WO2006030981A1 - 透明導電性カーボンナノチューブフィルムとその製造方法 - Google Patents
透明導電性カーボンナノチューブフィルムとその製造方法 Download PDFInfo
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- WO2006030981A1 WO2006030981A1 PCT/JP2005/017549 JP2005017549W WO2006030981A1 WO 2006030981 A1 WO2006030981 A1 WO 2006030981A1 JP 2005017549 W JP2005017549 W JP 2005017549W WO 2006030981 A1 WO2006030981 A1 WO 2006030981A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/269—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension including synthetic resin or polymer layer or component
Definitions
- the present invention relates to a new carbon nanotube film and a method for producing the same, which can have high conductivity with a small amount of carbon nanotubes disposed, and can also have transparency and flexibility. And its application. Background art
- carbon nanotubes are nanoscale materials, it has been studied to use them as conductive materials and to use flexible resin films as their substrates (for example, see Non-Patent Document 1). .
- Non-Patent Document 1 Cheol Park, et al, Chemical Physics Letter 364 (2002), 303 Disclosure of the Invention
- the present invention is characterized by the following in order to solve the above problems.
- step (A) Dispersing and disposing carbon nanotubes on the substrate surface in step (A) is carried out by at least one of the following methods: growth, plating, spraying of carbon nanotubes on the substrate surface, or casting or ing of the carbon nanotube dispersion solution. .
- the resin film in step (B) is formed by at least one of spin coating, roll coating, dipping, or vapor phase film formation.
- the carbon nanotube is a single-walled carbon nanotube.
- a manufacturing apparatus for any one of the above methods wherein a carbon nanotube substrate forming portion that disperses and disposes carbon nanotubes on a base surface, and a carbon nanotube substrate that disperses and disposes carbon nanotubes A film deposition unit for depositing a resin film on the surface and a film separation unit for separating the deposited resin film are provided.
- a conductive film in which carbon nanotubes are dispersed or embedded as a layer only on the surface portion of a resin film, and the surface resistance of the surface portion in which the carbon nanotubes are embedded has a surface resistance of 100 / mouth or less. It is a conductive carbon nanotube film having high conductivity.
- the resistance of the surface portion in which the carbon nanotubes are dispersed and embedded is less than 10 k ⁇ / mouth.
- the maximum thickness (t) of the surface portion where the carbon nanotubes are dispersed and embedded is 10% of t ZT with respect to the maximum thickness (T) of the entire film.
- the carbon nanotube is a single-walled carbon nanotube.
- the electric resistance value does not change before and after the scotch tape peeling test, or the fluctuation is within 10%, and the dispersion is embedded.
- the carbon nanotubes have high adhesion.
- the surface portion of the resin film in which the force ponnanotube is dispersed and embedded is divided into a patterned plane area of the entire plane of the resin film. It is drawn.
- any of the above conductive carbon nanotube films is a conductive material that is at least a part of the configuration.
- any of the above conductive carbon nanotube films is a heating element in which at least a part of the structure is formed.
- FIG. 1 is a conceptual diagram illustrating a method for producing a transparent conductive carbon nanotube film of the present invention and a conventional production method, and comparing the characteristics thereof.
- FIG. 2 is a cross-sectional view schematically illustrating (a) the laminated conductive force-bonn nanotube film of the present invention. (B) It is sectional drawing which illustrated typically about the laminated type conductive carbon nanotube film of another form.
- FIG. 3 is an atomic force microscope image obtained by observing the state of the surface of the transparent conductive carbon nanotube film and the carbon nanotube in each step of the production process of the transparent conductive carbon nanotube film in Example 1.
- A An atomic force microscope image showing the state of carbon nanotubes dispersed on the substrate in step (A).
- B It is the atomic force microscope image which observed the state of the resin film surface isolate
- C An atomic force microscope image obtained by observing the state of the surface of the separated substrate in step (C).
- FIG. 4 is a graph showing surface resistance characteristics against bending of the transparent conductive carbon nanotube film of Example 1.
- FIG. 5 is a view showing the visible light region light transmission characteristics of the transparent conductive force-bonbon nanotube film having a surface resistance of 20 kQ / mouth of Example 1.
- FIG. 6 is a diagram showing the electrical transport properties up to 40 V of the 2 cm square transparent conductive carbon nanotube film of Example 1.
- FIG. 7 is a view showing the appearance of SWCNT conductive films of various resins exemplified in Example 2.
- FIG. 8 is a diagram illustrating the light transmission characteristics of the SWCNT ⁇ PVC conductive film in Example 2.
- FIG. 9 is a diagram illustrating the electrical transport characteristics of the SWCNT ⁇ PVC conductive film in Example 2.
- FIG. 10 is an atomic force microscope photograph and a Raman spectrum diagram at the time of molding and after film peeling in the case of a PVC conductive film.
- FIG. 11 is a schematic diagram showing a bending (bending) test method in Example 3.
- FIG. FIG. 12 is a diagram illustrating the relationship between the bending radius (r) and the back surface resistance in the case of the SWCNT ⁇ PVC conductive film in Example 3.
- Fig. 13 is a diagram illustrating the relationship between the number of bending iterations and the resistance change.
- Figure 14 shows a schematic diagram and a photograph showing an example of the configuration of an evening panel.
- Figure 15 illustrates the dependence of temperature and resistance on the applied voltage for the heater example. It is a figure.
- the present invention has the features as described above, and an embodiment thereof will be described below.
- CNT carbon nanotubes
- a resin film forming solution in which carbon nanotubes (CNT) are dispersed is used to form a thin film, the CNTs are dispersed throughout the formed film. Therefore, carbon nanotubes (CNTs) cannot be selectively arranged as a network or as a layer only on the surface portion of the formed resin film. And of course, even when a large amount of CNT is used, the bond of CNT inevitably decreases, and it is difficult to improve conductivity. Moreover, transparency is lowered by adding a large amount of CNT.
- the resin is dispersed in a state where CNTs are dispersed as a mutual network only on the surface of the film, or in an equivalent state, or in a denser layer state.
- the resin is embedded in an inseparable state by impregnation and solidification into the above-mentioned network or layer, and is present only on the surface of the resin film. Is obtained, and the conductivity is high. Moreover, high transparency can be obtained because only a small amount of CNT is required.
- the meaning of “embedding” means that carbon nanotubes (CNT) are adsorbed or adhered to the surface of the resin film. Not.
- the CNTs in a dispersed state are entirely or at least partially surrounded by the resin, embedded in the surface of the resin film, and embedded and integrated. is doing. In this embedding, a part of the surface of the CNT may be exposed to the outside.
- the step (A) may be performed by various means.
- the carbon nanotube on the substrate surface in the step (A) is preferably used.
- the dispersive arrangement is performed by at least one of the method of growing, plating, and dispersing carbon nanotubes on the substrate surface or casting the carbon nanotube dispersion solution.
- the chemical vapor deposition method is considered for the growth of carbon nanotubes on the substrate surface.
- an electric field is applied to a carbon nanotube dispersion using two electrodes (usually parallel plates), and the carbon nanotubes migrate through the solution by this electric field.
- step (B) a bonano tube in a solvent can be deposited on a substrate placed in place.
- the resin film formation in step (B) is applied by spin coating, roll coating, dipping, or vapor phase deposition. It is considered that the film is formed by at least one of the methods.
- Various means may be employed for the separation in the step (C), that is, for removing the resin film in which the carbon nanotubes are embedded by so-called transfer. For example, mechanical stripping or chemical etching is considered. At the time of peeling, if the sacrificial layer on the substrate side is attached, it is removed. The use of various cleaning agents and etching agents is considered.
- the substrate does not cause deterioration or deterioration of the formed resin film and that the separation in step (C) is relatively easy. Good.
- Such a substrate examples include semiconductors such as Si (silicon), metals, alloys, or appropriate ceramics or inorganic materials such as oxides, carbides, nitrides, or composite oxides. . Further, it may be a peelable resin or a composite of resin and metal, ceramics or the like.
- the polymer components that make up the resin film Alternatively, it may be natural or a mixture thereof, or may be crosslinked and cured by heat or light. These types and configurations may be selected according to the use of the conductive film provided with the carbon nanotubes and the required properties.
- polyethylene resins such as polyethylene, polypropylene, polybutylene, polystyrene resins, polyvinyl chloride, polyvinylidene chloride, polyvinyl fluoride, polyhalogenated polyolefin resins such as polytetrafluoroethylene, polyacrylonitrile, etc.
- Nitryl resin acrylic resin, methacrylic resin, polyvinyl ester resin, polyester resin, epoxy resin, urethane resin, urea resin, polycarbonate resin, polyether resin, polysulfone resin, polyimide resin, polyamide resin, polysilicon resin, cellulose resin It may be selected from various thermoplastic or thermosetting materials such as gelatin.
- a conductive film in which carbon nanotubes are dispersed and embedded only in the surface portion of the resin film is formed.
- the carbon nanotube embedded in the surface portion of the resin film (CNT ) May be of various diameters, lengths, aspect ratios, etc., open at both ends, or closed at least at one end, or with an opening in the middle, Further, it may be a modified body having a solid part, or a single-walled or multi-walled carbon nanotube is considered. One of these or two or more of them may be used.
- each of the above-described process units may be connected to each other in a patch manner, or may be configured in a continuous manner with conveying means such as a belt conveyor.
- a conductive carbon nanotube film having a high electrical conductivity of a surface portion containing a single-bonn nanotube and having an electrical resistance of 100 ° C. or lower.
- the surface resistance in this case is the surface resistance measured by the four probe method.
- such a resistance value of less than 1 O k Q / port, and even less than 3 k QZ port is provided.
- a transparent conductive carbon nanotube film characterized by having a high light transmittance (visible light) of 80% or more.
- the thickness of the surface portion on which the carbon nanotubes are dispersed and embedded is not particularly limited, and the application purpose, characteristics, workability to use, or production efficiency is taken into consideration. Can be determined. In general, considering the handling, conductivity, etc. of the film, the maximum thickness (t) in the longitudinal section of the surface where carbon nanotubes are dispersed and embedded is the maximum thickness (T ) Is preferably taken into account that t / T ⁇ 10%.
- the present invention also provides a flexible conductive film that can be completely bent in a bending (bending) test. The following is noteworthy about this excellent bending property.
- the endurance of the bending test is 100 times or more of complete bending, and whether the electric resistance value of the surface portion in which the carbon nanotube is embedded fluctuates before and after the complete bending. , Or a variation of 10% or less is realized.
- the electrical resistance value does not change before or after the scott tape peeling test, or the fluctuation is within a range of 10% or less.
- a conductive carbon nanotube film having high adhesion of buried carbon nanotubes is realized.
- the surface of the resin film in which the carbon nanotubes are dispersed and embedded is also shown.
- the surface portion can be divided into a patterned plane area out of the entire plane of the resin film, and such a patterned conductive film can be used for applications such as a latch panel. Very useful in deployment.
- FIG. 2 is a cross-sectional view schematically illustrating the conductive carbon nanotube film of the present invention.
- the carbon nanotube-containing part (1) in which the carbon nanotubes are dispersed and embedded in the resin film and the carbon nanotube-free part (2) in which the carbon nanotubes are not dispersed and embedded are shown.
- a transparent conductive carbon nanotube film comprising a carbon nanotube-free portion (2) on both sides of a carbon nanotube-containing portion (1) and a carbon nanotube-containing portion (1) on both sides of the carbon nanotube-free portion. It is clamped by (2).
- the carbon nanotube is covered with a resin film in which carbon nanotubes are not dispersed and embedded from both sides of a resin film in which force-bonn nanotubes are dispersed and embedded. It may be converted.
- the respective carbon nanotube embedded surface portions are laminated and integrated. It may be.
- a transparent conductive force-bonn nanotube film having such a structure also has high conductivity and high transparency.
- the carbon nanotube-containing portion (1) is disposed on both sides of the carbon nanotube-free portion (2), and the carbon nanotube-free portion (2) is located on both sides of the carbon nanotube-containing portion (1).
- a transparent conductive carbon nanotube film for example, the carbon nanotubes are laminated and integrated so that the carbon nanotubes are covered with a resin film in which carbon nanotubes are dispersed and embedded from both sides of the resin film. It may be what was done.
- the surfaces opposite to the respective carbon nanotube-containing surface portions are laminated and integrated. It may be what was done. Even with such a transparent conductive carbon nanotube film, high conductivity and high transparency It is what has.
- the transparent conductive carbon nanotube film of the present invention has high conductivity, can have high transparency, has excellent flexibility and adhesion, and can be patterned. Therefore, in various industrial fields, for example, evening panels, reinforced polymer films, contact lenses, electrodes for batteries (especially anodes for solar cells), field emission electron sources in the form of transparent films, flat panel displays LCD drive electrode, electromagnetic shielding material (used to prevent internal and external display noise), aircraft material (lightweight, electromagnetic shielding), sensor electrode, transparent heating sheet (cold area LCD display Can be used for artificial muscles, etc.) It can be used effectively. Therefore, an example will be shown below and will be described in more detail. Of course, the invention is not limited by the following examples. Example
- a transparent conductive carbon nanotube film was formed under the following conditions and process.
- Substrate The substrate, a silicon substrate having a thickness of S I_ ⁇ 2 film having a thickness of 6 0 0 nm (maximum 2 cm X 6 cm).
- CNT dispersion method Carbon nanotubes were directly synthesized on a silicon oxide substrate using chemical vapor synthesis. That is, first, an iron fine particle catalyst was synthesized on a silicon oxide substrate by the method of tt Dai et al. (H. Dai, et al, Nano Letters Vol 3, P157, (2003)). Next, a silicon oxide substrate on which an iron fine particle catalyst is fixed is placed in a 1 inch chemical vapor phase reactor, and the temperature is raised to 75 ° C. in an argon and hydrogen atmosphere, using ethylene gas as a carbon source, Carbon nanotubes were grown on it for 1-2 minutes.
- This technique enables high-density and uniform single-walled carbon nanotube (SWCNT) networks to be fabricated directly on a silicon oxide substrate.
- the surface resistance of a carbon nanotube (SWCNT) network on a silicon oxide substrate reaches even below the I k QZ port. Catalyst amount, growth conditions By adjusting the conditions, the surface resistance of the carbon nanotube network can be adjusted from 1 kQZ to infinity.
- C NT layer thickness The thickness of the SWC NT layer was estimated by measurement with a scanning atomic force microscope (DIMENSION made by National Instruments). By adjusting the growth conditions, it is possible to create SWC NT layers with a thickness of several nanometers to 10 micrometers.
- Resin type As the resin, polystyrene (average amount 28,000, Aldrich) was used. Polystyrene was dissolved in toluene at a weight ratio (1: 1 to 1: 3), vacuum degassed, and used as a film resin.
- Film deposition method Toluene-dissolved polystyrene resin is spin-coated (1 00 0 to 2 0 00 RPM, 60 to 1: 20 seconds, 1 to 2 times), and 1 0 0 0 0 3 0 Minute heating molding.
- Film thickness could be adjusted between 10 meters and 5 O jii meters by selecting the mixing ratio of polystyrene and toluene, and the spin coat rotation speed, time and frequency.
- the polystyrene thin film could be easily peeled off from the silicon substrate after molding.
- the polystyrene thin film and silicon substrate can be separated by immersing the sample in diluted hydrofluoric acid (5%) overnight and etching the natural oxide film layer. In either case, almost all of the carbon nanotubes are transferred to the polystyrene thin film and do not remain on the silicon substrate.
- FIG. 3 shows atomic force microscope images observing the surface of the transparent conductive carbon nanotube film and the state of the carbon nanotubes at each stage of the production process of the transparent conductive carbon nanotube film.
- Figure 3 (a) shows the state of the carbon nanotubes dispersed on the substrate in step (A). It can be seen that a uniform and dense network of carbon nanotubes is formed on the surface.
- Fig. 3 (b) shows the state of the resin film surface separated in step (C), and Fig. 4 (c) shows the separated state of step (C). The state of the surface of the substrate is shown. Both figures show that the carbon nanotubes are completely transferred (transferred) from the substrate to the resin.
- Figure 4 shows the relationship of the surface resistance characteristics to the bending of the transparent conductive carbon nanotube film. Even if the film is bent to a radius of curvature of 0.2 to 5 mm, the conductivity is hardly changed. In addition, the film itself yielded and destroyed at 0.25 mm.
- Figure 5 shows the results of measuring the visible light region light transmission characteristics of a transparent conductive carbon nanotube film with a high surface resistance of 20 kQ / mouth. It is. It can be seen that it has a constant and high transparency (88%) over the entire visible light range. The light transmittance of the resin film not embedded with carbon nanotubes was 90%.
- Figure 6 shows the results of measuring the electron transport properties of a transparent conductive carbon nanotube film with a 2 cm square surface resistance of 20 kQ / mouth. It was found that ideal ohmic characteristics can be obtained up to 40 V. In addition, in the case of the above transparent conductive carbon nanotube polystyrene film, a surface resistance of 4 k ⁇ / cm] could be produced.
- Conductive carbon nanotube films were produced using various resins in the same manner as in Example 1.
- FIG. 7 is an external view illustrating the obtained conductive film.
- the display in the figure is P S: Polystyrene
- Examples of film forming conditions for the above conductive PVC film are as follows.
- plasticizer di--2-ethylhexyl phthalate also known as dioctyl phthalate, D-2-ethylhexyl Phtahlate, C 6 H 4 (CO OC 8 H 17 ) 2 , Kanto Chemical Co., Inc., 99.5%
- 10-20 1;% and 2-4 times volume of cyclohexanone (Cyclohexanone, C 6 H w O, Wako Pure Chemi cal industries, Ltd., 99.0%).
- the substrate was spin-coated at 500 rpm 30 sec. Heat at 60 to 2-5 hours on a hot plate to dry.
- Figure 8 shows the wavelength dependence of the light transmission of the transparent conductive carbon nanotube film of Case No. 1 in Table 1. (1) in the figure shows the transmittance of the PVC film itself, and (2) shows the case of the SWCNT ⁇ PVC film. As can be seen from Fig. 8, it has a very constant light transmittance characteristic in the visible region.
- Figure 9 shows the electrical transport characteristics of SWCNT ⁇ PVC film (2 cm square) in Case No. 2-2 in Table 1.
- Table 2 shows the characteristics of conductive films in the case of other resins. TJP2005 / 017549 Table 2
- Figure 10 shows the atomic force micrograph and Raman spectroscopic spectrum when forming the conductive PVC film formed by the above method using the same substrate as in Example 1, and after peeling the film from the substrate. Is illustrated.
- the resin in this case is PVC
- the film thickness is 50 m
- the SWCNT layer thickness is 100-200 nm.
- various resins can be formed with a SWCNT layer thickness of 30 nm to 2000 nm and a film thickness of 1 to 5000 m. .
- the SWCNT ⁇ PVC film of Case No. 2-3 in Example 2 was evaluated for bendability and change in surface resistance due to bend by the bend test method shown in Fig. 11.
- a 20 mm square conductive carbon nanotube film was used for the test.
- the film is made of resin and has a thickness of 10 to 50 nm (usually 30 to 40 m).
- a conductive paste (manufactured by Chemtronics) was applied to both ends of the film in a width of about 2 mm to form an electrode.
- This film should have a single-walled carbon nanotube layer on the outside. And then sandwiched between clamps and fixed with double-sided tape. Finally, the electrodes on both ends of the film were connected to both terminals of the resistance meter. For the connection, gold wire or copper wire (diameter 2 mm) and the conductive paste described above were used.
- the bending test was performed by tightening the clamp little by little and measuring the clamp distance (2r in Fig. 10) and the resistance value.
- the clamp distance 2 r is equal to the diameter of the curved film.
- Figure 11 shows a plot of the results. The test was conducted with the clamp fully tightened, that is, until the bending radius reached 0 mm.
- the apparatus described above was also used for the repeat test. Tighten the clamp, bend the film to a bending radius of 1 mm, measure the resistance, and then return to the bending radius of 5 mm. This was repeated once and repeated 100 times, and the change in resistance value was plotted in the ratio to the resistance value before bending (Fig. 12).
- the SWCNT ⁇ PS film of Example 1 had a bending radius (r) of 0.25 mm and the film itself yielded, but in the case No. 2-3 above, Complete bending, that is, the left and right bent pieces of the sample film in FIG. 11 can be brought into contact with each other by surface contact, and the bending radius (r) can be substantially zero.
- 20 mm square conductive carbon nanotube film was used for the test.
- the film is made of resin and has a thickness of about 50 jm.
- a conductive paste was applied to both ends of the film with a width of about 2 mm to form an electrode.
- Gold or copper wire (diameter 0.2 mm G) was adhered to the electrode using a conductive paste and connected to both terminals of the resistance meter.
- a Scotch tape manufactured by 3EM Co., Ltd. having a width of 1.2 ⁇ 15 mm was attached to the surface of the film where the single-walled carbon nanotube layer exists.
- the substrate was changed to niobium (Nb), stainless steel (SUS), or nickel chrome alloy, and a SWC NT ⁇ PVC conductive film was produced.
- the film properties in this case were substantially the same.
- metal substrates are relatively inexpensive, easy to scale up, flexible, and easy to separate even with hard materials.
- a SWCNT layer was formed by a plating method instead of the method of forming the SWCNT layer by the CVD method in step (A) in Example 1.
- a single-walled nanotube dispersion was prepared based on the document of Penicaud et al. (JACS, 2005 (Penicaud et al., Journal of American Ch. Eiical Society 127, 8-9). Prepare a tetrahydrofuran solution of sodium metal and naphthalenes, add single-walled nanotubes, stir for 1 day, remove the supernatant (single-walled carbon nanotubes) by vacuum filtration of the supernatant, and wash with dimethyl The resultant was dispersed in formamide, and aggregates were removed by centrifugation.
- An aluminum plate having a width of 1 cm and a length of 4 cm was placed as an electrode in the obtained single-walled nanotube dispersion.
- the electrode spacing was l mm.
- a voltage of 5 V was applied and allowed to stand for 18 hours, a SWCNT thin film with a thickness of 1 m or less was formed on the anode. All of this treatment was performed in an anaerobic atmosphere.
- Example 6 A SWCNT conductive film was patterned as shown in Fig. 14, and a conductive panel was overlaid to form a latch panel.
- the type of resin is polyvinyl chloride, the thickness of the film is 40 to 80 / Am (one is 20 to 40 trn), and the thickness of the single-walled carbon nanotube layer is 200 to 300 nm .
- the manufacturing method is as follows.
- a fine silicon particle serving as a catalyst was fractionated into a patterned plane region on a silicon substrate with a 20 mm square oxide film having a thickness of 600 nanometers.
- the catalyst was placed by applying a mask to the substrate in some way in advance. Iron fine particles are not arranged in the masked area.
- a 2 ⁇ 20 mm tape was pasted so as to divide the substrate to form a mask.
- an iron fine particle catalyst was synthesized on a substrate by the method of H Dai et al. (II Dal. Et al, Nano Letters Vol 3. P157. (2003)). At this time, the catalyst is disposed only on the substrate portion not covered with the mask. Remove the mask tape after placing the fine iron catalyst.
- a silicon oxide substrate with an iron fine particle catalyst placed in a 1 inch diameter chemical vapor reactor is placed, heated to 75 ° C. in an atmosphere of argon and hydrogen, and ethylene gas is used as a carbon source.
- the carbon nanotubes were grown for 1-2 minutes.
- a dense and uniform single-walled carbon nanotube (SWCNT) network can be fabricated directly on a silicon oxide substrate, but SWCNT grows on the part that was covered by the mask when iron fine particles were placed. do not do.
- an arbitrary carbon nanotube pattern can be formed on the substrate.
- the substrate after growth by the applied mask has a band-like region in the center where no single-walled carbon nanotubes having a width of 2 mm are present.
- a PVC resin film was formed on the substrate in the same manner as in Example 2.
- the formed resin was separated from the substrate to obtain a conductive carbon nanotube film.
- the resulting film has the patterned single-walled nanotubes on the substrate transferred as it is.
- the region where single-walled carbon nanotubes exist on both sides of the band is a conductive band where electricity flows.
- One copper wire was bonded to each of the two conductive bands of the obtained conductive carbon nanotube film with a conductive pace rod to form an electrode for resistance measurement.
- Two conductive carbon nanotube films were fabricated, crossed so that their conductive bands were perpendicular, and fixed to a slide glass to create a dinner panel. At this time, the faces of the two films where the single-walled nanotubes are present face each other. When pressing the panel, the two conductive bands facing each other come into contact with each other and electricity flows.
- a SWC N T conductive film was used as a heating element.
- the structure of this heating element was as follows.
- Resin type Polyimide resin (Pier M. L. R C-5 0 5 7 (Wako Pure Chemical Industries, Ltd.)) Film thickness: 2 0
- Figure 15 illustrates the variation in temperature (A) and resistance (B), and it can be seen that heat is generated when voltage is applied.
- the temperature can be increased to 100 or more.
- a heater that can be used at higher temperatures can be realized, and a flexible heater can also be realized.
Abstract
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JP2006535251A JP4617479B2 (ja) | 2004-09-17 | 2005-09-16 | 透明導電性カーボンナノチューブフィルムを用いたタッチパネル |
US11/663,061 US20070298253A1 (en) | 2004-09-17 | 2005-09-16 | Transparent Conductive Carbon Nanotube Film and a Method for Producing the Same |
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