CN110942921B - Preparation method of three-dimensional composite aerogel electrode material - Google Patents
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Abstract
The invention designs a preparation method of a three-dimensional composite aerogel electrode material, and particularly designs a preparation method of a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode material. Under the current density of 1A/g, the NiCo-LDH/MXene/rGO composite aerogel electrode has the specific capacitance of 2675F/g, the capacity retention rate of 87.5 percent after 5000 cycles and the coulombic efficiency of 94 percent. The preparation method has the advantages of simple equipment, easy control, good process repeatability, stable product quality and the like, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a preparation method of a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode material.
Background
In recent years, super capacitors have been widely noticed by people as an energy storage and conversion device with a great development prospect due to the characteristics of high power density, high charging and discharging speed, good cycle stability, high reliability and the like. However, the conventional two-dimensional structure electrode cannot store much energy due to the small volume of the active material, and thus has a bottleneck in terms of area energy density. In order to obtain a higher area energy density, a three-dimensional structure electrode becomes a possible solution. In recent years, three-dimensional structure electrodes made of graphene derivatives and other two-dimensional materials have attracted much attention in the relevant professional and academic fields. The three-dimensional structure electrode has high-load active materials, abundant porous structures and larger specific surface area, and can prevent poor self-repairing of two-dimensional materials. Therefore, the method for manufacturing the supercapacitor electrode by using the three-dimensional structure material is an effective strategy for improving the energy storage capacity of the supercapacitor electrode. However, the mechanical properties of the three-dimensional electrode are generally poor, and the resilience is poor. The subject group of polymer university in Zhejiang university in 2013 is to manufacture the ultra-light substance graphene aerogel. The graphene aerogel generally has excellent mechanical properties and high conductivity, and can be combined with other active materials to be applied to catalysis and supercapacitors.
At present, MXene/rGO composite aerogel is adopted to prepare a three-dimensional supercapacitor, the MXene material has high elastic modulus and high carrier mobility according to theoretical prediction, and the MXene material combines the metal conductivity of transition metal carbide and the hydrophilicity of the surface of a hydroxyl group or an oxygen end thereof, and the two-dimensional morphology and good conductivity of MXene make the MXene material become an electrode material with great prospect for lithium ion batteries, hybrid batteries and supercapacitors. However, from the current research results, the three-dimensional supercapacitor made of the MXene/rGO composite aerogel has some defects in the aspects of electrochemical performance and cycling stability. The transition metal Layered Double Hydroxide (LDH) has the characteristics of high surface volume ratio, short carrier transmission diffusion length, easy customization, low cost and the like. Nickel hydroxide and cobalt hydroxide are the most studied positive electrode materials in recent years because of their high reversible charge-discharge capacity, high efficiency, and environmental properties. The nickel-cobalt layered double hydroxide (NiCo-LDH) combines the advantages of the two materials in the electrochemical process and is superior to any one material, so the nickel-cobalt layered double hydroxide (NiCo-LDH) is reported to be one of super-capacitor materials with great development prospects, and can effectively solve the problems of the super-capacitor in the aspects of electrochemical performance and cycling stability.
Disclosure of Invention
The invention provides a preparation method of a three-dimensional composite aerogel electrode material, aiming at the problems of electrochemical performance and cycling stability of a super capacitor.
In order to achieve the purpose, the invention provides the following technical scheme:
(1) with Ti3AlC2MAX phase is used as raw material, and the layered Ti is prepared by selective etching of Al layer3C2MXene colloidal solution: adding lithium fluoride into hydrochloric acid solution, stirring until the lithium fluoride is completely dissolved, and then slowly adding Ti3AlC2MAX phase (titanium aluminum carbide) powder is prevented from being stirred by overheating, the obtained product is centrifugally washed by deionized water until the pH value of the supernatant is close to neutral, then the obtained solid is dispersed in the deionized water, nitrogen is introduced for ultrasonic treatment, and after centrifugation, dark green supernatant is collected to obtain layered Ti3C2Filling MXene colloidal solution with nitrogen, and storing in refrigerator;
(2) preparing MXene/NiCo-LDH composite material: dissolving cobalt salt and nickel salt in MXene solution, carrying out hydrothermal reaction, carrying out centrifugal separation after reaction to obtain a product A, and carrying out freeze drying on the product A to obtain an MXene/NiCo-LDH composite material;
(3) preparing NiCo-LDH/MXene/rGO three-dimensional composite aerogel: dispersing graphene oxide in deionized water, adding ethylenediamine and MXene/NiCo-LDH composite materials into graphene oxide dispersion liquid, sealing the mixed liquid in a glass bottle, heating the mixed liquid in an air drying box to synthesize NiCo-LDH/MXene/rGO three-dimensional composite hydrogel, dialyzing the NiCo-LDH/MXene/rGO three-dimensional composite hydrogel in a mixed liquid of ethanol and deionized water, freezing the dialyzed hydrogel, carrying out freeze drying treatment in a freeze dryer, and removing the solution to obtain the NiCo-LDH/MXene/rGO three-dimensional composite aerogel.
Preferably, in the step (1), the dosage of lithium fluoride is 1-2 g, the dosage of titanium aluminum carbide is 1-2 g, the concentration of the hydrochloric acid solution is 6-9M, and the dosage is 20-40 mL.
Preferably, in the step (1), overheating stirring is avoided, the stirring temperature is controlled to be 25-45 ℃, and the stirring time is 24-48 hours.
Preferably, in the step (1), the centrifugal washing speed is 3500rpm, the dispersion is carried out in 150-300 mL of deionized water, and ultrasonic treatment is carried out for 1-2 hours under nitrogen.
Preferably, in the step (1), the speed of the second centrifugation is 1500-2500 rpm, and the time is 0.5-2 hours.
Preferably, in the step (2), the cobalt salt is Co (NO)3)2·6H2O, Ni salts being Ni (NO)3)2·6H2O, the molar ratio is 1: (0.5-2). The amount of MXene is 20-40 mL, the hydrothermal reaction temperature is 120-180 ℃, and the reaction time is 10-15 hours.
Preferably, in the step (3), the concentration of the graphene oxide dispersion liquid is 3mg/mL, the dosage is 5-10 mL, the dosage of ethylenediamine is 20-40 microliter, and the dosage of the MXene/NiCo-LDH composite material is 10-20 mg.
Preferably, in the step (3), the heating temperature is 95-120 ℃ and the time is 3-6 hours.
Preferably, in the step (3), the dialysis time is 3 to 6 hours, and the freeze-drying time is 36 to 48 hours. The invention has the advantages and beneficial effects that:
1. the invention provides a preparation method of a three-dimensional composite aerogel electrode material, MXene is added to be beneficial to improving the conductivity of the material, the contact area of the MXene and an electrolyte is increased due to the three-dimensional porous structure, the specific capacity of the material is improved, the preparation process is simple, and the repeatability is high.
2. The invention provides a preparation method of a three-dimensional composite aerogel electrode material, wherein the NiCo-LDH/MXene/rGO composite aerogel electrode has the specific capacitance of 2675F/g under the current density of 1A/g, the capacity retention rate is 87.5% after 5000 cycles, and the coulombic efficiency is 94%.
Drawings
FIG. 1: the flow schematic diagram of the preparation method of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel provided by the invention is shown in the specification;
FIG. 2: scanning electron microscope photos of NiCo-LDH/MXene/rGO three-dimensional composite aerogel are obtained in the embodiment 1 of the invention;
FIG. 3: scanning electron microscope photos of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel are obtained in the embodiment 2 of the invention;
FIG. 4: scanning electron microscope photos of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel are obtained in the embodiment 3 of the invention;
FIG. 5: the charge-discharge curve diagram of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode obtained in the embodiment 1-3 of the invention;
FIG. 6: the charging and discharging curve diagrams of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode obtained in the embodiment 1 of the invention under different current densities are obtained;
FIG. 7: the cycle performance diagram of the NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode obtained in the embodiment 1 of the invention.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited to the following examples.
Example 1:
(1) with Ti3AlC2MAX phase is used as raw material, and the layered Ti is prepared by selective etching of Al layer3C2MXene colloidal solution: 1g of lithium fluoride was added to 9M 20mL of hydrochloric acid solution, stirred until the lithium fluoride was completely dissolved, and then 1g of Ti was slowly added3AlC2MAX phase (titanium aluminum carbide) powder, avoiding over-heating stirring, and stirring for 24 hours at 35 ℃. The resulting product was washed with deionized water and centrifuged (3500rpm) until the supernatant pH was near neutral. Then, the finished product is dispersed in 150mL of deionized water, and nitrogen is introduced for ultrasonic treatment for 1 hour. After centrifugation at 2000rpm for 1 hour, the dark green supernatant was collected to obtain layered Ti3C2And filling the MXene colloidal solution with nitrogen, and storing in a refrigerator.
(2) Preparing MXene/NiCo-LDH composite material: 0.015mol of nickel nitrate and 0.03mol of cobalt nitrate are dissolved in 30mL of MXene solution, hydrothermal reaction is carried out for 10 hours at 120 ℃, a product A is obtained by centrifugal separation after the reaction, and the MXene/NiCo-LDH composite material is obtained by freeze drying the product A.
(3) Preparing NiCo-LDH/MXene/rGO three-dimensional composite aerogel: graphene oxide was dispersed in deionized water to a concentration of 3mg/mL, and 20. mu.L of ethylenediamine and 10mg of MXene/NiCo-LDH composite material were added to the graphene oxide dispersion. And sealing the mixed solution in a glass bottle, and heating the mixed solution in a blast drying oven at 95 ℃ for 6 hours to synthesize the NiCo-LDH/MXene/rGO three-dimensional composite hydrogel. The mixture was dialyzed for 6 hours against a mixture of ethanol and deionized water. Freezing the dialyzed hydrogel, and then carrying out freeze drying treatment in a freeze dryer for 36 hours to remove the solution to obtain the NiCo-LDH/MXene/rGO three-dimensional composite aerogel.
(4) Electrochemical testing: a three-electrode system is adopted for testing in a KOH solution, a platinum sheet is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode piece is used as a working electrode. Mixing NiCo-LDH/MXene/rGO three-dimensional composite aerogel with acetylene black and PVDF, and adding N-methyl pyrrolidone, wherein the mass ratio of the active material to the acetylene black to the PVDF is 8:1: 1. And coating the nickel foam on the nickel foam, and performing vacuum drying to obtain the electrode plate. In FIG. 5, the curve a is a charge-discharge curve diagram of a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode, and the specific capacity is 2675F/g under the current density of 1A/g. Fig. 7 shows that the capacity retention after 5000 cycles was 87.5% and the coulombic efficiency was 94%.
Example 2:
(1) with Ti3AlC2MAX phase is used as raw material, and the layered Ti is prepared by selective etching of Al layer3C2MXene colloidal solution: 1g of lithium fluoride was added to 9M 20mL of hydrochloric acid solution, stirred until the lithium fluoride was completely dissolved, and then 1g of Ti was slowly added3AlC2MAX phase (titanium aluminum carbide) powder, avoiding over-heating stirring, and stirring for 24 hours at 35 ℃. The resulting product was washed with deionized water and centrifuged (3500rpm) until the supernatant pH was near neutral. Then, the finished product is dispersed in 150mL of deionized water, and nitrogen is introduced for ultrasonic treatment for 1 hour. After centrifugation at 2000rpm for 1 hour, the dark green supernatant was collected to obtain layered Ti3C2And filling the MXene colloidal solution with nitrogen, and storing in a refrigerator.
(2) Preparing MXene/NiCo-LDH composite material: 0.03mol of nickel nitrate and 0.015mol of cobalt nitrate are dissolved in 30mL of MXene solution, hydrothermal reaction is carried out for 10 hours at 120 ℃, a product A is obtained by centrifugal separation after the reaction, and the MXene/NiCo-LDH composite material is obtained by freeze drying the product A.
(3) Preparing NiCo-LDH/MXene/rGO three-dimensional composite aerogel: graphene oxide was dispersed in deionized water to a concentration of 3mg/mL, and 20. mu.L of ethylenediamine and 10mg of MXene/NiCo-LDH composite material were added to the graphene oxide dispersion. And sealing the mixed solution in a glass bottle, and heating the mixed solution in a blast drying oven at 95 ℃ for 6 hours to synthesize the NiCo-LDH/MXene/rGO three-dimensional composite hydrogel. The mixture was dialyzed for 6 hours against a mixture of ethanol and deionized water. Freezing the dialyzed hydrogel, and then carrying out freeze drying treatment in a freeze dryer for 36 hours to remove the solution to obtain the NiCo-LDH/MXene/rGO three-dimensional composite aerogel.
(4) Electrochemical testing: a three-electrode system is adopted for testing in a KOH solution, a platinum sheet is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode piece is used as a working electrode. Mixing NiCo-LDH/MXene/rGO three-dimensional composite aerogel with acetylene black and PVDF, and adding N-methyl pyrrolidone, wherein the mass ratio of the active material to the acetylene black to the PVDF is 8:1: 1. And coating the nickel foam on the nickel foam, and performing vacuum drying to obtain the electrode plate. In the graph of FIG. 5, the curve b is a charge-discharge curve diagram of a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode, and the specific capacity is 2589.7F/g under the current density of 1A/g.
Example 3:
(1) with Ti3AlC2MAX phase is used as raw material, and the layered Ti is prepared by selective etching of Al layer3C2MXene colloidal solution: 1g of lithium fluoride was added to 9M 20mL of hydrochloric acid solution, stirred until the lithium fluoride was completely dissolved, and then 1g of Ti was slowly added3AlC2MAX phase (titanium aluminum carbide) powder, avoiding over-heating stirring, and stirring for 24 hours at 35 ℃. The resulting product was washed with deionized water and centrifuged (3500rpm) until the supernatant pH was near neutral. Then, the finished product is dispersed in 150mL of deionized water, and nitrogen is introduced for ultrasonic treatment for 1 hour. After centrifugation at 2000rpm for 1 hour, the dark green supernatant was collected to obtain layered Ti3C2And filling the MXene colloidal solution with nitrogen, and storing in a refrigerator.
(2) Preparing MXene/NiCo-LDH composite material: 0.0225mol of nickel nitrate and 0.0225mol of cobalt nitrate are dissolved in 30mL of MXene solution, hydrothermal reaction is carried out for 10 hours at 120 ℃, a product A is obtained by centrifugal separation after the reaction, and the MXene/NiCo-LDH composite material is obtained by freeze drying of the product A.
(3) Preparing NiCo-LDH/MXene/rGO three-dimensional composite aerogel: graphene oxide was dispersed in deionized water to a concentration of 3mg/mL, and 20. mu.L of ethylenediamine and 10mg of MXene/NiCo-LDH composite material were added to the graphene oxide dispersion. And sealing the mixed solution in a glass bottle, and heating the mixed solution in a blast drying oven at 95 ℃ for 6 hours to synthesize the NiCo-LDH/MXene/rGO three-dimensional composite hydrogel. The mixture was dialyzed for 6 hours against a mixture of ethanol and deionized water. Freezing the dialyzed hydrogel, and then carrying out freeze drying treatment in a freeze dryer for 36 hours to remove the solution to obtain the NiCo-LDH/MXene/rGO three-dimensional composite aerogel.
(4) Electrochemical testing: a three-electrode system is adopted for testing in a KOH solution, a platinum sheet is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, and a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode piece is used as a working electrode. Mixing NiCo-LDH/MXene/rGO three-dimensional composite aerogel with acetylene black and PVDF, and adding N-methyl pyrrolidone, wherein the mass ratio of the active material to the acetylene black to the PVDF is 8:1: 1. And coating the nickel foam on the nickel foam, and performing vacuum drying to obtain the electrode plate. In FIG. 5, the curve c is a charge-discharge curve diagram of a NiCo-LDH/MXene/rGO three-dimensional composite aerogel electrode, and the specific capacity of the electrode is 1819.3F/g under the current density of 1A/g.
Although the specific embodiments of the present invention have been described with reference to the examples, the scope of the present invention is not limited thereto, and those skilled in the art will appreciate that various modifications and variations can be made without inventive effort by those skilled in the art based on the technical solution of the present invention.
Claims (9)
1. A preparation method of a three-dimensional composite aerogel electrode material is characterized by comprising the following specific steps:
(1) with Ti3AlC2 MAPreparing layered Ti by selectively etching Al layer with X phase as raw material3C2MXene colloidal solution: adding lithium fluoride into hydrochloric acid solution, stirring until the lithium fluoride is completely dissolved, and then slowly adding Ti3AlC2MAX phase (titanium aluminum carbide) powder is prevented from being stirred by overheating, the obtained product is centrifugally washed by deionized water until the pH value of the supernatant is close to neutral, then the obtained solid is dispersed in the deionized water, nitrogen is introduced for ultrasonic treatment, and after centrifugation, dark green supernatant is collected to obtain layered Ti3C2Filling MXene colloidal solution with nitrogen, and storing in refrigerator;
(2) preparing MXene/NiCo-LDH composite material: dissolving cobalt salt and nickel salt in MXene solution, carrying out hydrothermal reaction, carrying out centrifugal separation after reaction to obtain a product, and then carrying out freeze drying to obtain an MXene/NiCo-LDH composite material;
(3) preparing NiCo-LDH/MXene/rGO three-dimensional composite aerogel: dispersing graphene oxide in deionized water, adding ethylenediamine and MXene/NiCo-LDH composite materials into graphene oxide dispersion liquid, sealing the mixed liquid in a glass bottle, heating the mixed liquid in an air drying box to synthesize NiCo-LDH/MXene/rGO three-dimensional composite hydrogel, dialyzing the NiCo-LDH/MXene/rGO three-dimensional composite hydrogel in a mixed liquid of ethanol and deionized water, freezing the dialyzed hydrogel, carrying out freeze drying treatment in a freeze dryer, and removing the solution to obtain the NiCo-LDH/MXene/rGO three-dimensional composite aerogel.
2. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (1), the dosage of lithium fluoride is 1-2 g, the dosage of titanium aluminum carbide is 1-2 g, the concentration of a hydrochloric acid solution is 6-9M, and the dosage is 20-40 mL.
3. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (1), overheating stirring is avoided, the stirring temperature is controlled to be 25-45 ℃, and the stirring time is 24-48 hours.
4. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (1), the centrifugal washing speed is 3500rpm, the obtained solid is dispersed in 150-300 mL of deionized water, and ultrasonic treatment is carried out for 1-2 hours under nitrogen.
5. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (1), the speed of the second centrifugation is 1500-2500 rpm, and the time is 0.5-2 hours.
6. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (2), the cobalt salt is Co (NO)3)2·6H2O, Ni salts being Ni (NO)3)2·6H2O, the molar ratio is 1: (0.5-2), the amount of MXene is 20-40 mL, the hydrothermal reaction temperature is 120-180 ℃, and the reaction time is 10-15 hours.
7. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (3), the concentration of the graphene oxide dispersion liquid is 3mg/mL, the dosage is 5-10 mL, the dosage of ethylenediamine is 20-40 microliter, and the dosage of the MXene/NiCo-LDH composite material is 10-20 mg.
8. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (3), the heating temperature is 95-120 ℃ and the time is 3-6 hours.
9. The method of preparing a three-dimensional composite aerogel electrode material of claim 1, wherein: in the step (3), the dialysis time is 3-6 hours, and the freeze-drying time is 36-48 hours.
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| CN111269516B (en) * | 2020-04-02 | 2021-01-15 | 北京航空航天大学 | MXene composite gel material, preparation method and application |
| CN111799095B (en) * | 2020-06-15 | 2022-03-15 | 桂林电子科技大学 | Hollow MXenes-based metal oxide composite material and preparation method and application thereof |
| CN112079338B (en) * | 2020-09-17 | 2022-02-18 | 齐鲁工业大学 | Three-dimensional foam-like composite material, preparation method and application thereof in sodium-ion battery |
| CN112834088B (en) * | 2021-01-21 | 2022-06-28 | 南开大学 | Bionic MXene aerogel-based sensing material and preparation method and application thereof |
| CN113054187A (en) * | 2021-03-19 | 2021-06-29 | 东北大学 | V-shaped groove2Preparation method of C-MXene/cobalt-nickel double metal hydroxide composite material |
| CN113394029B (en) * | 2021-06-22 | 2022-07-22 | 清华大学深圳国际研究生院 | MXene electrode preparation method based on 3D printing |
| CN113621989B (en) * | 2021-08-20 | 2023-08-25 | 中国科学院过程工程研究所 | Synthesis method for preparing nickel-based layered structure electrocatalyst based on Mxene/graphene hydrogel electrodeposition |
| CN113823781A (en) * | 2021-08-23 | 2021-12-21 | 惠州锂威新能源科技有限公司 | Composite negative electrode material and preparation method thereof |
| CN115483037B (en) * | 2022-09-19 | 2023-10-31 | 常州大学 | Polypyrrole/two-dimensional titanium carbide/sodium alginate aerogel composite material and preparation method and application thereof |
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