CN112928279A - Three-dimensional lithium battery current collector and preparation method and application thereof - Google Patents
Three-dimensional lithium battery current collector and preparation method and application thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
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- H01M4/667—Composites in the form of layers, e.g. coatings
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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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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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Abstract
The invention discloses a three-dimensional lithium battery current collector and a preparation method and application thereof. The adopted flexible self-supporting three-dimensional layered Mxene membrane has a three-dimensional layered structure which can provide more nucleation sites and provide an effective and better buffer layer, and the substance has high conductivity, good hydrophilicity and better mechanical flexibility. In addition, the MXene membrane is prepared without any conductive agent or additive, and is assembled into a self-supporting, hydrophilic, flexible and conductive membrane through simple suction filtration to form an integrated three-dimensional flexible electrode, so that the preparation cost of the electrode is greatly saved.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metal composite material preparation and lithium metal batteries, relates to a three-dimensional lithium battery current collector and a preparation method and application thereof, and particularly relates to a preparation method and application of an MXene/gold composite current collector for a high-safety lithium metal battery system without dendrites.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the increasing demand of electric vehicles, large-scale energy storage, light electric vehicles and the like, and the decreasing of global non-renewable resources, the development of secondary energy storage chargeable and dischargeable batteries with high performance and large capacity is urgent based on the urgent demand of current green, efficient and practical energy storage materials. The lithium ion battery which is charged and discharged is the energy storage system which is most widely researched and has the market application value at present. It has a series of advantages of high energy density, high safety factor, light weight, etc., but still cannot meet the demand of people for higher energy density, so researchers have started to shift the research focus to lithium metal secondary batteries.
The lithium metal negative electrode has 3860mAhg-1The theoretical capacity and the low potential (-3.04vs standard hydrogen electrode) are the most ideal negative electrode material of the high-energy density battery. However, uncontrolled lithium dendrite growth, infinite volume expansion, high reactivity, and formation of an unstable SEI film degrade the coulombic efficiency and cycle life of the lithium metal battery.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a three-dimensional lithium battery current collector and a preparation method and application thereof.
To solve the above technical problem, one or more of the following embodiments of the present invention provide the following technical solutions:
in a first aspect, the invention provides a three-dimensional layered MXene @ Au composite film, which comprises a flexible self-supporting three-dimensional layered MXene film and a nanogold particle layer loaded on the flexible self-supporting three-dimensional layered MXene film.
In a second aspect, the invention provides a preparation method of the three-dimensional layered MXene @ Au composite film, which comprises the steps of preparing the three-dimensional layered MXene film and then sputtering gold nanoparticles on the three-dimensional layered MXene film.
In a third aspect, the invention provides a lithium metal negative electrode current collector, which comprises the three-dimensional layered MXene @ Au composite film.
In a fourth aspect, the present invention provides a lithium metal battery negative electrode comprising a lithium metal battery negative electrode current collector and metallic lithium supported on the lithium metal battery negative electrode current collector.
In a fifth aspect, the present invention provides a lithium metal battery, wherein the negative electrode is the negative electrode of the lithium metal battery.
Compared with the prior art, one or more technical schemes of the invention have the following beneficial effects:
(1) the flexible self-supporting three-dimensional layered Mxene (a metal carbide and metal nitride material with a two-dimensional layered structure, good mechanical flexibility, high specific surface area, stable chemistry, high conductivity and unique photoelectric property) film adopted by the invention has a three-dimensional layered structure which can provide more nucleation sites and an effective and good buffer layer, and the substance has high conductivity, good hydrophilicity and good mechanical flexibility. In addition, the MXene membrane is prepared without any conductive agent or additive, and is assembled into a self-supporting, hydrophilic, flexible and conductive membrane through simple suction filtration to form an integrated three-dimensional flexible electrode, so that the preparation cost of the electrode is greatly saved.
(2) The invention adopts an ion sputtering vapor deposition method to load gold particles on MXene to be used as a current collector of a lithium metal cathode, the operation is simple, the nano gold particles can be alloyed with metal lithium, the gold has excellent lithium affinity, the nucleation barrier can be effectively reduced, the deposition uniformity is improved, the internal lithium ion transmission rate is improved, the battery safety problem caused by the penetration of lithium dendrites on a diaphragm is relieved, and the composite material has a better effect of inhibiting the growth of the lithium dendrites.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a microscopic morphology of an ion-sputter-deposited gold particle to a three-dimensional layered MXene film prepared in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a copper foil according to a comparative example of the present invention on which lithium of 4mAh/cm2 was deposited;
FIG. 3 is a scanning electron microscope image of an MXene film prepared in example 1 according to the present invention, deposited with 4mAh/cm2 lithium onto an MXene @ Au composite film;
fig. 4 is an electrochemical performance diagram of the MXene @ Au composite film prepared in example 1 of the present invention used as a current collector of a lithium metal negative electrode.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In a first aspect, the invention provides a three-dimensional layered MXene @ Au composite film, which comprises a flexible self-supporting three-dimensional layered MXene film and a nanogold particle layer loaded on the flexible self-supporting three-dimensional layered MXene film.
In some embodiments, the gold nanoparticles have a particle size of 2 to 8 nm.
Furthermore, the thickness of the nano gold particle layer is 9-35 nm.
In a second aspect, the invention provides a preparation method of the three-dimensional layered MXene @ Au composite film, which comprises the steps of preparing the three-dimensional layered MXene film and then sputtering gold nanoparticles on the three-dimensional layered MXene film.
In some embodiments, a method of making a three-dimensional layered MXene film comprises the steps of: preparing MXene colloidal solution, and preparing a three-dimensional layered Mxene film by carrying out suction filtration and drying on the MXene colloidal solution; and then ion sputtering a nano gold particle layer on the three-dimensional layered Mxene film.
Further, the preparation method of the MXene colloidal solution comprises the following steps: the MAX phase powder is mixed with acid and fluoride and stirred, water is added, and centrifugation is carried out to form a peeled MXene body solution with few layers or a single layer.
Still further, the powder of the MAX phase is selected from Ti3AlC2、Nb4AlC3、Ti3SiC2、Ta4SiC3、Nb4SiC3、Ti2AlC、Ta4AlC3、TiNbAlC、(V0.5Cr0.5)3A1C2、Mo3A1C2、V2A1C、Nb2AlC、Ti3AlCN、Ti2SiC、TiNbSiC、(V0.5Cr0.5)3SiC2、V2SiC、Nb2SiC or Ti3One or a mixture of more of SiCN.
Still further, the acid is one or more of hydrochloric acid, acetic acid, gluconic acid, citric acid, oxalic acid, carbonic acid or sulfuric acid.
Still further, the fluoride is one or more of lithium fluoride, sodium fluoride, potassium fluoride, zinc fluoride, aluminum fluoride or calcium fluoride.
Still further, the mass ratio of the MAX phase powder to the fluoride is 1: 1-5.
Still further, the rotating speed of the centrifugation is 3000-4000 r/min, preferably 3500 r/min.
Further, the drying temperature of the MXene colloidal solution after suction filtration is 50-70 ℃, preferably 60 ℃.
In some embodiments, the deposition current for ion sputtering a layer of nanogold particles on a three-dimensional layered Mxene film is 2-4mA, preferably 2 mA.
Further, the time of ion sputtering is 30-300 s.
In a third aspect, the invention provides a lithium metal negative electrode current collector, which comprises the three-dimensional layered MXene @ Au composite film.
In a fourth aspect, the present invention provides a lithium metal battery negative electrode comprising a lithium metal battery negative electrode current collector and metallic lithium supported on the lithium metal battery negative electrode current collector.
In a fifth aspect, the present invention provides a lithium metal battery, wherein the negative electrode is the negative electrode of the lithium metal battery.
Experiments prove that after the three-dimensional layered MXene @ Au composite film prepared by the method is used as a lithium metal negative electrode current collector to load lithium, the growth of metal lithium dendrites can be effectively inhibited. And the material composite is prepared into a flexible self-supporting film with better mechanical flexibility.
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited thereto in any way.
Example 1
Take 0.5g Ti3AlC2And stirring the powder in a mixed solution of 10ml of 6M hydrochloric acid and 0.5g of lithium fluoride, adding water, centrifuging (3500r/min), washing to remove redundant acid and fluoride, ultrasonically stripping, separating to obtain a small-layer MXene colloidal solution, filtering, and drying in a vacuum oven at 60 ℃ overnight to obtain the flexible self-supporting three-dimensional layered MXene film.
And depositing the nano gold particles on the three-dimensional layered MXene film by vapor deposition for 3min in an ion sputtering instrument at a current of 2mA to obtain the flexible self-supporting three-dimensional layered MXene @ Au composite film.
And finally, assembling the battery in a glove box, cutting the flexible self-supporting three-dimensional layered MXene @ Au film current collector into a wafer with the diameter of 1cm, and pre-depositing metal lithium on the composite film to obtain the replaceable lithium metal cathode. Then, a lithium wafer with a diameter of 1cm was used as a reference electrode, and a 2032 type button cell was assembled under an argon atmosphere using 1M LiTFSI in1,3-dioxolane/1,2-dimethoxyethane (DOL/DME,1:1byvolume) with 2 wt% LiNO3 as an electrolyte.
Example 2
Take 0.5gV2And stirring AlC powder in a mixed solution of 10ml of 6M hydrochloric acid and 0.5g of lithium fluoride, adding water, centrifugally washing to remove redundant acid and fluoride, ultrasonically stripping, separating to obtain a small-layer MXene colloidal solution, filtering, and drying in a vacuum oven at 60 ℃ overnight to obtain the flexible self-supporting three-dimensional layered MXene film.
And (3) depositing gold nanoparticles on the three-dimensional layered MXene film by vapor deposition for 4min in an ion sputtering instrument at a current of 5mA to obtain the flexible self-supporting three-dimensional layered MXene @ Au composite film.
And finally, assembling the battery in a glove box, cutting the flexible self-supporting three-dimensional layered MXene @ Au film current collector into a wafer with the diameter of 1cm, and pre-depositing metal lithium on the composite film to obtain the replaceable lithium metal cathode. Then, a lithium wafer with a diameter of 1cm was used as a reference electrode, and a 2032 type button cell was assembled under an argon atmosphere using 1M LiTFSI in1,3-dioxolane/1,2-dimethoxyethane (DOL/DME,1:1byvolume) with 2 wt% LiNO3 as an electrolyte.
Example 3
Take 0.5gV2And stirring AlC powder in a mixed solution of 10ml of 6M hydrochloric acid and 0.5g of lithium fluoride, adding water, centrifugally washing to remove redundant acid and fluoride, ultrasonically stripping, separating to obtain a few-layer MXene colloidal solution, filtering, and drying in a vacuum oven at 60 ℃ to obtain the flexible self-supporting three-dimensional layered MXene film.
And depositing the nano gold particles on the three-dimensional layered MXene film by vapor deposition for 2min in an ion sputtering instrument at a current of 5mA to obtain the flexible self-supporting three-dimensional layered MXene @ Au composite film.
And finally, assembling the battery in a glove box, cutting the flexible self-supporting three-dimensional layered MXene @ Au film current collector into a wafer with the diameter of 1cm, and pre-depositing metal lithium on the composite film to obtain the replaceable lithium metal cathode. Then, a lithium wafer with a diameter of 1cm was used as a reference electrode, and a 2032 type button cell was assembled under an argon atmosphere using 1M LiTFSI in1,3-dioxolane/1,2-dimethoxyethane (DOL/DME,1:1byvolume) with 2 wt% LiNO3 as an electrolyte.
Comparative example:
the cell was assembled in a glove box, a commercial copper foil was cut into a wafer having a diameter of 1cm, and metallic lithium was pre-deposited on the commercial copper foil to obtain a replaceable lithium metal negative electrode. Then, a lithium wafer having a diameter of 1cm was used as a reference electrode, and 1M LiTFSI 1,3-dioxolane/1,2-dimethoxyethane (DOL/DME,1:1byvolume) with 2 wt% LiNO was used3As electrolyte, under argon atmosphere2032 type button cell.
Performance testing
(1) Characterization of the microstructure of the MXene @ Au composite current collector:
the microscopic morphology of the prepared MXene @ Au composite current collector is observed by a scanning electron microscope, and as can be seen in FIG. 1, the nano-gold particles deposited on the MXene thin film through ion sputtering are uniformly distributed, and the MXene thin film still keeps a complete flexible film structure.
(2) And (3) characterizing the lithium deposition morphology:
the batteries prepared in example 1 and comparative example methods were used to deposit 4mA/cm2 of lithium onto a current collector at a current density of 0.5mA/cm 2. And then disassembling the battery under the argon atmosphere to obtain a deposited lithium sheet, and observing the growth morphology of lithium on the lithium sheet by using a scanning electron microscope. The results are shown in FIG. 2 (comparative example) and FIG. 3 (example 1). As can be seen in fig. 2, lithium deposited on commercial copper foil produces dendritic lithium dendrites. As can be seen in fig. 3, the lithium deposited on the MXene @ Au composite current collector is morphologically flat with no dendrite generation. The results show that the MXene @ Au composite current collector can inhibit the generation of lithium dendrites and induce uniform lithium deposition, which is beneficial to improving the coulombic efficiency of the battery, prolonging the cycle life of the battery and reducing the occurrence of the safety problem of lithium dendrite induction.
(3) The button cell prepared in example 1 was used as an example, and the coulombic efficiency of the cell was evaluated using a charge and discharge device (novacar CT-4008). The results are shown in FIG. 4. The initial charge and discharge cycle needs to form an SEI film initially, so the coulombic efficiency is not high, and the coulombic efficiency after 100 cycles is more than 95%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A three-dimensional layered MXene @ Au composite film is characterized in that: the self-supporting three-dimensional layered MXene film comprises a flexible self-supporting three-dimensional layered MXene film and a nanogold particle layer loaded on the flexible self-supporting three-dimensional layered MXene film.
2. The three-dimensional layered MXene @ Au composite film according to claim 1, wherein: the particle size of the nano gold particles is 2-8 nm;
furthermore, the thickness of the nano gold particle layer is 9-35 nm.
3. The method for preparing the three-dimensional layered MXene @ Au composite film according to any one of claims 1 and 2, wherein: the method comprises the steps of preparing a three-dimensional layered MXene film and then sputtering nano-gold particles on the three-dimensional layered MXene film.
4. The method for preparing the three-dimensional layered MXene @ Au composite film according to claim 3, wherein: the preparation method of the three-dimensional layered MXene film comprises the following steps: preparing MXene colloidal solution, and preparing a three-dimensional layered Mxene film by carrying out suction filtration and drying on the MXene colloidal solution; and then ion sputtering a nano gold particle layer on the three-dimensional layered Mxene film.
5. The method for preparing the three-dimensional layered MXene @ Au composite film according to claim 4, wherein: the preparation method of the MXene colloidal solution comprises the following steps: mixing and stirring MAX phase powder with acid and fluoride, adding water, and centrifuging to form a stripped MXene solution with few layers or a single layer;
still further, the powder of the MAX phase is selected from Ti3AlC2、Nb4AlC3、Ti3SiC2、Ta4SiC3、Nb4SiC3、Ti2AlC、Ta4AlC3、TiNbAlC、(V0.5Cr0.5)3A1C2、Mo3A1C2、V2A1C、Nb2AlC、Ti3AlCN、Ti2SiC、TiNbSiC、(V0.5Cr0.5)3SiC2、V2SiC、Nb2SiC or Ti3One or a mixture of more of SiCN;
still further, the acid is one or a mixture of hydrochloric acid, acetic acid, gluconic acid, citric acid, oxalic acid, carbonic acid or sulfuric acid;
still further, the fluoride is one or a mixture of more of lithium fluoride, sodium fluoride, potassium fluoride, zinc fluoride, aluminum fluoride or calcium fluoride;
further, the mass ratio of MAX phase powder to fluoride is 1: 1-5;
still further, the rotating speed of the centrifugation is 3000-4000 r/min, preferably 3500 r/min.
6. The method for preparing the three-dimensional layered MXene @ Au composite film according to claim 3, wherein: the drying temperature of the MXene colloidal solution after suction filtration is 50-70 ℃, and preferably 60 ℃.
7. The method for preparing the three-dimensional layered MXene @ Au composite film according to claim 3, wherein: the deposition current of ion sputtering the nano gold particle layer on the three-dimensional layered Mxene film is 2-4mA, preferably 2 mA;
further, the time of ion sputtering is 30-300 s.
8. A lithium metal negative current collector characterized by: comprising the three-dimensional layered MXene @ Au composite film according to claim 1 or 2.
9. A lithium metal battery negative electrode, characterized by: comprising the lithium metal battery negative electrode current collector of claim 8 and metallic lithium supported on the lithium metal battery negative electrode current collector.
10. A lithium metal battery, characterized in that: the negative electrode of the lithium metal battery according to claim 9.
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