CN110911683A - Lithium metal with rigid-elastic interface layer and preparation method and application thereof - Google Patents

Lithium metal with rigid-elastic interface layer and preparation method and application thereof Download PDF

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Publication number
CN110911683A
CN110911683A CN201911093493.7A CN201911093493A CN110911683A CN 110911683 A CN110911683 A CN 110911683A CN 201911093493 A CN201911093493 A CN 201911093493A CN 110911683 A CN110911683 A CN 110911683A
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lithium
lithium metal
rigid
interface layer
elastic interface
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晏成林
于淼
章琛
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Sichuan Chuangwei Zhishang Technology Co Ltd
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Sichuan Chuangwei Zhishang Technology Co Ltd
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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
    • 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
    • H01M10/058—Construction or manufacture
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides lithium metal with a rigid-elastic interface layer and a preparation method and application thereof, belonging to the field of lithium metal batteries. The invention enables lithium metal to simultaneously have a rigid-elastic interface layer by forming an inorganic-polymer structure through in-situ electrochemical deposition of diallyl disulfide (DADS) on the surface of the lithium metal. The polymer network improves the elasticity and toughness of the interface layer, and the formed inorganic unit can provide higher mechanical strength to resist the damage of lithium dendrite. Therefore, the interfacial layer can not only suppress the formation of lithium dendrites, but also allow the deposition/exfoliation behavior of lithium to proceed more rapidly and stably.

Description

Lithium metal with rigid-elastic interface layer and preparation method and application thereof
Technical Field
The invention belongs to the field of lithium metal batteries, and particularly relates to a lithium metal negative electrode with a rigid-elastic interface layer, and a preparation method and application thereof.
Background
Lithium metal has a large theoretical capacity (3860mAh g)-1) Low reduction potential (-3.04V/standard hydrogen electrode), heavyThe mass density is low (0.534g cm)-3) And the like, and becomes an irreplaceable negative electrode material of the next generation of rechargeable batteries. However, to put it into practice, two fundamental challenges also need to be addressed: (1) the high activity and irreversible reaction between lithium metal and the organic electrolyte can cause low coulombic efficiency and short cycle life of the battery; (2) the irregular lithium deposition/stripping behavior can cause the generation of lithium dendrites, although a Solid Electrolyte Interface (SEI) can be formed on the surface of the negative electrode in the first cycle process, the SEI is repeatedly broken and regenerated due to the unstable and fragile characteristics of the SEI, and the liquid electrolyte and lithium are continuously consumed; in addition, the lithium dendrites formed may penetrate the separator, forming short circuits, creating a serious fire and explosion safety hazard. The protection strategy commonly used at present is to cover a protective layer on the surface of lithium metal. However, most of lithium metals prepared by physical or chemical pretreatment have limited interfacial layer ionic conductivity and poor connection between an electrolyte and an electrode; in addition, conventional interfacial layers exhibit a single characteristic, either being too hard to cause the interfacial layer to be brittle, or too soft to inhibit dendrite growth, and thus cannot sustain a long-term stable cycle of the lithium metal battery.
The ideal interfacial protection layer for a lithium metal negative electrode should have the following basic characteristics: (1) chemically/electrochemically stable in an electrolyte; (2) the diffusion rate of lithium ions is fast, and the fast and uniform deposition of the lithium ions is ensured; (3) the mechanical strength is high, and the growth of lithium dendrites can be inhibited; (4) has good compatibility with electrolyte and electrode. Therefore, the novel lithium metal negative electrode protective layer has enough mechanical properties and is beneficial to the rapid progress of lithium deposition/stripping behavior, and has important significance.
Disclosure of Invention
Aiming at the problem that the conventional lithium metal negative electrode protective layer in the background technology cannot simultaneously have good mechanical property and good electrochemical property, the invention aims to provide a lithium metal negative electrode with a rigid-elastic interface layer, and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method of making lithium metal with a rigid-elastic interfacial layer comprising the steps of:
step 1, mixing lithium salt, an organic solvent and diallyl disulfide to prepare a solution A, wherein the content of the diallyl disulfide in the electrolyte is 5-20 wt%;
step 2, assembling to form a lithium symmetrical battery by taking metal lithium as an electrode and the solution A in the step 1 as electrolyte;
and 3, performing charging deposition on the lithium symmetrical battery obtained in the step 2, disassembling the battery after the deposition is finished, taking out a lithium electrode, and repeatedly washing by using 1, 3-dioxolane to obtain the lithium metal with the rigid-elastic interface layer.
Further, the lithium salt in step 1 is lithium bis (trifluoromethanesulfonate) imide (LiTFSI), lithium bis (fluorosulfonyl) imide (Li FSI), lithium difluoro oxalato borate (liddob), lithium bis (oxalato) borate (LiBOB) and lithium hexafluorophosphate (LiPF)6) One of the like; the organic solvent is one or more of 1, 3-Dioxolane (DOL), ethylene glycol dimethyl ether (DME), tetraethylene glycol dimethyl ether (TETRAGLYME), triethylene glycol dimethyl ether (TRIGLYME), methyl ethyl carbonate (EMC), diethyl carbonate (DEC), dimethyl carbonate (DMC) and Ethylene Carbonate (EC).
Further, the content of the diallyl disulfide in the solution A in the step 1 is preferably 5 wt%, 10 wt% or 20 wt%.
Further, the concentration of the lithium salt in the solution A in the step 1 is 1 mol/L.
Further, the content of the electrolyte in the step 2 is 10-50 mu L.
Further, the current density of the charging deposition in the step 3 is 0.1-2 mA cm-2The deposition time is 5-15 h.
The lithium metal with the rigid-elastic interface layer is characterized by comprising a lithium metal substrate and the rigid-elastic interface layer formed on the surface of the lithium metal substrate, wherein the thickness of the rigid-elastic interface layer is 20-80 mu m.
Further, the rigid-elastic interface layer is formed by polymerizing diallyl disulfide (DADS) by an in-situ electrochemical method.
The method for preparing the lithium metal battery based on the lithium metal with the rigid-elastic interface layer comprises the following specific steps: LiFePO using lithium metal with a rigid-elastic interface layer as the negative electrode4(LFP)、LiNi0.8Co0.1Mn0.1O2Either (NCM) or C/S composite material is used as a positive electrode, and a lithium metal battery is assembled together with an electrolyte.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the lithium metal with the rigid-elastic interface layer is an inorganic-polymer structure formed by in-situ electrochemical deposition of DADS on the surface of the lithium metal, wherein the polymer network improves the elasticity and toughness of the lithium metal and can adapt to the volume change of the lithium metal in the charging/charging process, and the formed inorganic unit provides higher mechanical strength to inhibit lithium dendrites, and the interface layer enables the deposition/stripping behavior of the lithium to be carried out more quickly and stably.
2. The invention can realize the preparation of different rigid-elastic interface layers by adjusting the DADS content, the current density and the deposition time in the preparation method, namely a defective rigid-elastic interface layer (DIL-Li), an optimized rigid-elastic interface layer (HEIL-Li) and a compact rigid-elastic interface layer (ODIL-Li), wherein the HEIL-Li layer is required by the invention.
Drawings
FIG. 1 is an IR spectrum of a rigid-elastic interfacial layer of lithium metal prepared in example 5.
FIG. 2 is a two-dimensional plot of an in-situ Raman spectrum of an electrochemically deposited rigid-elastic interfacial layer of example 5.
Fig. 3 is an SEM image before and after 100 cycles of a lithium symmetrical battery assembled from HEIL-Li provided in example 5 and normal lithium metal (bare Li) provided in a comparative example.
Fig. 4 is an Electrochemical Impedance Spectrum (EIS) of a lithium symmetric battery assembled based on lithium metal before and after 100 cycles;
wherein (A) is HEIL-Li provided in example 5, and (B) is bare Li provided in a comparative example.
FIG. 5 shows the HEIL-Li provided by example 5 and the bare Li provided by a comparative example, respectively, with LiFePO4Electrochemical performance of the positive assembled full cell.
FIG. 6 is HEIL-Li provided by example 5 and bare Li provided by a comparative example, respectively with LiNi0.8Co0.1Mn0.1O2Electrochemical performance of the assembled full cell.
Fig. 7 is an electrochemical performance of a full cell assembled with the HEIL-Li provided in example 5 and the bare Li provided in comparative example, respectively, with a C/S composite.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
The lithium metal with the rigid-elastic interface layer comprises a lithium metal matrix and the rigid-elastic interface layer formed on the surface of the lithium metal matrix, wherein the rigid-elastic interface layer is formed by electrochemically depositing DADS on the lithium surface through an in-situ electrochemical method to form polyolefin and inorganic lithium sulfide. Wherein the polymer network of the polyolefin improves the elasticity and toughness of the lithium metal, and the formed inorganic units provide higher mechanical strength to inhibit dendritic growth; the elastic properties are derived from the double bond polymerization of DADS to form polyolefins, and the rigid properties are due to the electrochemical polymerization process which also produces organosulfur lithium and inorganic lithium sulfide components.
The polymerization of DADS in the invention needs to be carried out under a constant potential, and can be stably polymerized on the surface of lithium only in a lithium symmetrical battery, if the battery is directly assembled, the battery voltage is constantly changed in the charging and discharging process of the battery, and the stable polymerization of DADS can not be satisfied; secondly, the electrolyte used in the polymerization process is a solution containing DADS, and if the battery is directly assembled for battery cycle test, the unreacted DADS can cause the battery cycle to be unstable; in addition, the method of the present invention provides a universal method for preparing stable lithium metal, and the lithium metal prepared by the method can be used for negative electrodes of various lithium metal batteries without being limited to a specific electrolyte system.
Example 1
A method of making lithium metal with a rigid-elastic interfacial layer comprising the steps of:
step 1, mixing LiTFSI and DOL/DME with a volume ratio of 1:1 to enable the concentration of LiTFSI to be 1mol/L, and then adding 10mg of DADS into 190mg of mixed solution to prepare solution A;
step 2, putting common lithium metal, a diaphragm, the common lithium metal, a gasket, an elastic sheet and a negative electrode shell on a positive electrode shell of the button cell in sequence, adding 30 mu L of the solution A obtained in the step 1 as electrolyte into the cell, and assembling the button cell into a glove box to form a symmetrical button cell;
step 3, the button cell obtained in the step 2 is at 1mAcm-2And charging for 5 hours under current for deposition, disassembling the battery after the deposition is finished, taking out the lithium electrode, and repeatedly washing by using DOL (lithium ion implantation) to obtain the lithium metal with the rigid-elastic interface layer.
Example 2
Lithium metal having a rigid-elastic interfacial layer was prepared according to the preparation method of example 1, and only the deposition time in step 3 was adjusted to 10 hours, and the other steps were not changed.
Example 3
Lithium metal having a rigid-elastic interface layer was prepared according to the preparation method of example 1, and only the deposition time in step 3 was adjusted to 15h, while the other steps were unchanged.
Example 4
Lithium metal having a rigid-elastic interface layer was prepared according to the preparation method of example 1, and only the amount of DADS added in step 1 was adjusted to 20mg, while the other steps were not changed.
Example 5
Lithium metal having a rigid-elastic interface layer was prepared according to the preparation method of example 4, and the deposition time in step 3 was adjusted to 10h, while the other steps were unchanged.
The material prepared in this example had a rigid-elastic interfaceThe lithium metal of the layer is used as a negative electrode, and LiFePO is adopted as a positive electrode4、LiNi0.8Co0.1Mn0.1O2Or the C/S composite, were assembled into button cells in a glove box and subjected to electrochemical cycling tests, comparative results are shown in fig. 5, 6 and 7.
Example 6
Lithium metal having a rigid-elastic interface layer was prepared according to the preparation method of example 4, and the deposition time in step 3 was adjusted to 15h, while the other steps were unchanged.
Example 7
Lithium metal having a rigid-elastic interface layer was prepared according to the preparation method of example 1, and only the amount of DADS added in step 1 was adjusted to 20mg, the amount of the mixed solution was adjusted to 160mg, and the other steps were not changed.
Example 8
Lithium metal having a rigid-elastic interfacial layer was prepared according to the preparation method of example 7, and the deposition time in step 3 was adjusted to 10 hours, while the other steps were unchanged.
Example 9
Lithium metal having a rigid-elastic interfacial layer was prepared according to the preparation method of example 7, and the deposition time in step 3 was adjusted to 15h, while the other steps were unchanged.
Comparative example
Lithium metal with a rigid-elastic interface layer was prepared according to the preparation method of example 1, only D ADS in step 1 was removed and the other steps were not changed, and lithium metal was prepared.
The lithium metal with the rigid-elastic interface layer prepared by the comparative example is used as a negative electrode, and LiFePO is adopted as a positive electrode4、LiNi0.8Co0.1Mn0.1O2Or the C/S composite, were assembled into button cells in a glove box and subjected to electrochemical cycling tests, comparative results are shown in fig. 5, 6 and 7.
Figure 1 shows the fourier transform infrared spectroscopy (FT-IR) of the DADS and rigid-elastic interface layer. 3085cm-1Vibration of point and 990cm-1And 910cm-1The planar bending vibration at (a) corresponds to the C-H group. 1635cm-1Characteristic ofThe peak is caused by stretching vibration of C ═ C due to allyl groups. For the rigid-elastomeric interfacial layer, all these characteristic peaks were not detectable, indicating double bond polymerization of the allyl groups.
FIG. 2 is a two-dimensional intensity plot of an in situ Raman spectrum during polymerization, clearly showing the variation in peak intensity. 320-460 cm-1The decrease in intensity of the range indicates a gradual decrease in DADS, indicating continued depletion of DADS to form polyolefin and organosulfur lithium.
FIG. 3 shows the surface morphology of bare Li and HEIL-Li before and after 100 cycles. The surface of the common lithium metal becomes rough and is full of dendrites after circulation. Lithium metal with a rigid-elastic interfacial layer has a flat surface, indicating that the interfacial layer is very stable during lithium deposition/stripping.
FIG. 4 shows the impedance spectra before and after cycling 100 cycles of bare Li and HEIL-Li in a symmetric cell. After 100 cycles, the impedance of the common lithium symmetrical battery is obviously increased, and the impedance of the lithium metal with the rigid-elastic interface layer is almost unchanged after the cycle, which shows that the optimized rigid-elastic interface layer is highly stable.
Fig. 5, fig. 6 and fig. 7 show the cycle performance of the full cell assembled by the HEIL-Li provided in example 5 and the normal lithium metal provided in the comparative example with the LF P, NCM and S positive electrodes, respectively, and all show that the lithium metal with the rigid-elastic interfacial layer obtained based on the present invention has a significant effect on improving the electrochemical performance of the lithium metal cell.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.

Claims (7)

1. A method of making lithium metal having a rigid-elastic interfacial layer, comprising the steps of:
step 1, mixing lithium salt, an organic solvent and diallyl disulfide to prepare a solution A, wherein the content of the diallyl disulfide in the solution A is 5-20 wt%;
step 2, assembling to form a lithium symmetrical battery by taking metal lithium as an electrode and the solution A in the step 1 as electrolyte;
and 3, performing charging deposition on the lithium symmetrical battery obtained in the step 2, disassembling the battery after the deposition is finished, taking out a lithium electrode, and repeatedly washing by using 1, 3-dioxolane to obtain the lithium metal with the rigid-elastic interface layer.
2. The method of claim 1, wherein the lithium salt in step 1 is one of lithium bis (trifluoromethanesulfonate) imide, lithium bis (fluorosulfonyl) imide, lithium difluoro-oxalato-borate, lithium bis-oxalato-borate, and lithium hexafluorophosphate; the organic solvent is one or more of 1, 3-dioxolane, ethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, triethylene glycol dimethyl ether, methyl ethyl carbonate, diethyl carbonate, dimethyl carbonate and ethylene carbonate.
3. The method of claim 1, wherein the diallyl disulfide is present in solution a in an amount of 5 wt%, 10 wt% or 20 wt% in step 1.
4. The method according to claim 1, wherein the electrolyte in step 2 is 10 to 50 μ L.
5. The method according to claim 1, wherein the current density of the charge deposition in step 3 is 0.1-2 mA cm-2The deposition time is 5-15 h.
6. A lithium metal with a rigid-elastic interface layer prepared by the method of any one of claims 1 to 5, wherein the lithium metal comprises a lithium metal matrix and the rigid-elastic interface layer is formed on the surface of the lithium metal matrix, and the thickness of the rigid-elastic interface layer is 20 to 80 μm.
7. A method for preparing a lithium metal battery based on the lithium metal with the rigid-elastic interface layer as claimed in claim 6, is characterized by comprising the following specific steps: LiFePO using lithium metal with a rigid-elastic interface layer as the negative electrode4、LiNi0.8Co0.1Mn0.1O2Or any one of the C/S composite materials is used as a positive electrode and is assembled with an electrolyte to obtain the lithium metal battery.
CN201911093493.7A 2019-11-11 2019-11-11 Lithium metal with rigid-elastic interface layer and preparation method and application thereof Pending CN110911683A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112786841A (en) * 2021-01-28 2021-05-11 宁波大学 Modification method of lithium metal surface and lithium metal battery
CN113707847A (en) * 2021-06-22 2021-11-26 浙江工业大学 Method for protecting lithium metal by electrochemical carbon deposition and application thereof

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JP2016189269A (en) * 2015-03-30 2016-11-04 日本電気株式会社 Estimation method for lithium ion secondary battery
US20190051905A1 (en) * 2017-08-14 2019-02-14 Nanotek Instruments, Inc. Anode-Protecting Layer for a Lithium Metal Secondary Battery and Manufacturing Method
CN109449486A (en) * 2018-10-15 2019-03-08 苏州大学 A kind of application of electrolysis additive
CN109585786A (en) * 2018-12-04 2019-04-05 安徽盟维新能源科技有限公司 A kind of guard method and its application of lithium an- ode
US20190190004A1 (en) * 2017-12-18 2019-06-20 The Hong Kong Polytechnic University Electrodes for batteries
CN110190243A (en) * 2019-05-29 2019-08-30 华中科技大学 A kind of preparation and application of the lithium an- ode with composite membrane

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CA1101443A (en) * 1977-11-08 1981-05-19 Hans-Gerhard Creutz Composition for electrodeposition of metal deposits, its method of preparation and uses thereof
JP2016189269A (en) * 2015-03-30 2016-11-04 日本電気株式会社 Estimation method for lithium ion secondary battery
US20190051905A1 (en) * 2017-08-14 2019-02-14 Nanotek Instruments, Inc. Anode-Protecting Layer for a Lithium Metal Secondary Battery and Manufacturing Method
US20190190004A1 (en) * 2017-12-18 2019-06-20 The Hong Kong Polytechnic University Electrodes for batteries
CN109449486A (en) * 2018-10-15 2019-03-08 苏州大学 A kind of application of electrolysis additive
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112786841A (en) * 2021-01-28 2021-05-11 宁波大学 Modification method of lithium metal surface and lithium metal battery
CN113707847A (en) * 2021-06-22 2021-11-26 浙江工业大学 Method for protecting lithium metal by electrochemical carbon deposition and application thereof
CN113707847B (en) * 2021-06-22 2022-10-04 浙江工业大学 Method for protecting lithium metal by electrochemical carbon deposition and application thereof

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