CN113314709A - Supermolecule polymer modified metal negative electrode and preparation method and application thereof - Google Patents
Supermolecule polymer modified metal negative electrode and preparation method and application thereof Download PDFInfo
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- CN113314709A CN113314709A CN202110575427.4A CN202110575427A CN113314709A CN 113314709 A CN113314709 A CN 113314709A CN 202110575427 A CN202110575427 A CN 202110575427A CN 113314709 A CN113314709 A CN 113314709A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of metal batteries, and mainly discloses a method for modifying a metal cathode by a supramolecular polymer. The method comprises the following steps: (1) dissolving a supramolecular polymer crosslinked by a non-covalent bond in an organic solvent to obtain a supramolecular polymer solution; (2) removing impurity compounds on the metal surface, uniformly coating the supramolecular polymer solution on the metal surface, and volatilizing the solvent to form a layer of supramolecular polymer interface to obtain the metal cathode modified by the supramolecular polymer. All the steps are carried out under the protection of inert gas. The method can eliminate the hidden trouble that the artificial SEI film of the metal cathode is broken in the circulating process, enhance the mechanical strength of the artificial SEI film and prolong the service life.
Description
Technical Field
The invention relates to the technical field of metal batteries, in particular to a supermolecular polymer modified metal cathode and a preparation method and application thereof.
Background
With the rapid development of electronic products and electric automobiles, the theoretical specific capacity of the graphite cathode in the lithium ion battery is only 372 mAh g-1And the requirement of high energy density of the lithium ion battery is difficult to meet. The metallic lithium has a g of as high as 3860 mAh-1The theoretical specific capacity and the lowest electrode potential (-3.04V) are the next generation lithium secondary battery cathode material with development prospect. However, lithium metal has very strong chemical activity and can react with almost all electrolytes, the structure of the SEI film formed after the reaction has non-uniformity, which causes dendrites to form, resulting in low coulombic efficiency and short circuit of the battery, and repeated cracking and recombination of the SEI film are the main reasons for short circuit, capacity attenuation and low coulombic efficiency of the battery, and it is urgently needed to establish a stable interface between the lithium metal negative electrode and the electrolyte. Therefore, constructing an artificial SEI film on the surface of lithium metal becomes a focus of attention of researchers.
Polymer layers for lithium negative electrode protection have attracted considerable attention because of good flexibility, polymer can accommodate poor interfacial fluctuations during battery cycling, form a good compatible interface with metallic lithium. Furthermore, polar functional groups in the polymer (e.g., -COOH, -OH, -CO-NH, -NH2) Has good lithium affinity and plays a great role in the uniform deposition of lithium ions. However, the cracking of the polymer artificial SEI film during the cycling of the battery is a difficult problem facing now. The uneven deposition of metallic lithium generates large local stress, while the mechanical modulus of the polymer is low, and the growth of lithium dendrites cannot be completely inhibited in practical work. There are researchers observing lithium polymer batteries (m. Rosso, c. Brissot, et. al. electrochimica acta, 51 (2006) 5334-. Therefore, fundamentally improving the mechanical strength of the polymer protective film and endowing the protective film with certain self-repairing capability is the key for increasing the functional reliability of the artificial SEI film.
Disclosure of Invention
The invention aims to provide a method for modifying a metal cathode by a supramolecular polymer, which can eliminate the hidden trouble of cracking of an artificial SEI film of the metal cathode in the circulating process, enhance the mechanical strength of the artificial SEI film and prolong the service life.
In order to achieve the purpose, the invention provides the following technical scheme:
in one aspect, a method for modifying a metal negative electrode by a supramolecular polymer comprises the following steps:
(1) dissolving a supramolecular polymer crosslinked by a non-covalent bond in an organic solvent to obtain a polymer solution;
(2) removing impurity compounds on the metal surface, uniformly coating the supramolecular polymer solution on the metal surface, and volatilizing the solvent to form a layer of supramolecular polymer interface to obtain the metal cathode modified by the supramolecular polymer.
All the steps are carried out under the protection of inert gas.
Preferably, the non-covalent bonds in step 1) include one or more of electrostatic interactions, hydrogen bonds, metal coordination bonds, host-guest interactions, pi-pi bond stacking, and hydrophobic-hydrophobic interactions.
More preferably, the electrostatically interacting supramolecular polymer may be a complex formed in water of an organic compound with opposite charges (anions such as sulfonate and carboxylate, cations such as quaternary ammonium salt) as supramolecular interaction sites, for example a block copolymer-surfactant complex formed by interaction of a hydrophilic polyethylene oxide (PEO)/sodium polymethacrylate diblock copolymer with various cationic surfactants.
The hydrogen bonded supramolecular polymer may be: upy (2-urea-4-pyrimidinone) modified poly (ethylene-co-butene), Upy modified polyethylene glycol/propylene glycol ether; a polystyrene core dispersed in a phase separated form in a polyacrylamide matrix; urea, carboxylic acid, thymine/2, 6-diaminotriazine, amidoethylimidazolidone, bis (aminoethyl) urea, diamine tetraethyltriurea modified polymers; upy modified Polydimethylsiloxane (PDMS); one or more of triple hydrogen bond polymer constructed by melamine and polyimide and supermolecular polymer monocrystal formed by hydrogen bonding of a series of carboxyl and pyridyl.
The supermolecular polymer with metal coordinate bond can be 2, 6-bis (1-methylbenzimidazolyl) pyridine ligand and Zn (NTf)2The 2, 6-pyridinedicarboxamide ligand is bonded to a Polydimethylsiloxane (PDMS) backbone and then to Fe3+The complex coordination cross-linked polymer, the coordination cross-linked polymer of an azacyclo carbene (NHC) ligand and a transition metal monomer, the metal coordination cross-linked polymer of a bifunctional ligand of phenanthroline and a positive copper ion, the polymethyl methacrylate with a terpyridine functional group on a side chain and the metal ion Fe2+、Zn2+The ionic coordination cross-linked polymer, the polymethyl methacrylate (PMMA) copolymer with terpyridine ligand functional groups and metal coordination cross-linked polymer, and one or more of o-diphenol and Fe coordination cross-linked polymer.
The supermolecule polymer with the host-guest interaction can be one or more of crown ether, cyclodextrin, calixarene, pillararene, cucurbituril and the like as a common macrocyclic host compound, and one or more of N-vinylimidazole, ferrocene, N-adamantan-1-yl acrylamide, N-butyl acrylate, bis-ammonio-polymethylmethacrylate, benz-methyl viologen, N-vinylimidazole, adamantane, naphthoxy derivatives and the like as a guest compound. For example: the cyclodextrin main body and n-butyl acrylate are polymerized and put into a supramolecular polymer, an organogel polymer formed by mixing a crown ether main body and diammonium polymethyl methacrylate, a macrocyclic main body cucurbituril and a radical polymer of a benzyl viologen or a naphthoxy derivative.
The supramolecular polymer stacked by pi-pi bonds may be a supramolecular polymer formed by tweezer type interaction between bispyrene end groups and naphthalene diimine chains, a supramolecular polymer formed by non-tweezer type interaction of monoalkynyl groups, a supramolecular polymer based on porphyrin derivatives formed by interaction between electron deficient trinitrofluorene and electron rich porphyrin, a supramolecular polymer formed by pi-pi bond interaction between electron deficient naphthalimide and electron rich pyrene, and the like.
The hydrophobic-hydrophobic interaction supramolecular polymer may be a polymer formed by multiple charge transfer interactions between cucurbituril and a multifunctional monomer, a polymer formed by hydrophobic interactions of hydrophobic inner cavities of cucurbituril and anthracene groups, a polymer formed by hydrophobic interactions of bis-2-N-methylpyridine units and cucurbituril, a polymer formed by hydrophobic interactions of naphthyloxy units and cucurbituril, and the like.
Preferably, the mass fraction of the supramolecular polymer in the supramolecular polymer solution in the step 1) is 5-50%.
Preferably, the organic solvent in step 1) may include, but is not limited to, one or more selected from dimethyl carbonate, diethyl carbonate, ethylene carbonate, ethyl methyl carbonate, propyl methyl carbonate, propylene carbonate, methyl ethyl ether ethylene glycol diethyl ether, 1, 3-dioxolane, tetrahydrofuran, sulfolane, dimethyl sulfoxide, ethylene sulfite, and N, N-dimethylformamide.
Preferably, the elementary metal in step 2) is lithium, sodium, potassium, zinc, aluminum or magnesium.
More preferably, the elementary metal is lithium, sodium or potassium.
Preferably, the coating thickness in the step 2) is 5 nm-50 μm.
Preferably, the inert gas in step 3) is one or more of nitrogen, helium, neon and argon.
On the other hand, the invention also provides a supramolecular polymer modified metal cathode, and the supramolecular polymer modified metal cathode is prepared by the method.
The invention also provides a metal battery, which comprises the supermolecular polymer modified metal negative electrode.
The scheme of the invention has the following beneficial effects:
(1) the preparation steps and the process of the supermolecule polymer modified metal cathode provided by the invention are simple, the operation conditions are simple, and the advantages of industrialization and scale production are achieved;
(2) the artificial SEI film of the metal cathode modified by the supramolecular polymer provided by the invention has ultrahigh mechanical strength, reduces local damage and microcrack of the protective film in the long-term circulation process of the battery, and improves the stability of the protective film.
(3) The artificial SEI film of the metal cathode modified by the supramolecular polymer has extremely strong self-repairing capability, effectively reduces side reactions among interfaces, and can spontaneously repair mechanical damage and cracks of the metal cathode in the repeated electroplating stripping process.
(4) The supermolecule polymer modified metal negative electrode artificial SEI film provided by the invention has a great deal of polar chemical bonds, and the polar chemical bonds can enable lithium deposition to be more uniform, inhibit the growth of dendrites, improve the safety performance of a battery and prolong the service life of the battery.
Detailed Description
The technical solutions of the present invention are described clearly and completely by the following embodiments, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
On one hand, the preparation method of the supermolecular polymer modified lithium metal negative electrode comprises the following steps:
(1) under the protection gas of helium, dissolving a block copolymer-surfactant complex formed by the interaction of a hydrophilic polyethylene oxide (PEO)/sodium polymethacrylate diblock copolymer and various cationic surfactants in dimethyl carbonate to prepare a polymer solution with the mass fraction of 5.0%;
(2) then removing impurity compounds on the surface of the lithium metal, uniformly coating 20 mu L of supramolecular polymer solution on the surface of the elemental lithium cathode by using a liquid-transferring gun, and uniformly coating to form a layer of interface crosslinked by non-covalent bonds;
(3) standing at room temperature for 20h to obtain the supramolecular polymer modified lithium metal cathode, wherein the thickness of the supramolecular polymer modified layer is 50 nm.
On the other hand, the invention also provides a supramolecular polymer modified lithium metal cathode, which is prepared by adopting the method.
The invention also provides a lithium metal battery, which comprises the supermolecule polymer modified lithium metal negative electrode, wherein a button battery is assembled by sequentially arranging a positive electrode shell, a positive electrode plate, electrolyte, a diaphragm, electrolyte, a modified lithium plate, a nickel net and a negative electrode shell from bottom to top, and the preparation method of the positive electrode comprises the following steps:
(1) lithium iron phosphate (LiFePO)4) Uniformly grinding conductive carbon black (Super P) and polyvinylidene fluoride (PVDF) according to a mass ratio of 80:10:10, and stirring for 1 h at a speed of 600 rpm in a stirrer by taking N-methylpyrrolidone (NMP) as a dispersing agent to obtain slurry;
(2) and uniformly coating the obtained slurry on a carbon-containing aluminum foil of a current collector, and then drying for 24 hours in a vacuum box at 120 ℃ to obtain the cathode.
Still further, the separator is Celgard 2400.
Further, the electrolyte comprises 1mol/L electrolyte salt of lithium hexafluorophosphate and an electrolyte solvent, wherein the electrolyte solvent is a mixed solution of dimethyl carbonate and ethylene carbonate, and the volume ratio of the dimethyl carbonate to the ethylene carbonate is 1: 1.
example 2
On one hand, the preparation method of the supermolecular polymer modified lithium metal negative electrode comprises the following steps:
(1) under the protection gas of helium, Upy modified Polydimethylsiloxane (PDMS) is dissolved in dimethyl carbonate to prepare a polymer solution with the mass fraction of 10.0%;
(2) then removing impurity compounds on the surface of the lithium metal, uniformly coating 20 mu L of supramolecular polymer solution on the surface of the elemental lithium cathode by using a liquid-transferring gun, and uniformly coating to form a layer of interface crosslinked by non-covalent bonds;
(3) standing at room temperature for 20h to obtain the supramolecular polymer modified lithium metal cathode, wherein the thickness of the supramolecular polymer modified layer is 100 nm.
On the other hand, the invention also provides a supramolecular polymer modified lithium metal cathode, which is prepared by adopting the method.
The invention also provides a lithium metal battery which is a symmetrical battery, the symmetrical battery comprises the supermolecule polymer modified lithium metal cathode, and the anode and the cathode of the symmetrical battery are the same.
The invention also provides a lithium metal battery, and the preparation method of the lithium metal battery comprises the following steps: assembling the obtained supramolecular polymer modified lithium metal electrode into a 2032 type symmetrical battery, wherein the symmetrical battery refers to a situation that a negative electrode and a positive electrode are both supramolecular polymer modified lithium metal electrodes, 50 microliters of ethylene glycol dimethyl ether and 1, 3-dioxolane are added into electrolyte, and the volume ratio of the ethylene glycol dimethyl ether to the 1, 3-dioxolane is 1: 1, electrolyte salt is 1mol/L lithium bistrifluoromethanesulfonylimide (LiTFSI).
Example 3
On one hand, the preparation method of the supermolecular polymer modified sodium metal negative electrode comprises the following steps:
(1) under the protection of neon gas, dissolving Upy modified poly (ethylene-co-butylene) in tetrahydrofuran to prepare a polymer solution with the mass fraction of 5.0%;
(2) then removing impurity compounds on the surface of the sodium metal, taking 15 mu L of supramolecular polymer solution by using a liquid-transfering gun, uniformly coating the supramolecular polymer solution on the surface of the metal sodium simple substance cathode, and uniformly coating to form a layer of interface crosslinked through non-covalent bonds;
(3) standing at room temperature for 24h to obtain the supermolecular polymer modified sodium metal cathode, wherein the thickness of the supermolecular polymer modified layer is 100 nm.
On the other hand, the invention also provides a supramolecular polymer modified sodium metal electrode which is prepared by adopting the method.
The invention also provides a sodium metal battery, which is a symmetrical battery, wherein the symmetrical battery comprises the supermolecule polymer modified sodium metal cathode, and the anode and the cathode of the symmetrical battery are the same.
The invention also provides a sodium metal battery, and the preparation method of the sodium metal battery comprises the following steps: assembling the obtained supramolecular polymer modified sodium metal electrode into a 2032 type symmetrical battery, wherein the symmetrical battery refers to a situation that a negative electrode and a positive electrode are both supramolecular polymer modified sodium metal electrodes, adding ethylene glycol dimethyl ether and 1, 3-dioxolane with 50 mu L of electrolyte, and the volume ratio of the ethylene glycol dimethyl ether to the 1, 3-dioxolane is 1: 1 sodium perchlorate (NaClO) with electrolyte salt of 1mol/L4)。
Example 4
On one hand, the preparation method of the supermolecular polymer modified potassium metal negative electrode comprises the following steps:
(1) under the protection of argon, the 2, 6-pyridine dicarboxamide ligand is combined with Polydimethylsiloxane (PDMS) skeleton and then Fe3+Dissolving the complex coordination cross-linked polymer in dimethyl sulfoxide to prepare a polymer solution with the mass fraction of 10.0%;
(2) then removing impurity compounds on the surface of the potassium metal, uniformly coating 30 mu L of supramolecular polymer solution on the surface of the elemental potassium metal cathode by using a liquid-transferring gun, and uniformly coating to form a layer of interface crosslinked by non-covalent bonds;
(3) standing at room temperature for 30h to obtain the supermolecular polymer modified potassium metal cathode, wherein the thickness of the supermolecular polymer modified layer is 150 nm.
On the other hand, the invention also provides a supermolecular polymer modified potassium metal negative electrode which is prepared by adopting the method.
The invention also provides a potassium metal battery, which comprises the supermolecule polymer modified potassium metal negative electrode, and the button battery is assembled by sequentially assembling a positive electrode shell, a positive electrode plate, electrolyte, a diaphragm, the electrolyte, a modified potassium plate, a nickel net and a negative electrode shell from bottom to top, wherein the preparation method of the positive electrode comprises the following steps:
(1) will K3V2(PO4)3Uniformly grinding conductive carbon and a polyvinylidene fluoride binder according to a mass ratio of 70:20:10, putting the ground conductive carbon and the polyvinylidene fluoride binder into a beaker, and magnetically stirring the mixture for 8 hours by taking N-methylpyrrolidone (NMP) as a dispersing agent to obtain slurry;
(2) and uniformly coating the obtained slurry on a current collector aluminum foil, and then drying in a vacuum box at 110 ℃ for 12 hours to obtain the cathode.
Still further, the membrane is a Whatman GF/D glass fiber membrane.
Further, the electrolyte is 0.8M KPF6 / EC + DEC(v∶v=1∶1)。
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A method for modifying a metal negative electrode by a supramolecular polymer is characterized by comprising the following steps:
under the protection of inert gas, the reaction kettle is,
(1) dissolving a supramolecular polymer crosslinked by a non-covalent bond in an organic solvent to obtain a supramolecular polymer solution;
(2) removing impurity compounds on the metal surface, uniformly coating the supramolecular polymer solution on the metal surface, and volatilizing the solvent to form a layer of supramolecular polymer interface to obtain the metal cathode modified by the supramolecular polymer.
2. The method for modifying a metal anode by using a supramolecular polymer as claimed in claim 1, wherein the non-covalent bond in step (1) comprises one or more of electrostatic interaction, hydrogen bonding, metal coordination bonding, host-guest interaction, pi-pi bond stacking and hydrophobic-hydrophobic interaction.
3. The method for modifying the metal negative electrode by using the supramolecular polymer as claimed in claim 1, wherein the mass fraction of the supramolecular polymer solution in the step (1) is 5% -50%.
4. The method for modifying a metal negative electrode by using a supramolecular polymer as claimed in claim 1, wherein the organic solvent is selected from one or more of dimethyl carbonate, diethyl carbonate, ethylene carbonate, ethyl methyl carbonate, propyl methyl carbonate, propylene carbonate, ethyl methyl carbonate, ethylene glycol diethyl ether, 1, 3-dioxolane, tetrahydrofuran, sulfolane, dimethyl sulfoxide, ethylene sulfite, and N, N-dimethylformamide.
5. The method for modifying a metal negative electrode by using a supramolecular polymer as claimed in claim 1, wherein the metal is lithium, sodium, potassium, zinc, aluminum or magnesium.
6. The method for modifying a metal cathode by using a supramolecular polymer as claimed in claim 1, wherein the coating thickness in the step (2) is 5 nm-50 μm.
7. A supramolecular polymer-modified metal negative electrode prepared by the method of any one of claims 1-6.
8. A metal battery comprising the supramolecular polymer-modified metal negative electrode of claim 7.
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Cited By (1)
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| CN116376046A (en) * | 2023-05-10 | 2023-07-04 | 五邑大学 | Method for preparing metal-organic polymer based on cage-shaped supermolecular monomer |
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| US20170062830A1 (en) * | 2015-08-31 | 2017-03-02 | The Board Of Trustees Of The Leland Stanford Junior University | High performance battery anodes with polymeric coatings |
| CN110582871A (en) * | 2017-02-20 | 2019-12-17 | 纳米技术仪器公司 | Lithium secondary battery containing protected anode active material particles and method of manufacturing the same |
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