WO2022032745A1 - Matériau composite vo2/mxene, son procédé de préparation et son utilisation - Google Patents
Matériau composite vo2/mxene, son procédé de préparation et son utilisation Download PDFInfo
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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
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Definitions
- the invention belongs to the technical field of nanomaterials, and in particular relates to a VO 2 /MXene composite material and a preparation method thereof.
- potassium ion batteries At present, with the continuous development of economy, lithium-ion batteries have been widely used in people's daily life. At the same time, the large consumption of metal lithium has caused people's concerns. Therefore, the development of new secondary alkali metal batteries has become the current research focus. It has been found that potassium ions are abundant on earth, more than 1,000 times that of lithium ions. Due to their relatively low cost, long cycle life, and high energy density, potassium ion batteries can meet the needs of the energy storage field. , is a new type of secondary alkali metal battery with great potential. Based on the above advantages, potassium ion battery is considered to be a promising large-scale electrochemical energy storage technology in the future, which is of great value to the development of new energy storage fields.
- the radius of potassium ions is larger than that of lithium ions, and the graphite anode materials that have been commercially used in lithium ion batteries cannot meet the rapid deintercalation of potassium ions due to their small interlayer spacing (0.335 nm).
- Anode materials for potassium-ion batteries with excellent cycle performance have become a research hotspot in this field.
- MXene is a new type of two-dimensional transition metal carbide or nitride, which stands out because of its unique physicochemical properties.
- this new material can be obtained by selective chemical etching, using HF to etch the A layer in the MAX phase to obtain an "accordion-like" MXene material with hydroxyl, oxygen, and fluorine functional groups on its surface, rich in chemical composition and abundant
- the functional groups of MXene give MXene a hydrophilic surface, excellent chemical properties, and good mechanical properties. However, its interlayer spacing is small, and the surface functional groups have certain adsorption properties, so the ideal rapid ion migration effect cannot be achieved when used alone.
- transition metal compounds have been widely studied due to their high reversible specific capacity.
- pure transition metal compounds generate huge volume expansion during the repeated de-intercalation process of potassium ions, resulting in the crushing and shedding of electrode materials and easy agglomeration. resulting in poor electrochemical performance.
- one of the objectives of the present invention is to provide a VO 2 /MXene composite material.
- Another object of the present invention is to provide a preparation method of the VO 2 /MXene composite material.
- the present invention provides an application of a VO 2 /MXene composite material, and the VO 2 /MXene composite material is applied to a negative electrode of a potassium ion battery.
- the present invention adopts following technical scheme:
- a preparation method of VO 2 /MXene composite material comprising the following steps:
- step (1) The vanadium source and the reducing agent are added to the dispersion liquid obtained in step (1) according to the molar ratio of 1:2-6, preferably 1:2-4, and more preferably 1:4-6, and stir 6-20h, such as 6h, 12h, 16h, 20h, to obtain a mixed solution;
- step (3) Transfer the mixed solution described in step (2) to the reaction kettle, put it in an oven, heat up to 110-240°C, such as 120°C, 150°C, 180°C, 220°C, and react for 10-30h, such as 10h , 15h, 20h, 24h, 28h, and then naturally cooled to room temperature to obtain a suspension;
- step (3) the suspension described in step (3) is centrifuged, and the filter residue is thoroughly cleaned with a cleaning agent to obtain a precipitate;
- step (4) the sediment described in step (4) is placed in a vacuum drying oven and dried to obtain a crude product
- step (6) the crude product described in step (5) is placed in a quartz boat, the quartz boat is placed in a tube furnace, a protective gas is introduced, and heated to 400-1100 DEG C at a heating rate of 5-8 DEG C/min, For example, at 400°C, 600°C, 800°C, and 1100°C, keep the temperature for 2-12h, such as 2h, 6h, 10h, 12h, and then naturally cool to room temperature to obtain VO 2 /MXene composite material.
- a protective gas is introduced, and heated to 400-1100 DEG C at a heating rate of 5-8 DEG C/min, For example, at 400°C, 600°C, 800°C, and 1100°C, keep the temperature for 2-12h, such as 2h, 6h, 10h, 12h, and then naturally cool to room temperature to obtain VO 2 /MXene composite material.
- the vanadium source is at least one of NH 4 VO 3 and NaVO 3 .
- the MXene is at least one of Ti 3 C 2 T x , V 3 C 2 T x , and Mo 3 N 2 T x , preferably Ti 3 N 2 T x , V 3 C 2 T x , Tx is a surface functional group -O, -F or -OH.
- the reducing agent is at least one of oxalic acid and ascorbic acid.
- the dispersant is at least one of N,N-dimethylformamide, ethanol, and ethylene glycol.
- step (3) the dispersion liquid is transferred to the reaction kettle, put into an oven, heated to 110-240°C, preferably 150-200°C, such as 130°C, 150°C, 180°C, and reacted for 10-30h , preferably 15-24h, such as 10, 14, 18, 20, 30h.
- the protective gas is Ar or N 2
- the gas flow rate is 150-300ml/min, such as 170ml/min, 190ml/min, 200ml/min, 220ml/min, 240ml/min, 260ml/min, 280ml/min , 300ml/min.
- the cleaning agent is at least one of water and ethanol, preferably, the suspension obtained in step (3) is thoroughly cleaned with deionized water and absolute ethanol, and deionized water and absolute ethanol can be used for alternate cleaning 3-10 times, preferably 4-7 times.
- the rotational speed used for centrifugation in step (4) is 4000-8000r/min, preferably 6000r/min, and the centrifugation time is 4-8min, preferably 6min.
- the temperature of vacuum drying in step (5) is 50-70°C, preferably 60°C, and the drying time is 5-12h, preferably 10h, such as 6h, 8h, 10h, 12h.
- the degree of vacuum does not exceed 131Pa, preferably 130Pa, 125Pa, 100Pa, 90Pa.
- the loading amount of VO 2 in the VO 2 /MXene composite material is 40-180wt%, preferably 40-100wt%, 80-130wt%, 100-180wt%.
- a potassium ion battery negative electrode comprising the VO 2 /MXene composite material prepared by the above preparation method.
- a potassium ion battery comprising the above-mentioned battery negative electrode.
- the VO 2 /MXene composite material of the present invention can effectively suppress the volume expansion of the electrode material during the cycle, prevent the VO 2 material from falling off and agglomeration, improve the cycle stability, increase the Reversible specific capacity; compared with pure MXene material, VO 2 material can grow crystals between MXene layers, which is beneficial to the increase of interlayer spacing and the expansion of specific surface area. It can be seen that VO 2 material and MXene material have a synergistic effect.
- the VO 2 /MXene composite material of the present invention exhibits good electrical conductivity, high reversible specific capacity, and excellent cycle stability.
- the composite material of the present invention has low cost of raw materials, high production efficiency and simple preparation method, and has great practical significance for the large-scale development and application of potassium ion batteries.
- Fig. 1 is the scanning electron microscope image of VO 2 /MXene composite material in embodiment 3;
- Fig. 2 is the cycle performance diagram measured under the current density of 100mA/g of potassium ion battery assembled with VO 2 /Mxene composite material in Example 3;
- Figure 3 is a graph of the cycle performance measured at a current density of 100 mA/g for a potassium-ion battery assembled with a pure VO 2 material in Comparative Example 1;
- Figure 4 is a graph of the cycle performance of the potassium-ion battery assembled with pure MXene material in Comparative Example 2 at a current density of 100 mA/g.
- the Ti 3 C 2 T x nanoparticles were purchased from Beijing Beike New Material Technology Co., Ltd., number BK2020011814, size: 1-5 ⁇ m, purity: 99%, product application fields: energy storage, catalysis, analytical chemistry, etc.
- a preparation method of VO 2 /MXene composite material comprising the following steps:
- step (1) (2) adding 0.3 mol NH 4 VO 3 and 0.6 mol oxalic acid to the dispersion described in step (1), and stirring for 6 hours to obtain a mixed solution;
- step (3) transferring the mixed solution of step (2) into a reaction kettle with a capacity of 50ml and sealing, placing it in an oven, heating to 110°C, keeping the temperature for 12h, and then cooling to room temperature to obtain a suspension;
- step (3) the suspension described in step (3) was centrifuged for 4 minutes under the condition of 4000r/min, and the filter residue was washed 3 times with deionized water and absolute ethanol alternately, and the precipitate was collected;
- step (4) drying the precipitate obtained in step (4) in a vacuum drying oven at a drying temperature of 60° C. and a drying time of 6 hours to obtain a crude product;
- step (6) the crude product obtained in step (5) is placed in a quartz boat, the quartz boat is placed in a tube furnace, high-purity Ar is introduced, and the flow rate is 150ml/min, and heated to 400 °C with a heating rate of 5°C/min °C, kept for 3h, and then naturally cooled to room temperature to obtain VO 2 /MXene composites.
- the electrochemical test of the VO 2 /MXene composite prepared in this example shows that at a current density of 100 mA/g, after 100 cycles, the reversible specific capacity is 338 mAh/g, which is a pure VO 2 (103.6 mAh/g ) is 3.26 times that of undoped MXene (61.1 mA h/g), and 5.5 times that of undoped MXene (61.1 mA h/g), and the VO 2 /MXene composite in this example exhibits excellent potassium storage performance.
- a preparation method of VO 2 /MXene composite material comprising the following steps:
- step (2) adding 0.5mol NH 4 VO 3 and 2mol oxalic acid to the dispersion described in step (1), and stirring for 14 hours to obtain a mixed solution;
- step (3) transfer the mixed solution obtained in step (2) into a reaction kettle with a capacity of 50ml and seal it, place it in an oven, heat to 180°C, keep the temperature for 20h, and then cool to room temperature to obtain a suspension;
- step (3) the suspension obtained in step (3) is centrifuged for 6 minutes under the condition of 6000 r/min, and after alternately washing the filter residue 3 times with deionized water and absolute ethanol, the precipitate is collected;
- step (4) drying the precipitate obtained in step (4) in a vacuum drying oven at a drying temperature of 60° C. and a drying time of 9 hours to obtain a crude product;
- step (6) place the crude product obtained in step (5) in a quartz boat, place the quartz boat in a tube furnace, feed high-purity Ar, flow rate is 220ml/min, heat to 800 with a heating rate of 7°C/min °C, kept for 8 h, and then naturally cooled to room temperature to obtain VO 2 /MXene composites.
- the electrochemical test of the VO 2 /MXene composite prepared in this example shows that at a current density of 100 mA/g and 100 cycles, the reversible specific capacity is 466 mAh/g, which is a pure VO 2 (103.6 mAh/g ) is 4.50 times that of undoped MXene (61.1 mA h/g), and 7.6 times that of undoped MXene (61.1 mA h/g), and the VO 2 /MXene composite in this example exhibits excellent potassium storage performance.
- a preparation method of VO 2 /MXene composite material comprising the following steps:
- step (2) adding 0.5mol NH 4 VO 3 and 3mol oxalic acid to the dispersion described in step (1), and stirring for 20 hours to obtain a mixed solution;
- step (3) transferring the mixed solution obtained in step (2) into a reaction kettle with a capacity of 50ml and sealing, placing it in an oven, heating to 240° C., keeping the temperature for 24h, and then cooling to room temperature to obtain a suspension;
- step (3) the suspension obtained in step (3) was centrifuged for 8 minutes under the condition of 8000 r/min, and after alternately washing the filter residue 3 times with deionized water and absolute ethanol, the precipitate was collected;
- step (4) drying the precipitate obtained in step (4) in a vacuum drying oven at a drying temperature of 60° C. and a drying time of 12 hours to obtain a crude product;
- step (6) place the crude product obtained in step (5) in a quartz boat, place the quartz boat in a tube furnace, feed high-purity Ar, flow rate is 300ml/min, heat to 1000 with a heating rate of 8°C/min °C, kept for 10 h, and then naturally cooled to room temperature to obtain VO 2 /MXene composites.
- the electrochemical test of the VO 2 /MXene composite prepared in this example shows that the reversible specific capacity is 421mAh/g after 100 cycles at a current density of 100mA/g, which is a pure VO 2 (103.6mAh/g) ) is 4.06 times that of undoped MXene (61.1 mA h/g), and the VO 2 /MXene composite in this example exhibits excellent potassium storage performance.
- the preparation method of pure VO material includes the following steps:
- step (2) The dispersion liquid obtained in step (1) is transferred into a reaction kettle with a capacity of 50ml, sealed and placed in an oven, heated to 240° C., maintained for 24h, and then cooled to room temperature;
- step (3) the product obtained in step (2) was washed 3 times with deionized water and dehydrated alcohol alternately, and centrifuged for 8 minutes under the condition of 8000 r/min with a centrifuge;
- step (3) Drying the centrifuged product obtained in step (3) in a vacuum drying oven at a drying temperature of 60° C. and a drying time of 12 hours.
- step (4) placing the product obtained in step (4) in a quartz boat, placing the quartz boat in a tube furnace, feeding high-purity Ar, the flow rate of 300ml/min, and heating to 1000°C with a temperature increase rate of 8°C/min , kept for 10h, and then naturally cooled to room temperature to obtain the VO 2 composite material.
- the electrochemical test of the VO 2 material prepared in this comparative example shows that the reversible specific capacity is 103.6mAh/g after 100 cycles at a current density of 100mA/g.
- Figure 1 is the scanning electron microscope image of the VO 2 /MXene composite material in Example 3. It can be seen from Figure 1 that the VO 2 nanomaterial in the VO 2 /MXene composite material is uniformly distributed on the surface of the MXene material sheet, and the VO 2 nanomaterial is 20nm. Around, the VO2 nanomaterials are well combined with the matrix, which can expand the distance between the lamellae without agglomeration, indicating that the layered structure of the VO2/ MXene composite was successfully prepared and effectively increased the interlayer spacing and specific surface area.
- Figures 2-4 are graphs of the cycle performances of the potassium ion batteries of Example 3, Comparative Example 1, and Comparative Example 2 measured at a current density of 100 mA/g, respectively.
- the VO2/ MXene composites show high battery capacity and good cycling performance compared to the pure VO2 material.
- the potassium-ion battery assembled with MXene material exhibits good cycling stability during charge-discharge at a current density of 100 mA/g, but has a small specific capacity.
- the layered structure of the VO 2 /MXene material contributes to the specific surface area and the active sites for ion attachment in the electrolyte, there is van der Waals force between the VO 2 material and MXene, and the surface functional groups can form chemical bonds with the material; compared with pure MXene materials , VO2 material can grow crystals between MXene layers, which is beneficial to the increase of interlayer spacing, enlarges the specific surface area, prevents agglomeration by interaction, still maintains stable capacity after 200 cycles, and larger transfer and ion adsorption area, double
- the electric layer capacitance has good performance, which improves the ability to store potassium ions and significantly increases the specific capacity of the material. It can be seen that the VO2 material has a synergistic effect with the MXene material.
- test methods are:
- the specific surface area was measured by the BET specific surface area test method, and the VO2 load was analyzed by X-ray energy dispersive spectroscopy (EDS).
- the performance test results of each group are shown in Table 1.
Abstract
La présente invention concerne un matériau composite VO2/MXene et son procédé de préparation. Le procédé de préparation comprend les étapes suivantes : (1) ajouter un matériau de MXene dans un dispersant pour formuler une solution de dispersion ayant une concentration de 10 à 100 mg/mL, puis agiter celle-ci pendant 1 à 6 h; (2) ajouter une source de vanadium et un réducteur dans la solution de dispersion de l'étape (1) selon un rapport molaire de 1 : 2 à 6, et l'agiter pendant 6 à 20 h pour obtenir une solution mixte; (3) faire réagir la solution mixte de l'étape (2) à 110-240 °C pendant 10 à 30 h, et refroidir pour obtenir une suspension; (4) laver la suspension de l'étape (3) au moyen d'un détergent, centrifuger celle-ci à 4000-8000 r/min pendant 4-8 min, et collecter le précipité; (5) sécher le précipité de l'étape (4) pour obtenir un produit brut; et (6) chauffer le produit brut de l'étape (5) à 400-1100 °C à une vitesse de chauffage de 5-8 °C/min dans une atmosphère protectrice, maintenir la température pendant 2 à 12 min, et refroidir celle-ci, de façon à obtenir le matériau composite VO2/MXene. Ledit composite présente d'excellentes performances de vitesse, une capacité spécifique réversible supérieure et une bonne stabilité de cyclage.
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CN114784455A (zh) * | 2022-04-06 | 2022-07-22 | 山东大学 | 一种隔膜及其制备方法与电池应用 |
CN115020115A (zh) * | 2022-07-15 | 2022-09-06 | 东华理工大学 | 一种基于水热法合成的电极复合材料及其制备方法 |
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CN113461013B (zh) * | 2021-07-01 | 2022-09-06 | 中国科学院上海硅酸盐研究所 | 一种自组装MXene非晶化纳米片超结构及其制备方法 |
CN114314664B (zh) * | 2021-11-30 | 2023-09-29 | 松山湖材料实验室 | 钒氧化物包覆碳化物复合材料及其制备方法和应用 |
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