CN115285973B - Method for synthesizing carbon chain - Google Patents
Method for synthesizing carbon chain Download PDFInfo
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- CN115285973B CN115285973B CN202210964082.6A CN202210964082A CN115285973B CN 115285973 B CN115285973 B CN 115285973B CN 202210964082 A CN202210964082 A CN 202210964082A CN 115285973 B CN115285973 B CN 115285973B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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, organic molecules and open single-walled carbon nanotubes are subjected to high-temperature heat treatment under vacuum sealing conditions, and the organic molecules are vaporized or sublimated and then filled into the carbon nanotubes to obtain single-walled carbon nanotubes internally filled with the organic molecules; then annealing conversion treatment is carried out, and the single-walled carbon nanotube filled with organic molecules is subjected to heat treatment under the condition of vacuum or inert gas, so that carbon chains can be formed in the single-walled carbon nanotube. The invention provides a new method for converting organic molecules into carbon chains in single-walled carbon nanotubes, which solves the technical defect that the carbon chains cannot be directly synthesized in the single-walled carbon nanotubes in the prior art, 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
A carbon chain is a one-dimensional sp hybridized material consisting of carbon atoms-triple bonds. Currently, one of the ways to synthesize carbon chains is to perform limited-domain synthesis in carbon nanotubes, 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, the inside of the single-wall carbon nano tube is firstly synthesized into a carbon nano tube inner tube with small diameter, and then a carbon chain is formed in the inner tube. That is, even though single-walled carbon nanotubes are initially used, the synthesized carbon chains are present in the double-walled carbon nanotubes, not in the single-walled carbon nanotubes, after the final high temperature anneal. When the carbon nano tube is 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 a muffle furnace, a tube furnace, or the like, or by laser irradiation, or by voltage application, as long as the temperature reaches 1400 ℃ or higher, and generally about 1500 ℃ is preferable. However, such high temperature annealing places high demands on the equipment and therefore a new method for synthesizing carbon chains at lower temperatures is needed. In addition, there is 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 in the prior art, the invention provides a method for synthesizing a carbon chain, which converts an organic molecule 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 below 700 ℃.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for synthesizing a carbon chain, which specifically comprises the following steps: simultaneously placing the open single-wall carbon nano tube and the organic molecules under a vacuum airtight condition, and filling the organic molecules into the carbon nano tube through vaporization or sublimation by high-temperature heat treatment to prepare the single-wall carbon nano tube internally filled with the organic molecules; and then placing the single-walled carbon nanotube filled with the organic molecules in a vacuum or inert gas environment, and forming carbon chains in the single-walled carbon nanotube after annealing and conversion treatment.
Preferably, the organic molecule includes p-terphenyl, m-terphenyl, biphenyl, o-methylbenzonitrile, 1, 2-dicyanobenzene, and the like. More preferably, the organic molecule comprises p-terphenyl, o-methylbenzonitrile.
The invention converts the organic molecules into the carbon chains in the single-walled carbon nanotubes by 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 nanotubes in the prior art, overcomes the requirement that the synthesis temperature is always 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 vaporize or sublimate. Preferably, the high temperature heat treatment is carried out at a temperature of 200-400 ℃ for 70-80 hours.
Preferably, the annealing conversion treatment is carried out at a temperature of 500-700 ℃ for 1-3 hours.
The heating mode is not limited, and the high-temperature environment can be provided by a muffle furnace, a tube furnace and the like, or can be provided by laser irradiation, or can be generated by applying voltage.
Preferably, the diameter of the single-walled carbon nanotubes is 0.6-1.1nm. The method of the present invention is not limited to the method of preparing single-walled carbon nanotubes used, as long as a portion of the single-walled carbon nanotubes have a diameter ranging from 0.6 to 1.1nm.
Preferably, the annealing conversion treatment is performed under a vacuum environment.
The vacuum degree of the vacuum environment of the invention has no strict requirement. Preferably, the vacuum degree in step S1 is 9.0X10 -1 -5.0×10 -3 Pa. The vacuum degree in step S2 was 1.0X10 -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 carbon chains, which comprises the steps of firstly carrying out high-temperature heat treatment on organic molecules and open single-wall carbon nanotubes under vacuum sealing conditions, and filling the vaporized or sublimated organic molecules into the carbon nanotubes to obtain single-wall carbon nanotubes internally filled with the organic molecules; then annealing conversion treatment is carried out, and the single-walled carbon nanotube filled with organic molecules is subjected to heat treatment under the condition of vacuum or inert gas, so that carbon chains can be formed in the single-walled carbon nanotube. The invention provides a new method for converting organic molecules into carbon chains in single-walled carbon nanotubes, which solves the technical defect that the carbon chains cannot be directly synthesized in the single-walled carbon nanotubes in the prior art, 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 of a carbon chain synthesis;
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 describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1A method of synthesizing a carbon chain
According to the process flow of fig. 1, the method comprises the steps of:
(1) 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 at the bottom and middle of the glass tube, respectively, with a mass ratio of carbon nanotubes to p-terphenyl of 1:3, under vacuum conditions (vacuum degree of 2.3X10) -3 Pa), sealing the tube, and then carrying out heat treatment at 230 ℃ for 72 hours to obtain the p-terphenyl filled single-walled carbon nanotube.
(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 performed 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 a carbon chain.
As can be seen from the raman spectrum of fig. 2, the carbon chain was successfully synthesized by the method of this example.
Example 2A method of synthesizing a carbon chain
According to the process flow of fig. 1, the method comprises the steps of:
(1) O-methylbenzonitrile filling: open single-walled carbon nanotubes (HiPco type, diameterThe range of 0.8-1.2nm, the powder purchased from Xianfeng nanometer) and the powder of o-methyl benzonitrile (purchased from Meilin) are respectively arranged at the bottom and the middle part of a glass tube, the mass ratio of the carbon nano tube to the o-methyl benzonitrile is 1:5, and the glass tube is subjected to vacuum condition (the vacuum degree is 2.7X10) -3 Pa), sealing the tube, and then carrying out heat treatment at 350 ℃ for 72 hours to obtain the o-methylbenzonitrile filled single-walled carbon nanotube.
(2) High-temperature annealing conversion: annealing the o-methylbenzonitrile filled single-walled carbon nanotube in the step (1) at 650 ℃ for 1h, wherein the heat treatment is performed in vacuum, and the vacuum degree is 4.1 multiplied by 10 -3 Pa. The o-methylbenzonitrile molecules are decomposed at high temperature in the carbon nano tube and then assembled into a carbon chain.
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, according to the carbon chain synthesis method provided by the invention, firstly, organic molecules are filled into single-wall carbon nanotubes, and then annealing is performed in vacuum, so that the organic molecules are decomposed in the carbon nanotubes and assembled into carbon chains. The carbon chain synthesis method provided by the invention converts organic molecules into carbon chains in the single-walled carbon nanotubes, solves the technical defect that the carbon chains cannot be directly synthesized in the single-walled carbon nanotubes 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 above, 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 to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (5)
1. A method for synthesizing carbon chains is characterized in that an open single-wall carbon nanotube and an organic molecule are simultaneously placed under a vacuum sealing condition, and the organic molecule is filled into the carbon nanotube through vaporization or sublimation by high-temperature heat treatment, so that the single-wall carbon nanotube with the organic molecule filled inside is prepared; then placing the single-walled carbon nanotube filled with the organic molecules in a vacuum or inert gas environment, and forming carbon chains in the single-walled carbon nanotube after annealing and conversion treatment; the diameter of the single-wall carbon nano tube is 0.6-1.1nm; the organic molecule is selected from p-terphenyl, m-terphenyl, biphenyl, o-methylbenzonitrile and 1, 2-dicyanobenzene; the annealing conversion treatment temperature is 500-700 ℃ and the time is 1-3h.
2. A method of synthesizing a carbon chain according to claim 1, wherein the high temperature heat treatment is carried out at a temperature of 200-400 ℃ for a time of 70-80 hours.
3. A method of synthesizing a carbon chain according to claim 1, wherein the annealing conversion treatment is performed in a vacuum environment.
4. A method of synthesizing a carbon chain according to claim 1, wherein the vacuum level during the filling of the organic molecules is 9.0 x 10 -1 -5.0×10 -3 Pa。
5. A method of synthesizing a carbon chain according to claim 1, wherein the vacuum level during the annealing conversion treatment is 1.0 x 10 -3 -5.0×10 -3 Pa。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| US6683783B1 (en) * | 1997-03-07 | 2004-01-27 | William Marsh Rice University | Carbon fibers formed from single-wall carbon nanotubes |
| WO2003090255A2 (en) * | 2002-04-18 | 2003-10-30 | Northwestern University | Encapsulation of nanotubes via self-assembled nanostructures |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| "Single-wall-carbon-nanotube/single-carbon-chain molecular junctions";Felix Börrnertet al.;Felix Börrnertet al.;第085439-1至085439-5页 * |
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