CN112573564B - Preparation method of magnesium hydroxygallate nanosheet material, product and application thereof - Google Patents
Preparation method of magnesium hydroxygallate nanosheet material, product and application thereof Download PDFInfo
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- CN112573564B CN112573564B CN202011575067.XA CN202011575067A CN112573564B CN 112573564 B CN112573564 B CN 112573564B CN 202011575067 A CN202011575067 A CN 202011575067A CN 112573564 B CN112573564 B CN 112573564B
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- H—ELECTRICITY
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- 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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- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
The invention provides a preparation method of a magnesium hydroxygallate nanosheet material, a product and an application thereof, wherein the preparation method of the magnesium hydroxygallate nanosheet material provided by the invention comprises the following steps: the hydroxyl magnesium gallate nanosheet material is prepared through a strong base and surfactant two-way auxiliary microwave method. The product structure obtained by the method has larger specific surface area and better conductivity, and further can improve the electrochemical performance of the material. The first discharge specific capacity is 415 mAh/g under the multiplying power of 1C, and after 40 times of circulation, the discharge specific capacity is 340 mAh/g. The problem that the specific capacity is attenuated relatively fast and the electrochemical performance is relatively poor in the circulation process of the magnesium ion battery is solved. And the preparation method is simple and quick, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Description
Technical Field
The invention relates to the technical field of magnesium electrode materials, in particular to a preparation method of a magnesium hydroxygallate nanosheet material, a product and application thereof.
Background
With the development of human society, the contradiction between the global shortage of energy resources and the increasing demand of people for energy is more and more acute. The development of battery systems with high energy density is a major goal of current power supply systems. Although lithium ion batteries having high specific energy and being environmentally friendly have been widely used in portable mobile appliances such as mobile phones and notebook computers, and in power sources for electric bicycles and electric vehicles. However, because the safety of the lithium ion battery is not well solved, the application of the lithium ion battery as a power battery still has much work to be done. Magnesium, one of the most abundant light metal elements on earth, is widely used in many fields due to its good physical and chemical properties. Much research is now done on secondary magnesium batteries, all based on secondary lithium ion batteries. Since magnesium and lithium are located diagonally in the periodic table of elements, the melting point of magnesium (648.8 ℃) is much higher than that of lithium (180.5 ℃) and there is no metal mobility of lithium, in addition to having similar atomic radius and chemical properties, so that the secondary magnesium battery is better in safety. Although the specific mass capacity was not as high as lithium (3862 mAh/g), it was also quite considerable (2205 mAh/g). In addition, the magnesium resource is very rich in China, the price of magnesium is far lower than that of lithium, and the magnesium is environment-friendly, so that secondary magnesium batteries are more and more concerned by people.
Magnesium hydroxygallate is commonly used as a wide bandgap semiconductor as a magnesium ion electrode material, which is considered to be a promising magnesium ion electrode material. However, the magnesium hydroxygallate nano-material is easy to agglomerate, collapse and pulverize in the circulation process, which results in poor electrochemical performance of the material.
Disclosure of Invention
In order to overcome the defect that the electrochemical performance of the magnesium hydroxygallate nano-material is poor due to easy agglomeration, structural collapse and pulverization in the circulating process, the invention aims to provide a preparation method of a magnesium hydroxygallate nano-sheet material.
Yet another object of the present invention is to: provides a hydroxyl gallium acid magnesium nanometer sheet material product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a method for preparing a magnesium hydroxygallate nanosheet material by a strong base and surfactant two-way auxiliary microwave method comprises the following steps,
the first step is as follows: adding 0.001-0.002 mol of gallium oxide, 0.006-0.012 mol of strong base, 2-4 g of surfactant and 0.003-0.006 mol of magnesium salt into 50 mL of deionized water, and magnetically stirring for 10-30 min to mark as solution A;
the second step is that: transferring the solution A into a round-bottom flask, putting the round-bottom flask into a microwave oven, heating for 10-20 min by 40-60% of the maximum power, and naturally cooling to obtain a suspension B;
the third step: and centrifuging the suspension B, washing the suspension B for 3 times by using deionized water and ethanol, and drying the suspension B in an oven at the temperature of 60-80 ℃ for 24 hours to obtain the final product, namely the magnesium hydroxygallate nanosheet material.
In the first step, the strong base is one or the combination of potassium hydroxide or sodium hydroxide.
In the first step, the active surface agent is one or the combination of cetyl trimethyl ammonium bromide or octadecyl diester quaternary ammonium salt.
In the first step, the magnesium salt is one or the combination of magnesium acetate, magnesium citrate or magnesium formate.
The invention provides a magnesium hydroxygallate nanosheet material prepared according to any one of the methods.
The invention provides an application of a hydroxymagnesium gallate nanosheet material in preparation of a magnesium electrode positive electrode material.
The invention prepares the hydroxyl magnesium gallate nanosheet material by a strong base and surfactant two-way auxiliary microwave method. The structure has larger specific surface area and better conductivity, thereby improving the electrochemical performance of the material. The first discharge specific capacity is 415 mAh/g under the multiplying power of 1C, and after 40 times of circulation, the discharge specific capacity is 340 mAh/g. The problem that the specific capacity is attenuated relatively fast and the electrochemical performance is relatively poor in the circulation process of the magnesium ion battery is solved. And the preparation method is simple and quick, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Drawings
Fig. 1 is a graph of the cycle life of magnesium hydroxygallate nanosheets material of example 1.
Fig. 2 is a cycle life diagram of the magnesium hydroxygallate nanosheet material of example 2.
Fig. 3 is a graph of the cycle life of the magnesium hydroxygallate nanosheet material of example 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A hydroxyl magnesium gallate nanosheet material is prepared by a strong base and surfactant two-way auxiliary microwave method and is prepared by the following steps:
the first step is as follows: adding 0.001 mol of gallium oxide, 0.006 mol of strong base sodium hydroxide, 2 g of surfactant cetyl trimethyl ammonium bromide and 0.006 mol of magnesium acetate into 50 mL of deionized water, and magnetically stirring for 10 min to obtain a solution A;
the second step: transferring the solution A into a round-bottom flask, putting the round-bottom flask into a microwave oven, heating for 20 min at 40% of the maximum power, and naturally cooling to obtain a suspension B;
the third step: and centrifuging the suspension B, washing the suspension B for 3 times by using deionized water and ethanol, and drying the suspension B in an oven at the temperature of 80 ℃ for 24 hours to obtain the final product, namely the magnesium hydroxygallate nanosheet material.
Fig. 1 is a graph of the cycle life of magnesium hydroxygallate nanosheets at 1C magnification. The first discharge specific capacity is 376 mAh/g, and after 40 times of circulation, the discharge specific capacity is 321 mAh/g.
Example 2
A magnesium hydroxygallate nanosheet material, which is similar to the step of example 1, and is prepared by the following steps:
the first step is as follows: adding 0.002 mol of gallium oxide, 0.012 mol of potassium hydroxide, 2 g of octadecyl diester quaternary ammonium salt and 0.003 mol of magnesium formate into 50 mL of deionized water, and magnetically stirring for 10 min to mark as solution A;
the second step is that: transferring the solution A into a round-bottom flask, putting the round-bottom flask into a microwave oven, heating for 10 min at the maximum power of 60%, and naturally cooling to obtain a suspension B;
the third step: and centrifuging the suspension B, washing the suspension B for 3 times by using deionized water and ethanol, and drying the suspension B in an oven at the temperature of 80 ℃ for 24 hours to obtain the final product, namely the magnesium hydroxygallate nanosheet material.
Fig. 2 is a graph of the cycle life of magnesium hydroxygallate nanosheets at 1C magnification. The first discharge specific capacity is 385 mAh/g, and after 40 times of circulation, the discharge specific capacity is 324 mAh/g.
Example 3
A magnesium hydroxygallate nanosheet material, which is similar to the step of example 1, and is prepared by the following steps:
the first step is as follows: adding 0.002 mol of gallium oxide, 0.012 mol of sodium hydroxide, 4g of octadecyl diester quaternary ammonium salt and 0.006 mol of magnesium citrate into 50 mL of deionized water, and magnetically stirring for 10 min to mark as solution A;
the second step is that: transferring the solution A into a round-bottom flask, putting the round-bottom flask into a microwave oven, heating for 10 min at the maximum power of 60%, and naturally cooling to obtain a suspension B;
the third step: and centrifuging the suspension B, washing the suspension B for 3 times by using deionized water and ethanol, and drying the suspension B in an oven at the temperature of 80 ℃ for 24 hours to obtain the final product, namely the magnesium hydroxygallate nanosheet material.
Fig. 3 is a graph of the cycle life of magnesium hydroxygallate nanosheets at 1C magnification. The first discharge specific capacity is 415 mAh/g, and after 40 times of circulation, the discharge specific capacity is 340 mAh/g.
Claims (4)
1. A preparation method of a magnesium hydroxygallate nanosheet material is characterized in that the magnesium hydroxygallate nanosheet material is prepared by a strong base and surfactant two-way auxiliary microwave method, and comprises the following steps:
the first step is as follows: adding 0.001-0.002 mol of gallium oxide, 0.006-0.012 mol of strong base, 2-4 g of surfactant and 0.003-0.006 mol of magnesium salt into 50 mL of deionized water, and magnetically stirring for 10-30 min, wherein the solution is marked as solution A;
the second step is that: transferring the solution A into a round-bottom flask, putting the round-bottom flask into a microwave oven, heating for 10-20 min by 40-60% of the maximum power, and naturally cooling to obtain a suspension B;
the third step: centrifuging the suspension B, washing the suspension B for 3 times by using deionized water and ethanol, and drying the suspension B in an oven at the temperature of 60-80 ℃ for 24 hours to obtain a final product, namely the magnesium hydroxygallate nanosheet material; wherein, the first and the second end of the pipe are connected with each other,
in the first step, the strong base is one or the combination of potassium hydroxide or sodium hydroxide;
the active surface agent is one or the combination of cetyl trimethyl ammonium bromide or octadecyl diester quaternary ammonium salt.
2. The method for preparing magnesium hydroxygallate nanosheets material according to claim 1, wherein: in the first step, the magnesium salt is one or a combination of magnesium acetate, magnesium citrate or magnesium formate.
3. A magnesium hydroxygallate nanosheet material, characterized by being prepared according to the method of claim 1 or 2.
4. Use of the magnesium hydroxygallate nanosheet material of claim 3 in the preparation of a magnesium electrical positive electrode material.
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| CN202011575067.XA CN112573564B (en) | 2020-12-28 | 2020-12-28 | Preparation method of magnesium hydroxygallate nanosheet material, product and application thereof |
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