CN114759168A - Co-doped nano porous zinc-based alloy integrated negative electrode and preparation method thereof - Google Patents
Co-doped nano porous zinc-based alloy integrated negative electrode and preparation method thereof Download PDFInfo
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- CN114759168A CN114759168A CN202210275790.9A CN202210275790A CN114759168A CN 114759168 A CN114759168 A CN 114759168A CN 202210275790 A CN202210275790 A CN 202210275790A CN 114759168 A CN114759168 A CN 114759168A
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- H01M4/00—Electrodes
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- H01M4/24—Electrodes for alkaline accumulators
- H01M4/244—Zinc electrodes
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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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- H01M4/24—Electrodes for alkaline accumulators
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Abstract
The invention discloses a preparation method of a co-doped nano porous zinc-based alloy integrated negative electrode, which comprises the following steps: (1) preparing an alloy: preparing a multi-element zinc-based alloy ingot by adopting a melting casting method, wherein in the multi-element zinc-based alloy, a doping element is one or more of Cu, Ni or Al; (2) processing the alloy ingot prepared in the step (1) into an alloy strip or sheet with the thickness of 50 mu m-2 mm; (3) preparing the alloy sheet prepared in the step (2) into a nano porous zinc-based alloy integrated negative electrode with the aperture of about 50-300nm by adopting a chemical dealloying method; (4) and (4) carrying out heat treatment on the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3). The method used by the invention loads zinc on the nano-porous metal matrix in situ, so that the combination with the matrix is tighter, the zinc loading capacity is controllable, and the technical problems that excessive zinc dendrites are generated on the surface of the zinc cathode of the electrode of the nickel-zinc battery and side reactions occur are solved.
Description
Technical Field
The invention belongs to the technical field of nickel-zinc batteries, and particularly relates to a co-doped nano porous zinc-based alloy integrated negative electrode and a preparation method of the negative electrode.
Background
With the development of economic scale, fossil energy resources are scarce, which makes people's demand for energy continuously increase. In recent years, although electrochemical energy storage devices represented by lithium ion batteries have been widely studied, lithium resources have low reserves and are expensive, which hinders the application of lithium ion batteries.
The zinc-nickel battery is an alkaline secondary battery which is composed of zinc oxide as a negative electrode material, nickel hydroxide as a positive electrode material and a potassium hydroxide aqueous solution as an electrolyte. The zinc-nickel battery is not only applied to small loads such as household appliances, electric toys, electric doors and windows, but also has good commercial prospect in the fields of electric bicycles, electric automobiles, high-speed rail power supplies, energy storage base station standby power supplies and the like with high safety requirements.
Although the metal zinc (Zn) has the characteristics of high theoretical specific capacity, low oxidation-reduction potential, rich raw materials, natural safety and the like, the metal zinc (Zn) becomes one of the most ideal cathode materials of the nickel-zinc battery; however, metal Zn is easily corroded in water and reacts with hydrogen production, and thus the coulomb efficiency is reduced, water and metal Zn are consumed, and the growth of zinc dendrite is promoted, so that the performance of a corresponding device is reduced, and even the device cannot operate normally. The existing improvement method mainly comprises the following steps: protective layers such as metal, metal oxide and the like are introduced on the surface to inhibit hydrogen generation or zinc dendrite growth. However, these methods not only increase the quality of the whole zinc sheet, but also have complicated synthesis steps and harsh conditions, and cannot be mass-produced.
In order to solve the problems in the prior art, a co-doped nano porous zinc-based alloy integrated negative electrode and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to solve the problem of serious dendritic growth of the zinc negative electrode in the prior art, and provides a preparation method of a co-doped nano porous zinc-based alloy integrated negative electrode.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a co-doped nano porous zinc-based alloy integrated negative electrode comprises the following steps:
(1) preparing an alloy: preparing a multi-element zinc-based alloy by adopting a melt casting method, wherein in the multi-element zinc-based alloy, the atomic ratio of Zn is 60-90%, the doping elements are one or more of Cu, Ni or Al, and the atomic ratio of the doping elements is 0-40%;
(2) processing the alloy ingot prepared in the step (1) to prepare an alloy strip or sheet with the thickness of 50 mu m-2 mm;
(3) Preparing the alloy sheet prepared in the step (2) into a nano porous zinc-based alloy integrated negative electrode with the aperture of 50-300nm by adopting a chemical dealloying method;
(4) carrying out heat treatment on the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3), wherein the heat treatment process comprises the following steps: under the mixed atmosphere of argon and hydrogen, the proportion of hydrogen in the mixed gas is controlled to be 5-15%, the heating rate is 2-10 ℃/min, the heat treatment temperature is 150-500 ℃, the heat treatment time is 5-30min, and the co-doped nano porous zinc-based alloy integrated negative electrode is obtained after the heat treatment.
Preferably, the preparation method of the alloy ingot in the step (1) is to obtain a homogeneous multi-element zinc-based alloy ingot by utilizing electromagnetic induction melting, casting and uniform post-annealing processes, wherein the annealing temperature is controlled to be 500-.
Preferably, the preparation processing method in the step (2) is to effectively control the size of the alloy by using a smelting melt-spinning or wire cutting instrument to obtain an alloy strip or sheet with the thickness of 50 μm-2 mm.
Preferably, the chemical dealloying method in the step (3) comprises the following specific steps: 0.05-10mol/L hydrochloric acid is used as corrosive liquid, the alloy sheet is subjected to dealloying treatment at the temperature of 20-80 ℃, the treatment time is 2-72 hours, and then the alloy sheet is cleaned and dried.
Preferably, the morphology of the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3) is a nano-porous structure with the pore size distribution of 50-300 nm.
The invention also aims to provide a co-doped nano-porous zinc-based alloy integrated negative electrode prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that: 1. the nano porous metal is used as a conductive matrix, so that the transmission of electrons and ions is facilitated; 2. the nano porous metal is used as a growth matrix, and the problem of dendritic crystal growth of a zinc cathode can be inhibited by loading zinc in situ; 3. a nano porous zinc-based alloy negative electrode is formed, high specific surface area and controllable zinc loading capacity are provided, and therefore the stability of the nickel-zinc battery is improved; 4. the selected metal element resources are rich, and the method for preparing the electrode by dealloying is simple and has lower cost; 5. the integrated zinc-based negative electrode does not need a binder, has controllable size and can meet commercial requirements.
Drawings
Fig. 1 is an SEM image of a co-doped nanoporous copper zinc integrated negative electrode obtained in example 1 of the present invention;
fig. 2 is an EDAX diagram of the co-doped nanoporous copper zinc integrated negative electrode obtained in example 1 of the present invention;
Fig. 3 is an XRD pattern of the co-doped nanoporous copper zinc integrated negative electrode obtained in example 1 of the present invention;
fig. 4 is a constant current zinc deposition/peeling test characterization of the co-doped nanoporous copper zinc integral anode obtained in example 1 of the present invention;
fig. 5 is an SEM image of the co-doped nanoporous copper zinc integrated negative electrode obtained in example 1 of the present invention after deposition/lift-off test;
fig. 6 is an SEM image after deposition/peeling test of a co-doped nanoporous copper zinc integrated anode obtained in example 1 of the present invention compared to a commercially available zinc sheet.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
In the invention, various metals, alloys and various solvents and solutions are purchased from common chemical manufacturers. The electrochemical treatment may be performed using various models and brands of electrochemical stations, and the choice of electrochemical station itself has no essential effect on the present invention. The battery test was performed using a battery tester well known in the art.
The preparation method of the co-doped nano porous zinc-based alloy integrated negative electrode comprises the following steps:
(1) preparing an alloy: preparing a multi-element zinc-based alloy by adopting a melt casting method, wherein in the multi-element zinc-based alloy, the atomic ratio of Zn is 60-90%, the doped elements are one or more of Cu, Ni or Al, and the atomic ratio of the doped elements is 0-40%; the preparation method of the alloy ingot comprises the steps of obtaining a homogeneous multi-element zinc-based alloy ingot by utilizing electromagnetic induction melting, casting and uniform post-annealing processes, wherein the annealing temperature is controlled to be 500-900 ℃, and the annealing time is 0.5-3 h.
(2) Preparing and processing the alloy ingot prepared in the step (1) into an alloy strip or sheet with the thickness of 50 mu m-2 mm; the preparation method comprises the step of utilizing a smelting melt-spinning or linear cutting instrument to effectively control the size of the alloy, so as to obtain an alloy strip or sheet with the thickness of 50 mu m-2 mm.
(3) Preparing the alloy strip or sheet prepared in the step (2) into a nano porous zinc-based alloy integrated negative electrode with the aperture of about 50-300nm by adopting a chemical dealloying method; wherein the chemical dealloying method comprises the following specific steps: using 0.05-10mol/L hydrochloric acid as corrosive liquid, performing dealloying treatment on the alloy sheet at the temperature of 20-100 ℃, wherein the treatment time is 0.5-72 hours, and then cleaning and drying; the prepared nano-porous zinc-based alloy integrated negative electrode is in a nano-porous structure with the pore size distribution of about 50-300 nm.
(4) Carrying out heat treatment on the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3); wherein the heat treatment process comprises the following steps: in the mixed atmosphere of argon and hydrogen, the proportion of hydrogen in the mixed gas is controlled to be 5-15%, the heating rate is 2-10 ℃/min, the heat treatment temperature is 150-500 ℃, the heat treatment time is 5-30min, and the co-doped nano porous zinc-based alloy integrated negative electrode is obtained after the heat treatment.
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Example 1
A preparation method of a co-doped nano-porous zinc-based alloy integrated negative electrode comprises the following steps:
(1) preparing an alloy: the atomic content ratio of Cu to Zn is 30:70, Cu-Zn metal particles are smelted into an alloy ingot by an electromagnetic induction smelting process, and then the alloy ingot is annealed for 1h at the temperature of 600 ℃ to obtain a homogeneous Cu-Zn alloy ingot;
(2) wire cutting: preparing the alloy ingot in the step (1) into an alloy sheet with the thickness of 1mm by a wire cutting method;
(3) removing alloy: placing the alloy sheet prepared in the step (2) in 2mol/L hydrochloric acid solution, dealloying at the temperature of 50 ℃, wherein the dealloying time is 12 hours, and then cleaning and drying;
(4) electrochemical testing: using nano porous copper-zinc alloy and commercially available zinc sheet as working electrode, using commercially available zinc sheet with same area as counter electrode and reference electrode, and measuring the total volume at 1mol L -1KOH and 20mmol L of-1Zn (CH) of3COO)2And (4) carrying out charge-discharge test in the mixed electrolyte, and observing the dendritic crystal formation and growth process.
Fig. 1 is an SEM image of the co-doped nanoporous copper-zinc integrated negative electrode obtained in example 1, and it can be seen from the SEM image that a nanoporous structure with a pore size of about 100nm is formed after the material is dealloyed.
Fig. 2 is an EDAX diagram of the co-doped nanoporous copper-zinc integrated anode obtained in example 1, and the EDAX diagram can illustrate that the content of zinc in the co-doped nanoporous copper-zinc integrated anode is about 46.76 at%.
FIG. 3 is an XRD (X-ray diffraction) pattern of the co-doped nano-porous copper-zinc integrated negative electrode obtained in example 1, and the phase composition of the co-doped nano-porous copper-zinc integrated negative electrode can be determined to be a face-centered cubic structure Cu-Zn alloy and a small part of Cu through the XRD pattern5Zn8。
Fig. 4, 5 and 6 are SEM images of the co-doped nanoporous cu-zn monolithic anodes for constant current zinc deposition/exfoliation test characterization, the nanoporous cu-zn monolithic anodes after deposition/exfoliation test and the commercial zinc sheet after deposition/exfoliation test, respectively, obtained in example 1 at 2.0m amcm-2After 16h of deposition/stripping (500 times of charge-discharge circulation) under the current density, sharp dendrite grows on the surface of the commercial zinc sheet. In contrast, a uniform coating was present on the surface of the nanoporous cu-zn monolithic anode, and no evidence of dendrite formation was observed.
Example 2
(1) Preparing an alloy: the atomic content ratio of Ni to Zn is 20:80, Ni-Zn metal particles are smelted into an alloy ingot by an electromagnetic induction smelting process, and then the alloy ingot is annealed for 1h at 800 ℃ to obtain a homogeneous Ni-Zn alloy ingot.
(2) Wire cutting: and (3) preparing the alloy ingot in the step (1) into an alloy sheet with the thickness of 1mm by using a wire cutting method.
(3) Removing alloy: and (3) placing the alloy sheet prepared in the step (2) in 2mol/L hydrochloric acid solution, dealloying at the temperature of 50 ℃ for 8 hours, and then cleaning and drying.
(4) Electrochemical testing: using nano porous nickel-zinc alloy and commercially available zinc sheet as working electrode, using commercially available zinc sheet with same area as counter electrode and reference electrode, and measuring the total volume of the working electrode and the reference electrode at 1mol L-1KOH and 20mmol L of-1Zn (CH) of3COO)2And (4) carrying out charge and discharge tests in the mixed electrolyte, and observing the formation and growth processes of dendrites.
The test result shows that the nano-porous nickel-zinc integrated negative electrode can inhibit the growth of zinc dendrites, and is consistent with the embodiment 1.
Example 3
(1) Preparing an alloy: the atomic content ratio of Ni, Cu and Zn is 20:10:70, Ni-Cu-Zn metal particles are smelted into alloy ingots by an electromagnetic induction smelting process, and then the alloy ingots are annealed for 1h at 800 ℃ to obtain homogeneous Ni-Cu-Zn alloy ingots;
(2) Wire cutting: preparing the alloy ingot in the step (1) into an alloy strip with the thickness of 60 mu m by a smelting and strip-spinning method;
(3) removing the alloy: placing the alloy sheet prepared in the step (2) in 2mol/L hydrochloric acid solution, dealloying at the temperature of 50 ℃, wherein the dealloying time is 0.5 hour, and then cleaning and drying;
(4) electrochemical testing: using nano porous nickel-copper-zinc alloy and commercially available zinc sheets as working electrodes, using commercially available zinc sheets with the same area as counter electrode and reference electrode, and measuring the working electrode area at 1mol L-1KOH and 20mmol L of-1Zn (CH) of3COO)2And (4) carrying out charge and discharge tests in the mixed electrolyte, and observing the formation and growth processes of dendrites.
The test result shows that the nano-porous nickel-copper-zinc integrated negative electrode can inhibit the growth of zinc dendrites, and is consistent with the embodiment 1.
Example 4
(1) Preparing an alloy: the atomic content ratio of Cu, Al and Zn is 20:20:60, Cu-Al-Zn metal particles are smelted into an alloy ingot by an electromagnetic induction smelting process, and then the alloy ingot is annealed at 500 ℃ for 1.5h to obtain a homogeneous Cu-Al-Zn alloy ingot;
(2) wire cutting: preparing the alloy ingot in the step (1) into an alloy sheet with the thickness of 1mm by a wire cutting method;
(3) removing alloy: placing the alloy sheet prepared in the step (2) in 0.5mol/L hydrochloric acid solution, dealloying at the temperature of 50 ℃, wherein the dealloying time is 10 hours, and then cleaning and drying;
(4) Electrochemical testing: the nano-porous copper-aluminum-zinc alloy and the commercially available zinc sheet are used as working electrodes, the commercially available zinc sheet with the same area is used as a counter electrode and a reference electrode, and the total volume of the working electrodes is 1mol L-1KOH and 20mmol L of-1Zn (CH) of3COO)2And (4) carrying out charge-discharge test in the mixed electrolyte, and observing the dendritic crystal formation and growth process.
The test result shows that the nano porous copper aluminum zinc integrated negative electrode can inhibit the growth of zinc dendrites, and is consistent with the embodiment 1.
The multi-element zinc-based alloy is directly prepared, and then the multi-element zinc-based alloy is dealloyed, so that the nano porous zinc-based alloy negative electrode is directly obtained; by dealloying, zinc can be loaded on the nano-porous metal substrate in situ; and (3) combining arc induction melting to carry out element doping on the nano porous zinc-based alloy negative electrode. Compared with the method in the prior art, the method of the invention has the advantages that the problem of dendritic growth of the zinc cathode can be inhibited because the zinc is directly loaded on the nano porous metal matrix in situ, thereby improving the stability of the nickel-zinc battery; and the selected metal element resources are rich, and the method for preparing the electrode by dealloying is simple and has lower cost.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A preparation method of a co-doped nano porous zinc-based alloy integrated negative electrode is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing an alloy: preparing a multi-element zinc-based alloy by adopting a melt casting method, wherein in the multi-element zinc-based alloy, the atomic ratio of Zn is 60-90%, the doping elements are one or more of Cu, Ni or Al, and the atomic ratio of the doping elements is 0-40%;
(2) processing the alloy ingot prepared in the step (1) to prepare an alloy strip or sheet with the thickness of 50 mu m-2 mm;
(3) preparing the alloy sheet prepared in the step (2) into a nano porous zinc-based alloy integrated negative electrode with the aperture of 50-300nm by adopting a chemical dealloying method;
(4) carrying out heat treatment on the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3), wherein the heat treatment process comprises the following steps: in the mixed atmosphere of argon and hydrogen, the proportion of hydrogen in the mixed gas is controlled to be 5-15%, the heating rate is 2-10 ℃/min, the heat treatment temperature is 150-500 ℃, the heat treatment time is 5-30min, and the co-doped nano porous zinc-based alloy integrated negative electrode is obtained after the heat treatment.
2. The preparation method of the co-doped nanoporous zinc-based alloy integrated negative electrode according to claim 1, wherein the preparation method comprises the following steps: the preparation method of the alloy ingot in the step (1) is to obtain a homogeneous multi-element zinc-based alloy ingot by utilizing electromagnetic induction melting, casting and uniform post-annealing processes, wherein the annealing temperature is controlled at 500-.
3. The preparation method of the co-doped nanoporous zinc-based alloy integrated negative electrode according to claim 1, wherein the preparation method comprises the following steps: the preparation and processing method in the step (2) is to utilize a smelting melt-spinning or linear cutting instrument to effectively control the size of the alloy to obtain an alloy strip or sheet with the thickness of 50 mu m-2 mm.
4. The preparation method of the co-doped nanoporous zinc-based alloy integrated negative electrode according to claim 1, wherein the preparation method comprises the following steps: the chemical dealloying method in the step (3) comprises the following specific steps: 0.05-10mol/L hydrochloric acid is used as corrosive liquid, the alloy sheet is subjected to dealloying treatment at the temperature of 20-80 ℃, the treatment time is 2-72 hours, and then the alloy sheet is cleaned and dried.
5. The preparation method of the co-doped nanoporous zinc-based alloy integrated negative electrode according to claim 1, characterized in that: the morphology of the nano-porous zinc-based alloy integrated negative electrode prepared in the step (3) is a nano-porous structure with the pore size distribution of 50-300 nm.
6. The co-doped nanoporous zinc-based alloy monolithic negative electrode manufactured according to the manufacturing method of any one of claims 1 to 5.
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| CN113745520A (en) * | 2021-09-05 | 2021-12-03 | 浙江大学 | Preparation method and application of zinc cathode material for inhibiting zinc dendrites |
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2022
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| CN106099086A (en) * | 2015-12-18 | 2016-11-09 | 华南理工大学 | Micro-nano Porous Cu zinc-aluminum shape memory alloy composite and preparation method and application |
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