Preparation method, product and application of copper-loaded magnesium vanadate material

Abstract

The invention provides a preparation method of a copper-loaded magnesium vanadate material and a product and application of the copper-loaded magnesium vanadate material. Vanadate, magnesium salt and copper salt are fully mixed according to the stoichiometric molar ratio and ground in mortar, and A is obtained; transferring the obtained mixture into a 10ml glass vial, adding another 2ml open vial containing 1ml of distilled water, keeping the whole container in an oven at 70-80 DEG C, reacting for 24-30 hours, taking out the vial, drying at the same temperature for 8-10 hours, and regrinding to obtain B; and putting the B into a muffle furnace, heating to 400-600 DEG C at a heating rate of 1-2 DEG C / min, and calcining for 2-4 hours to obtain a final product, namely the copper-loaded magnesium vanadate material. Under the condition of 1 A / g current density, the first specific discharge capacity is 268.8 mAh / g, after 100 cycles, the specific discharge capacity is 248.8 mAh / g, and the capacity retention ratio is 92.6%.

Description

Technical Field

[0001] This invention belongs to the field of battery materials and relates to a method for preparing a magnesium cathode material, particularly a method for preparing a copper-supported magnesium vanadate material, its products, and applications. Background Technology

[0002] Developing battery systems with high energy density has become a major goal of current power systems.

[0003] Although lithium-ion batteries, with their high energy density and environmental friendliness, are widely used in portable mobile devices such as mobile phones and laptops, as well as power sources for electric bicycles and electric vehicles, their safety remains a significant concern, and much work remains to be done in their application as power batteries. Magnesium, one of the most abundant light metal elements on Earth, is widely used in many fields due to its excellent physicochemical properties.

[0004] Current research on rechargeable magnesium batteries is extensive, primarily building upon existing lithium-ion batteries. Since magnesium and lithium are diagonally opposite elements in the periodic table, besides having similar atomic radii and chemical properties, magnesium has a significantly higher melting point (648.8℃) than lithium (180.5℃) and is less reactive, making rechargeable magnesium batteries safer. Although their specific capacity is lower than lithium (3862 mAh•g...),... -1 That's quite high, but still considerable (2205mAh•g) -1 Moreover, my country has extremely abundant magnesium resources, and the price of magnesium is much lower than that of lithium. Furthermore, magnesium is environmentally friendly, so rechargeable magnesium batteries are attracting increasing attention.

[0005] Magnesium vanadate is a compound with a layered crystal structure. Due to its specific lattice structure, it has good physical and chemical properties and is often used as a semiconductor with a wide band gap. It can also be used as a cathode material for magnesium-ion batteries. This material is considered a promising magnesium-ion cathode material. Summary of the Invention

[0006] The purpose of this invention is to provide a method for preparing copper-supported magnesium vanadate materials, so as to improve the problem of insufficient electrochemical performance of existing magnesium vanadate materials.

[0007] Another object of the present invention is to provide a copper-supported magnesium vanadate product obtained by the above method.

[0008] Another object of the present invention is to provide an application of the above-mentioned product.

[0009] This invention provides a method for preparing copper-supported magnesium vanadate materials. The invention utilizes a special solid-state method, namely a wet-assisted solid-state method, to prepare copper-supported magnesium vanadate materials. Humidity plays a crucial role in the reaction of the solid-state method and can ultimately control the size and morphology of the material, thereby improving the electrochemical performance of the composite material. This preparation process is relatively simple and easy to operate.

[0010] This invention provides a method for preparing copper-supported magnesium vanadate material. The method utilizes a special solid-state method, namely a wet-assisted solid-state method, to prepare the copper-supported magnesium vanadate material. The specific steps of this method are as follows: (1) Mix vanadate, magnesium salt and copper salt thoroughly in a stoichiometric molar ratio (2:1:0.01 ~ 0.05) and grind them in mortar to obtain mixture A; (2) Transfer the obtained mixture A to a 10 mL glass vial, add another 2 mL open vial containing 1 mL of distilled water, and then keep the entire container in an oven at 70-80°C for 24-30 h. After that, remove the open vial, dry it at the same temperature for 8-10 h, and then re-grind it to obtain product B. (3) Place product B in a box furnace and heat it to 400-600℃ at a heating rate of 1-2℃ / min for 2-4 hours to obtain the final product, copper-supported magnesium vanadate material. The box furnace is a muffle furnace.

[0011] Vanadates are oxyacid salts of vanadium. Preferably, in step (1), the vanadate is one or a combination of diacetylacetone vanadate, isopropanol vanadate, or lactate vanadate.

[0012] Preferably, in step (1), the magnesium salt is one or a combination of magnesium diacetylacetonate, magnesium isopropoxide, or magnesium lactate.

[0013] Preferably, in step (1), the copper salt is one or a combination of copper acetate, copper nitrate, or copper nitrate.

[0014] This invention provides a copper-supported magnesium vanadate material, prepared according to any of the methods described above.

[0015] This invention provides an application of copper-supported magnesium vanadate in magnesium electrode materials. The copper-supported magnesium vanadate material prepared according to Example 1 of this invention exhibits excellent discharge specific capacity and stable capacity retention. The copper-supported magnesium vanadate materials obtained in Examples 2 and 3 also have similar discharge specific capacities.

[0016] The beneficial effects of this invention are as follows: This invention prepares copper-supported magnesium vanadate materials via a special solid-state method, namely the wet-assisted solid-state method. Humidity plays a crucial role in the solid-state reaction and can ultimately control the size and morphology of the material, thereby improving the electrochemical performance of the composite material. The preparation process is relatively simple and easy to operate. Under a current density of 1 A / g, the initial discharge specific capacity is 268.8 mAh / g, and after 100 cycles, the discharge specific capacity is 248.8 mAh / g, with a capacity retention of 92.6%. Attached Figure Description

[0017] Figure 1 This is a cycle life diagram of the copper-supported magnesium vanadate material in Example 1; Under a current density of 1 A / g, the initial discharge specific capacity is 268.8 mAh / g, and after 100 cycles, the discharge specific capacity is 248.8 mAh / g, with a capacity retention of 92.6%. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0019] Example 1 A copper-supported magnesium vanadate material is prepared by a wet-assisted solid-state method according to the following steps: (1) Mix diacetylacetone vanadium oxide salt, diacetylacetone magnesium and copper acetate thoroughly in a stoichiometric molar ratio (2:1:0.01) and grind them in mortar to obtain mixture A; (2) The obtained mixture A was transferred to a 10 ml glass vial, and another 2 ml open vial containing 1 ml of distilled water was added. The entire container was then reacted in an oven at 80 °C for 24 h. The vial was then removed, dried at the same temperature for 8 h, and then ground again to obtain product B. (3) Place product B in a muffle furnace and heat it to 400°C at a heating rate of 2°C / min for 4 hours to obtain the final product, copper-supported magnesium vanadate material.

[0020] Figure 1 This is a cycle life diagram of the copper-supported magnesium vanadate material obtained in this embodiment. Under a current density of 1 A / g, the initial discharge specific capacity is 268.8 mAh / g, and after 100 cycles, the discharge specific capacity is 248.8 mAh / g, with a capacity retention of 92.6%.

[0021] Example 2 A copper-supported magnesium vanadate material, similar to that in Example 1, is prepared according to the following steps: (1) Mix isopropoxide vanadium oxide, magnesium isopropoxide and copper acetate thoroughly in a stoichiometric molar ratio (2:1:0.03) and grind them in mortar to obtain mixture A; (2) The obtained mixture A was transferred to a 10 ml glass vial, and another 2 ml open vial containing 1 ml of distilled water was added. The entire container was then kept in an oven at 70 °C for 30 h. After the reaction, the vial was removed, dried at the same temperature for 8 h, and then ground again to obtain B. (3) Place B in a muffle furnace and heat it to 500 °C at a heating rate of 1 °C / min for 3 hours to obtain the final product, copper-supported magnesium vanadate material.

[0022] Example 3 A copper-supported magnesium vanadate material, similar to that in Example 1, is prepared according to the following steps: (1) Mix vanadium lactate, magnesium lactate and copper nitrate thoroughly in a stoichiometric molar ratio (2:1:0.05) and grind them in mortar to obtain A; (2) Transfer the obtained mixture to a 10 ml glass vial, add another 2 ml open vial containing 1 ml of distilled water, and then keep the entire container in an oven at 70 °C. After reacting for 30 h, remove the vial, dry it at the same temperature for 8 h, and then grind it again to obtain B. (3) Place B in a muffle furnace and heat it to 600 °C at a heating rate of 2 °C / min for 2 hours to obtain the final product, copper-supported magnesium vanadate material.

Claims

1. A method for preparing a copper-supported magnesium vanadate material, characterized in that, The preparation of copper-supported magnesium vanadate materials by a wet-assisted solid-state method includes the following steps: (1) Mix vanadate, magnesium salt and copper salt thoroughly in a stoichiometric molar ratio of 2:1:(0.01 ~ 0.05) and grind them in mortar to obtain mixture A; (2) Transfer the obtained mixture A to a glass vial, and add another open vial to it. The volume ratio of the glass vial to the open vial is (3-8):

1. The open vial contains distilled water, and the volume of the distilled water is 1:(2-5) of the volume of the open vial. Then, keep the entire container in an oven at 70-80°C for 24-30 hours to react. After that, take out the open vial, dry it at the same temperature for 8-10 hours, and then grind it again to obtain B. (3) Place B in a box furnace and heat it to 400-600℃ at a heating rate of 1-2℃ / min for 2-4 hours to obtain the final product, copper-supported magnesium vanadate material.

2. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, The vanadate is one or a combination of diacetylacetone vanadate, isopropanol vanadate, or lactate vanadate.

3. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, The magnesium salt is one or a combination of magnesium diacetylacetonate, magnesium isopropoxide, or magnesium lactate.

4. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, The copper salt is one of copper acetate, copper nitrate, or a combination thereof.

5. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, In step (1), the molar ratio of vanadium oxide salt, magnesium salt, and copper salt is 2:1:0.

03.

6. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, In step (2), mixture A is transferred to a 10 ml glass vial, into which another 2 ml open vial containing 1 ml of distilled water is added.

7. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, In step (3), the box furnace is a muffle furnace.

8. The method for preparing copper-supported magnesium vanadate material according to claim 1, characterized in that, In step (3), the calcination temperature is 500℃.

9. A copper-supported magnesium vanadate material, obtained by the preparation method according to any one of claims 1-8.

10. The application of the copper-supported magnesium vanadate material according to claim 9 in magnesium cathodes.

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