Super capacitor composite material and preparation method thereof, super capacitor and electric equipment
By fixing single-crystal FeLaO3 particles with holes distributed on the surface on a two-dimensional metal carbonized material to form a FeLaO3@CC structure, the problem of difficult balance of load and performance of electrode materials in the prior art is solved, and the performance and life of the supercapacitor is significantly improved.
Patent Information
- Application Number
- CN202411851120.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-16
- Publication Date
- 2025-03-07
AI Technical Summary
The prior art faces challenges in developing supercapacitor electrode materials that are high-load but still maintain high performance, especially in nano-scale material designs, where it is difficult to achieve a good balance of area and volume and weight performance.
A composite material of two-dimensional metal carbonized material and single-crystal FeLaO3 particles with holes distributed on the surface is used to form a FeLaO3@CC structure by fixing the single-crystal FeLaO3 particles on the two-dimensional metal carbonized material to improve the specific surface area and electrochemical properties of the electrode material.
It realizes the load capacity of the electrode material while maintaining high performance, significantly improves the energy density and power density of the supercapacitor, and extends its service life.
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Figure CN119581237A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of capacitor materials, and in particular relates to a supercapacitor composite material and a preparation method thereof, a supercapacitor and electrical equipment. Background Art
[0002] Supercapacitors occupy an important position in modern energy storage technology. With its advantages of fast charging and discharging, long life and high power density, they are widely used in various electronic devices and power systems. The performance of supercapacitors depends largely on the characteristics of their electrode materials, so the development of high-performance electrode materials has become a research focus in this field. The selection and design of electrode materials directly affect the energy density and cycle life of supercapacitors, so the scientific community has been committed to finding materials with excellent electrochemical properties to meet the growing market demand.
[0003] In the existing technology, researchers mainly focus on reducing electrode materials to nanoscale, hoping to improve electrochemical activity by increasing the surface area of the material. However, although these nanoscale electrode materials have high activity in theory, they face a series of challenges in practical application. The electrochemical activity load of current nanoscale materials is usually low, often less than 1 mg cm -2 , which is comparable to the approximately 10 mg cm required for commercial applications. -2 This makes the capacitance per unit area limited and difficult to meet the requirements of high energy density. In addition, as the material mass loading increases, the thickness of the electrode increases, resulting in limited ion diffusion and a rapid decrease in electrochemical performance, thus limiting the possibility of increasing the area capacitance by increasing the mass loading.
[0004] For these reasons, existing technologies face significant challenges in developing electrodes that can withstand high loads while still maintaining high performance. Traditionally, people have focused more on weight performance metrics, but for space-constrained systems such as power supplies for wearable electronic devices, area and volume performance metrics are more important. Recent studies have shown that area and volume performance metrics are as important as weight performance metrics in many applications, but the balance between the two is difficult to achieve in existing nanoscale material designs.
[0005] In summary, the existing technology has many defects in the development of supercapacitor electrode materials. Although nanoscale materials have high electrochemical activity in theory, the load in practical applications is low and it is difficult to meet the requirements of commercial applications. As the material mass load increases, the increase in electrode thickness leads to limited ion diffusion and a rapid decrease in electrochemical performance. In addition, area and volume performance indicators are more important than weight performance indicators in many applications, but it is difficult for existing technologies to achieve a good balance in these aspects. These problems indicate that further research and innovation are needed to develop electrode materials that can meet both high load and high performance requirements in order to promote the further development of supercapacitor technology. Summary of the invention
[0006] In order to solve the above problems, the present invention provides a supercapacitor composite material, comprising: a two-dimensional metal carbonization material, and a single crystal FeLaO fixed on the surface of the two-dimensional metal carbonization material. 3 Particles;
[0007] Wherein, the single crystal FeLaO 3 The particles are single crystal particles with holes distributed on the surface.
[0008] Preferably, the supercapacitor composite material is a particle structure, and the outer surface of the two-dimensional metal carbonized material particle is provided with a plurality of single crystal FeLaO 3 Particles.
[0009] Preferably, the supercapacitor composite material is a layered composite structure; in the layered composite structure, the single crystal FeLaO 3 Particles grow in the two-dimensional metal carbonization material and on the surface of the two-dimensional metal carbonization material, forming a series connection in the two-dimensional metal carbonization material to form a porous network structure.
[0010] Preferably, the single crystal FeLaO 3 The distribution density of particles on the surface of the two-dimensional metal carbonized material is not less than 10 mg cm -2 .
[0011] In addition, in order to solve the above problems, the present invention also provides a method for preparing the supercapacitor composite material as described above, comprising:
[0012] The two-dimensional metal carbide material is washed and dried to obtain a dry sheet;
[0013] soaking the dried sheet in a nitrogen-methylpyrrolidone solution to obtain an impregnated material;
[0014] In an organic solvent, lanthanum salt and iron salt are added and dissolved to obtain a precursor salt mixture;
[0015] placing the infiltration material into the precursor salt mixture, so that the precursor salt mixture melts on the surface of the infiltration material to obtain an intermediate product;
[0016] The intermediate product is subjected to a high temperature and high pressure heat preservation treatment, and then subjected to a calcination treatment after cooling, so as to obtain the composite material;
[0017] Preferably, the iron salt comprises at least one of ferric nitrate, ferric chloride and ferric oxalate;
[0018] Preferably, the lanthanum salt comprises at least one of lanthanum chloride, lanthanum nitrate, lanthanum sulfate, lanthanum carbonate and lanthanum hexaboride;
[0019] Preferably, the organic solvent comprises at least one of n-pentane, petroleum ether, isopropyl ether, isobutanol, tetrahydrofuran, pyridine, aniline and acetonitrile;
[0020] Preferably, the amount of the iron salt and the lanthanum salt added to the precursor salt mixture is 0.3 mmol to 0.9 mmol;
[0021] Preferably, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is (3-1):(1-3);
[0022] Preferably, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is 1:1.
[0023] Preferably, the two-dimensional metal carbide material is washed and dried to obtain a dry sheet, comprising:
[0024] Taking the two-dimensional metal carbide material, and washing it repeatedly with ethanol and water alternately;
[0025] Carrying out a drying process under a protective atmosphere to obtain the dried sheet;
[0026] Preferably, the temperature of the drying process is not less than 60°C.
[0027] Preferably, the high temperature and high pressure insulation treatment has the following treatment conditions:
[0028] The insulation temperature is 160℃~220℃;
[0029] The insulation time is not less than 48 hours.
[0030] Preferably, the calcination treatment is carried out under the following conditions:
[0031] The calcination temperature is 500°C to 800°C;
[0032] The calcination time is 12 to 24 hours.
[0033] In addition, the present invention also provides a supercapacitor, which is prepared using the supercapacitor composite material as described above.
[0034] In addition, the present invention also provides an electrical device, including the supercapacitor as described above.
[0035] The present invention provides a supercapacitor composite material and a preparation method thereof, a supercapacitor and electrical equipment. The supercapacitor composite material comprises: a two-dimensional metal carbonization material, and a single crystal FeLaO fixed on the surface of the two-dimensional metal carbonization material. 3 Particles; wherein the single crystal FeLaO 3 The particles are single crystal particles with holes distributed on the surface. The supercapacitor composite material provided by the present invention is prepared by 3 Fixed on two-dimensional metal carbide to form FeLaO 3 @CC, Single crystal eliminates the grain boundaries that cause electron scattering, thereby achieving improved electronic conductivity, single crystal FeLaO 3 The surface of the material is distributed with holes, which greatly increases the specific surface area and can further increase the load, thereby achieving the goal of increasing the load while maintaining high performance. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Figure 1 This is an electron microscope schematic diagram of the supercapacitor composite material in the embodiment of the present application;
[0037] Figure 2 This application aims to investigate the room temperature cycling performance of FeLaO3@CC material. DETAILED DESCRIPTION
[0038] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0039] refer to Figure 1 In an embodiment of the present application, a supercapacitor composite material is provided, comprising: a two-dimensional metal carbonized material, and a single crystal FeLaO fixed on the surface of the two-dimensional metal carbonized material. 3 Particles;
[0040] Wherein, the single crystal FeLaO 3 The particles are single crystal particles with holes distributed on the surface.
[0041] As mentioned above, the composition of the supercapacitor composite material includes a two-dimensional metal carbon material and a single crystal FeLaO fixed on its surface. 3Among them, the performance of supercapacitors is improved through nanoscale material design and specific preparation methods.
[0042] First, the two-dimensional metal carbon material itself has excellent conductivity. 3 The particles are fixed on the surface of the two-dimensional metal carbide material, which can utilize the high conductivity of the two-dimensional metal carbide material to improve the conductivity of the entire electrode material, thereby reducing the internal resistance of the electrode and improving the overall electrochemical performance of the electrode.
[0043] Secondly, the two-dimensional metal carbide material has high strength and high modulus mechanical properties, which can provide a single crystal FeLaO 3 The particles provide stable mechanical support. This can effectively prevent the single crystal particles from falling off and structural changes during the charge and discharge process, maintaining the stability and long life of the electrode material.
[0044] Again, single crystal FeLaO 3 The distribution of particles on the surface of the two-dimensional metal carbon material can transform the two-dimensional structure into a three-dimensional structure, which is conducive to the transmission and diffusion of electrolyte ions in the electrode material. Such a structural design is conducive to improving the fast charging and discharging performance of supercapacitors.
[0045] Single crystal FeLaO 3 The particles are fixed on the surface of the two-dimensional metal carbon material, which can effectively improve the electrochemical performance of the electrode material. The high conductivity of the two-dimensional metal carbon material and the single crystal FeLaO 3 This, combined with the high electrochemical activity of the particles, can significantly increase the energy density and power density of capacitors.
[0046] Single crystal FeLaO 3 The distribution of particles on the surface of the two-dimensional metal carbonized material increases the specific surface area of the electrode material. The larger specific surface area provides more electrochemical active sites, thereby increasing the capacitance of the electrode material.
[0047] Two-dimensional metal carbide materials as substrate materials can be single crystal FeLaO 3 The particles provide good mechanical support to prevent them from falling off during the cyclic charge and discharge process. This maintains the structural integrity of the electrode material and extends the service life of the supercapacitor.
[0048] Single crystal FeLaO 3 The particles are distributed on the surface of the two-dimensional metal carbonized material, and the porous structure formed helps to optimize the energy storage and release performance of the electrode material during the charging and discharging process. Such a structural design can improve the charging and discharging efficiency and energy utilization of supercapacitors.
[0049] Two-dimensional metal carbide materials have excellent mechanical properties and chemical stability and can remain stable during long-term cyclic use. 3 The particles are fixed on the surface of two-dimensional metal carbonized materials, which can significantly improve the cycle stability of electrode materials, reduce performance degradation, and enhance the reliability of supercapacitors.
[0050] In summary, single crystal FeLaO 3 The particles are fixed on the surface of two-dimensional metal carbide materials, which can fully utilize the advantages of both and significantly improve the electrochemical performance, structural stability and cycle life of supercapacitors, providing an effective solution for the development of high-performance supercapacitors.
[0051] In the single crystal FeLaO 3 The surface of the particles is densely covered with a large number of holes, which are used to: 3 The pores distributed on the particle surface significantly increase the specific surface area of the material. A larger specific surface area can provide more active sites, allowing the electrode material to contact more electrolyte ions during the electrochemical reaction, thereby increasing the capacitance of the capacitor.
[0052] The pore structure facilitates the diffusion of electrolyte ions within the material. When the traditional non-porous granular material is highly loaded, the ion diffusion is limited and the electrochemical performance decreases. The presence of pores can form more diffusion channels, reduce the resistance of the ion diffusion path, thereby increasing the diffusion rate of ions and enhancing the electrochemical performance of the material.
[0053] The pore structure can relieve the stress caused by volume change of the electrode material during the charge and discharge process, thereby improving the mechanical stability and cycle life of the material. The pores can act as a buffer zone, reducing the mechanical stress caused by volume change and helping to maintain the structural integrity of the electrode material.
[0054] Single crystal FeLaO with holes distributed on the surface 3 Particles can effectively increase the specific surface area and ion diffusion rate of the material, so that the electrode material can still maintain good electrochemical performance under high load. Compared with traditional materials, this structural design significantly improves the energy density and power density of the capacitor.
[0055] The pore structure allows electrolyte ions to more fully contact the electrode material, improving the utilization of active materials. The increase in material utilization means that a higher capacitance can be obtained under the same material weight, thereby improving the overall performance of the supercapacitor.
[0056] The pore structure helps to relieve the mechanical stress of the electrode material during the charge and discharge cycle, and improves the cycle stability and life of the material. This is particularly important for supercapacitors in practical applications, which can provide longer service life and higher reliability.
[0057] The structure with holes on the surface can optimize the energy storage and release performance of the electrode material during the charge and discharge process. The holes provide more electrochemically active sites, making the charge and discharge process more efficient, thereby improving the performance of the supercapacitor.
[0058] In summary, the single crystal FeLaO 3 The characteristic of "single crystal particles with holes on the surface" plays a key role in improving the electrochemical performance, material utilization, cycle life and energy storage efficiency of supercapacitor composite materials. This design combines the advantages of nanomaterials and pore structures, providing strong technical support for the development of high-performance supercapacitors.
[0059] The above-mentioned two-dimensional metal carbonized material can be a MXene material, such as a MXene sheet, which is a two-dimensional (2D) material having a layered structure similar to graphene. MXene is a general term for transition metal carbides, nitrides or carbonitrides, and its general formula is M n +1X n , where "M" represents transition metals, such as titanium (Ti), tantalum (Ta), hafnium (Hf), etc.; "X" represents carbon (C) or nitrogen (N). Among them, the most common MXene material is titanium carbide (Ti 3 C 2 ), but there are many other types of MXene materials that have been synthesized and studied.
[0060] Attach or directly grow FeLaO on two-dimensional metal carbide materials (such as Mxene) 3 This effective method can promote the transport of ions and electrons by reducing the resistance of the active material / current collector interface.
[0061] As mentioned above, supercapacitor, also known as electrochemical capacitor or double-layer capacitor, is a high-performance energy storage device. It combines the advantages of traditional capacitors and batteries, and has the characteristics of high power density, fast charge and discharge, and long cycle life. Supercapacitors have been widely used in many applications that require fast energy transfer and high power output, such as hybrid vehicles, renewable energy systems, backup power supplies, and portable electronic devices. In the embodiments of the present application, the supercapacitor composite material can be used to prepare a supercapacitor.
[0062] In summary, the supercapacitor composite material provided by the present invention is prepared by 3Fixed on two-dimensional metal carbide to form FeLaO 3 @CC, Single crystal eliminates the grain boundaries that cause electron scattering, thereby achieving improved electronic conductivity, single crystal FeLaO 3 The surface of the material is distributed with holes, which greatly increases the specific surface area and can further increase the load, thereby achieving the goal of increasing the load while maintaining high performance.
[0063] In one embodiment, the supercapacitor composite material is a particle structure, and the outer surface of the two-dimensional metal carbonized material particle is provided with a plurality of single crystal FeLaO having a porous structure. 3 Particles.
[0064] The supercapacitor composite material can be a particle structure, and each particle can include a core part, that is, a two-dimensional metal carbide material particle, and a plurality of single crystal FeLaO 3 Particles, the single crystal FeLaO 3 The particles have a porous structure.
[0065] In another embodiment, the supercapacitor composite material is a layered composite structure; in the layered composite structure, the single crystal FeLaO 3 Particles grow in the two-dimensional metal carbonization material and on the surface of the two-dimensional metal carbonization material, forming a series connection in the two-dimensional metal carbonization material to form a porous network structure.
[0066] As mentioned above, in the supercapacitor composite material, a two-dimensional metal carbon material with a plate structure and a single crystal FeLaO distributed on the surface of the two-dimensional metal carbon material may be included. 3 Particles. Among them, single crystal FeLaO 3 Adhere to the surface of the two-dimensional metal carbon material and penetrate into the two-dimensional metal carbon material during the preparation process. The two-dimensional metal carbon material can be, for example, a MXene material, i.e., single crystal FeLaO 3 Growing and attaching to the MXene sheet, thus forming single-crystalline FeLaO in and on the surface of the MXene sheet 3 The particles are connected in series to form a porous network structure.
[0067] Furthermore, the single crystal FeLaO 3 The distribution density of particles on the surface of the two-dimensional metal carbonized material is not less than 10 mg cm -2 .
[0068] In addition, the present application also provides a method for preparing the supercapacitor composite material as described above, comprising:
[0069] Step S1, washing and drying the two-dimensional metal carbide material to obtain a dry sheet;
[0070] Step S2, soaking the dried sheet in a nitrogen methyl pyrrolidone solution to obtain an impregnated material.
[0071] Step S3, adding lanthanum salt and iron salt into an organic solvent, and obtaining a precursor salt mixture after dissolution.
[0072] Step S4, placing the infiltration material into the precursor salt mixture, allowing the precursor salt mixture to melt on the surface of the infiltration material to obtain an intermediate product.
[0073] Step S5, subjecting the intermediate product to a high temperature and high pressure heat preservation treatment, and then subjecting it to a calcination treatment after cooling, so as to obtain the composite material.
[0074] Further, the iron salt includes at least one of ferric nitrate, ferric chloride and ferric oxalate;
[0075] Further, the lanthanum salt includes at least one of lanthanum chloride, lanthanum nitrate, lanthanum sulfate, lanthanum carbonate and lanthanum hexaboride;
[0076] Further, the organic solvent includes at least one of n-pentane, petroleum ether, isopropyl ether, isobutanol, tetrahydrofuran, pyridine, aniline and acetonitrile;
[0077] Further, the amount of the iron salt and the lanthanum salt added to the precursor salt mixture is 0.3 mmol to 0.9 mmol;
[0078] Further, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is (3-1):(1-3);
[0079] Furthermore, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is 1:1.
[0080] Furthermore, the two-dimensional metal carbide material is washed and dried to obtain a dry sheet, comprising:
[0081] Taking the two-dimensional metal carbide material, and washing it repeatedly with ethanol and water alternately;
[0082] Carrying out a drying process under a protective atmosphere to obtain the dried sheet;
[0083] Furthermore, the temperature of the drying process is not less than 60°C.
[0084] Furthermore, the high temperature and high pressure insulation treatment has the following treatment conditions:
[0085] The insulation temperature is 160°C to 220°C; for example, it can be 160°C, 180°C, 200°C, 210°C, 220°C, etc.
[0086] The insulation time is not less than 48 hours.
[0087] Furthermore, the calcination treatment is carried out under the following conditions:
[0088] The calcination temperature is 500°C to 800°C; for example, it can be 500°C, 600°C, 700°C, 800°C, etc.
[0089] The calcination time is 12 hours to 24 hours, for example, 12 hours, 16 hours, 18 hours, 20 hours, 24 hours, etc.
[0090] In addition, a supercapacitor is provided in an embodiment of the present application, which is prepared using the supercapacitor composite material as described above.
[0091] In addition, an electrical device is also provided in an embodiment of the present application, including the supercapacitor as described above.
[0092] The present invention is further described below by means of specific examples, but it should be understood that these examples are only used for more detailed description and should not be construed as limiting the present invention in any form.
[0093] Embodiment 1:
[0094] In this embodiment, a supercapacitor composite material was prepared by the following method. The parameters of each component in the preparation are shown in Table 2 and Table 3.
[0095] Experimental methods:
[0096] S1. Wash the Mxene sheet (two-dimensional metal carbonized material) alternately with ethanol and deionized water three times, and then completely dry it at 60 °C in a nitrogen atmosphere;
[0097] S2. Soak Mxene in 50 mL of nitrogen methyl pyrrolidone solution to fully wet it. The nominal size of a piece of two-dimensional metal carbonization material is 2 cm × 4 cm.
[0098] S3. Add x mmol FeCl to the organic solvent. 3 (iron salt) and LaCl 3 (lanthanum salt) precursor salt (x = 0.3) to form a precursor salt mixture. Among them, FeCl 3 With LaCl 3 The molar ratio of nitrate to carbon is 1:1. After the nitrate is completely melted and wets the two-dimensional metal carbonized material, it is transferred to a high-temperature and high-pressure reactor and kept at 200°C for 48 hours.
[0099] S4. After the product in the reaction kettle is cooled, it is transferred to a crucible and calcined at 600° C. for 18 hours to obtain the supercapacitor composite material.
[0100] Embodiment 2:
[0101] In this embodiment, a supercapacitor composite material is prepared by the method in Embodiment 1. The preparation method is basically the same as that in Embodiment 1, except that: x=0.6.
[0102] Embodiment 3:
[0103] In this embodiment, a supercapacitor composite material is prepared by the method in Embodiment 1. The preparation method is basically the same as that in Embodiment 1, except that: x=0.9.
[0104] Embodiment 4:
[0105] In this embodiment, a supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that: FeCl 3 With LaCl 3 The molar ratio is 1:2.
[0106] Embodiment 5:
[0107] In this embodiment, a supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that: FeCl 3 With LaCl 3 The molar ratio is:3:1.
[0108] Embodiment 6:
[0109] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that: FeCl 3 With LaCl 3 The molar ratio is: 1:3.
[0110] Embodiment 7:
[0111] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the short temperature in step S4 was 800°C.
[0112] Embodiment 8:
[0113] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was n-pentane.
[0114] Embodiment 9:
[0115] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was petroleum ether.
[0116] Embodiment 10:
[0117] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was isopropyl ether.
[0118] Embodiment 11:
[0119] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was isobutanol.
[0120] Embodiment 12:
[0121] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was pyridine.
[0122] Embodiment 13:
[0123] A supercapacitor composite material was prepared by the method in Example 1. The preparation method was basically the same as that in Example 1, except that the organic solvent was aniline.
[0124] Horizontal comparison test:
[0125] Experimental methods:
[0126] For the supercapacitor composite material prepared in the embodiment and the comparative example, a specific surface area test is performed, and the supercapacitor composite material is coated on a current collector and dried to form an electrode. Two electrodes (positive and negative electrodes) are assembled into a supercapacitor unit together with components such as an electrolyte and a diaphragm. Cyclic voltammetry (CV), constant current charge and discharge test (GCD), electrochemical impedance spectroscopy (EIS) and other tests are performed in the supercapacitor unit to evaluate its electrochemical performance.
[0127] (1) Cyclic voltammetry (CV): This is a technique used to study electrochemical systems by varying the voltage and measuring the current response. In a CV test, the voltage varies in a triangular waveform, and the surface capacitance of the material can be calculated by measuring the change in current.
[0128] (2) Constant current charge and discharge test (GCD): In this test, the supercapacitor is charged and discharged at a constant current, and the surface capacitance is calculated by measuring the change in voltage.
[0129] (3) Electrochemical impedance spectroscopy (EIS): The electrical conductivity of a material can be analyzed by measuring the impedance of the system under a small amplitude AC voltage.
[0130] (4) Nitrogen adsorption-desorption isotherm test: This is a physical adsorption technique that determines the specific surface area of the material by measuring the amount of nitrogen adsorbed at different pressures.
[0131] Experimental results and analysis:
[0132] Table 4 Performance test results of batteries prepared in Examples and Comparative Examples
[0133] Serial number <![CDATA[Surface capacitance (F·cm -2 )]]> <![CDATA[Equivalent resistance (Ω·cm -2 )]]> <![CDATA[BET(m 2 / g)]]> Example 1 9.77 4.60 65..9 Example 2 8.91 10.56 63.5 Example 3 11.02 2.08 67.1 Example 4 9.25 3.25 60.2 Example 5 4.23 7.65 57.5 Example 6 6.20 4.12 57.8 Example 7 2.35 6.22 59.1 Example 8 4.65 7.46 51.2 Example 9 5.19 5.09 52.0 Example 10 4.26 5.23 60.1 Embodiment 11 7.19 7.26 63.2 Example 12 5.28 4.65 59.4 Embodiment 13 5.22 8.23 52.3
[0134] analyze:
[0135] According to the data in Table 4 and reference Figure 2 The performance test results of the supercapacitor composite materials prepared in Examples 1 to 13 are listed, including the surface capacitance (F·cm -2 ), equivalent resistance (Ω·cm -2 ) and specific surface area (BET, m 2 / g).
[0136] Surface capacitance (F·cm -2 ) aspect: Example 3 has the highest surface capacitance, reaching 11.02F·cm -2 , while the surface capacitance of Example 7 is the lowest, which is 2.35F·cm -2 This indicates that different preparation conditions, such as the molar ratio of precursor salts and calcination temperature, have a significant impact on the electrochemical properties of the materials.
[0137] In the equivalent resistance (Ω·cm -2 ) aspect: Example 3 also exhibits the lowest equivalent resistance, which is 2.08Ω·cm -2 , while the equivalent resistance of Example 2 is the highest, which is 10.56Ω·cm -2 This shows that different preparation conditions have a direct impact on the electronic transport properties of the material.
[0138] In terms of specific surface area (BET, m 2 / g): Example 1 has the highest specific surface area, which is 65.9 m 2 / g, while the specific surface area of Example 7 is the lowest, which is 59.1m 2 This may be related to the calcination temperature and the choice of organic solvent, which may affect the pore structure of the material.
[0139] Although all embodiments achieved the desired technical effects, there were differences in performance between the different embodiments. These differences indicate that by adjusting the preparation parameters, such as the molar ratio of the precursor salt, the calcination temperature and the choice of the organic solvent, the performance of the material can be optimized to achieve higher area capacitance, lower equivalent resistance and better specific surface area.
[0140] The above are preferred implementation modes and corresponding embodiments of the present invention. It should be pointed out that, for those skilled in the art, without departing from the creative concept of the present invention, several modifications and improvements may be made, including but not limited to the adjustment of proportions, processes, dosages and reaction vessels, which all fall within the scope of protection of the present invention.
Claims
1. A supercapacitor composite material, characterized in that: include: A two-dimensional metal carbide material, and single crystal FeLaO3 particles fixed on the surface of the two-dimensional metal carbide material; Wherein, the single crystal FeLaO3 particles are single crystal particles with holes distributed on the surface.
2. The supercapacitor composite material according to claim 1, characterized in that: The supercapacitor composite material is a particle structure, and the outer surface of the two-dimensional metal carbonization material particle is provided with a plurality of single crystal FeLaO3 particles with a porous structure.
3. The supercapacitor composite material according to claim 1, characterized in that: The supercapacitor composite material is a layered composite structure; in the layered composite structure, the single crystal FeLaO3 particles grow in the two-dimensional metal carbide material and on the surface of the two-dimensional metal carbide material, forming a series connection in the two-dimensional metal carbide material to form a porous network structure.
4. The supercapacitor composite material according to claim 3, characterized in that: The distribution density of the single crystal FeLaO3 particles on the surface of the two-dimensional metal carbide material is not less than 10 mg·cm -2 .
5. The method for preparing the supercapacitor composite material according to any one of claims 1 to 4, characterized in that: include: The two-dimensional metal carbide material is washed and dried to obtain a dry sheet; soaking the dried sheet in a nitrogen-methylpyrrolidone solution to obtain an impregnated material; In an organic solvent, lanthanum salt and iron salt are added and dissolved to obtain a precursor salt mixture; placing the infiltration material into the precursor salt mixture, so that the precursor salt mixture melts on the surface of the infiltration material to obtain an intermediate product; The intermediate product is subjected to a high temperature and high pressure heat preservation treatment, and then subjected to a calcination treatment after cooling, so as to obtain the composite material; Preferably, the iron salt comprises at least one of ferric nitrate, ferric chloride and ferric oxalate; Preferably, the lanthanum salt comprises at least one of lanthanum chloride, lanthanum nitrate, lanthanum sulfate, lanthanum carbonate and lanthanum hexaboride; Preferably, the organic solvent comprises at least one of n-pentane, petroleum ether, isopropyl ether, isobutanol, tetrahydrofuran, pyridine, aniline and acetonitrile; Preferably, the amount of the iron salt and the lanthanum salt added to the precursor salt mixture is 0.3 mmol to 0.9 mmol; Preferably, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is (3-1):(1-3); Preferably, the molar ratio of the iron salt to the lanthanum salt in the precursor salt mixture is 1:
1.
6. The method for preparing the supercapacitor composite material according to claim 5, characterized in that: The two-dimensional metal carbide material is washed and dried to obtain a dry sheet, comprising: Taking the two-dimensional metal carbide material, and washing it repeatedly with ethanol and water alternately; Carrying out a drying process under a protective atmosphere to obtain the dried sheet; Preferably, the temperature of the drying process is not less than 60°C.
7. The method for preparing the supercapacitor composite material according to claim 5, characterized in that: The high temperature and high pressure insulation treatment, the treatment conditions are: The insulation temperature is 160℃~220℃; The insulation time is not less than 48 hours.
8. The method for preparing the supercapacitor composite material according to claim 5, characterized in that: The calcination treatment conditions are: The calcination temperature is 500°C to 800°C; The calcination time is 12 to 24 hours.
9. A supercapacitor, characterized in that: The supercapacitor composite material is prepared according to any one of claims 1 to 4.
10. An electrical equipment, characterized in that: Comprising the supercapacitor as claimed in claim 9.
