CN117326548B - Method for removing dispersing agent on surface of carbon nano tube - Google Patents
Method for removing dispersing agent on surface of carbon nano tube Download PDFInfo
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- CN117326548B CN117326548B CN202311637487.XA CN202311637487A CN117326548B CN 117326548 B CN117326548 B CN 117326548B CN 202311637487 A CN202311637487 A CN 202311637487A CN 117326548 B CN117326548 B CN 117326548B
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- temperature chamber
- dispersing agent
- nano tube
- pulse
- constant temperature
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 52
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 52
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 4
- 230000035485 pulse pressure Effects 0.000 claims description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000002071 nanotube Substances 0.000 abstract description 2
- 210000002381 plasma Anatomy 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
Classifications
-
- 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
- C01B32/17—Purification
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for removing a dispersing agent on the surface of a carbon nano tube, which belongs to the technical field of nano tube surface molecule removal, and comprises the following steps: placing carbon nanotubes with organic dispersing agents on the surfaces in a constant temperature chamber; vacuumizing the constant-temperature chamber; and introducing pulse gas into the constant temperature chamber to selectively adsorb the organic dispersing agent on the surface of the carbon nano tube, and removing the organic dispersing agent on the surface of the carbon nano tube. According to the method for removing the carbon nanotube surface dispersing agent, the organic dispersing agent on the surface of the carbon nanotube is selectively removed through the pulse gas based on the difference of adsorption capacity of the carbon nanotube surface and the organic dispersing agent on the surface of the gas molecule or the plasma, the damage to the carbon nanotube is reduced, the pulse electromagnetic valve controls the pulse gas to intermittently enter the constant temperature chamber to react with the organic dispersing agent on the surface of the carbon nanotube, and the controllability is better.
Description
Technical Field
The invention relates to the technical field of nanotube surface molecule removal, in particular to a method for removing a carbon nanotube surface dispersing agent.
Background
Most of the prior art removes the organic dispersing agent on the surface of the carbon nano tube by direct annealing or removing the organic dispersing agent on the surface of the carbon nano tube by direct annealing, however, the annealing can be performed by adjusting parameters such as atmosphere, temperature, pressure, time and the like, but the adjustable parameters are limited, so that the removal of the organic dispersing agent on the surface of the carbon nano tube is not clean.
Disclosure of Invention
The invention aims to provide a method for removing a carbon nano tube surface dispersing agent, which solves the defects in the prior art, and the technical problem to be solved by the invention is realized by the following technical scheme.
The method for removing the carbon nano tube surface dispersing agent provided by the invention comprises the following steps:
placing carbon nanotubes with organic dispersing agents on the surfaces in a constant temperature chamber;
vacuumizing the constant-temperature chamber;
and introducing pulse gas into the constant temperature chamber to selectively adsorb the organic dispersing agent on the surface of the carbon nano tube, and removing the organic dispersing agent on the surface of the carbon nano tube.
In the scheme, the time for vacuumizing the constant-temperature chamber is 5-10 min.
In the above scheme, after the constant temperature chamber is vacuumized, the pressure of the constant temperature chamber is 10 - 2 Pa～10 -4 Pa。
In the above scheme, the constant temperature chamber is externally connected with a pulse electromagnetic valve.
In the above scheme, the pulse electromagnetic valve controls the pulse gas to be intermittently introduced into the constant temperature chamber.
In the scheme, the interval time of each two times of pulse gas is 2s-2000s, the time of each time of pulse gas is 5ms-2000ms, the total times of pulse gas is 5-1000 times, and the pulse pressure of the pulse gas is 5Pa-20000Pa.
In the above scheme, the temperature in the constant temperature chamber is 200-900 ℃.
In the above-mentioned scheme, the pulse gas adopts oxygen, ozone or plasma gas.
In the above scheme, nitrogen is introduced as carrier gas before pulse gas is introduced into the thermostatic chamber.
In the scheme, the flow rate of the introduced nitrogen is 5sccm-1000sccm.
The embodiment of the invention has the following advantages:
according to the method for removing the carbon nanotube surface dispersing agent, provided by the embodiment of the invention, based on the difference of adsorption capacity of the carbon nanotube surface and the organic dispersing agent on gas molecules or plasmas, the organic dispersing agent on the carbon nanotube surface is selectively removed through pulse gas, so that the damage to the carbon nanotube is reduced, the pulse electromagnetic valve controls the pulse gas to intermittently enter the constant temperature chamber to react with the organic dispersing agent on the carbon nanotube surface, and the controllability is better.
Drawings
Fig. 1 is a step diagram of a method for removing a carbon nanotube surface dispersant according to the present invention.
FIG. 2 is a step diagram of a method for removing a carbon nanotube surface dispersant according to an embodiment of the present invention.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The invention will be described in detail below with reference to the drawings in connection with embodiments.
As shown in fig. 1, the present invention provides a method for removing a dispersant on a surface of a carbon nanotube, including:
step S1: placing a carbon nano tube with an organic dispersing agent on the surface in a constant temperature chamber, wherein the temperature in the constant temperature chamber is 200-900 ℃, the constant temperature chamber is externally connected with a pulse electromagnetic valve, and the pulse electromagnetic valve is used for controlling the pulse gas to be intermittently introduced into the constant temperature chamber;
step S2: vacuumizing the constant-temperature chamber, wherein the vacuumizing time of the constant-temperature chamber is 5-10 min, and the pressure of the constant-temperature chamber is 10 after the vacuumizing of the constant-temperature chamber -2 Pa～10 - 4 Pa；
Step S3: introducing nitrogen into the constant temperature chamber to serve as carrier gas, wherein the flow rate of the introduced nitrogen is 5sccm-1000sccm;
step S4: and introducing pulse gas into the constant temperature chamber to selectively adsorb the organic dispersing agent on the surface of the carbon nano tube and remove the organic dispersing agent on the surface of the carbon nano tube, wherein the pulse gas adopts oxygen, ozone or plasma gas, the interval time of introducing the pulse gas every two times is 2s-2000s, the time of introducing the pulse gas every time is 5ms-2000ms, the total times of introducing the pulse gas is 5-1000 times, and the pulse pressure of the pulse gas is 5Pa-20000Pa.
Specifically, because the carbon nanotube surface and the organic dispersing agent have different adsorption capacities on gas molecules or plasmas, the organic dispersing agent on the carbon nanotube surface can be selectively removed through pulse gas, the damage to the carbon nanotube is reduced, and the pulse electromagnetic valve controls the pulse gas to intermittently enter the constant temperature chamber to react with the organic dispersing agent on the carbon nanotube surface, so that the reaction progress can be better controlled.
Specifically, after step S4 is completed, the pulse electromagnetic valve externally connected to the constant temperature chamber is closed, nitrogen is introduced for a period of time, and then the carbon nanotubes are taken out.
In one embodiment of the present invention, a method for removing a carbon nanotube surface dispersant includes:
step S101: placing carbon nanotubes with organic dispersing agents on the surfaces in a constant temperature chamber with the temperature of 200 ℃;
step S102: vacuumizing the constant-temperature chamber for 5-10 min to ensure that the pressure of the constant-temperature chamber is 10 -3 Pa；
Step S103: introducing nitrogen into the constant temperature chamber to serve as carrier gas, wherein the flow rate of the introduced nitrogen is 20sccm;
step S104: oxygen is introduced into the constant temperature chamber as pulse gas to selectively adsorb the organic dispersing agent on the surface of the carbon nano tube, and the organic dispersing agent on the surface of the carbon nano tube is removed, wherein the interval time of oxygen introduction every two times is 2s-2000s, the time of oxygen introduction every time is 5ms, the total times of oxygen introduction is 100 times, and the pulse pressure of oxygen is 20Pa.
It should be noted that the foregoing detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, 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 belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is intended to include the plural unless the context clearly indicates otherwise. Furthermore, it will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, steps, operations, devices, components, and/or groups thereof.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or otherwise described herein.
Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those elements but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways, such as rotated 90 degrees or at other orientations, and the spatially relative descriptors used herein interpreted accordingly.
In the above detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, like numerals typically identify like components unless context indicates otherwise. The illustrated embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments may be utilized, and other changes may be made, without departing from the spirit or scope of the subject matter presented herein.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for removing a carbon nanotube surface dispersant, the method comprising:
placing the carbon nano tube with the organic dispersing agent on the surface in a constant temperature chamber, wherein the constant temperature chamber is externally connected with a pulse electromagnetic valve;
vacuumizing the constant-temperature chamber;
introducing pulse gas into the constant-temperature chamber to selectively adsorb the organic dispersing agent on the surface of the carbon nano tube and remove the organic dispersing agent on the surface of the carbon nano tube, wherein the pulse gas is controlled to be intermittently introduced into the constant-temperature chamber through the pulse electromagnetic valve;
the pulse gas adopts oxygen or ozone;
after removing the organic dispersing agent on the surface of the carbon nano tube, closing a pulse electromagnetic valve externally connected with the constant temperature chamber, introducing nitrogen for a period of time, and taking out the carbon nano tube.
2. The method for removing the carbon nanotube surface dispersant according to claim 1, wherein the time for evacuating the constant temperature chamber is 5min to 10min.
3. The method for removing a carbon nanotube surface dispersant according to claim 2, wherein after the constant temperature chamber is vacuumized, the pressure of the constant temperature chamber is 10 -2 Pa～10 -4 Pa。
4. The method for removing the surface dispersant of carbon nanotubes according to claim 1, wherein the interval time between each two pulse gas introduction is 2s-2000s, the time of each pulse gas introduction is 5ms-2000ms, the total number of times of pulse gas introduction is 5-1000 times, and the pulse pressure of the pulse gas is 5Pa-20000Pa.
5. The method for removing a carbon nanotube surface dispersant according to claim 1, wherein the temperature in the constant temperature chamber is 200 to 900 degrees.
6. The method for removing a carbon nanotube surface dispersant according to claim 1, wherein nitrogen is introduced as a carrier gas before the pulse gas is introduced into the constant temperature chamber.
7. The method for removing a carbon nanotube surface dispersant according to claim 6, wherein the flow rate of the introduced nitrogen gas is 5sccm to 1000sccm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311637487.XA CN117326548B (en) | 2023-12-01 | 2023-12-01 | Method for removing dispersing agent on surface of carbon nano tube |
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| CN202311637487.XA CN117326548B (en) | 2023-12-01 | 2023-12-01 | Method for removing dispersing agent on surface of carbon nano tube |
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| CN117326548B true CN117326548B (en) | 2024-02-23 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109225094A (en) * | 2018-08-29 | 2019-01-18 | 北京大学 | The minimizing technology and electronic device of the surface polymer of carbon nano-tube film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109225094A (en) * | 2018-08-29 | 2019-01-18 | 北京大学 | The minimizing technology and electronic device of the surface polymer of carbon nano-tube film |
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