CN109713369B - Low-cost aluminum-based electrolyte and application of low-cost aluminum-based electrolyte to aluminum battery - Google Patents
Low-cost aluminum-based electrolyte and application of low-cost aluminum-based electrolyte to aluminum battery Download PDFInfo
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Abstract
Low-cost aluminum-containing electrolyte and aluminum battery thereofApplication, which belongs to the technical field of electrochemical energy storage. The electrolyte is an ionic liquid formed by aluminum halide-A, preferably aluminum chloride, amide compound, preferably acetamide, and certain amount of additive, wherein the additive comprises aluminum halide-B (when the additive is aluminum halide-B, the extract of aluminum halide-B is different from aluminum halide-A), bis (trifluoromethane) sulfonyl imide aluminum (Al (TFSI))3) Sodium bis (trifluoromethanesulfonylimide) (Na (TFSI)), magnesium bis (trifluoromethanesulfonylimide) (Mg (TFSI))2) Bis (trifluoromethanesulfonyl) imide zinc (Zn (TFSI)2) Aluminum perchlorate (Al (ClO)4)3) Chloroaluminate, bromoaluminate, urea, aluminum triflate (Al (OTF))3) One or more of benzene, toluene, chlorobenzene, 1,2, 2-tetrafluoroethyl 2,2,3, 3-tetrafluoropropyl ether (HFE) can be used in the fields of aluminum ion batteries, aluminum-sulfur batteries and the like. The aluminum-sulfur battery assembled by the electrolyte provided by the invention has high capacity, good cycling stability and excellent rate capability. Meanwhile, the aluminum-sulfur battery is low in cost, does not contain high-pollution substances such as heavy metals and the like, is easy to assemble, is high in safety, and has a good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of electrolyte, and particularly relates to preparation of a novel low-cost aluminum-based electrolyte and application of the electrolyte in an aluminum battery, particularly an aluminum-sulfur battery.
Background
With the increasing demand of the modern society for high-efficiency energy storage equipment, lithium ion batteries based on lithium resources are increasingly restricted by the aspects of resource shortage, high cost and the like, and are difficult to meet future large-scale application. With the continuous and deep research on secondary batteries based on new materials, new structures and new systems, a variety of new battery systems based on multi-electron reaction are reported in succession, and it is expected to manufacture low-cost secondary batteries with higher energy density and power density. Aluminum, the highest metal content in the earth's crust, is considered to be an attractive metal due to its light weight, low cost, high safety, and other advantagesA cathode material, and aluminum can provide 3 electrons for electrochemical reaction, thereby having ultra-high theoretical volume capacity (8046mAh cm)–3) Far higher than the theoretical volume capacity (2062mAh cm) of lithium ion battery–3). In conclusion, the aluminum ion battery has the development potential due to the advantages of high capacity, low cost, high safety, abundant resources and the like, and the development of the aluminum ion battery technology has important significance for the development of power generation chemical energy storage devices.
Sulfur is a kind of material with high earth-crust content, low cost and high theoretical specific capacity (1675mAh g)-1) The substance (2) has attracted considerable attention as a positive electrode material for nonaqueous metal-sulfur batteries. The theoretical energy density of the aluminum-sulfur battery taking sulfur as the battery anode reaches 1300 Wh/kg–1. Therefore, the aluminum-sulfur battery is expected to become a battery with low cost, high safety and high energy density, which meets the requirements of modern electronic products, electric vehicles and power grids.
The development of the electrolyte is one of the key points of the development of the aluminum ion battery and the aluminum-sulfur battery. At present, the reported electrolyte of the aluminum-sulfur battery is based on room-temperature ionic liquid obtained by aluminum chloride and halogenated imidazole according to a certain proportion, but the cost of the ionic liquid is high, and the cycle stability, the capacity and the coulombic efficiency of the assembled aluminum-sulfur battery can not meet the actual requirements. Therefore, the development of the electrolyte of the aluminum ion battery and the aluminum-sulfur battery, which has good electrochemical performance and lower cost, has important scientific research and application values.
Disclosure of Invention
The invention provides a novel low-cost electrolyte and application of the electrolyte in aluminum-sulfur batteries, aluminum ion batteries and aluminum electrodeposition, aiming at overcoming the defects of high production cost, poor cycle life and low coulombic efficiency of the conventional electrolyte of aluminum-ion batteries, particularly aluminum-sulfur batteries.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides an electrolyte, which contains aluminum halide-A, an amide compound and an additive, wherein the aluminum halide-A is selected from the following components: one or more of aluminum fluoride, aluminum chloride, aluminum bromide and aluminum iodide, preferably AlCl3(ii) a The amide group compoundSelected from: one or more of acetamide, propionamide, butyramide, N-methylacetamide, N-dimethylacetamide, preferably acetamide; the additive is selected from: aluminum halide-B, bis (trifluoromethanesulfonylimide) aluminum (Al (TFSI)3) Sodium bis (trifluoromethanesulfonylimide) (Na (TFSI)), magnesium bis (trifluoromethanesulfonylimide) (Mg (TFSI))2) Bis (trifluoromethanesulfonyl) imide zinc (Zn (TFSI)2) Aluminum perchlorate (Al (ClO)4)3) Chloroaluminate, bromoaluminate, urea, aluminum triflate (Al (OTF))3) One or more of benzene, toluene, chlorobenzene, 1,2, 2-tetrafluoroethyl 2,2,3, 3-tetrafluoropropyl ether (HFE); the aluminum halide-B is selected from: when the additive is aluminum halide-B, the aluminum halide-B is taken out of the aluminum halide-A.
The molar ratio of the aluminum halide-A to the amide compound in the electrolyte is 1.0-2.0, preferably 1.2-1.5, the total mass of the additives is 0-50% of the total mass of the electrolyte, and the preferable ranges are different for different additives.
The electrolyte is prepared by the following steps: under the protection of inert atmosphere, adding the aluminum halide-A into the amide compound, continuously stirring, and after complete liquefaction, adding the additive and continuously stirring. The preferred scheme is as follows: slowly adding aluminum halide into the amide compound in a glove box (containing oxygen and water in an amount of less than 0.1ppm) under the protection of argon at room temperature, uniformly stirring and dissolving for 2-24h, adding the additive after complete liquefaction, and continuously stirring and dissolving for 2-24h to obtain a clear and transparent solution.
The invention also provides an aluminum-sulfur battery using the novel low-cost electrolyte, which comprises a positive electrode, a negative electrode and the electrolyte;
the positive electrode material of the aluminum-sulfur battery according to the present invention is various composite materials containing sulfur as an active material. For example, the positive electrode may be a composite of elemental sulfur or a compound of sulfur and a carbon material. When the elemental sulfur or the sulfur compound is compounded with the carbon material, the mass percentage of the sulfur is 10-90%.
The carbon material includes, but is not limited to, mesoporous carbon, activated carbon, carbon nanotubes, graphene assemblies, carbon micro/nanospheres, carbon nanohorns, carbon fibers; compounds of sulfur include, but are not limited to, aluminum sulfide, selenium sulfide, tellurium sulfide, organic sulfides.
According to the invention, the cathode of the aluminum-sulfur battery can be at least one of various aluminum-containing products, such as aluminum foil, foamed aluminum, porous aluminum, aluminum-containing alloy and aluminum-containing composite materials, the aluminum cathode comprises an aluminum product with an oxide layer covered on the surface, and the thickness of the cathode is 0.01-2 mm.
According to the present invention, the aluminum negative electrode is washed, dried, and subjected to various pretreatment processes according to different negative electrodes before use.
The electrolyte of the invention, an aluminum-sulfur battery filled with the electrolyte of amide compound and aluminum halide can carry out stable charge-discharge reaction, the capacity of the aluminum-sulfur battery is high, the cycling stability is good, the coulombic efficiency is high, in addition, the cost of the electrolyte is low, the potential window is wide, and the melting temperature range is wide.
The aluminum-sulfur battery assembled by the electrolyte provided by the invention has high capacity and good cycling stability, and meanwhile, the aluminum-sulfur battery has low production cost and good industrial application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a graph showing the cycle performance of an aluminum-sulfur battery according to example 1 of the present invention;
FIG. 2 is a charge-discharge curve of an aluminum-sulfur battery according to example 10 of the present invention.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any numerical values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass data approximating such ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Example 1
1.3 times the amount of substance equivalent of AlCl in an argon glove box at room temperature3Slowly adding into acetamide, magnetically stirring for 12h to obtain clear and transparent brown yellow liquid, and standing to serve as electrolyte.
Taking the solution as an electrolyte, taking S @ mesoporous carbon (CMK-3 type) with the sulfur content of 50% as a positive electrode composite material, mixing and grinding the composite material, a conductive agent Super P and a binder PTFE according to the ratio of 8:1:1 to manufacture a positive electrode pole piece, pressing the pole piece onto a positive electrode current collector molybdenum net to be used as a positive electrode, taking a washed and dried aluminum sheet with certain thickness and purity as a negative electrode, assembling a Whatman GF/A glass fiber diaphragm in an argon glove box to form a battery with an agenlok configuration, and then transferring out of the glove box. The cells were subjected to cyclic voltammetry tests on a Solartron electrochemical workstation. The battery was subjected to constant current charge and discharge test on a LAND battery tester with a cut-off voltage of 0.05-1.8V and a charge and discharge current of 100mA, and the results are shown in FIG. 1.
Example 2
The procedure is as in example 1, except that AlCl is added3Slowly adding the mixed solution into acetamide according to the mol ratio of 1.2:1, and standing the mixed solution after the mixed solution is completely dissolved to be used as an electrolyte.
The pole piece fabrication and cell assembly processes were the same as in example 1. Performing cyclic voltammetry test on a Solartron electrochemical workstation, performing constant current charge and discharge test on a LAND tester, wherein the cut-off voltage is 0.05-1.8V, and the charge and discharge current is 100mA, and the result shows that the first-circle discharge specific capacity reaches 1250 mAh.g–1And the specific capacity after 20 cycles of circulation is 777mAh g–1。
Example 3
According toExample 1 except that 2% by mass of Al (OTF) was added to the resulting clear, transparent, orange-yellow solution3And continuously stirring as an additive, and standing for use as an electrolyte after the additive is completely dissolved.
The room temperature eutectic liquid is used as electrolyte, and the pole piece manufacturing and battery assembling processes are the same as those in example 1. And performing constant current charge and discharge test on the LAND tester with cutoff voltage of 0.05-1.8V and charge and discharge current of 100mA, and the result shows that Al (OTF) is added3The coulombic efficiency increased after being used as an additive, and the coulombic efficiency increased from 84% to 90%.
Example 4
The procedure of example 1 was followed except that 10% toluene as an additive was added to the resulting clear and transparent orange-yellow solution, followed by stirring and, after complete dissolution, the solution was left to stand for use as an electrolyte.
The room temperature eutectic liquid is used as electrolyte, and the pole piece manufacturing and battery assembling processes are the same as those in example 1. And performing constant current charge and discharge test on the LAND tester with cutoff voltage of 0.05-1.8V, charge and discharge current of 100mA, first-loop discharge specific capacity of 1275 mAh.g–1。
Example 5
AlCl was prepared according to the method of example 13The electrolyte with the molar ratio of 1.3:1 to acetamide and S @ CMK-3 with the sulfur content of 50 percent are used as a positive electrode composite material, the manufacturing process of a positive electrode piece is the same as that in example 1, except that a negative electrode adopts three-dimensional foamed aluminum which is subjected to a series of pretreatment such as washing, drying and tabletting under different pressures, and the assembly process of other batteries is the same as that in example 1. And constant current charge and discharge tests are carried out on the LAND tester, and the three-dimensional porous structure of the foamed aluminum provides a space for deposition and dissolution of aluminum, so that the foamed aluminum is used as an aluminum electrical cathode, and the rate capability is improved.
Example 6
Adding AlCl at room temperature under argon atmosphere3Slowly adding the mixture into acetamide according to the mol ratio of 1.3:1, magnetically stirring for 12 hours to obtain clear and transparent orange-yellow liquid, and standing the liquid for use as electrolyte for aluminum electrodeposition.
The room temperature eutectic liquid is used as electrolyte, the electro-deposition matrix is copper, the copper foil is used as a positive electrode, the aluminum foil is used as a negative electrode, the system is positioned in a sealed electrolytic cell, the deposition time is 120min, and the current density is 3 mA-cm–2And taking out the deposited copper foil in an argon atmosphere, cleaning the copper foil with acetonitrile, drying, sealing and storing, and carrying out scanning electron microscope analysis, wherein the thickness of an aluminum deposition layer changes along with the deposition time, and the thickness of the deposition layer is about 5-10 mu m under the test time of 120 min.
Example 7
The procedure is as in example 1, except that 1.3 times the amount of substance equivalent of AlCl is used3Slowly adding the mixture into acetamide-based compound propionamide, magnetically stirring for 12 hours to obtain clear and transparent brown yellow liquid, and standing the liquid to be used as electrolyte.
Vanadium pentoxide (V) synthesized by hydrothermal method by using the solution as electrolyte2O5) The positive electrode active material is prepared by mixing and grinding the active material, conductive agent acetylene black and adhesive PVDF according to the mass ratio of 7:2:1, a positive electrode pole piece is prepared, the pole piece is coated on a current collector tantalum foil to be used as a positive electrode, a washed and dried aluminum sheet with certain thickness and purity is used as a negative electrode, a Whatman GF/A glass fiber diaphragm is assembled into an aluminum ion battery with a Swagelok configuration in an argon glove box, and then the battery is transferred out of the glove box. Cyclic voltammetry tests were performed on a Solartron electrochemical workstation and constant current charge and discharge tests were performed on a LAND battery tester.
Example 8
According to the method of example 1, 1.3 times the amount of substance equivalent of AlCl3Slowly adding into acetamide, magnetically stirring for 6 hr to obtain clear and transparent brown yellow liquid, and standing to obtain electrolyte.
Using the solution as electrolyte, and synthesizing layered molybdenum disulfide (MoS) by a hydrothermal method2) Directly attached to carbon fiber cloth to form self-supporting electrode material, using the electrode material as positive electrode, using washed and dried aluminum sheet with certain thickness and purity as negative electrode, and assembling Whatman GF/A glass fiber diaphragm in argon glove boxAn aluminum ion battery in the Swagelok configuration, and then transferred out of the glove box. Cyclic voltammetry tests were performed on a Solartron electrochemical workstation and constant current charge and discharge tests were performed on a LAND battery tester.
Example 9
According to the method of example 1, 1.3 times the amount of substance equivalent of AlCl3Slowly adding into acetamide, magnetically stirring for 6 hr to obtain clear and transparent brown yellow liquid, and standing to obtain electrolyte.
With the solution as an electrolyte, functional conductive fibers are arranged in a deionized water/ethanol/sulfur/carbon disulfide system, and a hydrothermal reaction is carried out at 180 ℃ for 24 hours to obtain a carbon fiber cloth sulfur particle-loaded composite material as a positive electrode, and the negative electrode and a diaphragm are prepared into the Swagelok battery in the same way as in example 1. Cyclic voltammetry tests were performed on a Solartron electrochemical workstation and constant current charge and discharge tests were performed on a LAND battery tester.
Example 10
According to the method of the embodiment 1, NaTFSI with the mass fraction of 1% is added into the obtained clear and transparent orange solution to be used as an additive to be continuously stirred, and after the NaTFSI is completely dissolved, the solution is kept still to be used as an electrolyte.
The solution was used as an electrolyte, graphite paper was used as a positive electrode, and the negative electrode and a separator were used in the same manner as in example 1 to fabricate a Swagelok double-cation battery. The cyclic voltammetry test is carried out on a Solartron electrochemical workstation, the constant current charge and discharge test is carried out on a LAND battery tester, the cut-off voltage is 0.05-1.8V, the charge and discharge current is 100mA, the charge and discharge curve is shown in figure 2, and the result shows that after NaTFSI is added, the discharge platform is increased from 0.6V to 0.7-0.8V, and the energy density of the battery is improved.
Example 11
To the resulting clear, transparent, orange-yellow solution was added 1% Mg (TFSI) as in example 12And continuously stirring as an additive, and standing for use as an electrolyte after the additive is completely dissolved.
The solution was used as an electrolyte, graphite paper was used as a positive electrode, and the negative electrode and a separator were used in the same manner as in example 1 to fabricate a Swagelok double-cation battery. In thatPerforming cyclic voltammetry test on a Solartron electrochemical workstation and constant current charge and discharge test on a LAND battery tester, wherein the cut-off voltage is 0.05-1.8V, the charge and discharge current is 100mA, and the first-circle discharge capacity is 1200 mAh.g–1The capacity after 20 cycles of circulation is 700mAh g–1。
Claims (11)
1. An electrolyte comprising an aluminum halide-a, an amide homolog, and an additive, wherein the aluminum halide-a is selected from the group consisting of: one or more of aluminum fluoride, aluminum chloride, aluminum bromide and aluminum iodide; the amide homologs are selected from: one or more of acetamide, propionamide, butyramide, N-methylacetamide, N-dimethylacetamide and the like; the molar ratio of the aluminum halide-A to the amide compound in the electrolyte is 1.0-2.0; the additive is selected from: aluminum halide-B, bis (trifluoromethanesulfonylimide) aluminum (Al (TFSI)3) Sodium bis (trifluoromethanesulfonylimide) (Na (TFSI)), magnesium bis (trifluoromethanesulfonylimide) (Mg (TFSI))2) Bis (trifluoromethanesulfonyl) imide zinc (Zn (TFSI)2) Aluminum perchlorate (Al (ClO)4)3) Chloroaluminate, bromoaluminate, urea, aluminum triflate (Al (OTF))3) One or more of benzene, toluene, chlorobenzene, 1,2, 2-tetrafluoroethyl 2,2,3, 3-tetrafluoropropyl ether (HFE); the aluminum halide-B is selected from: when the additive is aluminum halide-B, the aluminum halide-B is taken out of the aluminum halide-A; the total mass of the additive is 0-20% of the total mass of the electrolyte.
2. The electrolyte of claim 1, wherein the additive is sodium bistrifluoromethanesulfonylimide (na (tfsi)), and wherein the total mass of the additive is 1% of the total mass of the electrolyte.
3. The electrolyte of claim 1, wherein said additive is magnesium bistrifluoromethanesulfonylimide (Mg (TFSI)2) The total mass of the additive is 1% of the total mass of the electrolyte.
4. The electrolyte as claimed in claim 1, wherein the additive is aluminum triflate (Al (OTF))3) The total mass of the additive is 2% of the total mass of the electrolyte.
5. An electrolyte as claimed in claim 1, wherein the additive is toluene and the total mass of the additive is 10% of the total mass of the electrolyte.
6. The method for preparing the electrolyte according to claim 1, wherein the aluminum halide-A is slowly added to the amide compound under the protection of inert atmosphere, and is uniformly stirred and dissolved for 2 to 24 hours, and after the aluminum halide-A is completely liquefied, the additive is added and is continuously stirred and dissolved for 2 to 24 hours.
7. Use of the electrolyte according to claim 1 in an aluminium-sulphur battery.
8. An aluminum-sulfur battery based on the electrolyte of claim 1, wherein the aluminum-sulfur battery comprises a positive electrode, a negative electrode and the electrolyte.
9. The aluminum-sulfur battery according to claim 8, wherein the positive electrode is a composite material of elemental sulfur or a compound of sulfur and a carbon material; when the sulfur simple substance or the sulfur compound is compounded with the carbon material, the mass percentage of the sulfur is 10-90%.
10. The aluminum-sulfur battery of claim 9, wherein the carbon material comprises one or more of mesoporous carbon, activated carbon, carbon nanotubes, graphene assemblies, carbon micro/nano spheres, carbon nanohorns, and carbon fibers; the sulfur compound comprises one or more of aluminum sulfide, selenium sulfide, tellurium sulfide and organic sulfide.
11. The aluminum-sulfur battery as recited in claim 8, wherein the negative electrode of the aluminum-sulfur battery is at least one of aluminum foil, foamed aluminum, porous aluminum, aluminum-containing alloy, and aluminum-containing composite material, the aluminum negative electrode comprises an aluminum product covered with an oxide layer, and the thickness of the negative electrode is 0.01 to 2 mm.
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| CN110683977B (en) * | 2019-09-10 | 2021-04-16 | 山东大学 | Aluminum ion battery electrolyte, preparation method and application |
| CN112002937A (en) * | 2020-08-07 | 2020-11-27 | 山东科技大学 | Gel electrolyte for aluminum ion battery and preparation method and application thereof |
| CN112768775A (en) * | 2021-02-25 | 2021-05-07 | 中国科学院宁波材料技术与工程研究所 | Non-aqueous aluminum ion electrolyte and secondary battery |
| CN113097565A (en) * | 2021-03-29 | 2021-07-09 | 北京理工大学 | Ionic liquid-like electrolyte for aluminum secondary battery and preparation method thereof |
| CN114628787B (en) * | 2022-03-28 | 2024-04-05 | 宁德新能源科技有限公司 | Electrolyte, electrochemical device, and electronic device |
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