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CN116111068A - Zinc cathode material modified by three-dimensional antimony/antimony oxide composite layer and preparation method and application thereof - Google Patents

Zinc cathode material modified by three-dimensional antimony/antimony oxide composite layer and preparation method and application thereof Download PDF

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CN116111068A
CN116111068A CN202310160165.4A CN202310160165A CN116111068A CN 116111068 A CN116111068 A CN 116111068A CN 202310160165 A CN202310160165 A CN 202310160165A CN 116111068 A CN116111068 A CN 116111068A
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antimony
zinc
composite layer
oxide composite
dimensional
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赵钦
田孝萌
马天翼
孙晓东
孙颖
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Liaoning University
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Liaoning University
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/049—Manufacturing of an active layer by chemical means
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a zinc anode material modified by a three-dimensional antimony/antimony oxide composite layer, and a preparation method and application thereof. The zinc cathode material modified by the three-dimensional antimony/antimony oxide composite layer is prepared by a simple two-step self-assembly step: forming an antimony layer by in-situ displacement reaction between the zinc foil and the antimony trifluoride solution; simultaneously, the rapid oxidation reaction of the antimony layer in the reaction solution dissolved with oxygen causes the surface to generate a thin antimony oxide layer. Due to the unique three-dimensional nano skeleton structure of the designed antimony/antimony oxide composite layer, the zinc anode material modified by the antimony/antimony oxide composite layer provided by the invention can homogenize zinc ion circulation and electric field distribution at a zinc anode material-electrolyte micro-interface, further reduce polarization and inhibit zinc dendrite growth in the electroplating/stripping process, and finally realize reversible zinc deposition and dissolution of the zinc anode material. Therefore, the zinc cathode material modified by the antimony/antimony oxide composite layer improves the rate capability and long cycle life of the water-based zinc ion battery.

Description

Zinc cathode material modified by three-dimensional antimony/antimony oxide composite layer and preparation method and application thereof
Technical Field
The invention relates to the technical field of battery electrode materials, in particular to a zinc anode material modified by a three-dimensional antimony/antimony oxide composite coating, and a preparation method and application thereof.
Background
Battery systems with high energy density, safety and low cost are required for the growing industries of large stationary energy storage systems, electric vehicles, and portable consumer electronics. Compared with other battery systems, the electrolyte of the water-based zinc ion battery is safe and environment-friendly, and zinc metal is used as an anode, so that the water-based zinc ion battery has rich and proper standard electrode potential (-0.76V vs SHE) and higher theoretical capacity (820 mA h g) -1 ) Therefore, in recent years, aqueous Zinc Ion Batteries (ZIBs) have been widely studied. However, because zinc anode materials have high thermodynamic instability when in contact with aqueous electrolytes, this can lead to severe hydrogen evolution and self-corrosion side reactions. Meanwhile, the rough microenvironment of the surface of the zinc anode material causes inconsistent diffusion and nucleation of zinc ions, and serious dendrite growth of the zinc anode material is caused. These detrimental problems seriously affect the plating/stripping reversibility and long cycle stability of zinc ion batteries, preventing their large-scale application. To solve these troublesome problems, researchers in this field have implemented various improvement strategies, such as: electrolyte optimization, construction of galvanized current collectors, design of artificial protection layers, etc., wherein artificial interface layer design has recently been seen as a low cost solution. However, the existing protective layer still has many defects, such as a polymer layer can cause larger ion transmission resistance, and voltage polarization is further increased; stabilization of carbon-based conductive layersThe structure is easy to be destroyed in the repeated zinc electroplating-stripping process due to poor performance, more importantly, the current coating mostly has a two-dimensional disordered structure, and the problem of electrode volume expansion in the circulating process is difficult to adapt, so that a more ideal artificial protection layer is still required to be continuously searched at present to improve the zinc cathode, thereby further improving the electrochemical performance of the water-based zinc ion battery.
Disclosure of Invention
In order to solve a plurality of problems existing in the existing zinc negative electrode material artificial protective layer of the water-based zinc ion battery, the problems of dendrite, hydrogen evolution, corrosion and the like of the zinc negative electrode of the water-based zinc ion battery are solved. The invention aims to provide a zinc anode material modified by a three-dimensional antimony/antimony oxide composite coating, and the antimony/antimony oxide composite coating prepared by the invention has a unique three-dimensional nano skeleton structure, and can greatly adapt to volume expansion of an anode and inhibit generation of nano platy dendrites with different orientations in a circulation process when being constructed on the surface of a zinc anode material of a water-based zinc ion battery. Meanwhile, corrosion and hydrogen evolution can be inhibited, and byproducts such as basic zinc sulfate and the like are avoided, so that the long-cycle stability and the rate capability of the battery are improved.
In order to achieve the above purpose, the invention adopts the following technical scheme: a zinc negative electrode material modified by a three-dimensional antimony/antimony oxide composite layer, wherein the antimony/antimony oxide composite layer has a three-dimensional nano skeleton structure.
The preparation method of the zinc anode material modified by the three-dimensional antimony/antimony oxide composite layer is characterized by comprising the following steps of: immersing zinc foil in an antimony trifluoride solution, and self-assembling elemental antimony on the surface of the zinc foil through in-situ displacement reaction between the zinc foil and the antimony trifluoride solution; through the oxidation reaction of the elemental antimony and oxygen in the solution, the surface of the elemental antimony layer is oxidized into antimony oxide, and finally the elemental antimony and antimony oxide composite layer is obtained on the surface of the zinc foil.
Further, in the preparation method, after one surface of the zinc foil is sealed, the zinc foil is immersed in the antimony trifluoride solution, the unsealed side of the zinc foil is contacted with the antimony trifluoride solution, the zinc foil is stood for 2min, taken out, washed by absolute ethyl alcohol, stood and dried at room temperature.
Further, in the above preparation method, sealing one side of the zinc foil is: one side of the zinc foil is firmly bonded by using an insulating tape.
Further, according to the preparation method, the unsealed side of the zinc foil is polished by 2000-mesh sand paper before reaction, and the surface passivation film is removed.
Further, in the above preparation method, the concentration of the antimony trifluoride solution is 0.2mol/L.
Further, according to the preparation method, the thickness of the zinc foil is 0.07-0.10mm, and the purity is 99.9%.
The invention provides an application of a zinc anode material modified by a three-dimensional antimony/antimony oxide composite layer as an electrode material in a water-based zinc ion battery.
Compared with the prior art, the invention has the beneficial effects that:
1. based on the wide understanding of the zinc anode material-electrolyte interface modification strategy, the invention provides an in-situ interface modification strategy depending on time, namely: through the displacement reaction, metallic antimony ions are nucleated and grown on the surface of the zinc anode material in situ, a smooth metallic antimony layer with consistent structure is gradually formed, meanwhile, the characteristic that the metallic antimony layer is easy to oxidize in the air is ingeniously utilized, and oxygen dissolved in the reaction solution oxidizes the surface of the antimony layer to form an antimony oxide layer.
2. According to the invention, an antimony/antimony oxide composite layer is constructed on the surface of the zinc anode material for the first time, the nano layer has a three-dimensional nano skeleton structure, and the excellent structure endows the zinc anode material with large specific surface area, abundant zinc ion transmission channels and nucleation active sites, so that the local current density and concentration polarization of the surface of the zinc anode in the circulation process can be reduced, and the nucleation of the tip at the position with optimal energy can be avoided; and meanwhile, regularly arranged and mutually connected nano particles under the microcosmic condition are beneficial to promoting the transmission dynamics and the flow consistency of zinc ions at the cathode-electrolyte interface, and further ensuring that the zinc ions can be uniformly deposited in micropores of the three-dimensional nano framework, thereby inhibiting the growth of dendrites.
3. The uniformly arranged three-dimensional nano skeleton constructed by the invention has the advantages that the displayed abundant inter-pore micro-gaps improve the wettability of electrolyte, reduce the transmission resistance of interface ions, simultaneously, the proper nano ion channels can quickly reconstruct a solvation network, limit the penetration of unfavorable hydration molecules and free water molecules, and well inhibit the problems of hydrogen evolution and corrosion induced by active water.
4. The zinc cathode material modified by the three-dimensional antimony/antimony oxide composite layer prepared by the invention finally enhances the cycle stability and coulomb efficiency of the water-based zinc ion battery, and has a better application prospect in the field of new energy batteries.
Drawings
FIG. 1 is an X-ray photoelectron spectrum of a three-dimensional antimony/antimony oxide composite layer modified zinc anode material composite layer.
Fig. 2 is a scanning electron microscope image of a three-dimensional antimony/antimony oxide composite layer modified zinc anode material composite layer provided by the invention.
Fig. 3 is a constant current charge-discharge curve under different multiplying power currents when the three-dimensional antimony/antimony oxide composite layer modified zinc anode material and the pure zinc foil provided by the invention are used as electrodes of a water-based zinc ion battery.
Fig. 4 is an electrochemical impedance spectrum curve of a water-based zinc ion symmetric battery in a frequency range of 0.01Hz to 100000Hz when the zinc anode material modified by a three-dimensional antimony/antimony oxide composite layer and the pure zinc foil provided by the invention are used as electrodes of the water-based zinc ion symmetric battery.
FIG. 5 shows the current density of 5mA cm when the three-dimensional antimony/antimony oxide composite layer modified zinc anode material and the pure zinc foil provided by the invention are used as electrodes of a water-based zinc-ion battery -2 The surface capacity is 1mA h cm -2 And a constant current charge-discharge curve graph of the water system zinc ion symmetrical battery.
Detailed Description
Example 1 a zinc negative electrode material modified by a three-dimensional antimony/antimony oxide composite layer (one) was prepared as follows:
1. 0.2mol/L antimony trifluoride solution was prepared.
First, 3.5752g of antimony trifluoride powder is weighed by a dry and clean medicine spoon and placed in a clean 100mL beaker, then a proper amount of distilled water is added, the solution is stirred until the solution is clear and transparent, then the solution is transferred into a 100mL volumetric flask, and distilled water is used for constant volume, so that the antimony trifluoride solution with the concentration of 0.2mol/L is obtained.
2. Pretreatment of zinc foil.
Cutting 3X 3cm 2 The method comprises the steps of (1) grinding one surface of the zinc foil with sand paper to remove surface oxide films smoothly and uniformly, then washing the zinc foil with distilled water and absolute ethyl alcohol to remove impurities on the surface of the zinc foil, and then adhering an insulating tape on the unground surface of the zinc foil to enable only the ground surface to react with the solution in the reaction process.
3. And designing a three-dimensional antimony/antimony oxide composite layer on the surface of the zinc anode material.
Pouring an antimony trifluoride solution with the concentration of 0.2mol/L into a culture dish, immersing the treated zinc foil into the antimony trifluoride solution, enabling one surface which is not adhered with an insulating tape to contact with the antimony trifluoride solution, and enabling simple substance antimony to be self-assembled on the surface of the zinc foil through in-situ replacement reaction between the zinc foil and the antimony trifluoride solution to form an antimony layer. When the displacement reaction occurs, a large amount of oxygen is dissolved in the reaction liquid, so that the surface of the antimony layer is accompanied by rapid oxidation reaction, and the simple substance antimony is oxidized into antimony oxide, so that the surface of the antimony layer is spontaneously oxidized to form the antimony oxide layer. And after 2min of dipping, taking out the zinc foil, washing off the residual antimony trifluoride solution on the surface of the zinc foil by using absolute ethyl alcohol, and finally, successfully constructing a three-dimensional antimony and antimony oxide composite layer on the surface of the zinc foil, thereby obtaining the zinc anode material modified by the three-dimensional antimony/antimony oxide composite layer.
(II) characterization
FIG. 1 is an X-ray photoelectron spectrum of a three-dimensional antimony/antimony oxide composite layer modified zinc anode material composite layer. As can be seen from FIG. 1, the peak-to-peak ratios of the two pairs of binding energies are consistent with those of the related literature and correspond to Sb respectively 0 3d of (2) 3/2 ，3d 5/2 And Sb (Sb) 2 O 3 3d of (2) 3/2 ，3d 5/2 This result proves that the simple substance antimony and antimony oxide composite layer is successfully constructed on the surface of the zinc anode material.
Fig. 2 is a scanning electron microscope image of a three-dimensional antimony/antimony oxide composite layer modified zinc anode material composite layer provided by the invention. As can be seen from the surface scanning electron microscope image of a in fig. 2, under the scale of 2 micrometers, the elemental antimony/antimony oxide composite layer presents a size layered arrangement and a cross-linked nanoparticle structure, and as can be seen from the cross-section scanning electron microscope image of b in fig. 2, a large number of uniformly ordered and full-shaped nanoparticles can construct a three-dimensional nano skeleton which is regularly arranged.
Example 2 application of three-dimensional antimony/antimony oxide composite layer modified zinc cathode material in aqueous zinc ion battery
The zinc cathode material modified by the three-dimensional antimony/antimony oxide composite layer prepared in the example 1 is cut into a wafer with the diameter of 12mm for standby.
The button cell type used in this example was CR2032.
Symmetrical battery assembly
And taking two zinc cathode materials modified by the three-dimensional antimony/antimony oxide composite layer as the positive electrode plate and the negative electrode plate of the button cell respectively. Firstly, putting a positive plate into a positive shell, ensuring that one surface with a composite layer contacts a diaphragm, then putting a glass fiber diaphragm, and then dripping 150 mu L of ZnSO with the concentration of 2mol/L 4 Electrolyte is then put into the negative electrode plate above the diaphragm, one surface with the composite layer is contacted with the diaphragm, then a gasket and an elastic sheet are sequentially put into the negative electrode plate, finally the negative electrode shell is buckled, and the battery is packaged by a battery packaging machine, so that a three-dimensional zinc-ion symmetrical button battery with zinc negative electrode materials modified by the antimony/antimony oxide composite layer serving as positive/negative electrode plates is obtained, and the zinc-ion symmetrical button battery is marked as Zn@Sb/Sb 2 O 3 //Zn@Sb/Sb 2 O 3 Symmetrical button cells.
Comparative example 1-aqueous zinc ion symmetric coin cell of pure zinc electrode: the assembly method is the same as above, except that pure zinc foil is used for both the positive and negative plates, and the Zn// Zn symmetrical button cell is marked.
(III) Battery Performance test
And (3) testing constant current charge and discharge of the water system zinc ion symmetrical button cell and testing electrochemical impedance in a certain frequency range.
1. At 1mA cm -2 To 5mA cm -2 In the current density range of (2) for Zn@Sb/Sb containing 2 O 3 Or a symmetric cell with Zn electrodes was subjected to rate performance testing, the results are shown in figure 3. The results show that the voltage-time curve tends to stabilize all the time with increasing current density, at high current densities the polarization voltage increases slightly. Zn@Sb/Sb when returning to the original current density 2 O 3 The electrodes showed similar voltage hysteresis, indicating that the antimony/antimony oxide composite layer provided good rate performance for the cell. In contrast, pure Zn electrodes initially exhibit stable voltage fluctuations, but after current density increases, their polarization voltage increases rapidly and severely unstable voltage oscillations occur, due to extremely slow and uneven pure zinc-electrolyte interface zinc ion transport at large rates, resulting in greater concentration polarization and very poor plating/stripping reversibility.
2. Electrochemical impedance spectra were tested in the high and low frequency range of 0.01Hz to 100000Hz as shown in figure 4. The result shows that Zn@Sb/Sb 2 O 3 //Zn@Sb/Sb 2 O 3 The charge transfer resistance of the cell is significantly less than Zn// Zn due to the skeleton-rich electrolyte wettability and zinc ion affinity of the nanoparticle construction, accelerating zinc ion transport.
3. At a current density of 5mA cm -2 The surface capacity is 1mA h cm -2 Next, constant current charge and discharge tests were performed on the aqueous zinc ion symmetric coin cell, and the results are shown in fig. 5. Zn@Sb/Sb 2 O 3 //Zn@Sb/Sb 2 O 3 The symmetrical button cell can keep the long cycle life of 640h, and the average polarization voltage is always kept at a lower value (39 mV) in the whole cycle period, which shows that the three-dimensional composite layer designed by the invention has larger specific surface area and rich ion migration tunnels, can induce the zinc ions at the interface to uniformly circulate even under the high current density, simultaneously reduces the local current density at the interface,and finally, the circulation stability and reversibility of the water system zinc ion symmetrical battery are improved. The polarization voltage of the Zn// Zn symmetrical button cell is slightly higher than that of Zn@Sb/Sb at the initial stage 2 O 3 //Zn@Sb/Sb 2 O 3 But as the cycle was continued for around 30 hours, the polarization voltage began to suddenly increase and continued to maintain a large ripple value (300 mV), indicating that uneven deposition/dissolution was accompanied by an increase in corrosive hydrogen evolution, leading to the formation of flaky dendrites and mossy inert byproducts, ultimately leading to cell failure.

Claims (8)

1. The zinc anode material modified by the three-dimensional antimony/antimony oxide composite layer is characterized in that the antimony/antimony oxide composite layer has a three-dimensional nano skeleton structure.
2. The preparation method of the zinc anode material modified by the three-dimensional antimony/antimony oxide composite layer, which is characterized by comprising the following steps: immersing zinc foil in an antimony trifluoride solution, and self-assembling elemental antimony on the surface of the zinc foil through in-situ displacement reaction between the zinc foil and the antimony trifluoride solution; through the oxidation reaction of the simple substance antimony and oxygen in the solution, the surface of the simple substance antimony layer is oxidized into antimony oxide, and finally the simple substance antimony and antimony oxide composite layer is obtained on the surface of the zinc foil.
3. The method of claim 2, wherein the zinc foil is sealed on one side and then immersed in the antimony trifluoride solution, the unsealed side of the zinc foil is brought into contact with the antimony trifluoride solution, allowed to stand for 2 minutes, the zinc foil is removed, washed with absolute ethanol, allowed to stand and dried at room temperature.
4. A method of manufacture as claimed in claim 3, wherein sealing one side of the zinc foil is: one side of the zinc foil is firmly bonded by using an insulating tape.
5. A method of preparing according to claim 3, wherein the unsealed side of the zinc foil is sanded with 2000 mesh sand paper prior to the reaction to remove the surface passivation film.
6. The method according to claim 2, 3, 4 or 5, wherein the concentration of the antimony trifluoride solution is 0.2mol/L.
7. The method of claim 2, 3, 4 or 5, wherein the zinc foil has a thickness of 0.07-0.10mm and a purity of 99.9%.
8. The use of a zinc negative electrode material modified by a three-dimensional antimony/antimony oxide composite layer as claimed in claim 1 as an electrode material in an aqueous zinc ion battery.
CN202310160165.4A 2023-02-24 2023-02-24 Zinc cathode material modified by three-dimensional antimony/antimony oxide composite layer and preparation method and application thereof Pending CN116111068A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116666638A (en) * 2023-07-24 2023-08-29 首都师范大学 Artificial solid/liquid interface protective layer based on layer-by-layer self-assembly technology, metal electrode, battery, and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116666638A (en) * 2023-07-24 2023-08-29 首都师范大学 Artificial solid/liquid interface protective layer based on layer-by-layer self-assembly technology, metal electrode, battery, and preparation method and application thereof
CN116666638B (en) * 2023-07-24 2024-01-23 首都师范大学 Water system zinc ion secondary battery

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