CN113725419A - Al-Cu eutectic alloy electrode with lamellar structure, preparation method thereof and application thereof in water-based secondary aluminum ion battery - Google Patents
Al-Cu eutectic alloy electrode with lamellar structure, preparation method thereof and application thereof in water-based secondary aluminum ion battery Download PDFInfo
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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Abstract
The invention provides an Al-Cu eutectic alloy electrode with a lamellar structure, a preparation method thereof and application thereof in a water-based secondary aluminum ion battery, belonging to the technical field of electrode materials of the water-based secondary aluminum ion battery. The Al-Cu eutectic alloy electrode with laminated structure consists of one aluminum layer and one Al layer2Cu intermetallic compound layers are alternately arranged and stacked, wherein the aluminum layer has a thickness of 0.18 μm and Al2The thickness of the Cu intermetallic compound layer was 0.24 μm. The Al-Cu eutectic alloy electrode with the lamellar structure hasThe unique surface passivation film and the lamellar micro-galvanic couple structure ensure that the aluminum foil has higher conductivity, simultaneously maintains higher stability in the metal surface stripping and depositing process, and solves the problem of dendritic crystals which are easy to appear when the aluminum foil negative electrode influences long-term circulation.
Description
Technical Field
The invention belongs to the technical field of electrode materials of water-based secondary aluminum ion batteries, and particularly relates to preparation of an Al-Cu eutectic alloy electrode with a lamellar structure and application of the Al-Cu eutectic alloy electrode in a water-based secondary aluminum ion battery.
Background
Lithium ion batteries have dominated the world's commercial battery due to their higher energy density. However, the development of lithium ion batteries is limited by the limited resource reserves and high prices, and the safety problem of organic electrolytes is difficult to be solved completely. For this reason, interest in multivalent ion batteries such as aluminum ion batteries, zinc ion batteries, and magnesium ion batteries is increasing. These multivalent ions have higher charge loading, smaller ionic radius and lower deposition potential relative to lithium ions, and these multivalent batteries can use safer and better performing water as the electrolyte. Among these multivalent ions, the aluminum ion battery having the theoretically highest energy density naturally becomes the focus of attention.
Compared with commercial lithium ion batteries, the water system battery has the advantages of low raw material cost, safety, stability, environmental friendliness, low assembly environment requirement and the like. Commonly used positive electrode materials for aluminum ion batteries include manganese-based oxides, graphite, and prussian blue analogs, etc., and aluminum foil is generally used for the negative electrode. A great deal of research has been conducted on positive electrode materials for aluminum ion batteries, which can exhibit stable performance as a positive electrode for aluminum ion batteries, both in ionic liquid and water. However, the negative electrode of the aqueous secondary aluminum ion battery needs to be further studied. The aluminum foil cathode used by the traditional aluminum ion battery is easy to generate hydrogen evolution and passivation in aqueous solution, so that the battery is ineffective, and the development of the water-based secondary aluminum ion battery is greatly restricted. Also, aluminum foil cathodes can exhibit dendrite growth and severe self-discharge problems during long-term cycling.
Because the copper element in the aluminum alloy can effectively weaken the surface passivation layer, the stripping/electroplating process of the electrode can be promoted by participating in the formation of an intermetallic compound to form a galvanic couple with pure aluminum. During crystallization of the eutectic alloy, the later precipitated phase is precipitated by attaching to the surface of the leading phase, and a dual-phase core with a common growth interface of the two phases can be formed. And the two phases grow forwards together, and finally the lamellar tissue between the two phases can be formed. This provides the possibility of solving the problem of dendrites that the aluminum foil is very likely to appear in long-term circulation.
Disclosure of Invention
The invention aims to provide an Al-Cu eutectic alloy electrode with a lamellar structure, which consists of an aluminum layer and an Al layer2Cu intermetallic compound layers are alternately arranged and stacked, wherein the aluminum layer has a thickness of 0.18 μm and Al2The thickness of the Cu intermetallic compound layer was 0.24 μm.
The preparation method of the Al-Cu eutectic alloy electrode with the lamellar structure comprises the following specific steps:
1) determining the Al-Cu ratio (Al% is 66.8 wt%, Cu% is 33.2 wt%) according to the eutectic point, respectively weighing pure aluminum ingots and pure copper ingots, and removing surface oxide layers;
2) simultaneously putting the aluminum ingot and the copper ingot into a smelting furnace for deoxidization treatment;
3) and melting the metal ingot into a liquid state by heating, and preserving the heat for more than 1 min.
4) Cooling the liquid metal to room temperature in the mold by using circulating water, wherein the cooling speed is 100-300K/s;
5) and cutting the completely cooled metal block into sheets with the thickness of 200-300 mu m on a diamond wire cutting machine, and polishing off an oxide layer on the surface to prepare the Al-Cu eutectic alloy electrode with the lamellar structure, wherein the electrode can be used as the negative electrode of the water-based secondary aluminum ion battery.
Preferably, the heating temperature for melting the metal ingot into a liquid state by electric arc in the step 3) is 1700 ℃, and the temperature is kept for 2 min.
The cooling rate in the step 3) by circulating water cooling is 300K/s.
The invention has the beneficial effects that:
the preparation method of the material is simple, and a novel negative electrode material thought is provided for the water-based secondary aluminum ion battery. The Al-Cu eutectic alloy electrode with the lamellar structure provided by the invention has the unique surface passivation film and lamellar micro-galvanic couple structure, so that the Al-Cu eutectic alloy electrode has higher conductivity and maintains higher stability in the metal surface stripping and depositing process. Compared with a pure aluminum metal cathode, a symmetrical battery and a water-based secondary aluminum ion full battery which are prepared by using the laminar eutectic alloy electrode have higher electrochemical activity and structural stability.
Drawings
FIG. 1 is a laser confocal picture of an Al-Cu eutectic alloy electrode with a lamellar structure;
FIG. 2 is a field emission electron microscope (FESEM) picture of an Al-Cu eutectic alloy electrode having a lamellar structure;
FIG. 3 is an XRD spectrum of an Al-Cu eutectic alloy electrode with a lamellar structure; .
FIG. 4, EDS spectra of Al-Cu eutectic alloy electrodes with lamellar structure; .
FIG. 5 is HR-TEM pictures of Al-Cu eutectic alloy electrodes with lamellar structures.
FIG. 6 is a schematic diagram of the reaction of Al-Cu eutectic alloy electrodes with lamellar structures.
FIG. 7A symmetrical cell with standard Al-Cu eutectic alloy electrode composition with lamellar structure at 0.5mA cm-2Current density 2000h constant current charge and discharge test (Voltage-time curve)
FIG. 8 shows the Electrochemical Impedance (EIS) of a symmetrical cell based on the Al-Cu eutectic alloy electrode composition with a lamellar structure.
FIG. 9 Al-Cu eutectic alloy electrode with lamellar Structure and Al0.14MnO2Performing Cyclic Voltammetry (CV) test on a water-based secondary aluminum ion full cell with standard nanosheet composition at 0.1mV s-1;
FIG. 10 shows an Al-Cu eutectic alloy electrode having a lamellar structure and Al0.14MnO2The nano sheets form a standard aqueous secondary aluminum ion full cell, and Electrochemical Impedance (EIS) is carried out in a frequency range of 100kHz to 10 mHz;
FIG. 11 shows an Al-Cu eutectic alloy electrode having a lamellar structure and Al0.14MnO2The standard aqueous secondary aluminum ion full cell composed of nano sheets is 0.5A g-1Current density of (A) was subjected to a cyclic test
FIG. 12 shows an Al-Cu eutectic alloy electrode having a lamellar structure and Al0.14MnO2The standard aqueous secondary aluminum ion full cell composed of nano sheets is 0.5Ag-1Current density of (c) and stability test after 100 cycles.
Detailed Description
The technical solution of the present invention is further explained and illustrated below by way of specific examples.
Example 1
The preparation process and steps in this example are as follows:
A. 15g of pure aluminum block (Al, purity 99.994%) and 7.46g of pure copper block (Cu, purity 99.996%) were weighed out, and the surface oxide layer was removed.
B. Putting the two metals into a smelting furnace together for deoxidization treatment.
C. Heating to 1700 deg.C and keeping the temperature for 2min to ensure the metal is completely melted and mixed uniformly.
D. And rapidly cooling the high-temperature liquid metal to room temperature at the speed of 300K/s in the mould by using circulating water.
E. And cutting the completely cooled metal block into sheets with the thickness of 200-300 mu m on a diamond wire cutting machine, and polishing off the oxide layer on the surface.
Example 2
A. 668g of pure aluminum block (Al, purity 99.994%) and 332g of pure copper block (Cu, purity 99.996%) were weighed, and the surface oxide layer was removed.
B. The two metals are put into a smelting furnace together for deoxidization treatment.
C. Heating to 1150 deg.C and holding for 2h to ensure complete melting of the metal and uniform mixing.
D. And rapidly cooling the high-temperature liquid metal to room temperature at the speed of 100K/s in the mould by using circulating water.
E. And cutting the completely cooled metal block into sheets with the thickness of 200-300 mu m on a diamond wire cutting machine, and polishing off the oxide layer on the surface.
The lamella thickness of the high-temperature liquid metal at the cooling speed of 300K/s is distributed between 0.35 and 0.5 mu m and is concentrated near 0.42 mu m through verification of a laser confocal microscope.
Morphology and structural characterization of materials
Through laser Confocal (CLSM) characterization, an Al-Cu alloy sample obtained by smelting shows a lamellar structure as shown in figure 1, and the Al-Cu alloy sample is also proved to be a lamellar structure by combining a Field Emission Scanning Electron Microscope (FESEM) as shown in figure 2. The more visual test of the energy spectrum of the field emission scanning electron microscope proves that the alloy sample obtained by the invention is an aluminum layer and an Al layer2Cu layers are alternately arranged and stacked, wherein the thickness of the aluminum layer is-0.18 mu m, and Al2The thickness of the Cu layer was 0.24. mu.m. .
FIG. 3 is an XRD spectrum of a lamellar Al-Cu alloy sample, which proves that eutectic phenomenon of Al-Cu alloy exists only in pure aluminum phase and Al2A Cu metal compound phase. Figure 4 is an EDS spectrum of a sheet alloy sample,
the chemical compositions determined are shown in the following table,
this result demonstrates that the chemical composition of the lamellar alloy sample is Al82Cu18Combined with the phase diagram of Al-Cu binary alloyIt is clear that the lamellar Al-Cu alloy samples are at the eutectic point.
HR-TEM pictures of the lamellar Al-Cu alloy samples of FIG. 5 show Al lattice spacing of 0.234nm, respectively, corresponding to
Crystal face of Al2Cu lattice spacing of 0.303nm, corresponding to Al2The Cu (200) crystal plane.
Characterization of electrochemical Properties of the Material
The Al-Cu eutectic alloy electrode with lamellar structure prepared in example 1 was sliced into 200-300 μm thick slices on a diamond wire cutting machine, and the oxide layer on the surface was polished off. Then the Al-Cu eutectic alloy electrode slice with a lamellar structure is used as a working electrode, and 2mol L of the working electrode-1Al (OTF)3The solution is used as electrolyte to form a standard symmetrical battery for electrochemical test;
the Al-Cu eutectic alloy electrode symmetrical cell with a lamellar structure prepared in example 1 was charged at 0.5mA cm-2Current Density 2000h constant Current Charge/discharge test (Voltage-time Curve)
An Al-Cu eutectic alloy symmetrical battery with a lamellar structure prepared in example 1 is subjected to an Electrochemical Impedance Spectroscopy (EIS) test in a frequency range of 100kHz to 10 mHz;
the Al-Cu eutectic alloy electrode with a lamellar structure prepared in example 1 was used as a battery negative electrode, and Al0.14MnO22mol L of nanosheet as the positive electrode of the battery-1Al (OTF)3And 0.2mol L-1Mn(OTF)2The solution is used as electrolyte, and the electrochemical test is carried out on the water-based secondary aluminum ion full cell with standard composition
The Al-Cu eutectic alloy electrode having a lamellar structure prepared in example 1 was combined with Al0.14MnO2Placing a standard aqueous secondary aluminum ion full cell consisting of nanosheets in 0.1mV s-1Performing Cyclic Voltammetry (CV) testing at a scan rate of (a);
the Al-Cu eutectic alloy electrode having a lamellar structure prepared in example 1 was combined with Al0.14MnO2Performing Electrochemical Impedance Spectroscopy (EIS) on a water-based secondary aluminum ion full cell with standard nanosheet composition in a frequency range of 100kHz to 10 mHz;
the Al-Cu eutectic alloy electrode having a lamellar structure prepared in example 1 was combined with Al0.14MnO2The water-based secondary aluminum ion full cell with standard nanosheet composition is placed in a 0.5A g-1A 400-cycle stability test was performed at the current density of (a).
As can be seen from the results of the symmetrical cell in FIG. 7, the Al-Cu eutectic alloy electrode with the lamellar structure of the symmetrical cell is 0.5mA cm-2Can be tested for over 2000h without significant voltage hysteresis. In contrast, pure aluminum symmetrical cells quickly experienced severe voltage hysteresis just before the start of the test. Fig. 8 is an impedance comparison between a pure aluminum symmetrical cell and an Al-Cu eutectic alloy electrode symmetrical cell with a lamellar structure, the charge transfer resistance of the Al-Cu eutectic alloy electrode symmetrical cell with the lamellar structure is about 144 Ω, and in contrast, the charge transfer resistance of the pure aluminum symmetrical cell is about 3814 Ω, demonstrating that the Al-Cu eutectic alloy electrode with the lamellar structure has a stronger electrochemical activity than pure aluminum foil. FIG. 9 shows an Al-Cu eutectic alloy electrode pool with Al layer layered structure0.14MnO2The aqueous secondary aluminum ion battery composed of the nano sheets is at 0.1mV s in a voltage range of 0.5-1.9V-1The sweep rate of (a) was obtained. The reduction peak of the cell redox curve occurred at 1.5V and the oxidation peak at 1.61V. FIG. 10 shows an Al-Cu eutectic alloy electrode with a lamellar structure with Al in the frequency range of 100kHz to 10mHz0.14MnO2Comparing the aqueous secondary aluminum ions formed by the nanosheets with the Electrochemical Impedance (EIS) of the pure aluminum foil, the graph shows that the charge transfer resistance of the eutectic alloy sample in the full cell is only 72 omega, and the charge transfer resistance of the pure aluminum foil sample is about 1708 omega. The small charge transfer resistance and the polarization degree together indicate that the alloy sample full cell has excellent electrochemical activity. FIG. 11 shows an Al-Cu eutectic alloy electrode and a pure aluminum electrode with Al having a lamellar structure0.14MnO2The standard aqueous secondary aluminum ion full cell composed of nano sheets is 0.5A g-1The circulation curve of the current density of (A) is shown in the figure, and the Al-Cu eutectic alloy electrode with a lamellar structure is combined with Al0.14MnO2After the nano sheets form the water-based secondary aluminum ion battery, the temperature is 0.5A g-1The current density of the alloy can still keep 327mAh g after circulating for 400 circles-1The specific capacity of (A). In sharp contrast, the pure aluminum sheet electrode assembled aqueous secondary aluminum ion battery basically failed after only 80 cycles, leaving only 16mAh g-1The specific capacity of (A). This fully demonstrates the unique advantage of alloy electrodes in terms of structural stability. FIG. 12 shows an Al-Cu eutectic alloy electrode having a lamellar structure and Al0.14MnO2The standard aqueous secondary aluminum ion full cell composed of nano sheets is 0.5A g-1Current density of (a) and charge-discharge curve after circulating for 400 cycles. As can be seen, the battery is at 0.5A g-1The initial charge-discharge process can be basically maintained after the current passes through the 400-cycle circuit and only undergoes small attenuation. This proves that the Al — Cu eutectic alloy electrode having a lamellar structure has better structural stability. The alloy electrode can be used as a cathode of a water-based secondary aluminum ion battery, and has good application prospect in the field of water-based secondary batteries. The method can be expanded to other energy storage battery systems, and provides a new method and idea for improving the electrochemical activity and the structural stability of the metal electrode.
Claims (5)
1. The Al-Cu eutectic alloy electrode with the lamellar structure is characterized by comprising an aluminum layer and an Al layer2Cu layers are alternately arranged and stacked, wherein the thickness of the aluminum layer is 0.18 μm, and Al is2The thickness of the Cu layer was 0.24 μm, and the entire electrode was a 200-300 μm thick sheet.
2. The method 1 for preparing the Al-Cu eutectic alloy electrode with the lamellar structure according to claim 1 comprises the following steps:
1) respectively weighing pure aluminum ingots and pure copper ingots according to the proportion that Al% is 66.8 wt% and Cu% is 33.2 wt%, and removing surface oxide layers;
2) putting the two metals into a smelting furnace together for deoxidization treatment;
3) heating to 1150 deg.C to completely melt the metal, and keeping the temperature for 1 min;
4) cooling the high-temperature liquid metal to room temperature in the mold by using circulating water, wherein the cooling speed is 100-300K/s;
5) and cutting the completely cooled metal block into sheets with the thickness of 200-300 mu m on a diamond wire cutting machine, and polishing off the oxide layer on the surface.
3. The method for preparing an Al-Cu eutectic alloy electrode with a lamellar structure according to claim 1, characterized in that the heating temperature by melting the ingot into a liquid state in step 3) is 1700 ℃, and the temperature is maintained for 2 min.
4. The method for producing an Al — Cu eutectic alloy electrode with a lamellar structure according to claim 1, characterized in that the cooling rate in step 3) of claim 2 is 300K/s.
5. Use of the Al-Cu eutectic alloy electrode having a lamellar structure according to claim 1 as a negative electrode of an aqueous aluminum ion battery.
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