market potential and prospect, this method
With great industrial application value.
Brief description of the drawings
Fig. 1 is the embodiment of the present invention 1 by lithium metal surface optical photo before and after the processing.
The specific capacity voltage after lithium before and after the processing-lithium titanate battery first circle and the circle of circulation 30 is bent for embodiment 1 by Fig. 2
Line.
Fig. 3 specific capacity voltage curves after lithium-sulfur cell first circle before and after the processing and the circle of circulation 30 for embodiment 3.
Embodiment
Technical scheme is described further below in conjunction with drawings and examples.
Membrane is existing commercial all kinds of membranes, and Celgard 2325 has been selected in embodiment.
Test method described in following embodiments, if without specified otherwise, the reagent and material, are commercially obtained
.
Embodiment 1
(1) stable lithium anode is prepared：
Accurately 0.1g Kynoar (PVDF) is weighed to be substantially dissolved in 3.4g solvent N-methyl pyrilidones (NMP),
0.1g conductive blacks are added after being mixed evenly to be mixed evenly, and are added 0.8g fluorocarbons and are mixed evenly, are stirred overnight rear even spread
In copper foil current collector, the pole piece of 18mm is punched into；After drying metal lithium sheet is sequentially placed into CR2016 type button cell shells
With fluorocarbons pole piece, proper amount of electrolyte LiPF is added6(EC:DMC 3:7) dismantled after, standing 24h, metal after being handled
Lithium piece, there is one layer of grey matter on metal lithium sheet surface after processing as shown in Figure 1, may be the lithium fluoride protective layer after reaction.Should
Metal lithium sheet can be used as stable lithium anode after processing.
(2) lithium metal-lithium titanate (LTO) battery is assembled：
Metal lithium sheet after handling is sequentially placed into CR2016 type button cell shells, (existing commercial all kinds of membranes are equal for membrane
Can, such as 2325 membranes of Celgard) and metatitanic acid pole piece, add proper amount of electrolyte LiPF6(EC:DMC 3:7), it is compacted,
Obtain stable metal lithium-lithium titanate battery.
(3) electrochemical property test of lithium metal-lithium titanate battery：
Constant current charge-discharge test, operating voltage are carried out under 2C multiplying powers by lithium titanate quality in pole piece on charging/discharging apparatus
Section is 1-2.5V.Lithium metal after processing charge and discharge electric polarization smaller under 2C multiplying powers as shown in Figure 2, polarization is more original to be reduced
30mV, cyclical stability is also more preferable, and capacity retention ratio is 98.5% after 30 circles.
Into battery it is to test the performance of the lithium anode of preparation using lithium titanate electrode assembling：Metatitanic acid lithium electrode follows
Ring performance is stablized, and therefore, the decay of circulation is led mainly due to the side reaction (such as formation of Li dendrite, dead lithium) of lithium metal side
Cause.Show as described in Figure 2, the decay of lithium metal-lithium titanate battery circulation of the lithium cathode sheet after processing is obviously reduced, cycle performance
It is better than untreated cathode of lithium battery.
Embodiment 2
Stable metal cathode of lithium reaction time difference is prepared, to stand 12h, remaining is same as Example 1.
Embodiment 3
(1) stable lithium anode is prepared：
Accurately weigh 0.1g PVDF to be substantially dissolved in 3.4g NMP, 0.1g conductive blacks are added after being mixed evenly and are mixed
Uniformly, add 0.8g fluorocarbons to be mixed evenly, be uniformly coated on after being stirred overnight in copper foil current collector, be punched into the pole of 18mm
Piece；Metal lithium sheet and fluorocarbons pole piece are sequentially placed into CR2016 type button cell shells after drying, adds proper amount of electrolysis
Liquid bis trifluoromethyl sulfonamide Asia lithium LiTFSI (glycol dimethyl ether (DME)/1,3-dioxolane (DOL)), tears open after standing 24h
Open spare.
(2) metal lithium-sulfur cell (Li-S) is assembled：
Metal lithium sheet, membrane and sulphur carbon electrode piece after handling are sequentially placed into CR2016 type button cell shells, it is suitable to add
The electrolyte LiTFSI (DME/DOL) of amount, compacting, obtains stable metal lithium-sulfur cell.
(3) electrochemical property test of metal lithium-sulfur cell：
Sulphur quality in pole piece is pressed on charging/discharging apparatus constant current charge-discharge test, operating voltage section are carried out with 200mA/g
For 1.5-2.7V.As shown in figure 3, the lithium metal charge and discharge electric polarization smaller after processing, when the lithium piece after processing is circulated, polarization
More original reduction 15mV, capacity retention ratio improves 5% after circulation 30 is enclosed.
Stable lithium anode is applied in lithium-sulfur cell by the present embodiment, it was demonstrated that can be applied not only to lithium-ion electric
Pond (such as lithium titanate battery), can also be applied in the new systems such as lithium-sulfur cell, have wider application surface.
In conclusion method of the present invention by building lithium fluoride protective layer in metallic lithium surface, carries out lithium metal pre-
Processing, has obtained the lithium anode with very cycle performance.This method is simply easily amplified, workable, is had very big
Industrial application value.Lithium anode after processing has very excellent cycle performance, under larger multiplying power discharge and recharge still protect
Higher capacity and cyclical stability are held, a kind of excellent performance, the lithium metal material higher than energy are provided for fast charge secondary cell
Material.
Although present disclosure is discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read the above, for the present invention's
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a kind of preparation method of lithium anode, it is characterised in that this method includes：
Step 1, positive plate slurry is prepared by positive active material of fluorocarbons, by the coating of positive plate slurry on a current collector, punching
Cutting is for fluorocarbons pole piece；
Step 2, button cell is assembled with metal lithium sheet, fluorocarbons pole piece and lithium ion electrical conductance solution, wherein, metal lithium sheet,
Fluorocarbons pole piece directly contacts；
Step 3, a period of time is stood, dismantles button cell, metal lithium sheet is taken out, after the metal lithium sheet is the processing of perfluorinated carbon
Metal lithium sheet, its surface have lithium metal protective layer.
2. the preparation method of lithium anode as claimed in claim 1, it is characterised in that the positive plate slurry also includes
Conductive agent, conductive agent selection conductive black.
3. the preparation method of lithium anode as claimed in claim 1, it is characterised in that described collector selection copper foil or
Aluminium foil.
4. the preparation method of lithium anode as claimed in claim 1, it is characterised in that in step 2, the lithium-ion electric
The property led solution is lithium-ion battery electrolytes.
5. the preparation method of lithium anode as claimed in claim 1, it is characterised in that in step 2, the lithium-ion electric
The property led solution selects 1.2 M LiPF6Solution, solvent are the mixed liquor of EC and EMC, wherein, EC:EMC= 3:7, with volume ratio
Meter.
6. the preparation method of lithium anode as claimed in claim 1, it is characterised in that in step 3, time of repose is
When 0.01-48 is small.
7. the preparation method of lithium anode as claimed in claim 6, it is characterised in that in step 3, time of repose is
When 0.01-24 is small.
8. lithium anode made from the preparation method in a kind of 1-7 according to claim described in any one, its its feature exists
In the surface of lithium anode has lithium metal protective layer.
9. a kind of lithium battery, it is characterised in that the lithium battery pack contains：Membrane, organic electrolyte, anode pole piece and according to right will
Seek lithium anode pole piece made from the preparation method in 1-7 described in any one.
10. lithium battery as claimed in claim 9, it is characterised in that the active material selection ferric phosphate of the anode pole piece
Any one in lithium, sulphur carbon material, lithium titanate material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109004211A (en) * | 2018-07-23 | 2018-12-14 | 西安交通大学 | A kind of zero strain liquid for power grid energy storage consolidates metal battery and production method |
| CN109037626A (en) * | 2018-07-20 | 2018-12-18 | 浙江大学 | A kind of alkali metal base cathode and its preparation method and application |
| CN109686922A (en) * | 2018-12-06 | 2019-04-26 | 上海空间电源研究所 | A kind of preparation method and application of sandwich structure long-service-life metal lithium battery |
| CN109950476A (en) * | 2019-04-18 | 2019-06-28 | 电子科技大学 | A kind of lithium anode material and its preparation method and application |
| CN110660969A (en) * | 2019-09-20 | 2020-01-07 | 清华大学深圳国际研究生院 | Metallic lithium cathode and preparation method thereof |
| CN110718692A (en) * | 2019-10-24 | 2020-01-21 | 湖南科技大学 | Fluoride stabilizing layer of lithium-sulfur battery, preparation method of fluoride stabilizing layer and lithium-sulfur battery |
| CN110957492A (en) * | 2018-09-26 | 2020-04-03 | 中国科学院宁波材料技术与工程研究所 | Lithium metal interface protection, preparation method thereof and battery containing lithium metal interface protection |
| WO2020125516A1 (en) * | 2018-12-17 | 2020-06-25 | 深圳先进技术研究院 | Lithium metal electrode, preparation method therefor and lithium battery |
| CN111403716A (en) * | 2020-03-27 | 2020-07-10 | 清华大学深圳国际研究生院 | Self-supporting lithium-sulfur battery positive plate, preparation method thereof and lithium-sulfur battery |
| CN114284475A (en) * | 2021-12-20 | 2022-04-05 | 中南大学 | Preparation method of composite lithium metal cathode with three-dimensional structure and product thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037626B (en) * | 2018-07-20 | 2020-08-11 | 浙江大学 | Alkali metal-based negative electrode and preparation method and application thereof |
| CN109037626A (en) * | 2018-07-20 | 2018-12-18 | 浙江大学 | A kind of alkali metal base cathode and its preparation method and application |
| CN109004211A (en) * | 2018-07-23 | 2018-12-14 | 西安交通大学 | A kind of zero strain liquid for power grid energy storage consolidates metal battery and production method |
| CN109004211B (en) * | 2018-07-23 | 2020-06-19 | 西安交通大学 | Zero-strain liquid-solid metal battery for power grid energy storage and manufacturing method |
| CN110957492A (en) * | 2018-09-26 | 2020-04-03 | 中国科学院宁波材料技术与工程研究所 | Lithium metal interface protection, preparation method thereof and battery containing lithium metal interface protection |
| CN109686922A (en) * | 2018-12-06 | 2019-04-26 | 上海空间电源研究所 | A kind of preparation method and application of sandwich structure long-service-life metal lithium battery |
| WO2020125516A1 (en) * | 2018-12-17 | 2020-06-25 | 深圳先进技术研究院 | Lithium metal electrode, preparation method therefor and lithium battery |
| CN109950476A (en) * | 2019-04-18 | 2019-06-28 | 电子科技大学 | A kind of lithium anode material and its preparation method and application |
| CN109950476B (en) * | 2019-04-18 | 2022-10-14 | 电子科技大学 | Metallic lithium negative electrode material and preparation method and application thereof |
| CN110660969A (en) * | 2019-09-20 | 2020-01-07 | 清华大学深圳国际研究生院 | Metallic lithium cathode and preparation method thereof |
| CN110718692A (en) * | 2019-10-24 | 2020-01-21 | 湖南科技大学 | Fluoride stabilizing layer of lithium-sulfur battery, preparation method of fluoride stabilizing layer and lithium-sulfur battery |
| CN110718692B (en) * | 2019-10-24 | 2023-12-19 | 湖南科技大学 | Fluoride stabilizing layer of lithium-sulfur battery, preparation method of fluoride stabilizing layer and lithium-sulfur battery |
| CN111403716A (en) * | 2020-03-27 | 2020-07-10 | 清华大学深圳国际研究生院 | Self-supporting lithium-sulfur battery positive plate, preparation method thereof and lithium-sulfur battery |
| CN111403716B (en) * | 2020-03-27 | 2022-07-08 | 清华大学深圳国际研究生院 | Self-supporting lithium-sulfur battery positive plate, preparation method thereof and lithium-sulfur battery |
| CN114284475A (en) * | 2021-12-20 | 2022-04-05 | 中南大学 | Preparation method of composite lithium metal cathode with three-dimensional structure and product thereof |
| CN114284475B (en) * | 2021-12-20 | 2024-01-30 | 中南大学 | Preparation method of three-dimensional structured composite lithium metal anode and product thereof |
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