CN114023959B - Preparation method of magnesium-containing graphene lithium ion battery cathode material - Google Patents
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a magnesium-containing graphene lithium ion battery cathode material, which is characterized by comprising the following steps of: step one, adding a magnesium salt into a beaker filled with deionized water, and ultrasonically stirring until the magnesium salt is completely dissolved to obtain a solution A; step two, placing graphene in the solution A to form a mixed solution; stirring the mixed solution to a uniformly dispersed solution B; pouring the solution B into the lining of the reaction kettle to perform high-temperature hydrothermal reaction, repeatedly cleaning the reaction product obtained in the step three by using a cleaning solution to remove redundant acid radical ions and impurities, and finally drying the reaction product in a forced air drying oven at the temperature to obtain a precursor; and fifthly, grinding the precursor into fine powder by using a mortar for heat treatment, and cooling to room temperature to obtain the final product, namely the magnesium-containing graphene lithium ion battery cathode material. The method disclosed by the invention is simple in process, safe and environment-friendly, has high dispersion degree of the magnesium salt on the surface of the graphene, and is suitable for industrial development.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a magnesium-containing graphene lithium ion battery cathode material.
Background
The lithium ion battery has the advantages of high energy density, long cycle life, environmental protection and the like, and is widely applied to various fields of portable electronic products, electric automobiles, national defense equipment and the like. As an important component of a lithium battery, graphite is the most commonly used lithium battery negative electrode material at present due to the characteristics of low price, rich source, low lithium intercalation voltage and the like, but the graphite has the problems of low theoretical capacity and poor conductivity, and the material also has the problem of lithium dendrite crystal in the process of charging and discharging under high multiplying power, which seriously hinders the further development of the material in the lithium battery.
Graphene itself is a highly interconnected network structure, and has the characteristics of high conductivity, large specific surface area, excellent chemical stability and the like. In addition, the specific capacity of the material is about 2 times of that of a graphite electrode, and the material is hopeful to be applied to a lithium ion battery cathode material instead of graphite. It should be noted that graphene cannot be directly used as an electrode in practical applications, mainly because graphene sheets are easily stacked or even agglomerated during charging and discharging processes, so that the specific surface area of the graphene sheets is reduced, and the lithium intercalation capacity is reduced. Patents CN 111952573A, CN 108598444B and CN 106920932B disclose that MnO2, V2O3 and Co (OH) 2 are respectively introduced to the surface of graphene according to their advantages of high theoretical capacity, excessive electrochemical active sites, etc. to improve the characteristics of graphene material such as specific capacity and rate capability. Although the method obviously improves the problems of easy agglomeration of graphene and low lithium intercalation capacity, the cycle life of the material is low due to the fact that the transition metal compounds are actively and easily expanded in the rapid charging and discharging process.
CN 102390825A discloses that when magnesium ions are introduced into lithium cobaltate or lithium nickel cobalt manganese oxide, they can reversibly react with anions in the electrolyte to provide pseudo capacitance for the material, and also play a role in maintaining the structural stability of the material during the circulation process, but no one has explored the research on introducing a magnesium source into the surface of graphene, and the above synthesis process is complicated and the uniformity of particle size is difficult to control. Therefore, the search for a novel magnesium-containing graphene lithium ion negative electrode material which is simple in process, easy to control conditions and low in cost is a current key task.
Disclosure of Invention
The invention aims to solve the defects of insufficient specific capacity and energy density caused by the agglomeration problem of a graphene material, and provides a magnesium-containing graphene lithium ion battery cathode material, so that the electrochemical performance of a lithium ion battery is effectively improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a magnesium-containing graphene lithium ion battery cathode material comprises the following steps:
step one, adding a proper amount of magnesium salt into a beaker filled with 30-50 mL of deionized water, and ultrasonically stirring until the magnesium salt is completely dissolved to obtain a solution A;
step two, placing graphene in the solution A prepared in the step one to form a mixed solution; then transferring the mixed solution to a magnetic stirrer, and stirring the mixed solution to a uniformly dispersed solution B;
and step three, pouring the solution B obtained in the step two into the lining of the reaction kettle to carry out high-temperature hydrothermal reaction. Obtaining a reaction product when the high-temperature hydrothermal reaction is finished and the temperature is cooled to room temperature;
step four, repeatedly cleaning the reaction product obtained in the step three by using a cleaning solution to remove redundant acid radical ions and impurities, and finally drying the reaction product in a forced air drying box at the temperature of 60-80 ℃ for 10-12 hours to obtain a precursor;
and step five, grinding the precursor obtained in the step four by using a mortar into fine powder, and placing the powder into a tube furnace for heat treatment. And cooling to room temperature and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
The preparation method of the magnesium-containing graphene lithium ion battery cathode material provided by the invention also has the following technical characteristics:
for example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided by an embodiment of the present disclosure, in the step one, the magnesium salt is a soluble magnesium salt, specifically, any one or more of magnesium-containing acetate, sulfate, and nitrate.
For example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided in an embodiment of the present disclosure, the graphene in the second step includes: graphene oxide and chemically oxidizing or stripping the obtained graphene.
For example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided by an embodiment of the present disclosure, the mass ratio of the magnesium salt to the graphene in the second step is 2% to 5%:1.
for example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided in an embodiment of the present disclosure, when the solution B is stirred on a magnetic stirrer in the second step, ethanol with a total amount of 4 to 6mL should be added point by point as a dispersing agent, and the dispersion degree of the magnesium source may be adjusted by adjusting the dropping time.
For example, in the preparation method of the magnesium-containing graphene lithium ion battery anode material provided in an embodiment of the present disclosure, the hydrothermal reaction process in the third step specifically includes placing the inner liner of the reaction kettle in a vacuum drying oven, and vacuum-maintaining the inner liner at a temperature of 150 to 180 ℃ for 10 to 15 hours.
For example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided by an embodiment of the present disclosure, the washing solutions in the fourth step are deionized water and ethanol respectively, and the washing sequence is that the deionized water is washed for 3 times, and then the ethanol is washed for 3 times.
For example, in the preparation method of the magnesium-containing graphene lithium ion battery negative electrode material provided in an embodiment of the present disclosure, the heat treatment in the fifth step is: heating to 450 ℃ at a heating rate of 1-3 ℃/min in the atmosphere of inert gas and keeping for 3-5 h
For example, in the preparation method of the magnesium-containing graphene lithium ion battery anode material provided by an embodiment of the present disclosure, in the fifth step, the inert gas is any one of argon, nitrogen and helium.
Compared with the prior art, the invention provides a preparation method of a magnesium-containing graphene lithium ion battery cathode material, which has the following beneficial effects:
1. the invention not only prepares the magnesium-containing graphene lithium ion battery cathode material, but also prepares the magnesium-containing graphene lithium ion battery cathode material
A new idea is provided for the application of the novel magnesium-containing graphene negative electrode material in the field of lithium ion batteries. In the preparation process, magnesium ions can be uniformly and firmly doped into different active sites of graphene under the hydrothermal environment provided by the outside; the dropping of the absolute ethyl alcohol not only promotes the further development of the process, but also plays a role in inhibiting the agglomeration of the graphene; the defects introduced in the doping process can be eliminated by combining the heat treatment process of the tubular furnace, so that the synthesis of the high-dispersity magnesium-containing graphene lithium ion battery cathode material is promoted. And the introduction of magnesium ions can maintain the structural stability of graphene in a long cycle process, and reduce the diffusion internal resistance of electrons and ions in the charge-discharge process, so that the electronic and ionic conductivity of the material is effectively improved, and the multiplying power performance and the cycle life of the material are greatly improved. In addition, the method provided by the invention is simple in process, safe and environment-friendly, and the magnesium salt is high in dispersion degree on the surface of the graphene, so that the method is suitable for industrial development.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description relate only to some embodiments of the present disclosure and are not limiting to the present disclosure.
Fig. 1 is an SEM image of the magnesium-containing graphene lithium ion battery negative electrode material prepared in examples 1 to 3.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions of the embodiments of the present disclosure will be clearly and completely described below with reference to the drawings of the embodiments of the present disclosure. It is to be understood that the described embodiments are only a few embodiments of the present disclosure, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the disclosure without any inventive step, are within the scope of protection of the disclosure.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of "first," "second," and the like in this disclosure is not intended to indicate any order, quantity, or importance, but rather is used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
The first embodiment,
A preparation method of a magnesium-containing graphene lithium ion battery cathode material comprises the following steps:
step one, adding a proper amount of magnesium salt into a beaker filled with 30-50 mL of deionized water, and ultrasonically stirring until the magnesium salt is completely dissolved to obtain a solution A;
step two, placing graphene in the solution A prepared in the step one to form a mixed solution; then transferring the mixed solution to a magnetic stirrer, and stirring the mixed solution to a uniformly dispersed solution B;
and step three, pouring the solution B obtained in the step two into the inner liner of the reaction kettle for high-temperature hydrothermal reaction. Obtaining a reaction product when the high-temperature hydrothermal reaction is finished and the temperature is cooled to room temperature;
step four, repeatedly cleaning the reaction product obtained in the step three by using a cleaning solution to remove redundant acid radical ions and impurities, and finally drying the reaction product in a blast drying oven at the temperature of 60-80 ℃ for 10-12 h to obtain a precursor;
and step five, grinding the precursor obtained in the step four by using a mortar into fine powder, and placing the powder into a tube furnace for heat treatment. And cooling to room temperature and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
In the first step, the magnesium salt is a soluble magnesium salt, and specifically is any one or more of acetate, sulfate and nitrate containing magnesium.
The graphene in the second step comprises: graphene oxide and chemically oxidizing or stripping the obtained graphene.
The mass ratio of the magnesium salt to the graphene in the second step is 2% -5%: 1.
and in the second step, when the solution B is stirred on a magnetic stirrer, 4-6 mL of ethanol serving as a dispersing agent is added point by point, and the dispersion degree of the magnesium source can be regulated and controlled by regulating the dropping time.
The hydrothermal reaction process in the third step specifically comprises the steps of placing the inner liner of the reaction kettle in a vacuum drying oven, and keeping the inner liner of the reaction kettle in vacuum for 10 to 15 hours at the temperature of between 150 and 180 ℃.
In the fourth step, the washing liquid is respectively deionized water and ethanol, and the washing sequence is that the deionized water is firstly washed for 3 times and then the ethanol is washed for 3 times.
The heat treatment in the fifth step is as follows: heating to 450 ℃ at a heating rate of 1-3 ℃/min in the atmosphere of inert gas and keeping for 3-5 h
And in the fifth step, the inert gas comprises argon, nitrogen and helium, wherein the inert gas is any one of argon, nitrogen and helium.
Example II,
A preparation method of a magnesium-containing graphene lithium ion battery cathode material comprises the following steps:
step one, adding 2% -5% of Mg (CH 3 COO) 2.4H 2O into a beaker filled with 30mL of deionized water, and ultrasonically stirring until a magnesium source is completely dissolved to obtain a solution A;
step two, placing graphene oxide in the prepared solution A to form a mixed solution; transferring the mixed solution to a magnetic stirrer, dropwise adding 4-6 mL of ethanol (dispersant) under the stirring effect, and stirring for 2-3 h;
step three, pouring the solution B obtained in the step two into a 100mL polytetrafluoroethylene reaction kettle lining, and placing the solution B into a vacuum drying oven at the temperature of 150-180 ℃ for hydrothermal reaction for 10-15 h;
step four, when the hydrothermal reaction is finished and the reaction product is cooled to room temperature, the reaction product obtained in the step three is washed for 3 times by deionized water and ethanol to remove redundant acid radical ions and impurities, and then the reaction product is placed into a forced air drying oven with the temperature of 60-80 ℃ to be dried for 10-12 hours to obtain a precursor;
step five, grinding the precursor obtained in the step four by using a mortar into fine powder, and placing the powder into a tube furnace for heat treatment, wherein the treatment conditions are as follows: raising the temperature to 450 ℃ at a heating rate of 1-3 ℃/min in the atmosphere of inert gas and keeping the temperature for 3-5 h. And cooling to room temperature and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
EXAMPLE III
A preparation method of a magnesium-containing graphene lithium ion battery cathode material comprises the following steps:
step one, adding MgSO4 accounting for 2-5 percent into a beaker filled with 30mL of deionized water, and ultrasonically stirring until a magnesium source is completely dissolved to obtain a solution A;
step two, placing graphene oxide in the prepared solution A to form a mixed solution; transferring the mixed solution to a stirrer, dropwise adding 4-6 mL of ethanol (dispersant) under the stirring effect, and stirring for 2-3 h;
step three, pouring the solution B obtained in the step two into a 100mL polytetrafluoroethylene reaction kettle lining, and placing the solution B in a vacuum drying oven at the temperature of 150-180 ℃ for hydrothermal reaction for 10-15 h;
step four, when the hydrothermal reaction is finished and the reaction product is cooled to room temperature, the reaction product obtained in the step three is washed for 3 times by deionized water and ethanol to remove redundant acid radical ions and impurities, and then the reaction product is placed into a forced air drying oven with the temperature of 60-80 ℃ to be dried for 10-12 hours to obtain a precursor;
step five, grinding the precursor obtained in the step four into fine powder by using a mortar, and placing the powder in a tube furnace for heat treatment, wherein the treatment conditions are as follows: raising the temperature to 450 ℃ at a heating rate of 1-3 ℃/min in the atmosphere of inert gas and keeping the temperature for 3-5 h. And cooling to room temperature and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
Example four
Step one, adding 2-5 percent of Mg (NO 3) 2 into a beaker filled with 30mL of deionized water, and ultrasonically stirring until a magnesium source is completely dissolved to obtain a solution A;
step two, placing graphene oxide in the prepared solution A to form a mixed solution; transferring the mixed solution to a stirrer, dropwise adding 4-6 mL of ethanol (dispersing agent) under the stirring effect, and stirring for 2-3 h;
step three, pouring the solution B obtained in the step two into a 100mL polytetrafluoroethylene reaction kettle lining, and placing the solution B in a vacuum drying oven at the temperature of 150-180 ℃ for hydrothermal reaction for 10-15 h;
step four, when the hydrothermal reaction is finished and the reaction product is cooled to room temperature, the reaction product obtained in the step three is washed for 3 times by deionized water and ethanol to remove redundant acid radical ions and impurities, and then the reaction product is placed into a forced air drying oven with the temperature of 60-80 ℃ to be dried for 10-12 hours to obtain a precursor;
step five, grinding the precursor obtained in the step four by using a mortar into fine powder, and placing the powder into a tube furnace for heat treatment, wherein the treatment conditions are as follows: raising the temperature to 450 ℃ at a heating rate of 1-3 ℃/min in the atmosphere of inert gas and keeping the temperature for 3-5 h. And cooling to room temperature and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
Scanning Electron Microscope (SEM) tests were performed on several of the magnesium-containing graphene lithium ion battery negative electrode materials prepared in the examples. Fig. 1 is an SEM image of the magnesium-containing graphene lithium ion battery negative electrode material prepared in examples 1 to 3. As can be seen from the figure, after the high-temperature hydrothermal treatment, different soluble magnesium salts are successfully loaded and uniformly distributed on the surface of graphene in the form of tiny particles.
Subsequently, the products obtained in examples 1-3 were assembled into button cells, and performance tests were performed on the button cells in a blue tester (wherein the positive electrode: lithium sheet; the negative electrode: the material prepared in the above steps; separator: polypropylene microporous membrane; and electrolyte were prepared by using EC (ethylene carbonate), EDC (diethyl carbonate) and EMC (ethyl methyl carbonate) as solvents at a volume ratio of 1.
Table 1 shows the results of the tests of conductivity, specific capacity and cycle performance of the lithium ion batteries assembled from the materials obtained in examples 1 to 3.
Table 2 shows the results of rate capability tests of lithium ion batteries assembled with the materials obtained in examples 1 to 3.
Generally, the larger the diffusion capacity of lithium ions in an electrolyte during charge and discharge, the smaller the charge transfer resistance of electrons on the surface of a material, indicating that the rate capability and cycle life of the material are better. As can be seen from table 1-2, after the surface of graphene is doped with different soluble magnesium sources, the ionic conductivity of the composite material gradually decreases, and the electronic conductivity gradually increases, that is, the diffusion capability of lithium ions is enhanced in the charging and discharging processes, and the charge transfer impedance of electrons on the surface of the material decreases, so that the specific capacity and the rate capability of graphene are respectively improved from 740.1mAh g-1 and 46.9% to 850.0mAh g-1 and 76.0%, and the capacity retention rate reaches 93% after 100 cycles, which indicates that magnesium salt is introduced on the surface of graphene, not only can reduce the diffusion internal resistance of electrons and ions in the charging and discharging processes, enhance the ionic and electronic conductivities, but also plays a role in maintaining the stable structure of graphene in the long cycle process, so as to realize the rapid transmission and storage of lithium ions.
The following points need to be explained:
1. in the drawings of the embodiments of the present disclosure, only the structures related to the embodiments of the present disclosure are referred to, and other structures may refer to general designs.
2. Features of the disclosure in the same embodiment and in different embodiments may be combined with each other without conflict.
The above is only a specific embodiment of the present disclosure, but the scope of the present disclosure is not limited thereto, and any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present disclosure, and shall be covered by the scope of the present disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (9)
1. The preparation method of the magnesium-containing graphene lithium ion battery cathode material is characterized by comprising the following steps:
step one, adding a proper amount of magnesium salt into a beaker filled with 30-50 mL deionized water, and ultrasonically stirring until the magnesium salt is completely dissolved to obtain a solution A;
step two, placing graphene in the solution A prepared in the step one to form a mixed solution; then transferring the mixed solution to a magnetic stirrer, and stirring the mixed solution to a uniformly dispersed solution B;
step three, pouring the solution B obtained in the step two into a lining of a reaction kettle for high-temperature hydrothermal reaction, and obtaining a reaction product when the high-temperature hydrothermal reaction is finished and the temperature is cooled to room temperature;
step four, repeatedly cleaning the reaction product obtained in the step three by using a cleaning solution to remove redundant acid radical ions and impurities, and finally drying the reaction product in a forced air drying oven at the temperature of 60-80 ℃ for 10-12 h to obtain a precursor;
and fifthly, grinding the precursor obtained in the fourth step into fine powder by using a mortar, placing the powder into a tube furnace for heat treatment, cooling to room temperature, and collecting to obtain the final product magnesium-containing graphene lithium ion battery cathode material.
2. The preparation method of the magnesium-containing graphene lithium ion battery anode material according to claim 1, wherein the magnesium salt in the step one is a soluble magnesium salt, specifically any one or more of magnesium-containing acetate, sulfate and nitrate.
3. The preparation method of the magnesium-containing graphene lithium ion battery negative electrode material according to claim 1, wherein the graphene in the second step comprises: graphene oxide and chemically oxidizing or stripping the obtained graphene.
4. The preparation method of the magnesium-containing graphene lithium ion battery negative electrode material according to claim 1, wherein the mass ratio of the magnesium salt to the graphene in the second step is 2% -5%: 1.
5. the preparation method of the magnesium-containing graphene lithium ion battery anode material according to claim 1, wherein in the second step, ethanol with a total amount of 4-6 mL is added point by point as a dispersing agent when the solution B is stirred on a magnetic stirrer, and the dispersion degree of a magnesium source can be adjusted by adjusting the dropping time.
6. The preparation method of the magnesium-containing graphene lithium ion battery cathode material according to claim 1, wherein the hydrothermal reaction process in the third step specifically includes placing a liner of a reaction kettle in a vacuum drying oven, and vacuum-maintaining the liner at 150-180 ℃ for 10-15 h.
7. The preparation method of the magnesium-containing graphene lithium ion battery cathode material according to claim 1, wherein the washing solutions in the fourth step are deionized water and ethanol respectively, and the washing sequence is that the deionized water is firstly washed for 3 times, and then the ethanol is washed for 3 times.
8. The preparation method of the magnesium-containing graphene lithium ion battery negative electrode material according to claim 1, wherein the heat treatment in the fifth step is: heating to 450 ℃ at a heating rate of 1-3 ℃/min in an inert gas atmosphere and keeping the temperature at 3-5 h.
9. The method for preparing the magnesium-containing graphene lithium ion battery anode material according to claim 8, wherein in the fifth step, the inert gas is any one of argon, nitrogen and helium.
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| CN102390825A (en) * | 2011-08-18 | 2012-03-28 | 青岛瀚博电子科技有限公司 | Modified lithium iron phosphate material for lithium ion battery and preparation method thereof |
| CN104923796B (en) * | 2015-06-11 | 2017-03-29 | 中国石油大学(北京) | A kind of method of preparation of industrialization graphene coated nanometer aluminium powder |
| CN106920932B (en) * | 2017-03-10 | 2019-12-03 | 上海应用技术大学 | A kind of leaf of bamboo shape Co (OH)2/ graphene combination electrode material and preparation method thereof |
| CN108598444B (en) * | 2018-06-11 | 2021-06-18 | 中南大学 | Vanadium trioxide/graphene composite negative electrode material of lithium ion battery and preparation method |
| CN109593985A (en) * | 2019-01-14 | 2019-04-09 | 宝鸡市金得利新材料有限公司 | A kind of graphene enhancing magnesium-based composite material preparation method |
| CN111952573A (en) * | 2020-08-25 | 2020-11-17 | 山东大学 | Graphene-manganese dioxide-loaded composite material and preparation method and application thereof |
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