CN112086294A - Foam metal/MXene/NFC electrode material for supercapacitor and preparation method thereof - Google Patents
Foam metal/MXene/NFC electrode material for supercapacitor and preparation method thereof Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 38
- 239000002184 metal Substances 0.000 title claims abstract description 38
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 239000006260 foam Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 235000003270 potassium fluoride Nutrition 0.000 claims abstract description 12
- 239000011698 potassium fluoride Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000003990 capacitor Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229920001046 Nanocellulose Polymers 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000002356 single layer Substances 0.000 abstract description 4
- 229920002678 cellulose Polymers 0.000 abstract description 3
- 239000001913 cellulose Substances 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
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- 238000005530 etching Methods 0.000 abstract 1
- 238000000703 high-speed centrifugation Methods 0.000 abstract 1
- 239000007921 spray Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000001132 ultrasonic dispersion Methods 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 229910003266 NiCo Inorganic materials 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
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- 238000002604 ultrasonography Methods 0.000 description 2
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 1
- 229910009594 Ti2AlN Inorganic materials 0.000 description 1
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
The invention belongs to the technical field of energy storage materials, and particularly relates to a foam metal/Mxene/NFC electrode material for a supercapacitor and a preparation method thereof. Etching MAX with a mixed solution of potassium fluoride, hydrofluoric acid and hydrochloric acid to obtain MXene powder, stirring and mixing the MXene powder and nano-cellulose (NFC) in deionized water, performing ultrasonic treatment and high-speed centrifugation to obtain an NFC/MXene dispersion, spraying the dispersion onto a foamed metal substrate in an inert gas atmosphere through spray drying, placing the foamed metal/Mxene/NFC electrode material in a tubular furnace for calcination, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor. According to the invention, a natural renewable raw material NFC is selected, the material is degradable, pollution-free and environment-friendly, single-layer MXene can be obtained through NFC dispersion, the problem that the MXene is easy to agglomerate is avoided to a limited extent, and the NFC/MXene dispersion liquid is sprayed on the surface of the foam metal by adopting a spray drying method, so that the prepared electrode material has high conductivity, high specific capacity and excellent cycling stability.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a foam metal/Mxen e/NFC electrode material for a supercapacitor and a preparation method thereof.
Background
Since the new century, with the rapid development of human science and technology and industry, the energy crisis is becoming more serious, and at present, the world energy structure is dominated by fossil energy. The energy crisis is solved by two ways, namely, more deep development and utilization of renewable energy sources, improvement of the utilization rate of the existing energy sources and reduction of waste. Electric energy is one of the most practical energy forms, has the characteristics of high efficiency, convenience in transmission and the like, and in recent years, a Super Capacitor (SCs) becomes a new research hotspot in the field of energy storage, and has the advantages of higher power density, good cycle stability, shorter charging and discharging time consumption and the like.
The patent (CN 106531457B) discloses a NiCo for a super capacitor2O4The carbon nanotube/carbon nanotube composite electrode material is prepared by dispersing carbon nanotube in water solution of alcohol, and adding NiCo2O4Fully stirring and dispersing, then filtering, washing, drying, finally obtaining NiCo by high-temperature heat treatment in an atmosphere furnace2O4The carbon nanotube composite electrode material. The discharge capacity of the electrode material prepared by the method is lower in current density.
The patent (CN 108257791A) discloses an MXene paper electrode and a preparation method thereof, and a micro super capacitor and a preparation method thereof, wherein the preparation method of the MXene paper electrode adopts a spraying technology to prepare the MXene paper electrode, so that the MXene paper electrode has the advantages of lightness, thinness, flexibility and low cost. However, the method ignores the problem that MXene is easy to agglomerate, and the MXene lamellar structure is easy to generate the re-stacking phenomenon, so that the specific surface area of the material is greatly reduced, the diffusion of ions among MXene layers is influenced, and the electrochemical performance is reduced.
The low specific capacitance is a fatal defect of the carbon material, and the metal oxide can provide higher specific capacitance through a surface reversible faradaic reaction. In addition, the hydrophilic and lipophilic characteristics of the nano-cellulose (NFC) are added, the Mxene is peeled into a single-layer structure, the problem of easy aggregation of MXene is solved, and the electrical property of the MXene can be effectively improved.
Disclosure of Invention
Aiming at the problems, the invention provides a foam metal/Mxene/NFC electrode material for a super capacitor and a preparation method thereof. The preparation process is simple and convenient, and the obtained foam metal/Mxene/NFC electrode material has excellent performances of high conductivity, high specific capacity, superior cycling stability and the like.
The invention provides a foam metal/Mxene/NFC electrode material for a supercapacitor and a preparation method thereof, wherein the preparation method comprises the following steps:
step one, adding a mixed solution of potassium fluoride and hydrofluoric acid into 0.1mol/L hydrochloric acid, uniformly stirring, slowly adding a precursor MAX, stirring for 24 hours at 50 ℃, cleaning and drying to obtain MXene powder.
Step two, adding MXene powder and nano cellulose (NFC) into 1L of deionized water according to a certain proportion, stirring and mixing uniformly to obtain a suspension, carrying out ultrasonic treatment on the suspension, centrifuging the suspension in a high-speed centrifuge, and keeping a supernatant as a final NFC/MXene dispersion liquid.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto a foamed metal substrate in an inert gas atmosphere by a spray drying method, placing the foamed metal substrate onto a tubular furnace for calcining, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
Further, in the first step, the molar ratio of the potassium fluoride to the hydrofluoric acid is 1:1, and the mass ratio of the potassium fluoride to the hydrofluoric acid to the precursor MAX is 1: 1.
Further, the molecular formula of the MAX phase material in the first step is expressed as Mn+1AXnM is selected from any one or the combination of more than two of IIIB, IVB, VB and VIB group elements, A is any one or the combination of more than two of Cu, Ag, Co and Ni, X is C element and/or N element, and N is 1, 2, 3 or 4.
Furthermore, the mass ratio of MXene powder to the nano-cellulose in the second step is 5-9: 1.
Further, the power of the ultrasound in the second step is 50-80%, and the ultrasound time is 10-15 h.
Further, the rotating speed of the high-speed centrifuge in the second step is 5000-8000 r/min, and the centrifuging time is 20-40 min.
Further, the foam metal in the third step is treated according to the following method: soaking the foam metal in ethanol solution, performing ultrasonic treatment for 30min, and adding 10mol.L-1Reacting in HCl solution for 20min, removing oxide on the surface of the foamed nickel, repeatedly washing with deionized water for several times, and drying in a vacuum drying oven at 60 ℃ for 24h for later use.
Furthermore, the feeding concentration in the third step is 20 percent, the air inlet temperature is 150-.
Further, the inert gas in the third step is one or more of nitrogen, argon, helium and the like, and the preset temperature of the tubular furnace is 500-1200 ℃.
Further, the foam metal in the third step comprises at least one of foam nickel, foam copper, foam iron and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) the natural renewable raw material NFC is selected, the degradable pollution-free environment-friendly effect is achieved, single-layer MXene can be obtained through NFC dispersion, and the problem that the MXene is easy to agglomerate is limited.
(2) According to the invention, the NFC/MXene dispersion liquid is sprayed on the surface of the foam metal by adopting a spray drying method, so that the defects of low specific volume and poor cycle stability of the traditional carbon electrode material are overcome, and the prepared electrode material has high conductivity, high specific volume and excellent cycle stability.
Drawings
Fig. 1 is an SEM image of a single layer MXene lamellar structure.
FIG. 2 is a graph showing the relationship between the specific capacitance and the current density of five electrode materials prepared by the present invention.
Fig. 3 shows the capacity retention after 2000 cycles of five electrode materials prepared according to the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely through the following embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The treatment process of the foam metal comprises the following steps: soaking the foam metal in ethanol solution, performing ultrasonic treatment for 30min, and adding 10mol.L-1Reacting in HCl solution for 20min, removing oxide on the surface of the foamed nickel, repeatedly washing with deionized water for several times, and drying in a vacuum drying oven at 60 ℃ for 24h for later use.
The treatment of the foam metal in the following examples is performed by this method, and is not described in detail.
Example 1
Step one, adding a mixed solution of 3.0g of potassium fluoride and 8.7g of hydrofluoric acid into 0.1mol/L hydrochloric acid solution, uniformly stirring, and slowly adding a precursor Ti2AlN, stirred for 24 hours at 50 ℃, washed and dried to obtain MXene powder.
Step two, adding 20.0g of MXene powder and 4.0g of nano cellulose (NFC) into 1L of deionized water, stirring and mixing uniformly to obtain a suspension, dispersing the suspension for 12 hours by using an ultrasonic dispersion machine with the power of 60%, then placing the suspension in a 6000r/min high-speed centrifuge for centrifugation for 30min, and pouring out the supernatant to obtain the NFC/MXene dispersion liquid after the centrifugation is finished.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto the treated foamed iron substrate in a spray dryer with the feed concentration of 20%, the air inlet temperature of 150 ℃ and the atomizer rotating speed of 250r/s under the nitrogen atmosphere, placing the sprayed dispersion liquid into a tubular furnace preheated to 800 ℃ for calcination, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
Example 2
Step one, adding a mixed solution of 2.0g of potassium fluoride and 5.8g of hydrofluoric acid into a 0.1mol/L hydrochloric acid solutionUniformly stirring, and slowly adding a precursor Ti3CuC2And stirring for 24 hours at 50 ℃, and then cleaning and drying to obtain MXene powder.
Step two, adding 24.0g of MXene powder and 4.0g of nano cellulose (NFC) into 1L of deionized water, stirring and mixing uniformly to obtain a suspension, dispersing the suspension for 14h by using an ultrasonic dispersion machine with the power of 70%, then placing the suspension in a 7000r/min high-speed centrifuge for centrifugation for 40min, and pouring out the supernatant to obtain the NFC/MXene dispersion liquid after the centrifugation is finished.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto the treated foamed nickel substrate in a spray dryer with the feed concentration of 20%, the air inlet temperature of 160 ℃ and the atomizer rotating speed of 280r/s under the argon atmosphere, placing the sprayed dispersion liquid into a tubular furnace preheated to 1000 ℃ for calcination, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
Example 3
Step one, adding a mixed solution of 3.5g of potassium fluoride and 10.2g of hydrofluoric acid into 0.1mol/L hydrochloric acid solution, uniformly stirring, and slowly adding a precursor V2And stirring the obtained product for 24 hours at 50 ℃ with AlC, and then cleaning and drying the obtained product to obtain MXene powder.
Step two, adding 27.0g of MXene powder and 3.0g of nano cellulose (NFC) into 1L of deionized water, stirring and mixing uniformly to obtain a suspension, dispersing the suspension for 14h by using an ultrasonic dispersion machine with the power of 80%, then placing the suspension in a 8000r/min high-speed centrifuge for centrifugation for 30min, and pouring out the supernatant to obtain the NFC/MXene dispersion liquid after the centrifugation is finished.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto the treated foamed iron substrate in a spray dryer with the feed concentration of 20%, the air inlet temperature of 165 ℃ and the atomizer rotation speed of 290r/s under the argon atmosphere, placing the sprayed dispersion liquid into a tubular furnace preheated to 1100 ℃ for calcination, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
Example 4
Step one, adding 0.1mo of mixed solution of 2.8g of potassium fluoride and 8.1g of hydrofluoric acidL/L hydrochloric acid solution is evenly stirred, and then precursor Ti is slowly added2Stirring the mixture for 24 hours at 50 ℃ by CuN, and then cleaning and drying the mixture to obtain MXene powder.
Step two, adding 25.5g of MXene powder and 3.6g of nano cellulose (NFC) into 1L of deionized water, stirring and mixing uniformly to obtain a suspension, dispersing the suspension for 15 hours by using an ultrasonic dispersion machine with the power of 75%, then placing the suspension in a 7500r/min high-speed centrifuge for centrifugation for 40min, and pouring out the supernatant to obtain the NFC/MXene dispersion liquid after the centrifugation is finished.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto the treated foam copper substrate in a spray dryer with the feed concentration of 20%, the air inlet temperature of 170 ℃ and the atomizer rotating speed of 320r/s under the helium atmosphere, placing the spray dryer into a tubular furnace preheated to 700 ℃ for calcination, and cooling to obtain the foam metal/Mxene/NFC electrode material for the supercapacitor.
Example 5
Step one, adding a mixed solution of 4.1g of potassium fluoride and 8.6g of hydrofluoric acid into 0.1mol/L hydrochloric acid solution, uniformly stirring, and slowly adding a precursor Ti3AlC2And stirring for 24 hours at 50 ℃, and then cleaning and drying to obtain MXene powder.
Step two, adding 35.6g of MXene powder and 4.5g of nano cellulose (NFC) into 1L of deionized water, stirring and mixing uniformly to obtain a suspension, dispersing the suspension for 15 hours by using an ultrasonic dispersion machine with the power of 75%, then placing the suspension in a 6800r/min high-speed centrifuge for centrifugation for 40min, and pouring out the supernatant to obtain the NFC/MXene dispersion liquid after the centrifugation is finished.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto the treated foamed nickel substrate in a spray dryer with the feed concentration of 20%, the air inlet temperature of 168 ℃ and the atomizer rotating speed of 350r/s under the helium atmosphere, placing the sprayed dispersion liquid into a tubular furnace preheated to 1200 ℃ for calcination, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
Claims (6)
1. A foam metal/Mxene/NFC electrode material for a super capacitor and a preparation method thereof are characterized in that: the preparation method comprises the following steps:
step one, adding a mixed solution of potassium fluoride and hydrofluoric acid into 0.1mol/L hydrochloric acid, uniformly stirring, slowly adding a precursor MAX, stirring for 24 hours at 50 ℃, cleaning and drying to obtain MXene powder.
Step two, adding MXene powder and nano cellulose (NFC) into 1L of deionized water according to a certain proportion, stirring and mixing uniformly to obtain a suspension, carrying out ultrasonic treatment on the suspension, centrifuging the suspension in a high-speed centrifuge, and keeping a supernatant as a final NFC/MXene dispersion liquid.
And step three, spraying the NFC/MXene dispersion liquid obtained in the step two onto a foamed metal substrate in an inert gas atmosphere by a spray drying method, placing the foamed metal substrate onto a tubular furnace for calcining, and cooling to obtain the foamed metal/Mxene/NFC electrode material for the supercapacitor.
2. The foamed metal/Mxene/NFC electrode material for the super capacitor and the preparation method thereof according to claim 1 are characterized in that: in the first step, the molar ratio of the potassium fluoride to the hydrofluoric acid is 1:1, and the mass ratio of the potassium fluoride to the hydrofluoric acid to the precursor MAX is 1: 1.
3. The foamed metal/Mxene/NFC electrode material for the super capacitor and the preparation method thereof according to claim 1 are characterized in that: the molecular formula of the MAX phase material in the first step is expressed as Mn+1AXnM is selected from any one or the combination of more than two of IIIB, IVB, VB and VIB group elements, A is any one or the combination of more than two of Cu, Ag, Co and Ni, X is C element and/or N element, and N is 1, 2, 3 or 4.
4. The foamed metal/Mxene/NFC electrode material for the super capacitor and the preparation method thereof according to claim 1 are characterized in that: in the second step, the mass ratio of MXene powder to nano cellulose is 5-9: 1; the ultrasonic power is 50-80%, and the ultrasonic time is 10-15 h; the rotating speed of the high-speed centrifuge is 5000-8000 r/min, and the centrifugation time is 20-40 min.
5. The foamed metal/Mxene/NFC electrode material for the super capacitor and the preparation method thereof according to claim 1 are characterized in that: in the third step, the foam metal is treated according to the following method: soaking the foam metal in ethanol solution, performing ultrasonic treatment for 30min, and adding 10mol.L-1Reacting in HCl solution for 20min, removing oxide on the surface of the foamed nickel, repeatedly washing with deionized water for several times, and drying in a vacuum drying oven at 60 ℃ for 24h for later use.
6. The foamed metal/Mxene/NFC electrode material for the super capacitor and the preparation method thereof according to claim 1 are characterized in that: in the third step, the feeding concentration is 20 percent, the air inlet temperature is 150 ℃ and 180 ℃, and the rotational speed of the atomizer is 250r/s-350 r/s; the inert gas is one or more of nitrogen, argon, helium and the like, and the preset temperature of the tubular furnace is 500-1200 ℃; the foam metal includes at least one of nickel foam, copper foam, iron foam, and the like.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113218296A (en) * | 2021-03-23 | 2021-08-06 | 上海交通大学 | Elastic strain sensor and preparation method thereof |
| CN114671434A (en) * | 2020-12-24 | 2022-06-28 | 苏州北科纳米科技有限公司 | Method for preparing antioxidant MXene by soaking MAX phase in molten aluminum |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104795252A (en) * | 2015-03-27 | 2015-07-22 | 中国科学院金属研究所 | Preparation method for super-capacitor electrode assembled by ultrathin Ti3C2 nano-sheets |
| CN109679146A (en) * | 2018-08-31 | 2019-04-26 | 中国科学院金属研究所 | A kind of preparation method of MXene/ cellulose composite aerogel |
| CN110767465A (en) * | 2019-09-25 | 2020-02-07 | 洛阳师范学院 | Preparation method of supercapacitor based on two-dimensional niobium carbide nano composite material |
| CN110828654A (en) * | 2019-11-25 | 2020-02-21 | 齐鲁工业大学 | Composite piezoelectric film and preparation method thereof |
| WO2020142139A2 (en) * | 2018-11-08 | 2020-07-09 | Uwm Research Foundation, Inc. | Responsive interference coloration |
-
2020
- 2020-09-17 CN CN202010977957.7A patent/CN112086294A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104795252A (en) * | 2015-03-27 | 2015-07-22 | 中国科学院金属研究所 | Preparation method for super-capacitor electrode assembled by ultrathin Ti3C2 nano-sheets |
| CN109679146A (en) * | 2018-08-31 | 2019-04-26 | 中国科学院金属研究所 | A kind of preparation method of MXene/ cellulose composite aerogel |
| WO2020142139A2 (en) * | 2018-11-08 | 2020-07-09 | Uwm Research Foundation, Inc. | Responsive interference coloration |
| CN110767465A (en) * | 2019-09-25 | 2020-02-07 | 洛阳师范学院 | Preparation method of supercapacitor based on two-dimensional niobium carbide nano composite material |
| CN110828654A (en) * | 2019-11-25 | 2020-02-21 | 齐鲁工业大学 | Composite piezoelectric film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| WEIQIAN TIAN: "Multifunctional Nanocomposites with High Strength", 《ADVANCED MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114671434A (en) * | 2020-12-24 | 2022-06-28 | 苏州北科纳米科技有限公司 | Method for preparing antioxidant MXene by soaking MAX phase in molten aluminum |
| CN113218296A (en) * | 2021-03-23 | 2021-08-06 | 上海交通大学 | Elastic strain sensor and preparation method thereof |
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