CN114171798A - Method for improving lithium coating on surface of negative electrode, lithium-supplementing negative electrode and lithium ion secondary battery - Google Patents
Method for improving lithium coating on surface of negative electrode, lithium-supplementing negative electrode and lithium ion secondary battery Download PDFInfo
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- CN114171798A CN114171798A CN202111341622.7A CN202111341622A CN114171798A CN 114171798 A CN114171798 A CN 114171798A CN 202111341622 A CN202111341622 A CN 202111341622A CN 114171798 A CN114171798 A CN 114171798A
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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
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/058—Construction or manufacture
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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
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- 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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- 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
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Abstract
A method for improving the coating of lithium on the surface of a negative electrode, a lithium-supplementing negative electrode and a lithium ion secondary battery are disclosed. The method for improving the lithium coating on the surface of the negative electrode comprises the following steps: and forming a coarsening layer on the surface of the negative electrode active material layer of the negative electrode, wherein the coarsening layer has uniformly distributed nano-level roughness, and compounding the ultrathin metal lithium or lithium alloy film with the thickness of 1-50um onto the coarsening layer under pressure to obtain the lithium-supplement negative electrode. The process is simple, easy to operate and applicable to batch production.
Description
Technical Field
The invention belongs to the technical field of energy storage, and particularly relates to improvement of a lithium coating process of a negative electrode of a lithium ion secondary battery.
Background
The energy density of the power battery in 2025 reaches 400 wh/kg. In order to achieve high energy density, improvements are needed to be made on the positive electrode and the negative electrode of the battery, for example, the negative electrode adopts a silicon-doped lithium-supplementing technology, and the positive electrode adopts a ternary material (NCM, NCA) or lithium iron phosphate to form the battery. The silicon or silicon monoxide doped negative electrode has the problem of low first effect, and a lithium source needs to be additionally supplemented to improve the first effect of the battery and improve the energy density. At present, lithium can be supplemented to a negative electrode by adopting an ultrathin lithium foil/lithium alloy foil, and the ultrathin lithium foil/lithium alloy foil can be transferred to the surface of the negative electrode for lithium supplementation through pressure compounding, but the problem exists at present, because the negative electrode is a compacted negative electrode, gaps among negative electrode material particles become very small, and the transfer of metal lithium to the surface of the negative electrode through the pressure compounding has difficulty: when in compounding, high pressure is used, the metallic lithium can be completely transferred to the negative electrode, but the negative electrode sheet has the problem of partial crushing deformation; and the small pressure is used in combination, and the metallic lithium can only be partially transferred to the surface of the negative electrode. It is difficult to find a suitable pressure parameter to completely transfer the metallic lithium to the negative electrode without damaging the negative electrode itself.
Disclosure of Invention
Aiming at the problems, the invention provides a method for improving the lithium coating on the surface of a negative electrode, which comprises the steps of constructing a coarsened layer on the surface of the negative electrode, and compounding an ultrathin metal lithium or lithium alloy film on the coarsened layer under pressure to obtain the lithium-supplementing negative electrode with good compounding effect.
Specifically, one aspect of the present invention provides a method for improving lithium coating on the surface of a negative electrode, comprising:
forming a roughened layer on the surface of a negative electrode active material layer of a negative electrode, the roughened layer having a uniformly distributed nano-scale roughness;
and (3) compounding the ultrathin metal lithium or lithium alloy film with the thickness of 1-50um onto the coarsened layer under pressure to obtain the lithium-supplement negative electrode.
In the present invention, nano-scale roughness means that the maximum height difference in surface protrusions and/or depressions does not exceed 1000nm, preferably 500nm, even below 200 nm. Uniformly distributed roughness means that the roughness difference between the various regions on the surface is not more than 50%, preferably not more than 20%, even not more than 10%.
In some embodiments, the roughened layer is formed by applying the roughened layer on the surface of the anode active material layer or subjecting the surface of the anode active material layer to a roughening treatment.
In some embodiments, the step of applying the roughened layer comprises:
step 1: uniformly mixing conductive nanoparticles, a binder, and a solvent to form a slurry;
step 2: uniformly applying the slurry to the surface of a negative electrode active material layer of a negative electrode to form a surface roughened layer;
and step 3: and drying the cathode with the surface roughened layer to obtain the cathode with the surface roughened layer.
In some embodiments, the slurry comprises, by mass, 1-10% of conductive nanoparticles, 0.1-5% of a binder, and the balance of a solvent,
in some embodiments, the conductive nanoparticles comprise at least one of acetylene black, carbon black, graphene, carbon nanotubes.
In some embodiments, the binder comprises at least one of polyvinylidene fluoride, polytetrafluoroethylene.
In some embodiments, the solvent comprises at least one of N-methylpyrrolidone, N-hexane.
In some embodiments, the slurry is uniformly applied to the surface of the negative active material layer of the negative electrode by means of dimple coating, spray coating, ultrasonic atomization.
In some embodiments, the roughening treatment comprises at least one of physical sanding, grit blasting, laser etching.
In some embodiments, drying the negative electrode having the surface-roughened layer comprises drying in a vacuum oven at a drying temperature of 80-100 ℃ for 12-72 hours (to remove the solvent).
In some embodiments, the thickness of the roughened layer is 0.050-5 um.
In some embodiments, the ultra-thin lithium or lithium alloy film is supported with a film, wherein the metallic lithium or lithium alloy layer supported by the base film is continuous or intermittent in the length direction; or continuously or intermittently in the width direction.
In some embodiments, the lithium alloy is an alloy of metallic lithium with one or more of Ag, Al, Au, Ba, Be, Bi, C, Ca, Cd, Co, Cr, Cs, Fe, Ga, Ge, Hf, Hg, In, Ir, K, Mg, Mn, Mo, N, Na, Nb, Ni, Pt, Pu, Rb, Rh, S, Se, Si, Sn, Sr, Ta, Te, Ti, Y, V, Zn, Zr, Pb, Pd, Sb, and Cu, the content of metallic lithium being 1% to 99.9%.
In some embodiments, the anode comprises a graphite anode, a soft carbon anode, a hard carbon anode, a silicon carbon anode, a graphite-silica anode, a nano-silicon anode, a silica anode, or a tin-based anode.
In some embodiments, the pressure of the pressure recombination is from 0.1 to 20MPa, preferably from 3 to 10 MPa.
In some embodiments, the negative electrode has negative active material layers on both sides of a current collector, and an ultra-thin metallic lithium/lithium alloy film is pressure-compounded onto both sides of the negative electrode.
Another aspect of the present invention provides a lithium-supplementing negative electrode including a roughened layer formed on a surface of a negative electrode active material layer, and an ultra-thin metallic lithium or lithium alloy film having a thickness of 1-50um compounded onto the roughened layer, wherein the roughened layer includes conductive nanoparticles and a binder.
In some embodiments, the negative electrode comprises a graphite negative electrode, a soft carbon negative electrode, a hard carbon negative electrode, a silicon carbon negative electrode, a graphite-silica negative electrode, a nano-silicon negative electrode, a silica negative electrode, or a tin-based negative electrode.
In some embodiments, the negative active material layer of the graphite negative electrode comprises: at least one of natural graphite and/or artificial graphite.
In some embodiments, the anode active material layer of the soft carbon anode comprises: soft carbon.
In some embodiments, the anode active material layer of the hard carbon anode comprises: hard carbon.
In some embodiments, the negative active material layer of the silicon carbon negative electrode comprises: nano silicon and graphite; and mixing the nano silicon and the graphite according to a certain mass ratio to obtain the silicon-carbon cathode. Nano silicon: graphite (mass ratio) 0.1: 99.9-99.9: 0.1.
in some embodiments, the negative active material layer of the graphite-silica negative electrode comprises: silica and graphite; and mixing the nano silicon and the graphite according to a certain mass ratio to obtain the silicon-carbon cathode. Silicon monoxide: graphite (mass ratio) 0.1: 99.9-99.9: 0.1.
in some embodiments, the negative active material layer of the nano-silicon negative electrode comprises: and (4) nano silicon.
In some embodiments, the negative active material layer of the silica negative electrode comprises: and (3) silicon monoxide.
In some embodiments, the negative active material layer of the tin-based negative electrode comprises: tin oxide and/or tin alloy compound.
In some embodiments, the lithium-supplemented negative electrode is prepared by the above-described method of improving the coating of lithium on the surface of the negative electrode.
Still another aspect of the present invention provides a lithium ion secondary battery comprising the above lithium-complementary negative electrode.
The present invention may have at least one of the following advantageous effects:
(1) the roughened layer on the surface of the negative electrode makes the metal lithium or lithium alloy easier to transfer to the surface of the negative electrode without incomplete transfer or crushing deformation of the negative electrode.
(2) The surface of the lithium-supplement negative electrode is flat (metal lithium is easy to deform, and the influence of a coarsened layer on the surface morphology is counteracted).
(3) The lithium-supplementing negative electrode with the coarsened layer is characterized in that when the lithium-supplementing negative electrode is soaked in electrolyte, metal lithium and a negative electrode active substance are completely reacted, and the coarsened layer does not influence the electrochemical performance.
(4) The preparation process of the lithium-supplement cathode is simple and can be applied to batch production.
(5) The lithium-supplementing negative electrode, the positive electrode and the diaphragm can be directly assembled into a battery for use by adopting a winding or lamination process, no additional working procedure is added, and the method is consistent with the existing process.
(6) The lithium-supplement negative electrode can improve the first efficiency of the secondary battery.
Drawings
Fig. 1 shows a lithium-supplemented negative electrode product of example 1 of the present invention.
Fig. 2 shows a lithium-supplemented negative electrode product of example 2 of the invention.
FIG. 3 shows a lithium-supplemented product obtained by compounding comparative example 1 at a pressure of 5 MPa.
FIG. 4 shows a lithium-supplemented product obtained by compounding comparative example 1 at a pressure of 5.5 MPa.
Detailed Description
The present invention will be described more specifically with reference to examples. The following examples are typical examples of the product structure parameters, the reaction participants and the process conditions, but through the experiments of the present inventors, the other structure parameters, the reaction participants and other process conditions listed above are also applicable and all the claimed technical effects can be achieved.
Example 1:
preparing a surface roughening negative electrode 1: and (3) grinding and polishing the surface of the original cathode (the cathode doped with the silicon monoxide and having the thickness of 110um) by adopting 8000-mesh sand paper to obtain a surface-roughened cathode 1, wherein the average roughness of the surface of the roughened cathode 1 is 390 nm.
Preparation of lithium-supplement negative electrode 1: in a drying workshop with the dew point of-45 ℃, an ultrathin lithium foil with the thickness of 5um is used as a lithium supplement source, the cathode uses the surface roughened cathode 1, the upper and lower rolls of lithium foil and the dried surface roughened cathode 1 are compounded into a lithium supplement cathode under the pressure of 5MPa, as shown in figure 1, metal lithium is completely transferred to the surface of the cathode, and the surface of the lithium supplement cathode is relatively flat.
Example 2:
preparing a surface coarsening negative electrode 2: the method comprises the steps of mechanically mixing 30 g of acetylene black (Shenzhen, department of crystallography, Inc., with an average particle size of 30nm), 5 g of polyvinylidene fluoride (PVDF) (Shenzhen, department of crystallography, Inc.), and 1000 g of solvent N-methylpyrrolidone (NMP) (Shanghai, Allantin, Biotechnology, Inc.), obtaining uniform slurry, coating the surface of an original negative electrode (a negative electrode doped with silicon oxide and with a thickness of 110um) by virtue of a dimple coater to obtain a negative electrode 2 (a roughened layer with a thickness of 3um) with a roughened surface, wherein the average roughness of the roughened surface of the negative electrode is 450 nm; and drying the cathode with the roughened surface in a vacuum oven at 80 ℃ for 24 hours, and taking out for later use.
Preparation of lithium-supplement negative electrode 2: in a drying workshop with the dew point of-45 ℃, an ultrathin lithium foil with the thickness of 5um is used as a lithium supplement source, the cathode uses the surface roughened cathode 2, the upper and lower rolls of lithium foil and the dried surface roughened cathode 2 are compounded into the lithium supplement cathode under the pressure of 5MPa, as shown in figure 2, all the metal lithium is transferred to the surface of the cathode, and the surface of the lithium supplement cathode is relatively flat.
Assembling the battery and testing:
negative electrode lithium-doped negative electrode 1 and lithium-doped negative electrode 2 prepared as described above
Preparing a positive electrode: using lithium cobaltate (active material): acetylene black (conductive agent): polyvinylidene fluoride (binder) ═ 90: 5: adding a certain amount of N-methyl pyrrolidone according to the mass ratio of 5, and uniformly stirring and mixing to obtain anode slurry; coating the positive electrode slurry on an aluminum foil, and performing vacuum drying for 24 hours at 80 ℃ to obtain a positive electrode piece;
battery production and testing: die-cutting the lithium-supplement negative electrodes 1 and 2 into 45 mm by 58mm, die-cutting the positive electrode into 44 mm by 57mm, using celgard 2500 as a diaphragm, and forming a soft-package battery by 3 lithium-supplement negative electrodes and 4 positive electrodes by virtue of an automatic lamination machine; the electrolyte adopts ester electrolyte (multi-reagent). The ester electrolyte comprises the following components: ethylene Carbonate (EC): dimethyl carbonate (DMC): ethyl Methyl Carbonate (EMC) ═ 1:1:1, 1M lithium hexafluorophosphate. Voltage range 3.0-4.2V, charge and discharge cycle at 0.5C rate.
The original negative electrode (the negative electrode doped with the silicon monoxide and the thickness of 110um) and the positive electrode are assembled into the soft package battery, and the battery is prepared and tested as the lithium supplement battery
The test values are in the following table:
comparative example 1:
preparing a lithium-supplement negative electrode: in a drying workshop with the dew point of-45 ℃, an ultrathin lithium foil with the thickness of 5um is used as a lithium supplement source, a negative electrode doped with silicon oxide (the thickness is 110um, the thickness is the same as that of the negative electrode in the embodiment 1) is used, an upper roll of lithium foil, a lower roll of lithium foil and a dried negative electrode (dried in a vacuum oven at the temperature of 80 ℃ for 24 hours) are compounded into a lithium supplement negative electrode under the pressure of 5MPa, and the lithium supplement negative electrode product has the problem of incomplete metal lithium transfer as shown in figure 3; when the pressure is slightly increased to 5.5MPa, the lithium-supplemented negative electrode product is shown in FIG. 4, metal lithium is completely transferred to the surface of the negative electrode, but a part of the negative electrode is crushed.
It should be understood that the above-mentioned embodiments are merely preferred embodiments of the present invention, and not intended to limit the present invention, and 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 method for improving lithium coating on the surface of a negative electrode, comprising:
forming a roughened layer on the surface of a negative electrode active material layer of a negative electrode, the roughened layer having a uniformly distributed nano-scale roughness;
and (3) compounding the ultrathin metal lithium or lithium alloy film with the thickness of 1-50um onto the coarsened layer under pressure to obtain the lithium-supplement negative electrode.
2. The method according to claim 1, characterized in that the roughened layer is formed by applying the roughened layer on the surface of the negative electrode active material layer or subjecting the surface of the negative electrode active material layer to a roughening treatment.
3. The method of claim 2, wherein the step of applying the coarsening layer comprises:
step 1: uniformly mixing conductive nanoparticles, a binder, and a solvent to form a slurry;
step 2: uniformly applying the slurry to the surface of a negative electrode active material layer of a negative electrode to form a surface roughened layer;
and step 3: and drying the cathode with the surface roughened layer to obtain the cathode with the surface roughened layer.
4. The method according to claim 3, wherein the slurry comprises, by mass, 1-10% of conductive nanoparticles, 0.1-5% of a binder, and the balance of a solvent,
preferably, the conductive nanoparticles comprise at least one of acetylene black, carbon black, graphene, carbon nanotubes; the binder comprises at least one of polyvinylidene fluoride and polytetrafluoroethylene; the solvent comprises at least one of N-methylpyrrolidone and N-hexane.
5. The method according to claim 3, characterized in that the slurry is uniformly applied to the surface of the negative active material layer of the negative electrode by means of dimple coating, spray coating, ultrasonic atomization.
6. The method of claim 2, wherein the roughening comprises at least one of physical sanding, grit blasting, and laser etching.
7. A method according to claim 1, characterized in that the thickness of the coarsened layer is 0.050-5 um.
8. The method according to claim 1, characterized in that the pressure of the pressure recombination is 0.1-20MPa, preferably 3-10 MPa.
9. A lithium-supplementing negative electrode, characterized in that it comprises a roughened layer formed on the surface of a negative electrode active material layer and an ultrathin metallic lithium or lithium alloy film having a thickness of 1-50um compounded onto the roughened layer, wherein the roughened layer comprises conductive nanoparticles and a binder,
preferably, the negative electrode comprises a graphite negative electrode, a soft carbon negative electrode, a hard carbon negative electrode, a silicon carbon negative electrode, a graphite-silicon oxide negative electrode, a nano-silicon negative electrode, a silicon oxide negative electrode or a tin-based negative electrode.
10. A lithium ion secondary battery characterized in that it comprises the lithium-complementary negative electrode according to claim 9.
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2021
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| US20070204457A1 (en) * | 2006-01-10 | 2007-09-06 | Toshitada Sato | Non-aqueous electrolyte secondary battery and method for producing the same |
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