Method for removing carbon nanotube surface conjugated polymer material

Abstract

The application relates to a method for removing conjugated polymer materials on the surface of carbon nanotubes, and belongs to the technical field of nanotube surface molecule removal. The method comprises the following steps: annealing treatment is performed on carbon nanotubes with conjugated polymer materials on the surface under a protective atmosphere, so that carbon-carbon double bonds formed between the main chain of the conjugated polymer materials and the carbon nanotubes during the preparation of the carbon nanotubes are broken, so as to remove part of the conjugated polymer materials; a solvent is used to perform rotary flushing on the carbon nanotubes subjected to the annealing treatment; and the flushed carbon nanotubes are subjected to annealing treatment again under a protective atmosphere. The method can ensure that the carbon-carbon double bonds formed between the main chain of the conjugated polymer materials and the carbon nanotubes during the preparation of the carbon nanotubes are broken, so that the effect of removing the conjugated polymer materials on the surface of the carbon nanotubes is achieved; the conjugated polymer materials on the surface of the carbon nanotubes can be removed completely, and the morphology of the carbon nanotubes is not damaged during the removal process.

Description

Technical Field

[0001] This invention relates to the field of carbon nanotube surface molecular removal technology, and more particularly to a method for removing conjugated polymer materials from the surface of carbon nanotubes. Background Technology

[0002] In existing technologies, organic dispersants on the surface of carbon nanotubes are removed by direct annealing or by degradable molecules such as TFA. However, in the process of removing organic dispersants on the surface of carbon nanotubes by direct annealing, there is a problem that they cannot be completely removed; in the process of removing organic dispersants on the surface of carbon nanotubes by degradable molecules such as TFA, there is a problem that the morphology of the carbon nanotube film is damaged during the degradation process. Summary of the Invention

[0003] The present invention aims to provide a method for removing conjugated polymer materials from the surface of carbon nanotubes, so as to overcome the shortcomings of the prior art. The technical problem to be solved by the present invention is achieved through the following technical solution.

[0004] The method for removing conjugated polymer materials from the surface of carbon nanotubes provided by this invention includes the following steps:

[0005] The carbon nanotubes with conjugated polymer material on their surface are annealed under a protective atmosphere to break the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotube during the preparation of the carbon nanotubes, thereby removing some of the conjugated polymer material.

[0006] The annealed carbon nanotubes were spun and rinsed with a solvent.

[0007] The rinsed carbon nanotubes were then annealed again under a protective atmosphere.

[0008] In the above scheme, the method further includes the following steps:

[0009] The carbon nanotubes that have undergone re-annealing were spun and rinsed with a solvent.

[0010] Repeat the above steps until all conjugated polymer material on the surface of the carbon nanotubes is removed.

[0011] In the above scheme, the main chain of the conjugated polymer material is carbazole, fluorene, thiophene, pyridine, or bipyridine.

[0012] In the above scheme, the protective atmosphere is nitrogen, argon, or a mixture of both.

[0013] In the above scheme, the annealing temperature under a protective atmosphere is 400-800 degrees Celsius.

[0014] In the above scheme, the annealing time during annealing in a protective atmosphere is 5 to 200 minutes.

[0015] In the above scheme, the solvent is an organic solvent or water.

[0016] In the above scheme, the organic solvent includes ethanol and tetrahydrofuran.

[0017] In the above scheme, the rotation speed during rotary rinsing is 200rpm-6000rpm.

[0018] In the above scheme, the rotation rinsing time is 10 minutes.

[0019] This invention has the following advantages:

[0020] The method for removing conjugated polymer material from the surface of carbon nanotubes provided by this invention involves annealing the carbon nanotubes with conjugated polymer material on their surface under a protective atmosphere. This annealing process breaks the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotubes during the preparation of the carbon nanotubes, thereby removing the conjugated polymer material from the surface of the carbon nanotubes. The annealed carbon nanotubes are then subjected to a rotary rinse with a solvent to remove the remaining conjugated polymer material from their surface, thus completely removing the conjugated polymer material from the carbon nanotubes without damaging the morphology of the carbon nanotubes. Attached Figure Description

[0021] Figure 1 This is a flowchart illustrating the steps of a method for removing conjugated polymer material from the surface of carbon nanotubes according to the first embodiment of the present invention.

[0022] Figure 2 This is a flowchart illustrating the steps of a method for removing conjugated polymer material from the surface of carbon nanotubes according to a second embodiment of the present invention. Detailed Implementation

[0023] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0024] like Figure 1 As shown, the method for removing conjugated polymer material from the surface of carbon nanotubes provided in the first embodiment of the present invention includes:

[0025] Step S101: The carbon nanotubes with conjugated polymer material on their surface are annealed at a temperature of 400-800 degrees under a protective atmosphere to remove some of the conjugated polymer material on the surface of the carbon nanotubes.

[0026] Step S102: Use a solvent to spin-wash the annealed carbon nanotubes to remove the remaining conjugated polymer material on the surface of the carbon nanotubes;

[0027] Step S103: The rinsed carbon nanotubes are annealed again at a temperature of 400-800 degrees under a protective atmosphere.

[0028] In this embodiment, the carbon nanotubes with conjugated polymer material on their surface are annealed at a temperature of 400-800 degrees Celsius under a protective atmosphere. This ensures that the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotubes are broken, achieving a removal effect of more than 80% of the conjugated polymer material. The remaining material is then washed by high-speed rotation, which ensures that the conjugated polymer material has sufficient stability to meet the requirements of subsequent film preparation, while also removing it without damaging the carbon nanotubes.

[0029] The method for removing conjugated polymer material from the surface of carbon nanotubes provided in the second embodiment of the present invention includes the following steps:

[0030] Step S201: Annealing carbon nanotubes with conjugated polymer materials on their surface at a temperature of 400-800 degrees Celsius under a protective atmosphere;

[0031] Step S202: The annealed carbon nanotubes are spun and rinsed with solvent;

[0032] Step S203: The rinsed carbon nanotubes are annealed again at a temperature of 400-800 degrees under a protective atmosphere.

[0033] Step S204: The carbon nanotubes that have undergone re-annealing are spun and rinsed with solvent;

[0034] Step S205: Repeat the above steps until all conjugated polymer material on the surface of the carbon nanotubes is removed.

[0035] In this embodiment, carbon nanotubes with conjugated polymer material on their surface are subjected to cyclic annealing and rotary rinsing. During the annealing process, the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotube are broken, achieving partial removal of the conjugated polymer material. By high-speed rotary rinsing, most of the remaining conjugated polymer material can be removed. Annealing and rotary rinsing are performed again to ensure that the conjugated polymer material on the surface of the carbon nanotubes is completely removed.

[0036] A method for removing conjugated polymer material from the surface of carbon nanotubes, provided in a comparative embodiment of the present invention, includes:

[0037] Carbon nanotubes with conjugated polymer material on their surface are annealed at 400-800 degrees Celsius under a protective atmosphere to remove some of the conjugated polymer material from the carbon nanotubes.

[0038] In this embodiment, only carbon nanotubes with conjugated polymer material on their surface are annealed. This ensures that the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotube are broken, achieving a removal effect of more than 80% of the conjugated polymer material. However, the remaining conjugated polymer material is not removed.

[0039] Therefore, the second embodiment of the present invention is the preferred embodiment, which can ensure that the conjugated polymer material on the surface of carbon nanotubes is completely removed.

[0040] In various embodiments of the present invention, the carbon nanotubes are single-walled carbon nanotubes or multi-walled carbon nanotubes, etc. The carbon nanotube raw materials can be carbon nanotubes based on chemical vapor deposition, Hi pco tubes based on high-pressure chemical vapor deposition, small-diameter CoMocat tubes, or carbon nanotubes grown by arc discharge method, carbon nanotubes grown by laser scorching method, etc.

[0041] The main chain of the aforementioned conjugated polymer material consists of conjugated units such as carbazole, fluorene, thiophene, pyridine, and bipyridine. In the preparation process of carbon nanotubes, the aforementioned conjugated polymer material and carbon nanotube raw materials are added to a solvent and thoroughly mixed to form a mixture. Carbon nanotubes are then prepared based on this mixture. As a result, the surface of the formed carbon nanotubes has conjugated polymer material. Since the carbon nanotubes are prepared based on the mixture of the conjugated polymer material and the carbon nanotube raw materials, carbon-carbon double bonds are formed between the main chain of the aforementioned conjugated polymer material and the carbon nanotubes.

[0042] During the annealing process of carbon nanotubes with conjugated polymer materials on their surface at a temperature of 400-800 degrees Celsius under a protective atmosphere, the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotubes can be broken, thereby achieving the effect of removing the conjugated polymer material from the surface of the carbon nanotubes.

[0043] In the first and second embodiments of the present invention, the solvent used for the rotary rinsing of the annealed carbon nanotubes is an organic solvent or water; wherein the organic solvent includes ethanol, tetrahydrofuran, etc.; the rotary rinsing time of the annealed carbon nanotubes with the solvent is 10 minutes, and the rotation speed is 200rpm-6000rpm.

[0044] In various embodiments of the present invention, when performing annealing at a temperature of 400-800 degrees, the annealing time can be set to 5-200 minutes, specifically, the annealing temperature is preferably 500 degrees.

[0045] In various embodiments of the present invention, the protective atmosphere is a non-reactive gas such as nitrogen or argon, and a mixture of various non-reactive gases may be used.

[0046] It should be noted that the above detailed descriptions are exemplary and intended to provide further explanation of this application. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0047] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0048] It should be noted that the terms "first," "second," etc., used in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such terms can be used interchangeably where appropriate so that the embodiments of this application described herein can be implemented in sequences other than those illustrated or described herein.

[0049] Furthermore, the terms “comprising” and “having”, and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or apparatus that includes a series of steps or units is not necessarily limited to those steps or units that are explicitly listed, but may include other steps or units that are not explicitly listed or that are inherent to such process, method, product, or apparatus.

[0050] In the detailed description above, reference has been made to the accompanying drawings, which form part of this document. In the drawings, similar symbols typically identify similar parts unless the context otherwise indicates otherwise. The illustrated embodiments described in the detailed specification, drawings, and claims are not intended to be limiting. Other embodiments may be used and other changes may be made without departing from the spirit or scope of the subject matter presented herein.

[0051] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for removing conjugated polymer material from the surface of carbon nanotubes, characterized in that, The method includes the following steps: Step S1: The carbon nanotubes with conjugated polymer material on their surface are annealed under a protective atmosphere at a temperature of 400-800 degrees Celsius. This process breaks the carbon-carbon double bonds formed between the main chain of the conjugated polymer material and the carbon nanotubes during the preparation of the carbon nanotubes, thereby removing some of the conjugated polymer material. Step S2: The annealed carbon nanotubes are rinsed with solvent at a rotation speed of 200 rpm to 6000 rpm. Step S3: The rinsed carbon nanotubes are annealed again under a protective atmosphere at a temperature of 400-800 degrees Celsius. Step S4: Use the solvent to perform a rotary rinse of the carbon nanotubes that have undergone the second annealing treatment at a speed of 200 rpm to 6000 rpm. Step S5: Repeat steps S3 and S4 above until all conjugated polymer material on the surface of carbon nanotubes is removed.

2. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 1, characterized in that, The backbone of the conjugated polymer material is carbazole, fluorene, thiophene, pyridine, or bipyridine.

3. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 1, characterized in that, The protective atmosphere is nitrogen, argon, or a mixture of both.

4. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 1, characterized in that, Annealing time during annealing in a protective atmosphere is 5 to 200 minutes.

5. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 1, characterized in that, The solvent is an organic solvent or water.

6. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 5, characterized in that, The organic solvents include ethanol and tetrahydrofuran.

7. The method for removing conjugated polymer material from the surface of carbon nanotubes according to claim 1, characterized in that, The rinsing time is 10 minutes.

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