CN114823167A - Rapid preparation C @ MnO 2 Method and application of nanoparticles - Google Patents
Rapid preparation C @ MnO 2 Method and application of nanoparticles Download PDFInfo
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- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 15
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 10
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- 229910001925 ruthenium oxide Inorganic materials 0.000 description 2
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/32—Carbon-based
- H01G11/42—Powders or particles, e.g. composition thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/46—Metal oxides
Abstract
The invention discloses a method for quickly preparing C @ MnO 2 A method of nano particles and application thereof as an electrode active material of a super capacitor belong to the technical field of nano materials. Aims to quickly and conveniently obtain C @ MnO 2 And (3) nanoparticles. The main scheme comprises the steps of firstly treating the nano-carbon material in an oxidizing mixed acid solution, then adding the treated nano-carbon material into a permanganate solution, and carrying out ultrasonic treatment. Taking out the particles, washing and drying to obtain the C @ MnO 2 And (3) nanoparticles. The method is characterized by comprising the following steps: the whole preparation scheme is onlyAcetylene black is treated by ultrasonic wave, high-temperature heating is not needed, the preparation time is greatly shortened, and the obtained C @ MnO is 2 The nano-particles have strong stability, strong operability and excellent repeatability.
Description
Technical Field
The invention belongs to the technical field of nano material preparation,in particular to a core-shell structure C @ MnO 2 Nanoparticles and method for preparing same
Background
With the development of science and technology in the world today and the demand for miniaturization and long service life of electronic equipment, researchers have made higher demands on energy storage devices. Supercapacitors with the typical characteristics of high power density and comparable energy density certainly meet the above requirements, and therefore researchers in various countries are constantly looking for new materials as supercapacitor electrodes to obtain better electrochemical performance. Ruthenium oxide (RuO) 2 ) The material has excellent conductivity and specific capacitance and excellent stability, is an ideal electrode material of the super capacitor, but has toxicity and expensive Ru price, and limits large-scale application of the material. In order to seek alternatives, other transition metal oxides are continuously tried to be applied to supercapacitor electrode materials, wherein manganese oxide electrodes show unique pseudo-capacitance performance, have good electrochemical activity and wide electrochemical window, and supercapacitor devices assembled by taking the manganese oxide electrodes as positive electrode materials have large electrochemical window, so that higher energy density can be obtained. However, manganese oxide has a problem of low conductivity, and in order to improve the conductivity of the electrode material, it is necessary to compound it with other conductive materials, so carbon-based materials having a large specific surface area, such as porous carbon and graphene/carbon nanotubes, are often used as a base material for directly growing manganese oxide, so that a manganese oxide-based composite material having good conductivity can be obtained. In this last decade of research, a number of researchers have conducted many processes to prepare C @ MnO 2 The composite material is prepared by sol-gel process, hydrothermal synthesis, electrostatic spinning, redox reaction, chemical vapor deposition, electrodeposition, etc. Wherein, the method mainly aims to construct an electrode material with large specific surface area and proper pore size distribution and obtain C @ MnO with good electrochemical performance through a simple and feasible process 2 A composite electrode material.
CN201910347771 discloses a spherical core-shell structure C @ MnO 2 Method for preparing @ NiAl-LDH nanocomposite, although the product obtained by the method has higher specific surfaceThe product has good electrochemical performance, but the whole preparation process needs twice high-temperature hydrothermal and dropwise adding, mixing and stirring, the production process is too long and the yield is low, and the method cannot be used for commercial application of large-scale synthesis of nano materials. Therefore, the invention can quickly prepare C @ MnO 2 A nanoparticle approach is highly desirable.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide C @ MnO 2 The preparation method of the nano-particles and the application of the nano-particles as the super capacitor electrode aim at quickly and conveniently obtaining C @ MnO with higher specific capacitance and stronger stability 2 And (3) nanoparticles.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the invention discloses a method for quickly preparing C @ MnO 2 The method of the nano particles and the application of the nano particles as the electrode active material of the super capacitor comprise the following specific steps:
and (1) adding the nano carbon material into a mixed acid solution for treatment for a certain time, and drying for later use after cleaning.
Step (2), adding the nano carbon material treated in the step (1) into a permanganate solution, treating by using ultrasonic waves, cleaning and drying to obtain C @ MnO 2 And (3) nanoparticles.
In the step (1), the nano-carbon material is a material such as a carbon nanotube, a carbon fiber, a carbon sphere, acetylene black, graphene, and the like, and is preferably an acetylene black material.
In the step (1), the mixed acid is a mixture of multiple oxidizing acids, such as concentrated sulfuric acid, nitric acid, phosphoric acid, and the like, and preferably sulfuric acid and nitric acid in a volume ratio of 3: 1.
In the step (1), the treatment time is 2-15h, preferably 10 h.
In the step (1), deionized water is used for washing, and the drying temperature is 40-80 ℃, preferably 50 ℃.
In the step (1), the drying time is 12-48h, preferably 24 h.
In the step (2), the processing method of the nano carbon material obtained in the step (1) is ultrasonic waves.
In the step (2), the permanganate solution is a salt solution containing permanganate ions, such as potassium permanganate, sodium permanganate, calcium permanganate, zinc permanganate, magnesium permanganate, and the like, preferably a potassium permanganate solution.
In the step (2), the molar ratio of the nano carbon material to the permanganate is 2:1-1:2, preferably 1: 1.5.
In the step (2), the ultrasonic treatment temperature is 0-50 ℃, preferably 25 ℃, and the temperature change in the treatment process is controlled within +/-5 ℃.
In the step (2), the ultrasonic treatment time is 10-60min, preferably 40 min.
In the step (2), the washing manner is that deionized water and absolute ethyl alcohol are alternately washed, preferably 3 times each.
In the step (2), the drying temperature is 40-80 ℃, preferably 60 ℃.
In the step (2), the drying oven is a vacuum drying oven, and the drying time is 4-12h, preferably 8 h.
C @ MnO prepared by the preparation method 2 The nanoparticles can be used as electrode active materials in supercapacitors.
Compared with the prior art, the invention has the advantages that:
preparation of C @ MnO in the invention 2 The nano-particle scheme has the advantages of easily obtained raw materials, convenience and rapidness compared with methods such as hydrothermal synthesis and the like, simple and safe production process and instrument and equipment, strong operability and excellent repeatability, and can be obtained only by processing for dozens of minutes at normal temperature in an ultrasonic mode.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 shows C @ MnO obtained in example 1 of the present invention 2 Scanning electron micrographs of nanoparticles;
FIG. 2 shows C @ MnO obtained in example 1 of the present invention 2 Transmission electron microscopy of nanoparticles;
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the drawings and specific examples, which are implemented on the premise of the technical solution of the present invention, and the detailed implementation and specific operation procedures are provided, but the protection scope of the present invention is not limited to the following embodiments.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
C @ MnO prepared in the examples 2 The electrochemical test method of the nano-particle electrode material comprises cyclic voltammetry and constant current charging and discharging methods.
When the invention is used for testing the performance of the super capacitor, the three electrode systems are as follows: using calomel electrode as reference electrode, platinum sheet electrode as counter electrode, and using C @ MnO 2 Mixing the nano particles with acetylene black and polyvinylidene fluoride according to a mass ratio of 80:15:5, dispersing the mixture in N-methyl-2-pyrrolidone, fully grinding the mixture in an agate mortar, uniformly coating the mixture on foamed nickel, and drying the foamed nickel for 10 hours at 100 ℃ in a vacuum drying oven to be used as a working electrode. The electrolyte is CMC/Na 2 SO 4 And (4) gelling. The electrochemical tests were carried out on an electrochemical workstation (CHI760E, shanghai chenghua).
Example 1:
rapid preparation C @ MnO 2 A method of nanoparticles comprising the steps of:
and (1) mixing 300ml of sulfuric acid and 100ml of nitric acid to prepare a mixed acid solution, adding 50g of acetylene black into the mixed acid solution, standing for 10 hours to form a hydrophilic surface, taking out the acetylene black, washing with deionized water, and drying in an oven at 50 ℃ for 24 hours.
And (2) adding 35g of the acetylene black prepared in the step (1) into 1000ml of potassium permanganate solution, wherein the potassium permanganate solution is prepared by dissolving 592.204g of potassium permanganate in 1000ml of deionized water, the molar ratio of the acetylene black to the potassium permanganate is controlled to be 1:1.5, and ultrasonic treatment is carried out for 40min at 25 ℃. The process monitors and manages the whole environment temperature, so thatIt does not exceed 30 ℃. Taking out, washing the granules with deionized water and ethanol alternately, and drying in a vacuum drying oven at 60 ℃ for 8h to obtain C @ MnO 2 And (3) nanoparticles.
Example 2:
rapid preparation C @ MnO 2 A method of nanoparticles comprising the steps of:
and (1) mixing 300ml of sulfuric acid and 100ml of nitric acid to prepare a mixed acid solution, adding 50g of acetylene black into the mixed acid solution, standing for 10 hours to form a hydrophilic surface, taking out the acetylene black, washing with deionized water, and drying in an oven at 50 ℃ for 24 hours.
And (2) adding 35g of the acetylene black prepared in the step (1) into 1000ml of potassium permanganate solution, wherein the potassium permanganate solution is prepared by dissolving 493.504g of potassium permanganate in 1000ml of deionized water, the molar ratio of the acetylene black to the potassium permanganate is controlled to be 4:5, and ultrasonic treatment is carried out for 40min at 25 ℃. The process should monitor and manage the whole environmental temperature so that the temperature does not exceed 35 ℃. Taking out, washing the granules with deionized water and ethanol alternately, and drying in a vacuum drying oven at 60 ℃ for 8h to obtain C @ MnO 2 And (3) nanoparticles.
Example 3:
rapid preparation C @ MnO 2 A method of nanoparticles comprising the steps of:
and (1) mixing 300ml of sulfuric acid and 100ml of nitric acid to prepare a mixed acid solution, adding 50g of acetylene black into the mixed acid solution, standing for 10 hours to form a hydrophilic surface, taking out the acetylene black, washing with deionized water, and drying in an oven at 50 ℃ for 24 hours.
And (2) adding 35g of the acetylene black prepared in the step (1) into 1000ml of potassium permanganate solution, wherein the potassium permanganate solution is prepared by dissolving 592.204g of potassium permanganate in 1000ml of deionized water, the molar ratio of the acetylene black to the potassium permanganate is controlled to be 1:1.5, and ultrasonic treatment is carried out for 40min at the temperature of 0 ℃. The process should be carried out in an ice-water bath in the reaction vessel so that it does not exceed 10 ℃. Taking out, washing the granules with deionized water and ethanol alternately, and drying in a vacuum drying oven at 60 ℃ for 8h to obtain C @ MnO 2 And (3) nanoparticles.
Example 4:
rapid preparation C @ MnO 2 A method of nanoparticles comprising the steps of:
and (1) mixing 300ml of sulfuric acid and 100ml of nitric acid to prepare a mixed acid solution, adding 50g of acetylene black into the mixed acid solution, standing for 10 hours to form a hydrophilic surface, taking out the acetylene black, washing with deionized water, and drying in an oven at 50 ℃ for 24 hours.
And (2) adding 35g of the acetylene black prepared in the step (1) into 1000ml of potassium permanganate solution, wherein the potassium permanganate solution is prepared by dissolving 592.204g of potassium permanganate in 1000ml of deionized water, the molar ratio of the acetylene black to the potassium permanganate is controlled to be 4:6, and ultrasonic treatment is carried out for 60min at 25 ℃. The process should monitor and manage the whole environmental temperature to make it not exceed 30 ℃. Taking out, washing the granules with deionized water and ethanol alternately, and drying in a vacuum drying oven at 60 ℃ for 8h to obtain C @ MnO 2 And (3) nanoparticles.
Claims (4)
1. C @ MnO 2 A nanoparticle material, characterized in that the inside of the material is a nanocarbon material and the outside is MnO 2 A material.
2. The process of claim 1 for the rapid preparation of C @ MnO 2 A method of nanomaterials comprising the steps of:
and (1) adding the nano carbon material into a mixed acid solution for treatment, cleaning and drying for later use.
Step (2), adding the nano carbon material treated in the step (1) into a permanganate solution, treating by using ultrasonic waves, cleaning and drying to obtain C @ MnO 2 And (3) nanoparticles.
3. The method according to claim 2, wherein the pretreatment in the step (1) is to treat the nanocarbon material with an oxidizing acid, and the nanocarbon material is dried after being washed;
preferably, the nano-carbon material is a material such as a carbon nanotube, a carbon fiber, a carbon sphere, acetylene black, graphene, and the like, and the acetylene black material is preferred;
preferably, the mixed acid is a mixture of a plurality of oxidizing acids, such as concentrated sulfuric acid, nitric acid, phosphoric acid and the like, preferably sulfuric acid and nitric acid in a volume ratio of 3: 1;
preferably, the treatment time is 2-15h, preferably 10 h;
preferably, deionized water is used for cleaning, and the drying temperature is 40-80 ℃, preferably 50 ℃;
preferably, the drying time is 12-48h, preferably 24 h.
4. The production method according to claim 2 or 3, wherein the manner of processing the nanocarbon material in step (1) in step (2) is ultrasonic waves;
preferably, the permanganate solution is a salt solution containing permanganate ions, such as potassium permanganate, sodium permanganate, calcium permanganate, zinc permanganate, and magnesium permanganate, and preferably a potassium permanganate solution.
Preferably, the molar ratio of the nanocarbon material to permanganate is 2:1 to 1:2, preferably 1: 1.5;
preferably, the ultrasonic treatment temperature is 0-50 ℃, preferably 25 ℃, and the temperature change in the treatment process is controlled within +/-5 ℃;
preferably, the ultrasonic treatment time is 10-60min, preferably 40 min;
preferably, the cleaning mode is that deionized water and absolute ethyl alcohol are alternately cleaned, and 3 times of cleaning is preferred;
preferably, the drying temperature is 40-80 ℃, preferably 60 ℃;
preferably, the drying oven is a vacuum drying oven, and the drying time is 4-12h, preferably 8 h.
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