CN115101762B - Preparation method of carbon nano tube/metal selenide material - Google Patents

Preparation method of carbon nano tube/metal selenide material Download PDF

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CN115101762B
CN115101762B CN202210793106.6A CN202210793106A CN115101762B CN 115101762 B CN115101762 B CN 115101762B CN 202210793106 A CN202210793106 A CN 202210793106A CN 115101762 B CN115101762 B CN 115101762B
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carbon nano
nano tube
metal salt
mixed system
metal
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CN115101762A (en
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高江姗
何燕
张子明
田庆彬
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

The embodiment of the application provides a preparation method of a carbon nano tube/metal selenide material, which comprises the following steps: mixing the carbon nano tube with the prepared metal salt solution according to a preset proportion to obtain a micro-wetting carbon nano tube mixed system; filling a micro-moist carbon nano tube mixed system into a mixed system collector, placing the mixed system collector on a positive plate of an electric arc excitation device, and switching on a power supply to obtain an intermediate material of carbon nano tubes/metal salt particles, wherein the negative electrode of a tungsten wire is close to the carbon nano tube mixed system of the positive electrode; roasting the intermediate material of the carbon nano tube/metal salt particles to perform ion exchange treatment to obtain a carbon nano tube/metal selenide material; the carbon nano tube dispersion and the metal uniform immobilization can be realized in one step by using the electric arc excitation, and no toxic gas is generated in the process; and then the prepared carbon nano tube/metal salt particle intermediate material is placed in a tube furnace for ion exchange treatment to prepare the carbon nano tube/metal selenide, so that the operation is simple, and the industrialization is easy to realize.

Description

Preparation method of carbon nano tube/metal selenide material
Technical Field
The application belongs to the technical field of catalyst material preparation, and particularly relates to a preparation method of a carbon nano tube/metal selenide material.
Background
Hydrogen fuel proton exchange membrane fuel cells have received extensive attention for their advantages of high efficiency, zero emission, and the like. The catalyst in a fuel cell is the most critical component determining its catalytic performance, wherein the Oxygen Reduction Reaction (ORR) catalyst of the fuel cell cathode is responsible for reducing oxygen to lower oxygen for combination with positive hydrogen produced at the anode to produce water molecules, and thus the ORR catalyst is an important part in determining the catalytic rate. The composite material of the carbon nano material and the transition metal is a type with outstanding performance in the ORR catalyst, and the carbon nano tube in the carbon nano material has the characteristics of high conductivity, stable structure and the like and is often used as a carrier of the transition metal.
The preparation of metal catalysts with carbon nanotubes as carriers is often carried out by researchers by adopting hydrothermal method, electrochemical deposition method, gas-phase chemical deposition method and the like, however, the above methods can not disperse agglomerated carbon nanotubes, so that uniform dispersion and small particle size of metal particles on the carbon nanotubes are difficult to realize, and the method has the defects of tedious operation, high risk and strong pollution; in order to increase the dispersibility of a carrier, application number 201510959784.5 discloses an underwater arc discharge preparation method of a graphene-supported Pt catalyst, which uses a spectrum pure graphite rod as an electrode, wherein the arc discharge enables an anode to evaporate to provide a carbon source for the growth of a graphene structure, and metal cations in a salt solution are reduced to generate Pt metal particles which are supported on the surface of the graphene structure; however, the patent has the problems that the reduction of the salt solution can generate harmful gases such as chlorine, and the like, the recovery and the treatment are difficult, the operation steps are complex, the reduction reaction occurs, the energy consumption of graphite evaporation is high, and the like.
In view of this, the present application is specifically proposed.
Disclosure of Invention
In order to solve one of the technical defects, the embodiment of the application provides a preparation method of a carbon nano tube/metal selenide material.
According to a first aspect of the embodiments of the present application, there is provided a method for preparing a carbon nanotube/metal selenide material, which comprises the following steps:
mixing the carbon nano tube with the prepared metal salt solution according to a preset proportion to obtain a micro-wetting carbon nano tube mixed system;
filling a micro-moist carbon nano tube mixed system into a mixed system collector, placing the mixed system collector on a positive plate of an electric arc excitation device, and switching on a power supply to obtain an intermediate material of carbon nano tubes/metal salt particles, wherein the negative electrode of a tungsten wire is close to the carbon nano tube mixed system of the positive electrode;
and roasting the intermediate material of the carbon nano tube/metal salt particles to perform ion exchange treatment to obtain the carbon nano tube/metal selenide material.
Preferably, the dosage ratio of the metal salt to the liquid phase working medium is 0.2g-1.0g:10ml.
Preferably, the method comprises the following specific steps:
s1: mixing metal salt and liquid phase working medium according to a preset proportion to obtain a metal salt solution;
s2: mixing the carbon nano tube with the metal salt solution prepared in the step S1 according to a preset proportion to obtain a micro-wetting carbon nano tube mixed system;
s3: filling the micro-wet carbon nano tube mixed system prepared in the step S2 into a mixed system collector, placing the mixed system collector on a positive plate of an electric arc excitation device, and switching on a power supply to obtain a carbon nano tube/metal salt particle intermediate material;
s4: placing a porcelain boat containing selenium powder at an upper air port of a tube furnace, placing the porcelain boat containing the carbon nano tube/metal salt particle intermediate material prepared in the step S3 at a lower air port of the tube furnace, introducing protective gas, and heating to 400 ℃ for 3 hours to obtain the catalyst of the carbon nano tube/metal selenide.
Preferably, the mass ratio of the metal salt solution to the carbon nano tube is 4-10:1.
preferably, in step S3, after the power is turned on, a drop of the metal salt solution prepared in step S1 is dripped into the mixed system collector every 3-5min in the preparation process.
Preferably, the distance between the tungsten filament anode and the tungsten filament cathode is kept between 0.5 and 1.0mm.
Preferably, the liquid phase working medium is any one of water, ethanol and glycol, or a mixed solution of two or more solutions.
Preferably, the metal salt solution is a chloride of a metal.
The beneficial effects of this application:
1. firstly, mixing metal salt and a liquid phase working medium to prepare a micro-moist carbon nano tube mixed system, then exciting the carbon nano tube mixed system by adopting arc discharge, exciting the liquid phase working medium by an arc high-energy particle beam to generate phase change, vaporizing and rising so as to enable the carbon nano tube to obtain dispersion and rising kinetic energy, condensing the metal salt from an ionic state into nano particles so as to be fixedly supported on the carbon nano tube, realizing carbon nano tube dispersion and metal uniform solid support in one step by arc excitation, and then carrying out ion exchange treatment to prepare the catalyst of the carbon nano tube/metal selenide; the electric arc excitation can realize the dispersion of the carbon nano tube and the uniform immobilization of metal in one step, does not generate toxic gas, and has the characteristics of environmental protection; the electric arc excitation does not need long-time high-temperature high-pressure operation, and the like, is simple to operate and is easy to realize industrialization.
2. The traditional arc excitation in the solution is easy to generate caking phenomenon in the preparation process due to excessive solution, and the energy consumption is high; the method comprises the steps of mixing carbon nanotubes with a metal salt solution to a micro-wetting state, and then performing arc excitation treatment; at the moment, the carbon nano tube is fully mixed with the metal salt solution, so that massive crystallization is prevented from being generated after the subsequent arc treatment; the metal salt solution fully infiltrates into the gaps of the carbon nanotubes, and in the electric arc excitation process, the carbon nanotubes are driven to be dispersed and lifted by the vaporization force of the liquid phase working medium, so that the dispersibility of the carbon nanotubes is improved.
3. The method can realize carbon nanotube dispersion and metal uniform immobilization in one step by arc excitation, and toxic gas is not generated in the process; then placing the prepared carbon nano tube/metal salt particle intermediate material in a tube furnace for ion exchange treatment to prepare carbon nano tube/metal selenide, wherein in the process, the metal salt loaded on the carbon nano tube is replaced by the metal selenide, and the replaced chlorine or other gases can be concentrated for subsequent treatment, so that volatilization of toxic gases in the whole preparation process is stopped; preventing gas pollution in the preparation process.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
FIG. 1 is a CNTs-supported CoSe prepared in example 1 of the present application 2 SEM images of the material;
FIG. 2 is an SEM image of the CNTs feedstock material of the present application;
FIG. 3 is a CNTs-supported CoSe prepared in example 1 of the present application 2 A TEM image of the material;
FIG. 4 is a CNTs-supported CoSe prepared in example 1 of the present application 2 LSV plot at 400-2025rpm for material;
FIG. 5 is a CNTs-supported CoSe prepared in example 1 of the present application 2 I-t cycle stability profile of material, vs. commercial catalyst Pt/C comparison.
Detailed Description
In order to make the technical solutions and advantages of the embodiments of the present application more apparent, the following detailed description of exemplary embodiments of the present application is given with reference to the accompanying drawings, and it is apparent that the described embodiments are only some of the embodiments of the present application and not exhaustive of all the embodiments. It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other.
Example 1
The preparation method of the carbon nano tube/metal selenide material comprises the following specific steps:
s1: mixing 0.2g of cobalt chloride with 10ml of deionized water according to a preset proportion to obtain a metal salt solution;
s2: mixing the carbon nano tube with the metal salt solution prepared in the step S1 according to a ratio of 4:1 to obtain a micro-wetting carbon nano tube mixed system;
s3: filling the micro-moist carbon nanotube mixed system prepared in the step S2 into a mixed system collector, placing the mixed system on a positive plate of an electric arc excitation device, keeping the distance between a tungsten filament negative electrode and the carbon nanotube mixed system close to the positive electrode at 0.5-1.0mm, switching on a power supply, dropwise adding a drop of metal salt solution every 3-5min in the preparation process, and collecting to obtain a carbon nanotube/cobalt chloride particle intermediate material;
s4: placing a porcelain boat containing selenium powder at an upper air port of a tube furnace, placing the porcelain boat containing the carbon nano tube/cobalt chloride particle intermediate material prepared in the step S3 at a lower air port of the tube furnace, introducing protective gas, heating to 400 ℃ and maintaining for 3h to obtain the carbon nano tube/CoSe 2 Is a catalyst of (a).
Example two
The preparation method of the carbon nano tube/metal selenide material comprises the following specific steps:
s1: mixing 0.6g of cobalt chloride with 10ml of deionized water according to a preset proportion to obtain a metal salt solution;
s2: mixing the carbon nano tube with the metal salt solution prepared in the step S1 according to the ratio of 7:1 to obtain a micro-wetting carbon nano tube mixed system;
s3: filling the micro-moist carbon nanotube mixed system prepared in the step S2 into a mixed system collector, placing the mixed system on a positive plate of an electric arc excitation device, keeping the distance between a tungsten filament negative electrode and the carbon nanotube mixed system close to the positive electrode at 0.5-1.0mm, switching on a power supply, dropwise adding a drop of metal salt solution every 3-5min in the preparation process, and collecting to obtain a carbon nanotube/cobalt chloride particle intermediate material;
s4: placing a porcelain boat containing selenium powder at an upper air port of a tube furnace, placing the porcelain boat containing the carbon nano tube/cobalt chloride particle intermediate material prepared in the step S3 at a lower air port of the tube furnace, introducing protective gas, heating to 400 ℃ and maintaining for 3h to obtain the carbon nano tube/CoSe 2 Is a catalyst of (a).
Example III
The preparation method of the carbon nano tube/metal selenide material comprises the following specific steps:
s1: mixing 1g of cobalt chloride with 10ml of deionized water according to a preset proportion to obtain a metal salt solution;
s2: mixing the carbon nano tube with the metal salt solution prepared in the step S1 according to a ratio of 10:1 to obtain a micro-wetting carbon nano tube mixed system;
s3: filling the micro-moist carbon nanotube mixed system prepared in the step S2 into a mixed system collector, placing the mixed system on a positive plate of an electric arc excitation device, keeping the distance between a tungsten filament negative electrode and the carbon nanotube mixed system close to the positive electrode at 0.5-1.0mm, switching on a power supply, dropwise adding a drop of metal salt solution every 3-5min in the preparation process, and collecting to obtain a carbon nanotube/cobalt chloride particle intermediate material;
s4: placing a porcelain boat containing selenium powder at an upper air port of a tube furnace, placing the porcelain boat containing the carbon nano tube/cobalt chloride particle intermediate material prepared in the step S3 at a lower air port of the tube furnace, introducing protective gas, heating to 400 ℃ and maintaining for 3h to obtain the carbon nano tube/CoSe 2 A catalyst.
FIG. 1 is a CNTs-supported CoSe prepared in example 1 of the present application 2 SEM images of the material; FIG. 2 is an SEM image of the CNTs feedstock material of the present application; FIG. 3 is the present applicationCNTs-Supported CoSe prepared in example 1 2 A TEM image of the material; FIG. 4 is a CNTs-supported CoSe prepared in example 1 of the present application 2 LSV plot at 400-2025rpm for material; FIG. 5 is a CNTs-supported CoSe prepared in example 1 of the present application 2 The i-t cycle stability profile of the material was compared to the Pt/C of the commercial catalyst.
FIG. 1 shows carbon nanotubes/CoSe prepared after arc excitation 2 The catalyst was highly dispersed, and it can be seen from fig. 2 that the CNTs raw material was in an agglomerated form, and the carbon nanotubes were wound in a roll. Fig. 1 shows that the prepared catalytic material is dispersed from the carbon nanotube balls in the shape of curled and wound agglomerates into single carbon nanotubes which are mutually overlapped, and compared with fig. 2 and fig. 1, the catalytic material prepared by the method has a particularly remarkable dispersing effect.
FIG. 3 is a CNTs-supported CoSe prepared in example 1 of the present application 2 A TEM image of the material; also further indicate CoSe 2 The particles are loaded on the surface of the carbon nano tube, and the particle size is small and uniform.
FIG. 4 shows a carbon nanotube/CoSe prepared in example 2 of the present application 2 The LSV curve of the catalyst has a high half-wave potential and an initial potential.
FIG. 5 is a carbon nanotube/CoSe prepared according to the present application after 150000s of service 2 The catalyst has higher circulation stability compared with the Pt/C of the commercial catalyst.
Based on the above, the present application firstly mixes metal salt with liquid working medium to prepare a micro-moist carbon nanotube mixed system, then uses arc discharge to excite the carbon nanotube mixed system, the liquid working medium is excited by an arc high-energy particle beam to generate phase change, and is vaporized and lifted so as to enable the carbon nanotubes to obtain dispersion and lifting kinetic energy, the metal salt is condensed into nano particles from an ionic state so as to be immobilized on the carbon nanotubes, carbon nanotube dispersion and metal uniform immobilization can be realized in one step through arc excitation, and then ion exchange treatment is performed to prepare the catalyst of the carbon nanotubes/metal selenide; the electric arc excitation can realize the dispersion of the carbon nano tube and the uniform immobilization of metal in one step, does not generate toxic gas, and has the characteristics of environmental protection; the electric arc excitation does not need long-time high-temperature high-pressure operation, and the like, and has simple operation and easy operationRealizing industrialization. In addition, the carbon nano tube/CoSe prepared by the method 2 The catalyst has higher circulation stability.
It is worth noting that the present application can use sulfur powder to replace selenium powder in the ion exchange stage to prepare the carbon nanotube/metal sulfide material. The carbon nanotubes may be replaced by other materials such as graphene.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present application without departing from the spirit or scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims and the equivalents thereof, the present application is intended to cover such modifications and variations.

Claims (5)

1. The preparation method of the carbon nano tube/metal selenide material is characterized by comprising the following steps of:
mixing the carbon nano tube with the prepared metal salt solution according to a preset proportion to obtain a micro-wetting carbon nano tube mixed system;
filling a micro-moist carbon nano tube mixed system into a mixed system collector, placing the mixed system collector on a positive plate of an electric arc excitation device, and switching on a power supply to obtain an intermediate material of carbon nano tubes/metal salt particles, wherein the negative electrode of a tungsten wire is close to the carbon nano tube mixed system of the positive electrode;
roasting the intermediate material of the carbon nano tube/metal salt particles to perform ion exchange treatment to obtain a carbon nano tube/metal selenide material;
the preparation method of the carbon nano tube/metal selenide material comprises the following specific steps:
s1: mixing metal salt and liquid phase working medium according to a preset proportion to obtain a metal salt solution;
s2: mixing the carbon nano tube with the metal salt solution prepared in the step S1 according to a preset proportion to obtain a micro-wetting carbon nano tube mixed system;
s3: filling the micro-wet carbon nano tube mixed system prepared in the step S2 into a mixed system collector, placing the mixed system collector on a positive plate of an electric arc excitation device, and switching on a power supply to obtain a carbon nano tube/metal salt particle intermediate material;
s4: placing a porcelain boat containing selenium powder at an upper air port of a tube furnace, placing the porcelain boat containing the carbon nano tube/metal salt particle intermediate material prepared in the step S3 at a lower air port of the tube furnace, introducing protective gas, and heating to 400 ℃ for 3 hours to obtain a catalyst of the carbon nano tube/metal selenide;
the mass ratio of the metal salt solution to the carbon nano tube is 4-10:1, a step of;
the metal salt is cobalt chloride.
2. The method of claim 1, wherein the ratio of metal salt to liquid phase working medium is 0.2g-1.0g:10ml.
3. The preparation method according to claim 1, wherein in step S3, after the power is turned on, one drop of the metal salt solution prepared in step S1 is dropped into the mixed system collector every 3-5min during the preparation process.
4. The method of claim 1, wherein the distance between the negative electrode and the positive electrode of the tungsten filament is maintained between 0.5 and 1.0 and mm.
5. The method of claim 1, wherein the liquid working medium is any one of water, ethanol, and glycol, or a mixed solution of two or more solutions.
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Citations (1)

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CN111054418A (en) * 2019-12-19 2020-04-24 中南大学 Oxygen/hydrogen evolution two-dimensional cobalt monoxide @ cobalt diselenide @ nitrogen doped carbon nanotube/graphene dual-functional composite catalyst

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JP2011126718A (en) * 2009-12-15 2011-06-30 Hitachi Zosen Corp Method and apparatus for producing carbon nanotube
CN105552392A (en) * 2016-01-06 2016-05-04 复旦大学 Cobalt diselenide/graphite carbon composite material, namely oxygen reduction catalyst, and preparation method thereof
CN112553651B (en) * 2020-11-03 2022-02-15 常州大学 Preparation method of selenide coated carbon nanotube material
CN113327774B (en) * 2021-05-31 2022-11-11 青岛科技大学 Preparation method of carbon-based metal selenide composite material
CN113809304B (en) * 2021-09-17 2023-03-03 青岛科技大学 Preparation method and application of plasma-based tin dioxide/carbon nanotube composite material

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CN111054418A (en) * 2019-12-19 2020-04-24 中南大学 Oxygen/hydrogen evolution two-dimensional cobalt monoxide @ cobalt diselenide @ nitrogen doped carbon nanotube/graphene dual-functional composite catalyst

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