WO2016080327A1 - カーボンナノチューブ分散液、機能性膜および複合素材 - Google Patents

カーボンナノチューブ分散液、機能性膜および複合素材 Download PDF

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WO2016080327A1
WO2016080327A1 PCT/JP2015/082064 JP2015082064W WO2016080327A1 WO 2016080327 A1 WO2016080327 A1 WO 2016080327A1 JP 2015082064 W JP2015082064 W JP 2015082064W WO 2016080327 A1 WO2016080327 A1 WO 2016080327A1
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cnt
cnts
dispersion
functional film
dispersion liquid
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French (fr)
Japanese (ja)
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智大 古園
拓治 小向
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ニッタ株式会社
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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
    • 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
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

Definitions

  • the present invention relates to a dispersion containing carbon nanotubes (hereinafter referred to as CNT), a functional film, and a composite material.
  • CNT carbon nanotubes
  • a CNT dispersion containing CNT is known as a coating solution (see Patent Document 1).
  • CNT dispersions are conventionally used for the production of conductive films imparted with electrical conductivity derived from CNTs, and conductive films imparted with electrical conductivity can be referred to as functional films.
  • conductive films imparted with electrical conductivity can be referred to as functional films.
  • the dispersibility of the CNTs in the dispersion can be enhanced by the functional groups formed on the CNT surface or the dispersant added separately.
  • a solution containing a resin as a coating film formation is used as a dispersion medium in which CNTs are dispersed.
  • CNTs are present in the resin layer. If the content of CNT in the CNT dispersion increases, the CNT-derived characteristics in the resulting functional film are enhanced, but the inherent characteristics of the resin tend to be reduced. It is desirable that the CNT content in the CNT dispersion is as small as possible within a range in which a desired function is exhibited.
  • the CNT 104 in the CNT dispersion 100 is well dispersed in the dispersion medium 102, but the functional group is lost and the characteristics of the CNT are lost. It is not possible to obtain a functional film that sufficiently exhibits the above.
  • CNTs with few functional groups on the surface have poor dispersibility in the dispersion medium 102, and a bundle of aggregates 106 and aggregates 108 are generated.
  • the dispersant is used, as shown in FIG. 13, the CNTs 114 in the CNT dispersion liquid 110 are covered with the dispersant 116 and are well dispersed in the dispersion medium 112. However, since the contact resistance is increased by the dispersant 116, the characteristics of the CNT 114 are not sufficiently exhibited in the obtained functional film.
  • CNTs with a large aspect ratio generally have low dispersibility in the dispersion medium.
  • a plurality of CNTs 124 gather to form many bundled aggregates 126 and aggregates.
  • a network between the CNTs 124 cannot be obtained sufficiently. If the CNT aspect ratio is small, the problem of aggregation does not occur. However, even in a CNT dispersion containing CNT having a small aspect ratio and a dispersion medium, a network of CNTs cannot be sufficiently obtained.
  • the content in the CNT dispersion liquid is set for both CNTs having a large aspect ratio and CNTs having a small aspect ratio. Need to increase.
  • the CNT aggregates 108 exist in the resin layer 202 as shown in FIG.
  • the shape of the aggregate 108 becomes a convex portion 204 and appears on the surface of the functional film 200.
  • the flatness of the film surface is impaired and the film thickness varies.
  • the strength of the functional film 200 is reduced.
  • the CNT dispersion liquid which can produce the functional film which fully provided the characteristic derived from CNT, without impairing the original characteristic of a coating-film formation has not been obtained yet.
  • the present invention provides a CNT dispersion that can provide a functional film that sufficiently exhibits the characteristics derived from CNTs while sufficiently maintaining the original characteristics of the coating film formed product, a functional film using the same, and a composite material
  • the purpose is to provide.
  • the CNT dispersion according to the present invention is a CNT dispersion containing a dispersion medium containing a coating film formation product and a solvent, and CNTs dispersed in the dispersion medium, and the concentration x (volume%) of the CNT,
  • the thixo index y ( ⁇ 100 / ⁇ 400) satisfies the relationship of the following formulas (1), (2), (3), and (4).
  • ⁇ 100 is the viscosity (mPa ⁇ s) at a shear rate of 100 (1 / sec)
  • ⁇ 400 is the viscosity (mPa ⁇ s) at a shear rate of 400 (1 / sec).
  • the functional film according to the present invention is formed using the CNT dispersion liquid.
  • a composite material according to the present invention includes a base material and the functional film that covers the surface of the base material.
  • the CNT dispersion has a higher TI value y than the conventional one, a functional film in which the characteristics derived from CNT are sufficiently exhibited while sufficiently maintaining the original characteristics of the coating film formation, And a composite material provided with a functional film can be formed.
  • FIG. 2A is a schematic diagram illustrating the configuration of the functional film of the present embodiment
  • FIG. 2B is an enlarged view of a portion surrounded by a square frame in FIG. 2A.
  • FIG. 4A is an SEM (scanning electron microscope) photograph of the CNT used in the example
  • FIG. 4B is an enlarged photograph of FIG. 4A.
  • FIG. 5A is an SEM photograph of CNT used in the comparative example
  • FIG. 5B is an enlarged photograph of FIG. 5A.
  • 6A is an SEM photograph of CNT used in the comparative example
  • FIG. 6B is an enlarged photograph of FIG. 6A.
  • FIG. 7A is an SEM photograph of CNT used in the comparative example, and FIG. 7B is an enlarged photograph of FIG. 7A.
  • FIG. 8A is an SEM photograph of CNT used in the comparative example, and FIG. 8B is an enlarged photograph of FIG. 8A.
  • concentration (volume%) concentration (volume%)
  • the composite material 10 includes a base material 12 and a functional film 20 provided on the surface of the base material 12.
  • the base material 12 is not particularly limited, and can be any shape that requires electrical conductivity, thermal conductivity, or mechanical strength.
  • the material of the base material 12 can be selected from, for example, a polymer material such as a PET film, a metal material such as a stainless steel foil, and an inorganic material such as a glass plate and ceramics.
  • the functional film 20 has a film thickness t as shown in FIG. 2A.
  • the CNTs 34 are uniformly dispersed in the coating film 22 and entangled with each other to form a network structure 24. Yes.
  • a thin film thickness of about 0.1 to 100 ⁇ m, preferably 30 ⁇ m or less, and even if the contained CNT 34 is at a low concentration, it is derived from CNT such as electrical conductivity, thermal conductivity, or mechanical strength.
  • the functional film 20 of the present embodiment can suppress the strength reduction caused by the CNTs 34, and can maintain the original characteristics of the coating film 22 if the CNTs 34 have a low concentration.
  • the surface of the base material 12 on which the functional film 20 is provided is not limited to a flat surface, and may be a curved surface. Since the functional film 20 can be formed with a small film thickness, even if the surface of the base material 12 is a curved surface, the surface of the base material 12 can be covered well following the curved surface.
  • the base material 12 is a container having a predetermined shape, the functional film 20 may be formed on the inner surface of the container. Since the functional film 20 can be formed with a thin film thickness, even if it is formed on the inner surface of the container, the effect on the volume of the container is small.
  • the composite material 10 of this embodiment can be manufactured using the CNT dispersion 30 shown in FIG.
  • the CNT dispersion liquid 30 includes a dispersion medium 32 and CNTs 34 dispersed in the dispersion medium 32.
  • the dispersion medium 32 is a solution in which a resin as a coating film formation is dissolved in a solvent, and the resin and the solvent are used in a predetermined combination.
  • a resin as a coating film formation
  • NMP N-methyl-2-pyrrolidone
  • the concentration of PI in the entire dispersion medium 32 is preferably about 0.5 to 15% by volume, and more preferably about 2 to 10% by volume.
  • PVP polyvinyl pyrrolidone
  • water is used as the solvent, for example.
  • the concentration of PVP in the entire dispersion medium 32 is preferably about 9 to 70% by volume, more preferably about 20 to 60% by volume.
  • Polyamideimide can also be used as the resin, and NMP and dimethylacetamide are used as the PAI solvent, for example.
  • concentration of PAI in the entire dispersion medium 32 is preferably about 0.5 to 24% by volume, and more preferably about 3 to 15% by volume.
  • epoxy or urethane may be used as the resin.
  • MEK methyl ethyl ketone
  • acetone can be used as the solvent, respectively.
  • the resin in the dispersion medium 32 contained in the CNT dispersion 30 constitutes the coating film 22 in the functional film 20.
  • the CNT 34 is preferably about 1 to 100 ⁇ m in length and has a high aspect ratio.
  • the CNT dispersion liquid 30 of the present embodiment is prepared using a longer CNT 34 as a raw material.
  • the CNT 34 contained in the CNT dispersion 30 in FIG. 3 is obtained by shortening a longer material CNT by a dispersion process.
  • the length of the CNTs 34 in the CNT dispersion 30 is 1 ⁇ m or more, the CNTs 34 are entangled with each other in the functional film 20 and directly connected to each other, thereby forming a good network structure 24 (see FIG. 2B). Further, the CNTs 34 tend to aggregate when the length exceeds 100 ⁇ m.
  • the length of the CNT 34 is less than 1 ⁇ m, it is difficult to form the network structure 24 in the functional film 20.
  • the CNT 34 preferably has a diameter of about 30 nm or less. If the diameter of the CNT 34 is 30 nm or less, the CNT 34 is rich in flexibility and easily deforms, and therefore can exist in the CNT dispersion 30 without restriction. On the other hand, if the diameter of the CNT 34 exceeds 30 nm, the flexibility is lost and it becomes difficult to form the network structure 24. More preferably, the CNT 34 has a diameter of 20 nm or less.
  • the length and diameter of the CNT 34 are the average values measured using a transmission electron microscope (TEM) photo.
  • the surface of the CNT 34 has few defects.
  • Defects on the surface of CNT 34 are carboxyl group (—COOH), sulfone group (—SO 3 H), nitro group (—NO 2 ), aldehyde group (—CHO), amino group (—NH 2 ), and hydroxyl group (—OH).
  • the functional group is imparted by a surface treatment.
  • many functional groups existed on the surface for the purpose of improving the dispersibility in the CNT dispersion. Since the CNTs 34 contained in the CNT dispersion 30 of the present embodiment are not subjected to surface treatment, there are few defects due to functional groups.
  • a viscosity ⁇ 100 (mPa ⁇ s) at a shear rate of 100 (1 / sec) and a viscosity ⁇ 400 (at a shear rate of 400 (1 / sec)) ( mPa ⁇ s)) and a thixo index (TI value) represented by a ratio ( ⁇ 100 / ⁇ 400) and a CNT concentration (volume%) in the CNT dispersion 30 were found.
  • the following expressions (1), (2), (3), and (4) are present between the CNT concentration x (volume%) and the TI value y.
  • nano-dispersion means a state where CNTs 34 are physically separated and dispersed in a state where they are not entangled one by one. It means a state in which the proportion of objects is 10% or less.
  • the CNT dispersion liquid 30 of this embodiment can be prepared by dispersing predetermined CNTs 34 in the dispersion medium 32.
  • the raw material CNT used for the preparation of the CNT dispersion 30 is obtained by forming a catalyst film made of aluminum or iron on a silicon substrate using a thermal CVD method as described in, for example, Japanese Patent Application Laid-Open No. 2007-12611.
  • the catalyst metal for the growth of CNTs can be made fine and the hydrocarbon gas can be brought into contact with the catalyst metal in a heated atmosphere.
  • CNTs obtained by other manufacturing methods such as arc discharge method and laser evaporation method
  • impurities other than CNTs may be removed by high-temperature annealing in an inert gas after the CNTs are manufactured.
  • the CNTs 34 manufactured in this manufacturing example are long and linearly oriented with a high aspect ratio of a diameter of 30 nm or less and a length of several hundred ⁇ m to several mm.
  • the CNT 34 may be a single layer or a multilayer, but a multilayer is preferable.
  • the dispersion medium 32 can be prepared by dissolving the resin in a predetermined solvent at a predetermined concentration.
  • the CNT dispersion 30 is obtained by pulverizing the CNTs 34 produced as described above and adding them to the dispersion medium 32, and then nano-dispersing the CNTs 34 in the dispersion medium 32 using a wet disperser, a homogenizer, an ultrasonic disperser, or the like. Can be prepared.
  • the CNT 34 may be pretreated as long as a desired length is obtained and the functional groups on the surface are not lost.
  • wet dispersion in a viscous liquid.
  • wet dispersion it is possible to prevent entanglement between the CNTs and cutting or damage of the CNTs due to rubbing.
  • additives such as a dispersant, a surfactant, a thixotropic agent (viscoelasticity modifier) and the like are not necessarily required, but do not adversely affect the effects of the present invention. If so, such additives may be used.
  • the CNT dispersion 30 of the present embodiment as described above is applied on a predetermined base material 12 by bar coating, spraying, spin coating, knife coating, dip coating, or the like.
  • the CNTs 34 in the CNT dispersion 30 are nano-dispersed by receiving shear stress.
  • the amount of the CNT dispersion 30 to be applied can be adjusted so that the functional film 20 having a target film thickness can be obtained.
  • the functional film 20 can be formed by drying the applied CNT dispersion 30.
  • the CNT 34 is fixed in a state where the network structure 24 is formed. What is necessary is just to set drying conditions suitably according to the kind of resin and solvent which are contained in the dispersion medium 32 in the CNT dispersion liquid 30.
  • drying conditions suitably according to the kind of resin and solvent which are contained in the dispersion medium 32 in the CNT dispersion liquid 30.
  • the viscosity ⁇ 100 (mPa ⁇ s) at a shear rate of 100 (1 / sec) and the viscosity ⁇ 400 (mPa ⁇ s) at a shear rate of 400 (1 / sec)) A predetermined correlation is established between the ratio ( ⁇ 100 / ⁇ 400) and the CNT concentration (volume%).
  • the CNT dispersion 30 according to the present embodiment has a TI value y exceeding a predetermined value at a predetermined CNT concentration.
  • the functional film 20 that sufficiently exhibits the characteristics derived from the CNTs 34 while sufficiently maintaining the original characteristics of the resin. Can be formed.
  • the CNTs 34 are nano-dispersed when subjected to shear stress. Therefore, the CNT 34 is nano-dispersed by receiving shear stress when the CNT dispersion 30 is applied, and can be uniformly applied to the surface of the base material 12 even at a low concentration.
  • the shear stress is lowered, so that the CNTs 34 are gradually entangled with each other to form the network structure 24.
  • the viscosity of the CNT dispersion liquid 30 is increased, it is possible to prevent dripping or the like.
  • the functional film 20 includes the network structure 24 in which the CNTs 34 are entangled with each other, excellent electrical conductivity and mechanical strength derived from CNTs can be obtained even with a film thickness of about 0.1 to 100 ⁇ m.
  • the CNT dispersion 30 can form the composite material 10 having the characteristics derived from the CNTs 34, that is, electrical conductivity and mechanical strength, by providing the functional film 20 on the surface of an arbitrary base material 12.
  • the present invention is not limited to the above-described embodiment, and can be appropriately changed within the scope of the gist of the present invention.
  • the functional film 20 of the present embodiment can also be formed on a predetermined support so as to be peelable.
  • the functional film 20 is formed on the support by the same method as in the case of the composite material 10 and is peeled from the support, the functional film 20 can be obtained as an independent single body.
  • the coating film formation is a resin
  • the present invention is not limited to this and can be applied to a general viscous body.
  • CNT dispersions of Examples 1 to 7 were prepared by dispersing CNTs at a predetermined concentration in a dispersion medium containing a resin and a solvent.
  • the CNTs used here are MW-CNTs (multi-walled carbon nanotubes) grown on a silicon substrate by a thermal CVD method, and have a length of 350 ⁇ m and a diameter of 13 nm.
  • FIG. 4 the SEM photograph before the dispersion
  • CNT was mixed with a dispersion medium without performing surface treatment, and dispersed in the dispersion medium using a wet disperser. Neither a dispersant nor a thixotropic agent (viscoelasticity modifier) was blended, and wet dispersion treatment was performed 15 times to obtain a CNT dispersion of the example.
  • CNT dispersions of Comparative Examples 1 to 8 were prepared using commercially available CNTs at a predetermined concentration.
  • Nanocyl CNT product number NC7000, length 1.5 ⁇ m, diameter 9.5 nm
  • SWeNT CNT product number SMW200, length 3.5 ⁇ m
  • CNTs manufactured by Cano product number FloTube 9011, length 10 ⁇ m, diameter 11 nm
  • CNTs manufactured by JEIO product number JC-400, length 1 ⁇ m, diameter 20 nm
  • the numerical values of the length and the diameter of the CNT according to the comparative example are both catalog values.
  • the length and diameter of CNT in the obtained CNT dispersion were determined by TEM observation. Note that the CNTs in the CNT dispersions of Examples 1 to 7 are presumed to have few surface functional groups and few surface defects because they are not surface-treated.
  • Viscosity at 23 ° C. was measured for the CNT dispersions of Examples and Comparative Examples. Viscosity was measured using a Wellsbrookfield cone / plate viscometer, and the shear rate was varied to determine the viscosity at 100 / sec ( ⁇ 100) and the viscosity at 400 / sec ( ⁇ 400). It was. Let ( ⁇ 100 / ⁇ 400) be the thixo index (TI value).
  • Table 1 summarizes the CNTs and dispersion media contained in the CNT dispersions of Examples and Comparative Examples, together with the viscosity and TI value of the CNT dispersions.
  • NMP is an abbreviation for N-methyl-2pyrrolidone
  • PVP and PI are abbreviations for polyvinylpyrrolidone and polyimide, respectively.
  • (volume%) of resin is the density
  • the CNTs contained in the CNT dispersions of Examples 1 to 7 are as long as about 1 to 100 ⁇ m.
  • the CNT having a length of about 20 ⁇ m has a large aspect ratio exceeding 1000.
  • the CNT dispersions of Comparative Examples 1 to 8 contain CNTs having a length of about 0.1 to 1 ⁇ m and a small aspect ratio of about 100 at the maximum.
  • 5 to 8 show SEM photographs before dispersion treatment for the CNT used in Comparative Examples 1 to 3, the CNT used in Comparative Examples 4 to 6, the CNT used in Comparative Example 7, and the CNT used in Comparative Example 8. Each is shown.
  • island-shaped aggregates 140 to 143 formed by entanglement of individual CNTs are confirmed.
  • the CNT dispersion liquid of the examples is prepared using CNT having a high aspect ratio. Although the CNTs are shortened by carrying out the dispersion treatment, the CNT dispersion liquid of the example still has a length as long as about 20 ⁇ m and contains CNTs having a very large aspect ratio exceeding 1000.
  • the CNT dispersion of the comparative example was prepared using CNT containing aggregates that were entangled and aggregated.
  • FIG. 9 is a graph showing the relationship between the CNT concentration (volume%) and the TI value described in Table 1 above as the x-axis and y-axis, respectively.
  • the CNT dispersion liquid of the example has a larger TI value y than the CNT dispersion liquid of the comparative example.
  • the CNT dispersion liquid of the example contains CNT having a length of about 20 ⁇ m and a high aspect ratio. Since the CNT dispersion liquid of the example is long and has a large aspect ratio, when the shear stress is small, the CNT dispersion liquid entangles each other and easily forms the network structure 24, so that the viscosity can be increased. In addition, the CNT dispersion liquid of the example is subjected to shear stress, so that the network structure is easily disassembled and the CNTs are nano-dispersed, so that the viscosity decreases. Thus, since the viscosity of the CNT dispersion liquid of the example changes depending on the shear stress received, a large TI value y can be obtained.
  • the CNT dispersion liquid of the example a correlation as shown in FIG. 9 was obtained between the CNT concentration (volume%) and the TI value y. Since the CNTs are shortened by carrying out the dispersion treatment, the aspect ratio of the CNTs can be reduced when preparing the CNT dispersions of the examples. When the aspect ratio of the CNT is reduced, the viscosity when the shear stress is small can be reduced, so that the TI value y of the CNT dispersion is also reduced. In other words, the above formulas (12) and (13) correspond to the upper limit of the TI value y of the CNT dispersion liquid of the example. Moreover, the CNT dispersion liquid of an Example can obtain smaller TI value y by adjusting the length and aspect ratio of CNT.
  • the CNT dispersion liquid of the example satisfies the relationships of the above formulas (1), (2), (3), and (4).
  • the CNT dispersion of the comparative example had a low TI value y of about 1.1 to 1.39 (y ⁇ 5x + 1) as shown in FIG.
  • the CNTs used in the comparative example are entangled to form aggregates 140 to 143.
  • the CNT dispersion liquid of the comparative example has many aggregates, and originally, there are few CNTs effective for taking a network structure. Even if shear stress is applied, the aggregated CNTs are shortened to become CNTs having a small aspect ratio. Even if such CNTs are dispersed, it is difficult to adopt a network structure. Therefore, it is considered that the CNT dispersion liquid of the comparative example has a small change in viscosity due to the shear stress received and a low TI value y.
  • the TI value y of the CNT dispersion also depends on the affinity between the CNT surface and the solvent in the dispersion medium. For example, when the hydrophilicity of the CNT surface is high, the TI value y is high when water is contained as the solvent, and when the lipophilicity of the CNT surface is high, an organic solvent is contained as the solvent. At this time, the TI value y increases.
  • Examples 1 and 2 using PVP as the resin water is used as the solvent.
  • Examples 3 to 7 using PI as the resin an organic solvent is used.
  • a high TI value y can be obtained regardless of whether water or an organic solvent is used.
  • the TI value y is compatible with the solvent on the CNT surface. It has nothing to do with it.
  • a high TI value y is obtained by including CNT that can easily disassemble the network structure.
  • the CNT dispersion using two types of dispersion media that is, a dispersion medium containing PVP as a resin and a dispersion medium containing PI has been described.
  • the CNT dispersion liquid of the present embodiment is not limited to these. It is not something. If CNTs with a length of 1 to 100 ⁇ m are contained, the correlation between the CNT concentration (% by volume) and the TI value y is similar to that in the case of a CNT dispersion using a dispersion medium containing other resins. Become.
  • ⁇ Surface resistivity of functional film> The CNT dispersion liquid of Example 3 was applied onto the base material with a K hand coater to form a coating film. A glass substrate was used as the base material here. Using a hot plate, the film was dried at 90 ° C. for 30 minutes and then baked at 250 ° C. for 30 minutes to form a functional film having a predetermined film thickness. The surface resistivity of the obtained functional film was measured with a four-probe resistivity meter, and the result was plotted in the graph of FIG.
  • the functional film formed using the dispersion liquid of Example 3 has a surface resistivity of about (1.0E + 3.5) ⁇ / sq with a thickness of about 10 ⁇ m.
  • the functional film formed here is a conductive film in which electrical conductivity derived from CNT is imparted to the coating film (polyimide layer).
  • the CNT dispersion of the comparative example does not disassemble CNT aggregates even when subjected to shear stress. Therefore, when compared at the same CNT concentration, the TI value y is smaller than that of the CNT dispersion of the example.
  • the functional film formed with the CNT dispersion liquid of the comparative example since the CNT cannot form a network structure, a functional film that sufficiently exhibits the characteristics (electric conductivity) of the CNT is formed with a thin film thickness. I can't.
  • FIG. 11 is an SEM photograph of the surface of the functional film formed on the base material by the method described above. According to the SEM photograph of FIG. 11, it can be seen that a large amount of CNT having a length of 2.5 ⁇ m or more is present, and there are few aggregates and aggregates in which the CNTs are gathered in a bundle.
  • the CNT length here is the length of a part of the CNT existing in the vicinity of the film surface, not the entire length, so it is estimated that it is actually longer. It is presumed that the electrical conductivity of the functional film has been improved due to the fact that the CNTs are long and there are few defects on the CNT surface.
  • ⁇ Scratch strength of film> The CNT dispersion liquid of Example 3 was applied onto the base material by spray coating. Stainless steel was used as the base material here. It dried at 200 degreeC for 30 minutes using the dryer, and imidation was performed at 300 degreeC for 30 minutes. A functional film having a thickness of 17 to 18 ⁇ m was formed. For comparison, a thin film (polyimide film) having the same thickness was formed using only the dispersion medium without blending CNTs.
  • the strength was measured with a scratching needle with an arbitrary load applied to the obtained functional film and thin film. The strength when each film peels from the base material is compared.
  • the testing machine used was a Haydon friction measuring machine, the scratching needle was made of sapphire (0.05 mm, R60 °), and the scratching speed was 20 mm / min.
  • Example 3 Although the functional film using the CNT dispersion liquid of Example 3 was scraped at 0.98 N, it was confirmed that the scratch strength was improved without tearing to 2.45 N. On the other hand, the comparative polyimide film was scraped at 0.98N and was torn at 1.47N.

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PCT/JP2015/082064 2014-11-17 2015-11-16 カーボンナノチューブ分散液、機能性膜および複合素材 WO2016080327A1 (ja)

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