CN109360986B - Application of zinc selenide as anode material of aluminum ion battery - Google Patents
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- CN109360986B CN109360986B CN201811139119.1A CN201811139119A CN109360986B CN 109360986 B CN109360986 B CN 109360986B CN 201811139119 A CN201811139119 A CN 201811139119A CN 109360986 B CN109360986 B CN 109360986B
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to application of zinc selenide as an aluminum ion battery anode material, and belongs to the technical field of aluminum ion batteries. The zinc selenide is used as the anode material of the aluminum ion battery, so that the aluminum ion battery has a high discharge platform and a large specific capacity, wherein the discharge voltage platform is about 1.8V, and the first-loop specific capacity is about 164mAh/g under the current density of 200mA/g, so that the aluminum ion battery can be better applied to various fields, such as the electronic industry, the communication industry, electric automobiles and the like. Meanwhile, the preparation process of the zinc selenide is simple, the raw material source is wide, the cost is low, and the preparation method is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of aluminum ion batteries, and particularly relates to application of zinc selenide as an aluminum ion battery anode material.
Background
Aluminum ion batteries have many advantages and are receiving much attention compared to lithium ion batteries which are now widely used, such as that aluminum ion batteries can transfer three electrons in one redox reaction, thereby providing very high volumetric and mass energy densities. In addition, because aluminum is the most abundant metal element in the earth crust, the cost of the aluminum ion battery can be greatly reduced by taking the aluminum as a raw material, and the aluminum ion electrode material and the electrolyte used are not easy to combust, the aluminum ion battery has good safety.
Currently, a series of materials such as carbon-based materials, transition metal oxides/transition metal sulfides/transition metal selenides, and the like are used as positive electrode materials of aluminum ion batteries. However, there are disadvantages in using these materials as a positive electrode material for aluminum ion batteries. Such as graphite material, although it has a discharge voltage plateau as high as 2.0V, but its specific capacity is relatively low, and Dai et al, using graphite foam as the anode material of aluminum ion battery, shows extremely high cycle stability and high discharge voltage plateau, but the capacity of the battery assembled by the anode material is low, only 60mAh g-1(see Meng-Chang Lin, Ming Gong, Binganlu, Yingpeng Wu, Diyan Wang,Mingyun Guan,Michael Angell,Changxin Chen,JiangYang,Bing-Joe Hwang,Hongjie Dai.An ultrafast rechargeable aluminium-ionbattery[J]Nature,2015,520: 324-328). While metal sulfides/oxides/selenides, etc. have high specific capacities, their discharge voltage platforms are very low, usually below 1.0V (see Xuefeng Zhang, GuohuaZhang, Shuai Wang, Shijie Li and Shuqiang jiao. porous CuO microspirarchitectures as high performance catalyst materials for aluminum-materials [ J]Journal of Materials Chemistry A,2018,6, 3084-. Some metal sulfides/oxides/selenides have higher discharge voltage platforms, but the used positive electrode materials contain cobalt elements which are very expensive and have less and less reserves (see Tonghui Cai, Lianming Zhao, Haoyu Hu, Yanpeng Li, qingzhong xue, Wei Xing, Zifeng Yan, Lianzhou wang2/Carbon Nanodice@ReducedGraphene Oxide Composites for High-performance Rechargeable Aluminum-ionBatteries[J].Energy&Environmental Science,doi:10.1039/C8EE00822A)。
Zinc selenide can be used as an electrode material of a battery, but is mainly used as a negative electrode material of a lithium ion battery or a sodium ion battery, wherein when the zinc selenide is used as the negative electrode material of the lithium ion battery, the action mechanism of the zinc selenide is as follows (Yuk-Tae Kwon, chemical-Min park. electrochemical characteristics of ZnSe and its nanostructured composite for rechargeable Li-ion batteries [ J-Tae Kwon, K-Li-ion batteries, K-Na-Li-ion batteries]Journal of Power Sources,2014,251: 319-324)): during the discharge process: ZnSe → LiSe + Zn → Li2Se+LixZn→Li2Se + LiZn; in the charging process: li2Se+LiZn→Li2Se+LixZn → LiSe + Zn → ZnSe; however, at present, there is no report about the use of zinc selenide as an electrode material in an aluminum ion battery.
Disclosure of Invention
In view of the above, the present invention provides an application of zinc selenide as an anode material of an aluminum ion battery, in order to overcome the defects of the existing material technology.
In order to achieve the purpose, the invention provides the following technical scheme:
1. the zinc selenide is applied as the anode material of the aluminum ion battery.
Preferably, the particle size of the zinc selenide is 400-1000nm, and the zinc selenide is uniformly dispersed and has a regular shape.
Preferably, the zinc selenide is prepared by the following method:
(1) dissolving soluble zinc salt in methanol to obtain a solution A; dissolving dimethyl imidazole in methanol to obtain a solution B; pouring the solution A into the solution B, stirring uniformly to form a reaction solution, standing for reaction to obtain a precipitate, and drying the precipitate to obtain a precursor;
(2) and (2) mixing the precursor obtained in the step (1) with selenium powder, and calcining in a mixed atmosphere of hydrogen and argon.
Preferably, in step (1), the soluble zinc salt is one of zinc nitrate hexahydrate or zinc chloride.
Preferably, in the step (1), the mass ratio of zinc nitrate hexahydrate to dimethylimidazole in the reaction liquid is 42-64: 34-58.
Preferably, in the step (1), the standing reaction time is 10-30 h.
Preferably, in step (1), the temperature of the drying is less than 90 ℃.
Preferably, in the step (2), the mass ratio of the precursor to the selenium powder is 1: 1-4.
Preferably, in the step (2), the volume fraction of hydrogen in the mixed atmosphere is 3-10%.
Preferably, in the step (2), the calcination is carried out for 1-4h after the temperature is raised to 400-800 ℃ at the speed of 2-10 ℃/min.
In the invention, zinc selenide is used as the anode material of the aluminum ion battery, and after the battery is assembled, the reaction mechanism of the zinc selenide is probably as follows:
in the charging process:
negative electrode:
4Al2Cl7 -+3e-→Al+7AlCl4 -
and (3) positive electrode:
AlZnSe+7AlCl4 --3e-→ZnSe+4Al2Cl7 -
during the discharge process:
negative electrode:
Al+7AlCl4 --3e-→4Al2Cl7 -
and (3) positive electrode:
ZnSe+4Al2Cl7 -+3e-→AlZnSe+7AlCl4 -。
the invention has the beneficial effects that: the invention provides an application of zinc selenide as an aluminum ion battery anode material, and the zinc selenide is used as the aluminum ion battery anode material, so that the zinc selenide has a high discharge platform and a large specific capacity, wherein the discharge voltage platform is about 1.8V, and the first-loop specific capacity is about 164mAh/g under the current density of 200mA/g, so that the aluminum ion battery can be better applied to various fields, such as the electronic industry, the communication industry, electric automobiles and the like. Meanwhile, the preparation process of the zinc selenide is simple, the raw material source is wide, the cost is low, and the preparation method is suitable for large-scale industrial production.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is an XRD pattern of zinc selenide prepared in example 1;
FIG. 2 is an SEM image of zinc selenide prepared in example 1;
FIG. 3 is a graph of the charge and discharge curves at a current density of 200mA/g for an aluminum ion battery using zinc selenide prepared in example 1 as a positive electrode material;
fig. 4 is a graph of a cycle test at a current density of 200mA/g for an aluminum ion battery using zinc selenide prepared in example 1 as a positive electrode material.
Detailed Description
The preferred embodiments of the present invention will be described in detail below.
Example 1
(1) Dissolving 2g of zinc nitrate hexahydrate in 20mL of methanol to obtain a solution A; dissolving 1.6g of dimethylimidazole in 20mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 10 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:1, placing the mixture in a tube furnace, heating to 400 ℃ at the speed of 2 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 1h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 3%. The obtained zinc selenide is subjected to X-ray diffraction analysis, the result is shown in figure 1, the obtained product is zinc selenide (JCPDS #37-1463) as shown in figure 1, the obtained zinc selenide is detected by using a scanning electron microscope, the detection result is shown in figure 2, and the zinc selenide as shown in figure 2 has the diameter distribution within the range of 400 plus one 1000nm, is uniformly dispersed and is a polyhedron with regular appearance.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]And Cl is used as electrolyte to assemble the battery for performance test, the test result is shown in figures 3 and 4, as can be seen from figure 3, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform is 1.8V, as can be seen from figure 4, under the current density of 200mA/g, the first discharge specific capacity of the material is 164mAh/g, and after 60 cycles, the specific capacity of 82mAh/g is also provided.
Example 2
(1) Dissolving 2g of zinc nitrate hexahydrate in 30mL of methanol to obtain a solution A; dissolving 2g of dimethylimidazole in 30mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for reaction for 15 hours, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:2, placing the mixture in a tube furnace, heating to 600 ℃ at the speed of 4 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 1h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 3%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]Cl is electrolysisThe liquid is assembled into a battery for performance test, when zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform is 1.8V, the first discharge specific capacity of the material is 168mAh/g under the current density of 200mA/g, and the specific capacity of 81mAh/g is also obtained after 60 cycles.
Example 3
(1) Dissolving 2g of zinc nitrate hexahydrate in 40mL of methanol to obtain a solution A; dissolving 2.2g of dimethylimidazole in 40mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 18 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:2, placing the mixture in a tube furnace, heating to 700 ℃ at the speed of 5 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 3h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 4%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]The Cl is used as electrolyte to assemble a battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform of the zinc selenide is 1.8V, the first discharge specific capacity of the material is 172mAh/g under the current density of 200mA/g, and the specific capacity of 83mAh/g is also obtained after 60 cycles.
Example 4
(1) Dissolving 2g of zinc nitrate hexahydrate in 60mL of methanol to obtain a solution A; dissolving 2.3g of dimethylimidazole in 60mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 24 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:3, placing the mixture in a tube furnace, heating to 600 ℃ at the speed of 6 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 2h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 4%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrodeAluminum foil as cathode, AlCl3/[EMIm]The Cl is used as electrolyte to assemble a battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform of the zinc selenide is 1.8V, the first discharge specific capacity of the material is 162mAh/g under the current density of 200mA/g, and the specific capacity of 79mAh/g is also obtained after 60 cycles.
Example 5
(1) Dissolving 2g of zinc nitrate hexahydrate in 60mL of methanol to obtain a solution A; dissolving 2.5g of dimethylimidazole in 60mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 28 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:3, placing the mixture in a tube furnace, heating to 700 ℃ at the speed of 6 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 3h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 6%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]The Cl is used as electrolyte to assemble a battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform of the zinc selenide is 1.8V, the first discharge specific capacity of the material is 166mAh/g under the current density of 200mA/g, and the specific capacity of 83mAh/g is also obtained after 60 cycles.
Example 6
(1) Dissolving 2g of zinc nitrate hexahydrate in 80mL of methanol to obtain a solution A; dissolving 2.6g of dimethylimidazole in 80mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for reaction for 15 hours, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:4, placing the mixture in a tube furnace, heating to 700 ℃ at the speed of 6 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 4h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 6%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]The Cl is used as electrolyte to assemble a battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform of the zinc selenide is 1.8V, the first discharge specific capacity of the material is 162mAh/g under the current density of 200mA/g, and the specific capacity of 85mAh/g is also obtained after 60 cycles.
Example 7
(1) Dissolving 2g of zinc nitrate hexahydrate in 80mL of methanol to obtain a solution A; dissolving 2.6g of dimethylimidazole in 80mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 26 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:4, placing the mixture in a tube furnace, heating to 800 ℃ at the speed of 8 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 2h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 8%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]The Cl is used as electrolyte to assemble the battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform is 1.8V, the first discharge specific capacity of the material is 173mAh/g under the current density of 200mA/g, and the specific capacity of 82mAh/g is also obtained after 60 cycles.
Example 8
(1) Dissolving 2g of zinc nitrate hexahydrate in 90mL of methanol to obtain a solution A; dissolving 2.7g of dimethylimidazole in 90mL of methanol to obtain a solution B; quickly pouring the solution A into the solution B, uniformly stirring to form a reaction solution, standing for 30 hours for reaction, centrifuging to obtain a precipitate, and vacuum-drying the precipitate at 60 ℃ for 5 hours to obtain a precursor;
(2) and (2) mixing and grinding the precursor obtained in the step (1) and selenium powder according to the mass ratio of 1:4, placing the mixture in a tube furnace, heating to 800 ℃ at the speed of 10 ℃/min in the mixed atmosphere of hydrogen and argon, preserving heat for 4h, and cooling to room temperature to obtain the zinc selenide. Wherein the volume fraction of hydrogen in the mixed atmosphere is 10%.
(3) Taking the zinc selenide prepared in the step (2) as a positive electrode, the aluminum foil as a negative electrode and AlCl3/[EMIm]The Cl is used as electrolyte to assemble a battery for performance test, the zinc selenide is used as the anode material of the aluminum ion battery, the discharge potential platform of the zinc selenide is 1.8V, the first discharge specific capacity of the material is 163mAh/g under the current density of 200mA/g, and the specific capacity of 75mAh/g is also obtained after 60 cycles.
In the invention, zinc nitrate hexahydrate is used as a raw material for preparing zinc selenide, and zinc chloride can be used as a raw material for preparing the zinc selenide, so that the same technical effect can be realized.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. The zinc selenide is applied as the anode material of the aluminum ion battery.
2. The method as claimed in claim 1, wherein the zinc selenide has a particle size of 400-1000nm, is uniformly dispersed, and has a regular morphology.
3. The use of claim 2, wherein the zinc selenide is prepared by a process comprising:
(1) dissolving soluble zinc salt in methanol to obtain a solution A; dissolving dimethyl imidazole in methanol to obtain a solution B; pouring the solution A into the solution B, stirring uniformly to form a reaction solution, standing for reaction to obtain a precipitate, and drying the precipitate to obtain a precursor;
(2) and (2) mixing the precursor obtained in the step (1) with selenium powder, and calcining in a mixed atmosphere of hydrogen and argon.
4. The use according to claim 3, wherein in step (1), the soluble zinc salt is one of zinc nitrate hexahydrate or zinc chloride.
5. The use according to claim 4, wherein in the step (1), the mass ratio of zinc nitrate hexahydrate to dimethylimidazole in the reaction liquid is 42-64: 34-58.
6. The use according to claim 3, wherein in the step (1), the standing reaction time is 10-30 h.
7. Use according to claim 3, wherein in step (1) the temperature of drying is less than 90 ℃.
8. The use according to claim 3, wherein in the step (2), the mass ratio of the precursor to the selenium powder is 1: 1-4.
9. The use according to claim 3, wherein in step (2), the volume fraction of hydrogen in the mixed atmosphere is 3-10%.
10. The use as claimed in claim 3, wherein in step (2), the calcination is carried out by raising the temperature to 400-800 ℃ at a rate of 2-10 ℃/min and then maintaining the temperature for 1-4 h.
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| CN1877889A (en) * | 2006-05-11 | 2006-12-13 | 复旦大学 | Film lithium ion cell with zinc selenide film as anode and method for preparing same |
| WO2014121276A3 (en) * | 2013-02-04 | 2014-11-06 | Massachusetts Institute Of Technology | Metal sulfide electrodes and energy storage devices thereof |
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| WO2014121276A3 (en) * | 2013-02-04 | 2014-11-06 | Massachusetts Institute Of Technology | Metal sulfide electrodes and energy storage devices thereof |
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