A method for making patterns on the surface of a flexible carbon nanotube film
By covering the surface of the carbon nanotube film with a shielding module and performing vapor phase chemical deposition to grow an amorphous carbon layer, the problem of damage to the carbon nanotube film by the patterning method in the prior art is solved, and a low-cost and efficient patterning effect is achieved.
Patent Information
- Application Number
- CN202311298723.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-09
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2043-10-09
AI Technical Summary
Existing photolithography and nanoimprinting technologies are not suitable for patterning the surface of carbon nanotube films, which can easily lead to film damage and are costly.
A secondary growth method combined with a mask blocking mode is used to cover the surface of the carbon nanotube film with a specially shaped masking module. Then, a secondary vapor deposition is performed in a vapor chemical deposition furnace to grow an amorphous carbon deposition layer, forming an additive pattern that is bonded to the carbon nanotube film through CC chemical bonds.
Without damaging the carbon nanotube film, an additive pattern with controllable size and shape is formed to provide protection, improve the tolerance and stability of the film, and reduce manufacturing costs.
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Figure CN117344282B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of thin film patterning, and in particular to a method for manufacturing patterns on the surface of a flexible carbon nanotube film. Background Art
[0002] Photolithography is a common method for patterning substrate surfaces, but it is a relatively expensive method and is mostly applicable to silicon-based semiconductor surfaces. In addition, nanoimprint lithography is a relatively common and relatively low-cost method for patterning substrate surfaces. However, due to issues such as the force of the imprint during the patterning process, nanoimprint lithography is not suitable for filling large-area patterns or patterning high-aspect-ratio structures. Carbon nanotube films are relatively thin, and the two aforementioned methods of substrate surface patterning can easily damage the carbon nanotube films. Therefore, neither photolithography nor nanoimprint lithography is suitable for patterning carbon nanotube film surfaces. Summary of the Invention
[0003] The purpose of the present invention is to overcome the defects existing in the prior art and provide a method for manufacturing patterns on the surface of a flexible carbon nanotube film. Specifically, a method for processing arbitrary surface patterns by combining a secondary growth method with a shielding blocking mode is provided. That is, a specially shaped shielding module is covered on the surface of the carbon nanotube film, and then the carbon nanotube film and the shielding module are placed together in a vapor phase chemical deposition (CVD) furnace for secondary vapor deposition to grow a bright silver amorphous carbon deposition layer. This amorphous carbon deposition layer has good hardness and is bonded to the surface of the carbon nanotube film through CC chemical bonds, with good bonding strength. Without damaging the carbon nanotube film, an additive pattern with controllable size and shape is formed.
[0004] To achieve the above objectives, the technical solution of the present invention is to design a method for making patterns on the surface of a flexible carbon nanotube film, comprising the following steps:
[0005] S1: Lay the carbon nanotube film on a ceramic tray, trim and remove burrs from the edges of the carbon nanotube film, lay several shielding modules on the carbon nanotube film according to a certain array size, and then place the ceramic tray with the carbon nanotube film and shielding modules in the furnace of a tube furnace;
[0006] S2: Continuously introduce a certain flow of argon into the tube furnace, check the smooth flow of argon at the front and rear ends of the tube furnace, set the tube furnace heating rate, reaction temperature, reaction time, and then start the heating program;
[0007] S3: When the temperature inside the tubular furnace reaches the set reaction temperature, a certain flow of anhydrous ethanol is continuously injected into the furnace through injection pump 1. After 10 to 20 minutes, a certain flow of anhydrous methanol is continuously injected into the furnace through injection pump 2. At the same time, a certain flow of hydrogen is continuously introduced into the tubular furnace. After the set reaction time is reached, the introduction of anhydrous ethanol, anhydrous methanol and hydrogen is stopped, and the furnace is naturally cooled to room temperature to obtain a patterned carbon nanotube film.
[0008] A preferred technical solution is that in step S1, the shielding module used is a ceramic block.
[0009] Another preferred technical solution is that in step S2, the argon flow rate is 100-120 sccm, the heating rate is 8-15°C / min, the reaction temperature is 1000-1200°C, and the reaction time is 0.5-2h.
[0010] A further preferred technical solution is that in step S2, the argon flow rate is 110 sccm, the heating rate is 10°C / min, the reaction temperature is 1100°C, and the reaction time is 2 hours.
[0011] Another preferred technical solution is that in step S3, the flow rate of anhydrous ethanol is 0.05-0.15 mL / min, the flow rate of anhydrous methanol is 0.03-0.10 mL / min, and the flow rate of argon is 50-100 sccm.
[0012] A further preferred technical solution is that in step S3, the flow rate of anhydrous ethanol is 0.10 mL / min, the flow rate of anhydrous methanol is 0.05 mL / min, and the flow rate of argon is 70 sccm.
[0013] The advantages and beneficial effects of the present invention are:
[0014] 1. The present invention provides a method for fabricating patterns on the surface of a flexible carbon nanotube film, specifically providing a method for processing arbitrary surface patterns using a secondary growth method combined with a shielding mode. Specifically, a specially shaped shielding module is covered on the surface of the carbon nanotube film, and then the carbon nanotube film and the shielding module are placed together in a vapor phase chemical deposition (CVD) furnace for secondary vapor deposition to grow a bright silver amorphous carbon deposition layer. This amorphous carbon deposition layer has good hardness and is bonded to the surface of the carbon nanotube film through CC chemical bonds, resulting in a strong bond. Without damaging the carbon nanotube film, an additive pattern with controllable size and shape is formed.
[0015] 2. The present invention provides a method for manufacturing a pattern on the surface of a flexible carbon nanotube film. The patterned structure manufactured on the surface of the carbon nanotube film acts as an "armor" to protect the surface of the carbon nanotube film, and exhibits excellent tolerance and stable elastic deformation recovery ability.
[0016] 3. The method of the present invention for manufacturing patterns on the surface of a flexible carbon nanotube film has simple operating steps and low manufacturing cost. It can break some limitations of traditional two-dimensional materials, such as increasing the freedom of the substrate to manipulate electromagnetic waves and changing the original single properties of the substrate surface. It provides a development platform for further exploring the potential of two-dimensional materials and helps to expand the application fields of carbon nanotube film materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 is a photograph of the patterned carbon nanotube film prepared in Example 4;
[0018] Figure 2 yes Figure 1 Scanning electron microscope image at point A in the middle;
[0019] Figure 3 yes Figure 1 Scanning electron microscope image at point B in the middle;
[0020] Figure 4 The carbon nanotube film with an amorphous carbon layer deposited on the surface prepared in Comparative Examples 1 to 4 is Figure 4 (a) corresponds to the carbon nanotube film with an amorphous carbon layer deposited on the surface prepared in Comparative Example 1. Figure 4 (b) corresponds to the carbon nanotube film with an amorphous carbon layer deposited on the surface prepared in Comparative Example 2. Figure 4 (c) corresponds to the carbon nanotube film with an amorphous carbon layer deposited on the surface prepared in Comparative Example 3. Figure 4 (d) corresponds to the carbon nanotube film with an amorphous carbon layer deposited on the surface prepared in Comparative Example 4. DETAILED DESCRIPTION
[0021] The following embodiments are further described in conjunction with the accompanying drawings and examples. The following embodiments are only used to more clearly illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention.
[0022] The carbon nanotube film is produced by floating catalyst chemical vapor deposition (FCCVD). The specific production process is to use a syringe to inject an ethanol solution containing 2wt% ferrocene and 1vol% thiophene into a tubular reactor. The syringe serves as the carbon source and CNT growth catalyst, and hydrogen (2000sccm) is injected as the carrier gas. The catalyst and carbon source are decomposed, deposited, and grown at different temperatures in the tubular reactor. Subsequently, they are organized into a thin aerogel hollow tube in the reactor tube inside the furnace. Then, with the help of flowing gas, they are blown out of the reactor tube and finally collected by a roller to obtain the carbon nanotube film.
[0023] Example 1
[0024] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0025] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0026] S2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 0.5 h, and start the heating program.
[0027] S3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70sccm into the tubular furnace. After the set reaction time of 0.5h, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a patterned carbon nanotube film.
[0028] Example 2
[0029] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0030] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0031] S2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 1 hour, and start the heating program.
[0032] S3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 1 hour, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a patterned carbon nanotube film.
[0033] Example 3
[0034] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0035] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0036] S2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 1.5 h, and start the heating program.
[0037] S3: When the temperature inside the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 1.5 hours, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a patterned carbon nanotube film.
[0038] Example 4
[0039] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0040] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0041] S2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 2 h, and start the heating program.
[0042] S3: When the temperature inside the tube furnace reaches the set reaction temperature of 1100°C, turn on the first syringe pump and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on the second syringe pump and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, hydrogen is continuously introduced into the tube furnace at a flow rate of 70 sccm. After the set reaction time of 2 hours, the introduction of anhydrous ethanol, anhydrous methanol and hydrogen is stopped. After the temperature of the tube furnace drops to room temperature, the introduction of argon is stopped to obtain a patterned carbon nanotube film, a photo of which is shown in the attached figure. Figure 1 .
[0043] Attachment Figure 1 is a photograph of the patterned carbon nanotube film prepared in Example 4. Figure 1 It can be seen that a bright silver amorphous carbon layer is deposited on the surface of the carbon nanotube film, and the area covered by the ceramic block appears as a black square block, and the black square area appears to have a groove structure when touched. This is because there is no secondary growth of the amorphous carbon layer at the area covered by the ceramic block. Therefore, the area covered by the ceramic block shows the original black color of the carbon nanotube film.
[0044] Figure 2 yes Figure 1 Scanning electron microscope image at point A, from Figure 2 It can be seen that the amorphous carbon layer on the surface of the carbon nanotube film is uniform, dense and crack-free; Figure 3 yes Figure 1 The electron microscope scanning image at point B in the middle, from Figure 3 In the figure, we can see that the bright silver amorphous carbon layer is clearly distinguished from the black square, indicating that an amorphous carbon layer has been deposited on the surface of the carbon nanotube film due to secondary growth.
[0045] The photographs of the patterned carbon nanotube films prepared in Examples 1 to 3 are consistent with the photographs and electron microscope scanning results of the patterned carbon nanotube films prepared in Example 4, except that the color of the bright silver amorphous carbon layer grown on the surface of the patterned carbon nanotube films prepared in Examples 1 to 4 becomes more and more obvious. This is because the thickness of the bright silver amorphous carbon layer grown on the surface of the carbon nanotube films gradually increases with the extension of the reaction time.
[0046] Example 5
[0047] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0048] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0049] S2: Continuously introduce argon gas at a flow rate of 100 sccm into the tube furnace, check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed, set the heating rate of the tube furnace to 8°C / min, the reaction temperature to 1000°C, the reaction time to 2 h, and start the heating program;
[0050] S3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1000°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.05 mL / min. After 15 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.03 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 50 sccm into the tubular furnace. After the set reaction time of 2 hours, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a patterned carbon nanotube film.
[0051] Example 6
[0052] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0053] S1: Place a 10cm x 10cm carbon nanotube film on a ceramic tray and trim the edges of the carbon nanotube film to remove burrs. Place several ceramic blocks with a bottom surface size of 1cm x 1cm on the carbon nanotube film in an array with a spacing of 1mm. Then, place the ceramic tray with the carbon nanotube film and ceramic blocks in the furnace of a tube furnace.
[0054] S2: Continuously introduce argon gas at a flow rate of 120 sccm into the tube furnace, check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed, set the tube furnace heating rate to 15°C / min, the reaction temperature to 1200°C, the reaction time to 2 h, and start the heating program;
[0055] S3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1200°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.15 mL / min. After 20 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.10 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 100 sccm into the tubular furnace. After the set reaction time of 2 hours, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a patterned carbon nanotube film.
[0056] The photographs of the patterned carbon nanotube films prepared in Examples 5 and 6 are consistent with the photographs and electron microscopy results of the patterned carbon nanotube films prepared in Example 4.
[0057] Comparative Example 1
[0058] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0059] T1: Place a 15cm x 10cm carbon nanotube film on a ceramic tray, trim the edges of the film to remove burrs, and then place the ceramic tray with the carbon nanotube film in the furnace of a tube furnace.
[0060] T2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 15 min, and start the heating program.
[0061] T3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on the first injection pump and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on the second injection pump and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 15 minutes, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a carbon nanotube film with amorphous carbon deposited on the surface.
[0062] Comparative Example 2
[0063] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0064] T1: Place a 15cm x 10cm carbon nanotube film on a ceramic tray, trim the edges of the film to remove burrs, and then place the ceramic tray with the carbon nanotube film in the furnace of a tube furnace.
[0065] T2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the tube furnace heating rate to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 25 min, and start the heating program.
[0066] T3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 25 minutes, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a carbon nanotube film with amorphous carbon deposited on the surface.
[0067] Comparative Example 3
[0068] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0069] T1: Place a 15cm x 10cm carbon nanotube film on a ceramic tray, trim the edges of the film to remove burrs, and then place the ceramic tray with the carbon nanotube film in the furnace of a tube furnace.
[0070] T2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the tube furnace heating rate to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 30 min, and start the heating program.
[0071] T3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 30 minutes, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a carbon nanotube film with amorphous carbon deposited on the surface.
[0072] Comparative Example 4
[0073] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0074] T1: Place a 15cm x 10cm carbon nanotube film on a ceramic tray, trim the edges of the film to remove burrs, and then place the ceramic tray with the carbon nanotube film in the furnace of a tube furnace.
[0075] T2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the heating rate of the tube furnace to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 2 h, and start the heating program.
[0076] T3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 2 hours, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a carbon nanotube film with amorphous carbon deposited on the surface.
[0077] Comparative Example 5
[0078] The method of the present invention is used to create a pattern on the surface of a flexible carbon nanotube film. The specific operations are as follows:
[0079] T1: Place a 15cm x 10cm carbon nanotube film on a ceramic tray, trim the edges of the film to remove burrs, and then place the ceramic tray with the carbon nanotube film in the furnace of a tube furnace.
[0080] T2: Continuously introduce argon gas at a flow rate of 110 sccm into the tube furnace. Check the front and rear ends of the tube furnace to ensure that the argon flow is unobstructed. Set the tube furnace heating rate to 10°C / min, the reaction temperature to 1100°C, and the reaction time to 130 min, and start the heating program.
[0081] T3: When the internal temperature of the tubular furnace reaches the set reaction temperature of 1100°C, turn on injection pump 1 and inject anhydrous ethanol into the furnace at an injection rate of 0.1 mL / min. After 10 minutes, turn on injection pump 2 and inject anhydrous methanol into the furnace at an injection rate of 0.05 mL / min. At the same time, continuously introduce hydrogen at a flow rate of 70 sccm into the tubular furnace. After the set reaction time of 130 minutes, stop introducing anhydrous ethanol, anhydrous methanol and hydrogen. After the temperature of the tubular furnace drops to room temperature, stop introducing argon to obtain a carbon nanotube film with amorphous carbon deposited on the surface.
[0082] Table 1 Performance parameters of carbon nanotube films with amorphous carbon deposited on the surface prepared in Comparative Examples 1 to 5
[0083]
[0084] From the experimental data results in Table 1, it can be seen that the carbon nanotube films with amorphous carbon deposited on the surface prepared in Comparative Examples 1 to 2 still present the original black color. This is because the reaction time is short and the thickness of the amorphous carbon layer deposited on the surface of the carbon nanotube film is thin, so that the amorphous carbon layer does not cover the original black color of the carbon nanotube film; it can be seen from Comparative Examples 1 to 4 that as the reaction time increases, the thickness of the amorphous carbon layer deposited on the surface of the carbon nanotube film gradually increases, so that the color of the prepared carbon nanotube film with amorphous carbon deposited on the surface gradually changes from black to a distinct bright silver color; however, the color of the carbon nanotube film with amorphous carbon deposited on the surface prepared in Comparative Example 5 appears burnt black, and the overall toughness of the film deteriorates, and cracks appear when bent, indicating that the carbon nanotube film suffers brittle failure; in summary, the appropriate reaction time for the deposition of the amorphous carbon layer in the carbon nanotube film reaction is 0.5 to 2 hours.
[0085] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.
Claims
1. A method for making a pattern on the surface of a flexible carbon nanotube film, characterized in that: The steps are as follows: S1: Lay the carbon nanotube film on a ceramic tray, trim and remove burrs from the edges of the carbon nanotube film, lay several shielding modules on the carbon nanotube film, and then place the ceramic tray with the carbon nanotube film and shielding modules in the furnace of a tube furnace; S2: Continuously introduce argon into the tube furnace, check the smooth flow of argon at the front and rear ends of the tube furnace, set the tube furnace heating rate, reaction temperature, reaction time, and then start the heating program; S3: When the temperature inside the tube furnace reaches the set reaction temperature, anhydrous ethanol is continuously injected into the furnace through syringe pump 1. After 10 to 20 minutes, anhydrous methanol is continuously injected into the furnace through syringe pump 2. At the same time, hydrogen is continuously introduced into the tube furnace. After the set reaction time is reached, the introduction of anhydrous ethanol, anhydrous methanol and hydrogen is stopped, and the tube furnace is naturally cooled to room temperature to obtain a patterned carbon nanotube film. Wherein: the shielding modules are laid on the carbon nanotube film in an array with a pitch of 1 mm; In step S2, the argon flow rate is 100-120 sccm, the heating rate is 8-15°C / min, the reaction temperature is 1000-1200°C, and the reaction time is 0.5-2h; In step S3, the flow rate of anhydrous ethanol is 0.05-0.15 mL / min, and the flow rate of anhydrous methanol is 0.03-0.10 mL / min; In the step S3, the flow rate of hydrogen is 50 sccm, 70 sccm or 100 sccm.
2. The method for producing a pattern on the surface of a flexible carbon nanotube film according to claim 1, wherein: In the step S1, the shielding module used is a ceramic block.
3. The method for producing a pattern on the surface of a flexible carbon nanotube film according to claim 1, wherein: In step S2, the argon flow rate is 110 sccm, the heating rate is 10°C / min, the reaction temperature is 1100°C, and the reaction time is 2 h.
4. The method for producing a pattern on the surface of a flexible carbon nanotube film according to claim 1, wherein: In step S3, the flow rate of anhydrous ethanol is 0.10 mL / min, the flow rate of anhydrous methanol is 0.05 mL / min, and the flow rate of argon is 70 sccm.
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