CN111470492A - Preparation method of one-dimensional carbon chain - Google Patents
Preparation method of one-dimensional carbon chain Download PDFInfo
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- CN111470492A CN111470492A CN201911151182.1A CN201911151182A CN111470492A CN 111470492 A CN111470492 A CN 111470492A CN 201911151182 A CN201911151182 A CN 201911151182A CN 111470492 A CN111470492 A CN 111470492A
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Abstract
The invention belongs to the technical field of preparation of one-dimensional carbon chain materials, and particularly relates to a preparation method of a one-dimensional carbon chain. The invention provides a preparation method of a one-dimensional carbon chain, which comprises the following steps: step one, heat treatment: carrying out heat treatment on the single-walled carbon nanotube to obtain a first product; step two, solvent filling treatment: soaking the first product in an organic solvent, and filtering and drying the first product after soaking to obtain a second product; step three, high-temperature annealing: and after the second product is annealed at high temperature, cooling to room temperature to obtain a one-dimensional carbon chain product growing in the carbon nano tube. According to the invention, after the organic solvent filling treatment, molecules are filled in the single-walled carbon nano-tubes, and the single-walled carbon nano-tubes with the diameters within a limited range are filled by using a specific solvent, so that the controllable growth of one-dimensional carbon chains is realized; according to the preparation method provided by the invention, the yield of the carbon chain can be three times that of the prior art; the method solves the technical defects of low growth efficiency and low controllability existing in the preparation method of the one-dimensional carbon chain in the prior art.
Description
Technical Field
The invention belongs to the technical field of preparation of one-dimensional carbon chain materials, and particularly relates to a preparation method of a one-dimensional carbon chain.
Background
The one-dimensional carbon chain formed by sp orbital hybridization has excellent mechanical, electrical and optical properties theoretically, becomes one of new research hotspots of nano science and technology, and has a plurality of leading-edge application prospects in the fields of nano machinery, nano microelectronics and the like.
In the prior art, the preparation of one-dimensional carbon chains mainly has two methods: the two methods can reach the longest length respectively comprising 44 carbon atoms (5-6 nm) and more than 6000 carbon atoms (hundreds of nm) by chemical organic synthesis and growth in a limited environment in the carbon nano tube. The latter is relatively simpler, more convenient and faster and has controllable size, but the prior art has the problems of low carbon chain growth efficiency and low controllability.
Therefore, a method for preparing a one-dimensional carbon chain is developed to solve the technical defects of low growth efficiency and low controllability of the one-dimensional carbon chain preparation method in the prior art, and becomes a key scientific problem to be solved by the technical staff in the field.
Disclosure of Invention
In view of this, the invention provides a preparation method of a one-dimensional carbon chain, which is used for solving the technical defects of low growth efficiency and low controllability existing in the preparation method of the one-dimensional carbon chain in the prior art.
The invention provides a preparation method of a one-dimensional carbon chain, which comprises the following steps:
step one, heat treatment: carrying out heat treatment on the single-walled carbon nanotube to obtain a first product;
step two, solvent filling treatment: soaking the first product in an organic solvent, and filtering and drying the first product after soaking to obtain a second product;
step three, high-temperature annealing: and after the second product is annealed at high temperature, cooling to room temperature to obtain a one-dimensional carbon chain product growing in the carbon nano tube.
Preferably, in step two, the organic solvent is selected from: any one or more of alcohols, aldehydes, ketones, and benzene.
Preferably, in the step one, the diameter of the carbon nanotube is 1.3-2.0 nm.
Preferably, in step one, the heat treatment is performed in an oxygen-containing atmosphere; the oxygen-containing atmosphere is: air with humidity less than 80% or oxygen-argon mixed gas with oxygen content of 10% -80%.
Preferably, in the second step, the feeding ratio of the first product to the organic solvent is (0.1-10): 1 in parts by volume.
Preferably, in the first step, the temperature of the heat treatment is 350-500 ℃, and the time of the heat treatment is 0.5-2 hours.
Preferably, in the second step, the soaking method comprises: standing and soaking or ultrasonic soaking.
Preferably, the standing time is 1-24 h;
or the like, or, alternatively,
the ultrasonic time is 10 min-5 h.
Preferably, in the third step, the temperature of the high-temperature annealing is 1300-1550 ℃, and the time of the high-temperature annealing is 0.5-2 hours.
Preferably, in step three, the high-temperature annealing is performed in an inert gas protective atmosphere or in vacuum.
In summary, the invention provides a preparation method of a one-dimensional carbon chain, and the production method comprises the following steps: step one, heat treatment: carrying out heat treatment on the single-walled carbon nanotube to obtain a first product; step two, solvent filling treatment: soaking the first product in an organic solvent, and filtering and drying the first product after soaking to obtain a second product; step three, high-temperature annealing: and after the second product is annealed at high temperature, cooling to room temperature to obtain a one-dimensional carbon chain product growing in the carbon nano tube. According to the technical scheme provided by the invention, after solvent filling treatment, molecules are filled in the single-walled carbon nano-tubes, and the single-walled carbon nano-tubes with the diameters within a limited range are filled by using a specific solvent, so that the controllable growth of one-dimensional carbon chains is realized; furthermore, the carbon chain yield of the preparation method provided by the invention can be three times that of the prior art. The preparation method of the one-dimensional carbon chain provided by the invention solves the technical defects of low growth efficiency and low controllability existing in the preparation method of the one-dimensional carbon chain in the prior art.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for preparing a one-dimensional carbon chain according to an embodiment of the present invention;
FIG. 2 is a comparison graph of Raman spectrum lines of final products obtained by using single-walled carbon nanotubes filled with toluene molecules as raw materials, with test laser wavelengths of 633nm and 568nm respectively corresponding to long carbon chain and short carbon chain signals, and products obtained from single-walled carbon nanotubes which are not processed by the steps of the present invention;
FIG. 3 is a graph showing normalized area statistics of Raman spectral lines of a final product obtained from a single-walled carbon nanotube filled with toluene molecules corresponding to peak positions of carbon chains of different lengths, and comparing the normalized Raman spectral lines with the product obtained from the single-walled carbon nanotube not subjected to the step of the present invention;
FIG. 4 is a comparison graph of Raman spectrum lines of final products obtained from single-walled carbon nanotubes filled with methanol molecules, with test laser wavelengths of 633nm and 568nm corresponding to long carbon chain and short carbon chain signals, respectively, and products obtained from single-walled carbon nanotubes that have not been processed by the steps of the present invention;
FIG. 5 is a graph showing normalized area statistics of Raman spectral lines of a final product obtained from a single-walled carbon nanotube filled with methanol molecules corresponding to peak positions of carbon chains of different lengths, and comparing the normalized Raman spectral lines with a product obtained from a single-walled carbon nanotube not subjected to the step of the present invention;
FIG. 6 is a comparison graph of Raman spectrum lines of final products obtained from single-walled carbon nanotubes filled with acetone molecules, with test laser wavelengths of 633nm and 568nm corresponding to long carbon chain and short carbon chain signals, respectively, and products obtained from single-walled carbon nanotubes that were not processed by the steps of the present invention;
FIG. 7 is a graph showing normalized area statistics of Raman spectral lines of a final product obtained from a single-walled carbon nanotube filled with acetone molecules, corresponding to peak positions of carbon chains of different lengths, and comparing the normalized Raman spectral lines with a product obtained from a single-walled carbon nanotube which is not subjected to the step of the present invention;
FIG. 8 is a comparison graph of Raman spectrum lines of final products obtained from single-walled carbon nanotubes filled with propionaldehyde molecules, with test laser wavelengths of 633nm and 568nm corresponding to long carbon chain and short carbon chain signals, respectively, and products obtained from single-walled carbon nanotubes that have not been processed by the steps of the present invention;
fig. 9 is a graph showing normalized area statistics of raman spectral lines of a final product obtained from a single-walled carbon nanotube filled with propanal molecules, corresponding to peak positions of carbon chains of different lengths, and comparing the normalized area statistics with the product obtained from the single-walled carbon nanotube which is not subjected to the step of the present invention.
Detailed Description
The embodiment of the invention provides a preparation method of a one-dimensional carbon chain, which is used for solving the technical defects of low growth efficiency and low controllability existing in the preparation method of the one-dimensional carbon chain in the prior art.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to illustrate the present invention in more detail, the following examples are provided to describe the preparation method of a one-dimensional carbon chain according to the present invention.
Example 1
In this example, the raw material was a single-walled carbon nanotube having an average diameter of 1.7nm after purification, and the solvent was toluene.
And placing the purified single-walled carbon nanotube in a tube furnace, heating the single-walled carbon nanotube to 450 ℃ in oxygen-argon mixed gas with the oxygen content of 20%, keeping the temperature for 1 hour for heat treatment, and naturally cooling the single-walled carbon nanotube to room temperature to obtain a first product 1.
And (3) putting 10mg of the first product 1 into 10ml of toluene, carrying out water bath ultrasonic treatment for 60 minutes, and then sequentially filtering and drying the obtained material dispersion liquid to obtain the single-walled carbon nanotube containing toluene molecules inside, namely the second product 1.
The second product 1 is placed in an alumina crucible and in a tube furnace, and the pressure in the furnace tube is reduced to 10 ℃ by a molecular pump group-3And (3) the temperature is slowly increased to 1460 ℃ at the temperature increase speed of 10 ℃/min under Pa, high-temperature annealing is carried out for 1 hour, and then the temperature is reduced to room temperature in a natural cooling mode, so that the one-dimensional carbon chain obtained by growing in the carbon nano tube is obtained.
FIG. 2 is a comparison graph of Raman spectrum lines of final products obtained by using single-walled carbon nanotubes filled with toluene molecules as raw materials, with test laser wavelengths of 633nm and 568nm respectively corresponding to long carbon chain and short carbon chain signals, and products obtained from single-walled carbon nanotubes which are not processed by the steps of the present invention; fig. 3 is a summary of fig. 2, which is a histogram of normalized area statistics of the raman spectrum of the sample obtained in this example at five peak positions representing different length distributions of carbon chains, and it can be observed from fig. 3 that the single-walled carbon nanotube filled with toluene molecules in this example has more carbon chain content and the carbon chain yield of each length distribution is improved, taking the carbon chain grown by the single-walled carbon nanotube without molecules added inside as 100%.
Example 2
In this example, the raw material was a single-walled carbon nanotube having an average diameter of 1.3nm after purification, and the solvent was methanol.
And (3) placing the purified single-walled carbon nanotube in a tube furnace, heating to 400 ℃ in air with the humidity of 60%, keeping for 1 hour for heat treatment, and naturally cooling to room temperature to obtain a first product 2.
And (3) putting 1mg of the first product 2 into 2ml of methanol, carrying out ultrasonic treatment for 10 minutes, and then sequentially filtering and drying the obtained material dispersion liquid to obtain the single-walled carbon nanotube containing methanol molecules inside, namely the second product 2.
The second product 2 is placed in an alumina crucible and in a tube furnace, and the pressure in the furnace tube is reduced to 10 ℃ by a molecular pump group-4And Pa below, slowly raising the temperature to 1520 ℃ at a temperature rise speed of 10 ℃/min, carrying out high-temperature annealing for 1 hour, and then lowering the temperature to room temperature in a natural cooling mode to obtain the one-dimensional carbon chain grown in the carbon nano tube.
FIG. 4 is a comparison graph of Raman spectrum lines of final products obtained from single-walled carbon nanotubes filled with methanol molecules, with test laser wavelengths of 633nm and 568nm corresponding to long carbon chain and short carbon chain signals, respectively, and products obtained from single-walled carbon nanotubes that have not been processed by the steps of the present invention; FIG. 5 is a summary of FIG. 4, which is a histogram of normalized area statistics of Raman spectra of samples obtained in this example at five peak positions representing different length distributions of carbon chains, and it can be observed from FIG. 5 that the carbon chain content of the single-walled carbon nanotube filled with methanol molecules is higher in this example, and it can be found that the carbon chain content corresponds to 1790cm-1And 1800cm-1The growth efficiency of the longer carbon chain is improved more remarkably.
Example 3
In this example, the raw material was a single-walled carbon nanotube with an average diameter of 2.0nm after purification, and the solvent was acetone.
And (3) placing the purified single-walled carbon nanotube into a tube furnace, heating to 400 ℃ in air with the humidity of 65%, keeping for 1 hour for heat treatment, and naturally cooling to room temperature to obtain a first product 3.
And (3) putting 5mg of the first product 3 into 15ml of acetone, carrying out water bath ultrasonic treatment for 5 hours, and then sequentially filtering and drying the obtained material dispersion liquid to obtain the single-walled carbon nanotube containing acetone molecules inside, namely the second product 3.
And placing the second product 3 in an alumina crucible, placing the alumina crucible in a tubular furnace, slowly heating to 1500 ℃ at the heating rate of 5 ℃/min under the condition of inert gas, carrying out high-temperature annealing for 1 hour, and cooling to room temperature in a natural cooling manner to obtain the one-dimensional carbon chain grown in the carbon nano tube.
FIG. 6 shows the Raman spectrum of the final product obtained from single-walled carbon nanotube filled with acetone moleculesThe test laser wavelength is 633nm and 568nm, which respectively correspond to long carbon chain and short carbon chain signals, and are compared with the product obtained by the single-walled carbon nanotube which is not processed by the steps of the invention; FIG. 7 is a summary of FIG. 6, which is a histogram of normalized area statistics of Raman spectra of samples obtained in this example at five peak positions representing different length distributions of carbon chains, and it can be observed from FIG. 7 that the carbon chain content of the single-walled carbon nanotube with acetone molecules filled therein is higher in this example, and it can be found that the carbon chain content corresponds to 1790cm-1The growth efficiency of the longer carbon chain is improved more remarkably.
Example 4
In this example, the raw material was a single-walled carbon nanotube with an average diameter of 1.3nm after purification, and the solvent was propionaldehyde.
And (3) placing the purified single-walled carbon nanotube in a tube furnace, heating to 420 ℃ in air with the humidity of 55%, keeping for 1 hour for heat treatment, and naturally cooling to room temperature to obtain a first product 4.
And (3) putting 10mg of the first product 4 into 20ml of propionaldehyde, standing for more than 12 hours, and then sequentially filtering and drying the obtained material dispersion liquid to obtain the single-walled carbon nanotube containing propionaldehyde molecules inside, namely the second product 4.
The second product 4 is placed in an alumina crucible and in a tube furnace, and the pressure in the furnace tube is reduced to 10 ℃ by a molecular pump group-4And (3) the temperature is slowly increased to 1460 ℃ at the temperature increase speed of 5 ℃/min under Pa, high-temperature annealing is carried out for 1 hour, and then the temperature is reduced to room temperature in a natural cooling mode, so that the one-dimensional carbon chain obtained by growing in the carbon nano tube is obtained.
FIG. 8 is a comparison graph of Raman spectrum lines of final products obtained from single-walled carbon nanotubes filled with propionaldehyde molecules, with test laser wavelengths of 633nm and 568nm corresponding to long carbon chain and short carbon chain signals, respectively, and products obtained from single-walled carbon nanotubes that have not been processed by the steps of the present invention; FIG. 9 is a summary of FIG. 8, which is a histogram of normalized area statistics of Raman spectra of samples obtained in this example at five peak positions representing different length distributions of carbon chains, to provide a histogram of Raman spectraThe carbon chain growth of the single-walled carbon nanotube without the molecule added inside was 100%, and it can be observed from fig. 9 that the carbon chain content of the single-walled carbon nanotube with the propionaldehyde molecules filled therein in the present example was more, and it can be found that it corresponds to 1830cm-1、1840cm-1、1850cm-1The growth efficiency of the shorter carbon chains is improved more remarkably.
According to the technical scheme, the production method of the one-dimensional carbon chain has the following advantages:
1. in the production method provided by the invention, the yield of the one-dimensional carbon chain is successfully improved by using the single-walled carbon nanotube filled with different molecules for the first time;
2. in the production method provided by the invention, the controlled growth of the one-dimensional carbon chain with controllable length distribution is successfully realized by using the single-walled carbon nanotube filled with different molecules for the first time;
3. in the production method provided by the invention, a relevant mechanism influencing the growth length of the carbon chain is disclosed, namely the length of the carbon chain is related to the molecular species in the carbon nano tube;
4. in the production method provided by the invention, different filling molecules such as propionaldehyde are selected, so that the yield of the short carbon chain which is nearly three times higher than that of the prior art is successfully obtained;
5. the production process of the present invention successfully achieves a nearly three-fold higher yield of long carbon chains than the state of the art by selecting different filler molecules, such as acetone.
In summary, the invention provides a preparation method of a one-dimensional carbon chain, and the production method comprises the following steps: step one, heat treatment: carrying out heat treatment on the single-walled carbon nanotube to obtain a first product; step two, solvent filling treatment: soaking the first product in an organic solvent, and filtering and drying the first product after soaking to obtain a second product; step three, high-temperature annealing: and after the second product is annealed at high temperature, cooling to room temperature to obtain a one-dimensional carbon chain product growing in the carbon nano tube. According to the technical scheme provided by the invention, after solvent filling treatment, molecules are filled in the single-walled carbon nano-tubes, and the single-walled carbon nano-tubes with the diameters within a limited range are filled by using a specific solvent, so that the controllable growth of one-dimensional carbon chains is realized; furthermore, the carbon chain yield of the preparation method provided by the invention can be three times that of the prior art. The preparation method of the one-dimensional carbon chain provided by the invention solves the technical defects of low growth efficiency and low controllability existing in the preparation method of the one-dimensional carbon chain in the prior art.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a one-dimensional carbon chain is characterized by comprising the following steps:
step one, heat treatment: carrying out heat treatment on the single-walled carbon nanotube to obtain a first product;
step two, solvent filling treatment: soaking the first product in an organic solvent, and filtering and drying the first product after soaking to obtain a second product;
step three, high-temperature annealing: and after the second product is annealed at high temperature, cooling to room temperature to obtain a one-dimensional carbon chain product growing in the carbon nano tube.
2. The method according to claim 1, wherein in the second step, the organic solvent is selected from the group consisting of: any one or more of alcohols, aldehydes, ketones, and benzene.
3. The method of claim 1 or 2, wherein in the first step, the diameter of the carbon nanotube is 1.3-2.0 nm.
4. The method according to claim 1, wherein the heat treatment is carried out in an oxygen-containing atmosphere in step one; the oxygen-containing atmosphere is: air with humidity less than 80% or oxygen-argon mixed gas with oxygen content of 10% -80%.
5. The preparation method according to claim 1, wherein in the second step, the charging ratio of the first product to the organic solvent is (0.1-10): 1 in parts by volume.
6. The method according to claim 1, wherein in the first step, the temperature of the heat treatment is 350-500 ℃, and the time of the heat treatment is 0.5-2 h.
7. The preparation method according to claim 1, wherein in the second step, the soaking method comprises the following steps: standing and soaking or ultrasonic soaking.
8. The method according to claim 7, wherein the standing time is 1 to 24 hours;
or the like, or, alternatively,
the ultrasonic time is 10 min-5 h.
9. The method according to claim 1, wherein in the third step, the temperature of the high temperature annealing is 1300-1550 ℃, and the time of the high temperature annealing is 0.5-2 h.
10. The method according to claim 1 or 9, wherein the high-temperature annealing is performed in an inert gas atmosphere or in a vacuum in step three.
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