CN113346045A - Lithium metal anode modified by composite SEI layer and preparation method thereof - Google Patents
Lithium metal anode modified by composite SEI layer and preparation method thereof Download PDFInfo
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- CN113346045A CN113346045A CN202110590380.9A CN202110590380A CN113346045A CN 113346045 A CN113346045 A CN 113346045A CN 202110590380 A CN202110590380 A CN 202110590380A CN 113346045 A CN113346045 A CN 113346045A
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 6
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 239000011246 composite particle Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- ODNBVEIAQAZNNM-UHFFFAOYSA-N 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)ethanone Chemical compound C1=CC(Cl)=NN2C(C(=O)C)=CN=C21 ODNBVEIAQAZNNM-UHFFFAOYSA-N 0.000 claims abstract description 4
- GUNJVIDCYZYFGV-UHFFFAOYSA-K Antimony trifluoride Inorganic materials F[Sb](F)F GUNJVIDCYZYFGV-UHFFFAOYSA-K 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 29
- 238000007747 plating Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 4
- 229910012862 Li3Sb Inorganic materials 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002641 lithium Chemical class 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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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- 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
- H01M4/139—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
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- 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
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a lithium metal anode modified by a composite SEI layer and a preparation method thereof3Composite SEI layer composed of Sb/LiF composite particles, Li3The size of the Sb/LiF composite particles is 400-600 nm, and Li3The mass ratio of Sb to LiF is 3: 7; the preparation method is that antimony trifluoride is added into dimethyl ether to obtain Sb3+Sb with a concentration of 1 to 50mmol/L3+Precursor solution, soaking the polished Li metal in Sb3+And cleaning and drying the precursor solution for 180-360 seconds to obtain the nano-silver/nano-silver composite material. In Li3Under the synergistic effect of Sb and LiF, Li in the composite SEI layer is accelerated+Transport kinetics of and in the composite SEI layer and lithiumThe uniform Li deposition occurs on the interface of the metal, the interface mechanical strength is high, the lithium metal anode can be effectively stabilized, and the growth of dendritic crystals is prevented.
Description
Technical Field
The invention relates to the field of lithium metal batteries, in particular to a lithium metal anode modified by a composite SEI layer and a preparation method thereof.
Background
Since the lithium (Li) anode has a high theoretical specific capacity (3860mAh g)-1) And the lowest electrode potential (-3.04V, relative to the standard hydrogen electrode), therefore, the lithium metal battery is considered to be one of the next generation new energy storage devices with great development and application prospects. However, when the Li anode contacts a liquid organic electrolyte, it spontaneously reacts with organic and inorganic components to form a Solid Electrolyte Interphase (SEI) layer on the surface thereof. Such naturally formed SEI layers have fast Li+The local tips of conduction, resulting in uneven Li deposition, form Li dendrites that can crack the brittle SEI layer produced during cycling. Therefore, fresh Li anode surfaces will be exposed to the electrolyte again and cause more side reactions. More importantly, at high current densities, Li+The transport kinetics in the SEI layer are severely limited, leading to more pronounced Li dendrite problems.
Lithium fluoride (LiF) is the main component in the SEI layer, has low electronic conductivity and high chemical stability, and is a good passivation layer of the Li anode surface. However, the ionic conductivity of the LiF component is poor: (<10-9S cm-1) Much lower than other inorganic components in the SEI layer (e.g. Li)2O、Li2CO3) The ionic conductivity of (a). High Li of LiF+Diffusion energy barrier leading to Li+Is limited (especially at high current densities) and results in unstable Li plating/stripping performance. Thus, constructing a more stable LiF-rich SEI layer for Li enhancement+Diffusion kinetics in the SEI layer are crucial to achieve stable Li plating/stripping.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides a lithium metal modified by a composite SEI layerThe anode and the preparation method thereof, and the lithium metal anode is directly applied to the Li metal battery, thereby solving the problem that the Li metal battery has Li under high current density+Slow transport kinetics and poor stability of Li plating/stripping cycle.
The technical scheme of the invention is as follows:
a lithium metal anode modified by a composite SEI layer, comprising lithium metal and a composite SEI layer grown on the surface of the lithium metal, wherein the composite SEI layer is formed by Li3Sb/LiF composite particle composition, Li3Li in Sb/LiF composite particles3The mass ratio of Sb to LiF is 3:7, and Li3The size of the Sb/LiF composite particles is 400-600 nm.
Further, the thickness of the composite SEI layer is 2-10 mu m.
A method for preparing the above lithium metal anode modified with a composite SEI layer, comprising the steps of:
step 1: polishing Li metal and drying;
step 2: antimony trifluoride (SbF)3) Adding into dimethyl ether (DME), stirring to obtain Sb3+Sb with a concentration of 1 to 50mmol/L3+Precursor solution;
and step 3: soaking the Li metal obtained in the step 1 in the Sb obtained in the step 23+And taking out the precursor solution for 180-360 seconds, cleaning the surface residues with DME, and drying to obtain the lithium metal anode modified by the composite SEI layer.
Further, the specific step of polishing in step 1 is polishing in Tetrahydrofuran (THF) using a nylon brush.
Further, the drying temperature in the step 3 is 40-60 ℃.
The invention has the beneficial effects that:
the invention provides a lithium metal anode modified by a composite SEI layer, in Li3Under the synergistic effect of Sb and LiF, Li in the composite SEI layer is accelerated+And uniform Li deposition occurs at the interface of the composite SEI layer and the lithium metal; the composite SEI layer has high interface mechanical strength with the lithium metal anode, and can effectively stabilize the lithium metal anodeDendritic growth is prevented during repeated Li stripping/plating processes.
Drawings
Fig. 1 is an XRD pattern of a lithium metal anode modified with a composite SEI layer prepared in example 1 of the present invention;
fig. 2 is an SEM image of a lithium metal anode modified with a composite SEI layer according to example 1 of the present invention, (a) is an SEM image at a resolution of 100 μm, (b) is an SEM image at a resolution of 5 μm, and (c) is a cross-sectional SEM image at a resolution of 20 μm;
fig. 3 is a graph showing the cycle performance of the lithium metal anode modified with the composite SEI layer according to example 1 of the present invention applied to a symmetric battery, and is compared with a pure lithium metal anode symmetric battery.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example 1
This example provides a method for preparing a lithium metal anode modified by a composite SEI layer, which comprises the following steps:
step 1: polishing the Li foil in Tetrahydrofuran (THF) solvent using a nylon brush, removing surface oxides, and drying;
step 2: antimony trifluoride (SbF)3) Adding into dimethyl ether (DME), stirring for 1h to obtain Sb3+Sb concentration of 5mmol/L3+Precursor solution;
and step 3: soaking the Li foil obtained in the step 1 in the Sb obtained in the step 23+And taking out the precursor solution for 180s, cleaning the surface residues with DME, and drying at 60 ℃ for 12h to obtain the lithium metal anode modified by the composite SEI layer.
Example 2
Lithium metal anodes modified with a composite SEI layer were prepared according to the procedure of example 1, except that Sb was removed in step 23+Sb concentration of 5mmol/L3+Precursor solution adjusted to Sb3+Sb concentration of 1mmol/L3+Precursor solution; the other steps are unchanged.
Example 3
Prepared by following the procedure of example 1Modified lithium metal anode, except Sb in step 23+Sb concentration of 5mmol/L3+Precursor solution adjusted to Sb3+Sb concentration of 10mmol/L3+Precursor solution; the other steps are unchanged.
Example 4
Lithium metal anodes modified with a composite SEI layer were prepared according to the procedure of example 1, except that Sb was removed in step 23+Sb concentration of 5mmol/L3+Precursor solution adjusted to Sb3+Sb concentration of 50mmol/L3+Precursor solution; the other steps are unchanged.
Example 5
Lithium metal anodes modified with a composite SEI layer were prepared according to the procedure of example 1, and only Sb obtained in step 2 was soaked in step 33+Adjusting the precursor solution to be 180 s; the other steps are unchanged.
The lithium metal anode modified by the composite SEI layer prepared in the embodiment 1 of the invention is assembled into a symmetrical battery for stability test, and the obtained relevant characteristics and performance test results are as follows:
as can be seen from fig. 1, the diffraction peaks in the lithium metal anode modified by the composite SEI layer obtained in this example were located at 23.5 °, 27.2 °, 48.0 °, 61.6 ° and 70.2 °, which in turn correspond to Li3(111), (200), (222), (311), and (422) crystal planes of Sb (JCPDS card: 89-4221), proving that Li3The presence of a Sb component; diffraction peaks at 38.5 ° and 44.7 °, corresponding in turn to the (111) and (200) crystal planes of LiF (JCPDS cards: 89-3610), demonstrate the presence of the LiF component; in addition to this, lithium metal is also present. Thus, it was shown that the composite SEI layer in a lithium metal anode modified by the composite SEI layer is mainly composed of Li3Sb and LiF.
Fig. 2 is an SEM image of a lithium metal anode modified with a composite SEI layer according to example 1 of the present invention, and fig. 2(a) shows that the surface of the composite SEI layer is very dense; FIG. 2(b) shows that the composite SEI layer is made of Li3Sb/LiF composite particles; it can be concluded from the cross-sectional view shown in fig. 2(c) that the thickness of the composite SEI layer is about 5 μm.
As can be seen from FIG. 3, at 20mA cm-2High current density, 2mAh cm-2The symmetric cell assembled from the lithium metal anode modified with the composite SEI layer (modified Li symmetric cell) can cycle 1360 times compared to an unmodified pure lithium metal anode symmetric cell (pure Li symmetric cell), and has stable Li plating/stripping performance, exhibiting an ultra-low average charge-discharge overpotential (less than 100mV), indicating that the prepared composite SEI layer can enhance Li in SEI+Thereby stabilizing the Li plating/stripping performance.
Table 1 shows Li obtained by theoretical calculation3The interfacial properties of Sb and LiF with Li, respectively, include interfacial energy (σ) and work of adhesion (W)adh). If WadhThe higher the σ, the lower the interface mechanical strength. The results in Table 1 show that Li3The Sb/Li interface has a higher W than the LiF/Li interfaceadh(1.513J/m2) And lower sigma (0.159J/m)2) And further shows that the interface of the composite SEI layer and the lithium metal anode has better mechanical strength and is more stable.
TABLE 1 theoretical calculated interfacial energy (. sigma.) and work of adhesion (W)adh) Value of
Claims (6)
1. A lithium metal anode modified by a composite SEI layer, comprising lithium metal and Li grown on the surface of the lithium metal3Composite SEI layer composed of Sb/LiF composite particles, Li3Li in Sb/LiF composite particles3The mass ratio of Sb to LiF is 3:7, and Li3The size of the Sb/LiF composite particles is 400-600 nm.
2. The lithium metal anode modified by a composite SEI layer according to claim 1, wherein the composite SEI layer has a thickness of 2 to 10 μm.
3. A method for preparing a lithium metal anode modified with a composite SEI layer, comprising the steps of:
step 1: polishing Li metal and drying;
step 2: adding antimony trifluoride into dimethyl ether, and stirring to obtain Sb3+Sb with a concentration of 1 to 50mmol/L3+Precursor solution;
and step 3: soaking the Li metal obtained in the step 1 in the Sb obtained in the step 23+And taking out the precursor solution for 180-360 seconds, and then cleaning and drying to obtain the lithium metal anode modified by the composite SEI layer.
4. The method of preparing a lithium metal anode modified by a composite SEI layer according to claim 3, wherein the step of polishing in step 1 is polishing in tetrahydrofuran using a nylon brush.
5. The method for preparing a lithium metal anode modified by a composite SEI layer according to claim 3, wherein the drying temperature in the step 3 is 40-60 ℃.
6. The method for preparing a lithium metal anode modified by a composite SEI layer according to claim 3, wherein the step of washing in step 3 is washing surface residues with DME.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114784237A (en) * | 2022-04-02 | 2022-07-22 | 合肥工业大学 | Silicon-based negative electrode, preparation method and application thereof |
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