CN115282989B - Preparation method of ultrasonic-microwave water environment reconstruction iodine-doped carbon nanotube and iodine-doped carbon nanotube - Google Patents
Preparation method of ultrasonic-microwave water environment reconstruction iodine-doped carbon nanotube and iodine-doped carbon nanotube Download PDFInfo
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 116
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 title claims description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000011630 iodine Substances 0.000 claims abstract description 67
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 67
- 239000000126 substance Substances 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 11
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 3
- 229910052755 nonmetal Inorganic materials 0.000 abstract description 6
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 125000005842 heteroatom Chemical group 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 239000000463 material Substances 0.000 description 6
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- 230000003197 catalytic effect Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
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- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
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- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
-
- 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
Abstract
The application provides a preparation method of an ultrasonic-microwave water environment reconstruction iodine doped carbon nano tube, which adopts the following method: dispersing the carbon nano tube and excessive iodine simple substance in an aqueous solution, performing ultrasonic dispersion to prepare a simple substance mixture A, placing the mixture A in a microwave closed environment for one-time microwave treatment, and decomposing and reconstructing the iodine simple substance and the carbon nano tube into uniformly dispersed nano particles after the iodine simple substance and the carbon nano tube are impacted by microwaves to obtain an iodine-doped carbon nano tube B; and (3) placing the iodine-doped carbon nano tube B in a microwave environment for secondary microwave treatment, and removing unreacted iodine simple substance to obtain the pure iodine-doped carbon nano tube. The microwave method is innovatively applied to the preparation of directly forming the iodine-doped carbon nano tube by the non-metal simple substance, and the problem that the aperture of the carbon nano tube is blocked by the non-metal simple substance can be effectively reduced by applying the microwave method to the iodine-doped carbon nano tube; the preparation method is simple and rapid, has simple requirements on equipment, easily obtained raw materials, low cost and low energy consumption, and is suitable for large-scale production.
Description
Technical Field
The application belongs to the technical field of catalyst material preparation, and particularly relates to a preparation method of an ultrasonic-microwave water environment reconstruction iodine-doped carbon nanotube and the iodine-doped carbon nanotube.
Background
The heteroatom doped carbon material is one of the hot spots of research in recent years because of the advantages of low raw material price, rich earth resources, high ORR catalytic activity, good chemical stability, environmental friendliness and the like. For carbon materials without metal heteroatom doping, the heteroatom can induce charge density and spin density redistribution on adjacent carbon atoms, facilitating O adsorption 2 Enhancing ORR catalytic activity.
Carbon nanotubes are typically one-dimensional sp 2 The hybridized carbon nano material has the characteristics of unique structural characteristics, excellent physical and chemical properties, such as large specific surface area, good conductivity, good chemical stability, high mechanical property and the like. These properties make carbon nanotubes ideal carbon-based supports for ORR catalytically active species. When the hetero atoms are properly added into the carbon nano-tubeDesirable ORR performance can be achieved. The carbon nanotubes can enhance the oxygen mass transfer, water removal, corrosion resistance and electrical conductivity of the catalyst, thereby significantly improving the catalytic activity and durability of the catalyst. Compared with nonmetallic hetero atoms such as nitrogen atoms, halogen element iodine has higher electronegativity, and can polarize adjacent C atoms in the carbon framework, and the electronic structure is changed, so that the catalysis process is promoted. Iodine can also be produced by generating I - Formation of ionic bonds further enhances charge transfer.
The prior heteroatom doped carbon material mainly comprises a tubular furnace heat treatment method and a solvothermal method, the tubular furnace has the problems of uneven heating, insufficient contact between a sample and a dopant, complex hydrothermal operation and low yield. The reaction time of the two is longer, the condition is harsh, the large-scale production is difficult, and the cost is high.
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 an iodine-doped carbon nanotube by reconstructing an ultrasonic-microwave water environment and the iodine-doped carbon nanotube.
According to a first aspect of the embodiments of the present application, a method for preparing an iodine doped carbon nanotube by using an ultrasonic-microwave water environment reconstruction is provided, which comprises the following steps:
dispersing the carbon nano tube and excessive iodine simple substance in an aqueous solution, performing ultrasonic dispersion to prepare a simple substance mixture A, placing the mixture A in a microwave closed environment for one-time microwave treatment, and decomposing and reconstructing the iodine simple substance and the carbon nano tube into uniformly dispersed nano particles after the iodine simple substance and the carbon nano tube are impacted by microwaves to obtain an iodine-doped carbon nano tube B; and (3) placing the iodine-doped carbon nano tube B in a microwave environment for secondary microwave treatment, and removing unreacted iodine simple substance to obtain the pure iodine-doped carbon nano tube.
Preferably, the mass ratio of the iodine simple substance to the carbon nano tube is 0.2-7:1.
Preferably, the microwave power is 400-800W during one microwave treatment, and the microwave treatment time is 1-5min.
Preferably, microwave 50-150W is adopted for uncovering treatment for 1-4min during secondary microwave treatment so as to remove unreacted iodine simple substance.
Preferably, the carbon nano tube and the iodine simple substance are mixed and dispersed in the water solution, the ultrasonic dispersion is carried out for 20-60min, and the mass ratio of the carbon nano tube to the water is 1:50-200, wherein the mass of water is not higher than 4g.
Preferably, the method comprises the following specific steps:
s1: dispersing 20mg of carbon nano tubes and 60mg of iodine simple substance in an aqueous solution, and performing ultrasonic dispersion to obtain a simple substance mixture A;
s2: transferring the simple substance mixture A into a quartz crucible with a cover, and putting the quartz crucible into a microwave oven;
s3: adjusting the power to 800W, and carrying out microwave treatment for 3min; obtaining an iodine doped carbon nano tube B;
s4: taking out after the reaction is finished for 2min, and naturally cooling at room temperature;
s5: and (3) uncovering the cover under the microwave 160W for 2min to remove unreacted iodine simple substance to obtain the iodine-doped carbon nano tube.
According to a second aspect of embodiments of the present application, there is provided an iodine-doped carbon nanotube, prepared by the above method;
preferably, the carbon iodine in the iodine-doped carbon nanotubes is in a mixed bonding configuration, and has both covalent bonds and ionic bonds.
The beneficial effects of this application:
1. according to the method, firstly, the carbon nano tube and the iodine simple substance are dispersed in the aqueous solution, ultrasonic treatment is carried out, so that the carbon nano tube and the iodine simple substance are dispersed in the aqueous solution, the ultrasonic dispersion can enable iodine simple substance molecules to be uniformly distributed on the surface of the carbon nano tube, and in the microwave treatment, the water molecules can enhance the thermal motion of the iodine simple substance molecules, so that the doping efficiency is improved, then the microwave thermal shock method is adopted for absorbing microwaves by the carbon nano tube and the iodine simple substance, the instantaneous temperature can be increased to 1600K within 100ms, then the temperature is naturally cooled at room temperature, and the redundant iodine simple substance is removed by the secondary low-power microwaves. In the extreme temperature change, iodine simple substance is decomposed and reconstructed into iodine molecules with small particle size and uniform distribution, and C-C bonds on the carbon nano tube are broken due to microwave impact and molecular thermal motion, and the carbon nano tube is broken to generate positive bonds under the condition of sequential microwave impactNegative ions which reduce partial iodine simple substance into I - Neutral iodine and I - Is combined intoAnd combines with C positive ion to form ionic bond; covalent bonds exist between the carbon nano tube and part of iodine atoms, and the carbon atoms in the carbon layer structure of the carbon nano tube are replaced by part of iodine atoms, and the covalent bonds are formed by the carbon atoms around the carbon layer.
2. Compared with the traditional microwave method which is mostly used for thermal decomposition of precursor materials, the reduction of metal precursors and nucleation of metals are accelerated, the microwave method is creatively applied to the preparation process of directly forming the iodine-doped carbon nano tube by the non-metal simple substance, and the problem that the aperture of the carbon nano tube is blocked by the non-metal simple substance can be effectively reduced by applying the microwave method to the iodine-doped carbon nano tube; the preparation method is simple and rapid, has simple requirements on equipment, easily obtained raw materials, low cost and low energy consumption, and is suitable for large-scale production.
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 shows a high resolution XPS spectrum of I3 d of iodine doped carbon nanotubes prepared in example 1 of the present application;
FIG. 2 shows a high resolution XPS spectrum of C1s of iodine doped carbon nanotubes prepared in example 1 of the present application;
FIG. 3 XPS spectrum of iodine doped carbon nanotubes prepared in example 1 of the present application;
FIG. 4 shows the saturation of the saturated O with untreated CNTs and I-CNTs of example 1 of the present application 2 A lower CV curve;
FIG. 5 is a LSV curve of the I-CNTs prepared in example 1 of the present application at different rotational speeds;
FIG. 6 is a LSV plot for untreated CNTs at different rotational speeds;
FIG. 7 is an lsv curve of untreated CNTs prepared in example 1 of the present application at 1600 rpm.
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 iodine doped carbon nano tube by ultrasonic-microwave water environment reconstruction comprises the following specific steps:
s1: dispersing 20mg of carbon nano tube and 60mg of iodine simple substance in an aqueous solution, and performing ultrasonic dispersion for 30min to obtain a simple substance mixture A;
s2: transferring the simple substance mixture A into a quartz crucible with a cover, and putting the quartz crucible into a microwave oven;
s3: adjusting the power to 800W, and carrying out microwave treatment for 3min; obtaining an iodine doped carbon nano tube B;
s4: taking out after the reaction is finished for 2min, and naturally cooling at room temperature;
s5: and (3) uncovering the cover under the microwave 160W for 2min to remove unreacted iodine simple substance to obtain the iodine-doped carbon nano tube.
Example two
The preparation method of the iodine doped carbon nano tube by ultrasonic-microwave water environment reconstruction comprises the following specific steps:
s1: dispersing 20mg of carbon nano tube and 60mg of iodine simple substance in an aqueous solution, and carrying out ultrasonic treatment for 30min to obtain a simple substance mixture A;
as a specific implementation manner, 20mg of carbon nanotubes and 60mg of iodine simple substance can be respectively and independently dispersed in the aqueous solution by ultrasonic, and then the mixture A obtained by secondary ultrasonic dispersion can be subjected to independent ultrasonic dispersion, so that the dispersion degree of the carbon nanotubes and the iodine simple substance can be increased, and the subsequent iodine doping is facilitated.
S2: transferring the simple substance mixture A into a quartz crucible with a cover, and putting the quartz crucible into a microwave oven;
s3: adjusting the power to 600W, and carrying out microwave treatment for 3min; obtaining an iodine doped carbon nano tube B;
s4: taking out after the reaction is finished for 2min, and naturally cooling at room temperature;
s5: and (3) uncovering the cover under the microwave 160W for 2min to remove unreacted iodine simple substance to obtain the iodine-doped carbon nano tube.
Comparative example 1
Untreated CNTS.
FIG. 1 shows a high resolution XPS spectrum of I3 d of iodine doped carbon nanotubes prepared in example 1 of the present application;
FIG. 2 shows a high resolution XPS spectrum of C1s of iodine doped carbon nanotubes prepared in example 1 of the present application; FIG. 3 XPS spectrum of iodine doped carbon nanotubes prepared in example 1 of the present application; FIG. 4 shows the saturation of the saturated O with untreated CNTs and I-CNTs of example 1 of the present application 2 A lower CV curve; FIG. 5 is a LSV curve of the I-CNTs prepared in example 1 of the present application at different rotational speeds; FIG. 6 is a LSV plot for untreated CNTs at different rotational speeds; FIG. 7 is an lsv curve of untreated CNTs prepared in example 1 of the present application at 1600 rpm.
From FIGS. 1-3, it can be seen that iodine has been doped onto the carbon nanotubes, and that the C-I bonds, including ionic and covalent bonds, present between the carbon nanotubes and iodine are known from the high resolution XPS spectra of C1s and I3 d.
As can be seen from FIG. 4, the I-CNTs and CNTs have a reduction peak at 0.29V, indicating that they undergo an oxygen reduction reaction. The reduction peak area of the I-CNTs is obviously larger than that of the CNTs, which shows that the iodine doping enhances the oxygen reduction reaction activity. FIGS. 5 and 6 represent LSV curves for CNTs and I-CNTs, respectively, at different rotational speeds, with limiting current density increasing with increasing rotational speed due to the shortened diffusion layer at high speeds. FIG. 7 is a graph showing lsv curves of CNTs and I-CNTs at 1600rpm, and the limit current density of the I-CNTs is obviously higher than that of the CNTs, which shows that the larger the current which can pass in unit area and unit time of the I-CNTs, the faster the reaction kinetics. As a fuel cell cathode catalyst, it is possible to make the fuel cell have a larger power.
Based on the above, the heteroatom doping of the carbon nanotubes is conventionally performed by doping on the carbon nanotubes grown in situ, and thenThe doping report of the treated carbon nano tube is less, and most of the carbon nano tube is doped with nitrogen, boron, phosphorus and sulfur. The microwave rule is mostly used for thermal decomposition of precursor materials, and accelerates the reduction of metal precursors and the nucleation of metals; the application adopts a microwave thermal shock method to absorb microwaves by the carbon nano tube and iodine simple substance, the instantaneous temperature can be increased to 1600K within 100ms, then the microwave thermal shock method is naturally cooled at room temperature, and the redundant iodine simple substance is removed by secondary low-power microwaves. In the extreme temperature change, the iodine simple substance is decomposed and reconstructed into iodine molecules with small particle size and uniform distribution, and the C-C bonds on the carbon nano tube are broken due to microwave impact and molecular thermal motion, and the carbon nano tube generates C-C bond breaking under the sequential microwave impact to generate positive and negative ions, and the negative ions reduce part of the iodine simple substance into I - Neutral iodine and I - Is combined intoAnd combines with C positive ions to form ionic bonds. The high resolution XPS spectrum of I3 d shows that covalent bonds exist between the carbon nanotubes and part of iodine atoms, and the carbon atoms in the carbon layer structure of the carbon nanotubes are replaced by part of iodine atoms to form covalent bonds with carbon atoms around the carbon layer.
The ultrasonic dispersion can lead water molecules to drive iodine simple substance molecules to be uniformly distributed on the surface of the carbon nano tube, which is beneficial to the efficient doping of iodine during the microwave treatment, and the water molecules can enhance the thermal movement of the iodine simple substance molecules during the microwave treatment, thereby improving the doping efficiency.
Compared with the traditional microwave method which is mostly used for thermal decomposition of precursor materials, the reduction of metal precursors and nucleation of metals are accelerated, the microwave method is creatively applied to the preparation process of directly forming the iodine-doped carbon nano tube by the non-metal simple substance, and the problem that the aperture of the carbon nano tube is blocked by the non-metal simple substance can be effectively reduced by applying the microwave method to the iodine-doped carbon nano tube; the preparation method is simple and rapid, has simple requirements on equipment, easily obtained raw materials, low cost and low energy consumption, and is suitable for large-scale production.
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 (1)
1. The application of the iodine-doped carbon nano tube in the fuel cell cathode catalyst for the ultrasonic-microwave water environment reconstruction is characterized in that the iodine-doped carbon nano tube is prepared by adopting the following method:
dispersing the carbon nano tube and excessive iodine simple substance in an aqueous solution, performing ultrasonic dispersion to prepare a simple substance mixture A, placing the mixture A in a microwave closed environment for one-time microwave treatment, and decomposing and reconstructing the iodine simple substance and the carbon nano tube into uniformly dispersed nano particles after the iodine simple substance and the carbon nano tube are impacted by microwaves to obtain an iodine-doped carbon nano tube B; placing the iodine-doped carbon nano tube B in a microwave environment for secondary microwave treatment, and removing unreacted iodine simple substances to obtain a pure iodine-doped carbon nano tube;
the preparation method comprises the following specific steps:
s1: mixing and dispersing 20mg of carbon nano tubes and 60mg of iodine simple substance in an aqueous solution, and performing ultrasonic dispersion for 20-60min to obtain a simple substance mixture A of iodine and carbon nano tubes;
s2: transferring the simple substance mixture A of iodine and carbon nano tubes prepared in the step S1 into a 30mL quartz crucible with a cover, and putting the quartz crucible into a microwave oven;
s3: adjusting the power to 800W, and carrying out microwave treatment for 3min; obtaining an iodine doped carbon nano tube B;
s4: taking out after the reaction is finished for 2min, and naturally cooling at room temperature;
s5: uncapping under microwave 160W for 2min to remove unreacted iodine simple substance to obtain iodine doped carbon nanotube;
the carbon iodine in the iodine-doped carbon nano tube is in a mixed bonding configuration, and has covalent bonds and ionic bonds;
in step S1, the mass ratio of carbon nanotubes to water is 1:50-200, wherein the mass of water is not higher than 4g.
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| US9643165B2 (en) * | 2008-06-18 | 2017-05-09 | Board Of Trustees Of The University Of Arkansas | Doped-carbon composites, synthesizing methods and applications of the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6139919A (en) * | 1999-06-16 | 2000-10-31 | University Of Kentucky Research Foundation | Metallic nanoscale fibers from stable iodine-doped carbon nanotubes |
| CN102180462A (en) * | 2011-02-17 | 2011-09-14 | 无锡第六元素高科技发展有限公司 | Method for preparing modified graphene material in controlled atmosphere environment by microwave irradiation |
| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN107308961A (en) * | 2017-06-07 | 2017-11-03 | 华南师范大学 | A kind of I2 doping nanometer Bi4O5Br2Visible light catalyst, preparation method and applications |
| CN107892301A (en) * | 2017-10-26 | 2018-04-10 | 兰州理工大学 | A kind of phosphorus doping meso-porous carbon material and its microwave preparation and application |
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