CN115285973A - Method for synthesizing carbon chain - Google Patents
Method for synthesizing carbon chain Download PDFInfo
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- CN115285973A CN115285973A CN202210964082.6A CN202210964082A CN115285973A CN 115285973 A CN115285973 A CN 115285973A CN 202210964082 A CN202210964082 A CN 202210964082A CN 115285973 A CN115285973 A CN 115285973A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
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Abstract
The invention belongs to the technical field of carbon nano materials, and particularly relates to a method for synthesizing a carbon chain. In order to develop a method for directly synthesizing carbon chains in single-walled carbon nanotubes, the invention firstly carries out high-temperature heat treatment on organic molecules and the open single-walled carbon nanotubes under the vacuum sealing condition, and the organic molecules are vaporized or sublimated and then filled into the carbon nanotubes to obtain the single-walled carbon nanotubes filled with the organic molecules; then annealing conversion treatment is carried out, the single-walled carbon nanotube filled with organic molecules is subjected to heat treatment under the condition of vacuum or inert gas, and carbon chains can be formed in the single-walled carbon nanotube. The invention provides a novel method for converting organic molecules into carbon chains in a single-walled carbon nanotube, solves the technical defect that the carbon chains in the prior art cannot be directly synthesized in the single-walled carbon nanotube, overcomes the requirement that the synthesis temperature is often higher than 1400 ℃, and reduces the synthesis condition to below 700 ℃.
Description
Technical Field
The invention belongs to the technical field of carbon nano materials, and particularly relates to a method for synthesizing a carbon chain.
Background
The carbon chain is a one-dimensional sp hybrid material consisting of one triple bond of carbon atoms. At present, one of the ways of synthesizing carbon chains is to perform confined synthesis in a carbon nanotube, and the high temperature annealing temperature is generally higher than 1400 ℃. When the carbon nano tube is a single-wall carbon nano tube and the diameter of the carbon nano tube is 1.3-2.0nm, after high-temperature annealing, a small-diameter carbon nano tube inner tube is firstly synthesized in the single-wall carbon nano tube, and then a carbon chain is formed in the inner tube. That is, even if single-walled carbon nanotubes are initially used, the synthesized carbon chains are present in the double-walled carbon nanotubes, not the single-walled carbon nanotubes, after the final high-temperature annealing. When the carbon nano tube is a double-wall or multi-wall carbon nano tube and the diameter of the innermost carbon nano tube is 0.6-1.1nm, carbon chains can be formed in the double-wall or multi-wall carbon nano tube through high-temperature annealing. The high temperature annealing may be performed by providing a high temperature environment by a muffle furnace, a tube furnace, or the like, by providing a high temperature environment by laser irradiation, or by applying a voltage, as long as the temperature is 1400 ℃ or higher, and generally about 1500 ℃. However, such high temperature annealing has high requirements for instruments, and thus a new method for synthesizing carbon chains at a lower temperature is required. In addition, there is also a need for a method that can synthesize carbon chains directly in single-walled carbon nanotubes.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for synthesizing a carbon chain, which converts organic molecules into the carbon chain in a single-walled carbon nanotube, solves the technical defect that the carbon chain cannot be directly synthesized in the single-walled carbon nanotube in the prior art, overcomes the requirement that the synthesis temperature is often higher than 1400 ℃, and reduces the synthesis condition to be below 700 ℃.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a method for synthesizing a carbon chain, which comprises the following steps: placing the opened single-walled carbon nanotube and organic molecules under a vacuum closed condition at the same time, and performing high-temperature heat treatment to fill the organic molecules into the carbon nanotube through vaporization or sublimation so as to prepare the single-walled carbon nanotube filled with the organic molecules; then placing the single-walled carbon nanotube filled with organic molecules in a vacuum or inert gas environment, and forming carbon chains in the single-walled carbon nanotube after annealing conversion treatment.
Preferably, the organic molecule includes p-terphenyl, m-terphenyl, biphenyl, o-tolunitrile, 1, 2-dicyanobenzene, and the like. More preferably, the organic molecule comprises p-terphenyl, o-methyl benzonitrile.
The invention converts organic molecules into carbon chains in the single-walled carbon nanotube through high-temperature heat treatment and annealing conversion treatment, solves the technical defect that the carbon chains cannot be directly synthesized in the single-walled carbon nanotube in the prior art, overcomes the requirement that the synthesis temperature is often higher than 1400 ℃, and reduces the synthesis condition to below 700 ℃.
The temperature of the high temperature heat treatment should be higher than the temperature at which the organic molecules are vaporized or sublimated. Preferably, the high-temperature heat treatment is carried out at the temperature of 200-400 ℃ for 70-80h.
Preferably, the temperature of the annealing conversion treatment is 500-700 ℃ and the time is 1-3h.
The heating method of the present invention is not limited, and a high temperature environment may be provided by a muffle furnace, a tube furnace, or the like, a high temperature environment may be provided by laser irradiation, or a high temperature environment may be generated by applying a voltage.
Preferably, the single-walled carbon nanotubes have a diameter of 0.6 to 1.1nm. The method of the present invention is not limited to the method for preparing the single-walled carbon nanotubes, as long as the diameter of a part of the single-walled carbon nanotubes is in the range of 0.6 to 1.1nm.
Preferably, the annealing conversion treatment is performed in a vacuum environment.
The vacuum degree of the vacuum environment of the invention has no strict requirement. Preferably, the degree of vacuum of step S1 is 9.0X 10 -1 -5.0×10 -3 Pa. The degree of vacuum in step S2 was 1.0X 10 -3 -5.0×10 -3 Pa。
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a method for synthesizing a carbon chain, which comprises the steps of firstly carrying out high-temperature heat treatment on an organic molecule and an open single-walled carbon nano tube under a vacuum closed condition, and filling the vaporized or sublimated organic molecule into the carbon nano tube to obtain the single-walled carbon nano tube filled with the organic molecule; then annealing conversion treatment is carried out, the single-walled carbon nanotube filled with organic molecules is subjected to heat treatment under the condition of vacuum or inert gas, and carbon chains can be formed in the single-walled carbon nanotube. The invention provides a novel method for converting organic molecules into carbon chains in a single-walled carbon nanotube, solves the technical defect that the carbon chains in the prior art cannot be directly synthesized in the single-walled carbon nanotube, overcomes the requirement that the synthesis temperature is often higher than 1400 ℃, and reduces the synthesis condition to below 700 ℃.
Drawings
FIG. 1 is a process flow diagram for the synthesis of carbon chains;
FIG. 2 is a Raman spectrum of the carbon chain obtained in example 1;
fig. 3 is a raman spectrum of the carbon chain obtained in example 2.
Detailed Description
The following further describes embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
Example 1A method for synthesizing a carbon chain
According to the process scheme of fig. 1, the method comprises the following steps:
(1) And (3) filling p-terphenyl: open single-walled carbon nanotubes (CoMoCAT type, diameter range 0.6-1.3nm, purchased from Sigma-Aldrich) and p-terphenyl powder (purchased from Sigma-Aldrich) were placed in the bottom and middle of the glass tube, respectively, at a mass ratio of carbon nanotubes to p-terphenyl of 1 -3 Pa), sealing the tube, and then carrying out heat treatment at 230 ℃ for 72 hoursThen, the single-walled carbon nanotube filled with p-terphenyl is prepared.
(2) High-temperature annealing conversion: annealing the terphenyl filled single-walled carbon nanotube in the step (1) at 500 ℃ for 1h, wherein the heat treatment is carried out in vacuum and the vacuum degree is 3.2 multiplied by 10 -3 Pa. The p-terphenyl molecules are decomposed at high temperature in the carbon nano tube and then assembled into carbon chains.
As can be seen from the raman spectrum of fig. 2, the carbon chain was successfully synthesized by the method of this example.
Example 2 method for synthesizing carbon chain
According to the process scheme of fig. 1, the method comprises the following steps:
(1) Filling with o-methyl benzonitrile: open single-walled carbon nanotubes (HiPco type, diameter range 0.8-1.2nm, purchased from michael nanon) and o-methyl benzonitrile powder (purchased from michelin) were placed at the bottom and middle of the glass tube, respectively, the mass ratio of carbon nanotubes to o-methyl benzonitrile was 1 -3 Pa), and then carrying out heat treatment at 350 ℃ for 72 hours to prepare the o-methyl benzonitrile filled single-walled carbon nanotube.
(2) High-temperature annealing conversion: annealing the single-walled carbon nanotube filled with the o-tolunitrile in the step (1) at 650 ℃, wherein the heat treatment time is 1h, the heat treatment is carried out in vacuum, and the vacuum degree is 4.1 multiplied by 10 -3 Pa. The o-methyl benzonitrile molecules are decomposed at high temperature inside the carbon nanotubes and then assembled into carbon chains.
As can be seen from the raman spectrum of fig. 3, the carbon chain was successfully synthesized by the method of this example.
In summary, the method for synthesizing carbon chains provided by the present invention fills organic molecules into the single-walled carbon nanotubes, and then anneals the single-walled carbon nanotubes in vacuum to decompose the organic molecules in the carbon nanotubes and assemble the carbon chains. The carbon chain synthesis method provided by the invention enables organic molecules to be converted into carbon chains in the single-walled carbon nanotube, solves the technical defect that the carbon chains cannot be directly synthesized in the single-walled carbon nanotube in the prior art, overcomes the requirement that the synthesis temperature is often higher than 1400 ℃, and reduces the synthesis condition to below 700 ℃.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (8)
1. A method for synthesizing carbon chain is characterized in that single-walled carbon nanotubes with openings and organic molecules are simultaneously placed under vacuum sealing conditions, and the organic molecules are filled into the carbon nanotubes through vaporization or sublimation by high-temperature heat treatment to prepare the single-walled carbon nanotubes with the organic molecules filled inside; and then placing the single-walled carbon nanotube filled with the organic molecules in a vacuum or inert gas environment, and forming a carbon chain in the single-walled carbon nanotube after annealing and conversion treatment.
2. The method of claim 1, wherein the organic molecule comprises p-terphenyl, m-terphenyl, biphenyl, o-tolunitrile, 1, 2-dicyanobenzene.
3. The method for synthesizing carbon chains according to claim 1, wherein the high temperature heat treatment is performed at a temperature of 200-400 ℃ for 70-80h.
4. The method for synthesizing carbon chains according to claim 1, wherein the annealing conversion treatment is performed at a temperature of 500-700 ℃ for 1-3h.
5. The method for synthesizing carbon chains according to claim 1, wherein the single-walled carbon nanotubes have a diameter of 0.6 to 1.1nm.
6. The method for synthesizing carbon chains according to claim 1, wherein the annealing conversion treatment is performed in a vacuum environment.
7. The method for synthesizing carbon chains according to claim 1, wherein the degree of vacuum in step S1 is 9.0X 10 -1 -5.0×10 -3 Pa。
8. The method for synthesizing carbon chains according to claim 1, wherein the degree of vacuum in step S2 is 1.0X 10 -3 -5.0×10 -3 Pa。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020085968A1 (en) * | 1997-03-07 | 2002-07-04 | William Marsh Rice University | Method for producing self-assembled objects comprising single-wall carbon nanotubes and compositions thereof |
| US20040022718A1 (en) * | 2002-04-18 | 2004-02-05 | Stupp Samuel I. | Encapsulation of nanotubes via self-assembled nanostructures |
| CN111470492A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Preparation method of one-dimensional carbon chain |
| CN111470489A (en) * | 2019-11-05 | 2020-07-31 | 中山大学 | Conversion method for converting single-wall carbon nanotube into double-wall carbon nanotube |
| CN114506844A (en) * | 2022-02-24 | 2022-05-17 | 中山大学 | Method for quickly converting precursor molecules into graphene nanoribbons by using microwaves |
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- 2022-08-11 CN CN202210964082.6A patent/CN115285973B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020085968A1 (en) * | 1997-03-07 | 2002-07-04 | William Marsh Rice University | Method for producing self-assembled objects comprising single-wall carbon nanotubes and compositions thereof |
| US20040022718A1 (en) * | 2002-04-18 | 2004-02-05 | Stupp Samuel I. | Encapsulation of nanotubes via self-assembled nanostructures |
| CN111470489A (en) * | 2019-11-05 | 2020-07-31 | 中山大学 | Conversion method for converting single-wall carbon nanotube into double-wall carbon nanotube |
| CN111470492A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Preparation method of one-dimensional carbon chain |
| CN114506844A (en) * | 2022-02-24 | 2022-05-17 | 中山大学 | Method for quickly converting precursor molecules into graphene nanoribbons by using microwaves |
Non-Patent Citations (1)
| Title |
|---|
| FELIX BÖRRNERTET AL.: ""Single-wall-carbon-nanotube/single-carbon-chain molecular junctions"", FELIX BÖRRNERTET AL., pages 085439 - 1 * |
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