JP2013119505A - Low outgassing viscoelastic body - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a viscoelastic body which has excellent handleability because of small tack and generates a small amount of outgas even under high temperature conditions.SOLUTION: The viscoelastic body produces ≤20 mg/cmof outgas when stored at 400°C for 1 h. Probe tack of the viscoelastic body in a probe tack test is ≤200 gf at 25°C.

Description

  The present invention relates to a viscoelastic body. In detail, it is related with a viscoelastic body with little outgas amount.

  A viscoelastic body is useful as a material for an adhesive because it has an excellent balance between elasticity and viscosity, and has been actively researched and developed in various industrial fields. A pressure-sensitive adhesive made of a viscoelastic body wets and adheres to the adherend due to its low modulus and develops adhesive strength.

  Conventionally, acrylic resin, rubber resin, silicone resin, and the like are generally used as the material for the pressure-sensitive adhesive.

  As a material for the pressure-sensitive adhesive, a high molecular weight material of an organic material as described above is conventionally used, but a low molecular weight material remains in the pressure-sensitive adhesive as a solvent or by-product for increasing the molecular weight. . For this reason, when such a pressure-sensitive adhesive material is used under high temperature conditions, reduced pressure or vacuum conditions, or when used in a sealed space, the above-mentioned solvent or low molecular weight substance is generated as outgas, resulting in odor. Problems such as generation, contamination to other materials, and deterioration of adhesive properties occur. Further, under the high temperature conditions, the organic material itself as described above is decomposed, and this decomposition causes a problem that outgas is generated.

  For example, a specific cross-linked acrylic resin has been reported as a material for the pressure-sensitive adhesive with reduced outgas generation (see Patent Document 1). However, since this material is also a high molecular weight organic material as described above, it can only reduce the amount of outgas generated when heated at 120 ° C. for 1 hour, and can also reduce the amount of outgas generated under higher temperature conditions. It is not a thing.

  Moreover, since the conventional viscoelastic body has a strong tack, it adheres easily to a smooth surface and is difficult to handle.

JP 2011-202126 A

  An object of the present invention is to provide a viscoelastic body having a small tack, excellent handleability, and a low outgas generation amount even under high temperature conditions.

The viscoelastic body of the present invention has an outgas amount of 20 mg / cm ³ or less when stored at 400 ° C. for 1 hour.

  In a preferred embodiment, the viscoelastic body of the present invention has a probe tack in a probe tack test of 200 gf or less at 25 ° C.

  In a preferred embodiment, the viscoelastic body of the present invention includes a fibrous columnar structure.

  In a preferred embodiment, the fibrous columnar structure is a carbon nanotube aggregate including a plurality of carbon nanotubes.

  In a preferred embodiment, the carbon nanotube has a length of 50 μm or more.

  In a preferred embodiment, the viscoelastic body of the present invention includes a substrate.

  In a preferred embodiment, the viscoelastic body of the present invention is used for an analytical instrument.

  According to the present invention, it is possible to provide a viscoelastic body having a small tack, excellent handleability, and a low outgas generation amount even under high temperature conditions.

It is a schematic sectional drawing of an example in case the viscoelastic body in preferable embodiment of this invention contains a carbon nanotube aggregate. It is a schematic sectional drawing of this carbon nanotube aggregate manufacturing apparatus in case the viscoelastic body in preferable embodiment of this invention contains a carbon nanotube aggregate.

≪Viscoelastic body≫
The viscoelastic body of the present invention has an outgas amount of 20 mg / cm ³ or less when stored at 400 ° C. for 1 hour. The amount of outgas is preferably 10 mg / cm ³ or less, more preferably 5 mg / cm ³ or less, and even more preferably 1 mg / cm ³ or less.

  Since the amount of outgas when stored at 400 ° C. for 1 hour can be reduced to the above level, even when the viscoelastic body of the present invention is used under high temperature conditions, reduced pressure or vacuum conditions, generation of outgas is sufficient. And can avoid problems such as odor generation, contamination of other materials, and deterioration of adhesive properties.

  The viscoelastic body of the present invention has a probe tack in a probe tack test at 25 ° C. of preferably 200 gf or less, more preferably 10 gf to 200 gf, still more preferably 20 gf to 195 gf, and particularly preferably 30 gf to 190 gf. In this invention, when the said probe tack exists in the said range, the viscoelastic body of this invention has a moderate tack, and a handleability becomes favorable.

  The viscoelastic body of the present invention can preferably selectively collect particles having a specific particle size. Here, in the present invention, the “particle diameter” refers to a portion having the smallest particle diameter.

  The viscoelastic body of the present invention is preferably capable of selectively collecting particles having a particle size of less than 500 μm. Here, “adhesion collection” in the present invention means that the viscoelastic body of the present invention is pressure-bonded to particles that are adherends so that the particles are adhered to the viscoelastic body and collected. . The degree of pressure-bonding can be appropriately set according to the purpose, and for example, pressure-bonding by reciprocating once with a 5 kg roller can be mentioned.

  The viscoelastic body of the present invention is preferably capable of selectively adsorbing and collecting particles having a particle size of 200 μm or less. Here, “adsorption sampling” in the present invention means that the particles are adsorbed to the viscoelastic body and collected without adhering the viscoelastic body of the present invention to the adherend particles. . Specifically, for example, the particles as the adherend are brought into contact with the viscoelastic body at a low collision speed (for example, 1 m / s) to adsorb the particles to the viscoelastic body.

  In the viscoelastic body of the present invention, the contained gas component may be removed in advance under a high temperature environment, a reduced pressure environment or a vacuum environment before use, if necessary. Thus, even if the viscoelastic body of the present invention is previously exposed to a high temperature environment, a reduced pressure environment or a vacuum environment before use, its properties as a viscoelastic body are unlikely to be impaired.

  The viscoelastic body of the present invention preferably includes a fibrous columnar structure.

  Any appropriate material can be adopted as the material of the fibrous columnar structure. Examples thereof include metals such as aluminum and iron; inorganic materials such as silicon; carbon materials such as carbon nanofibers and carbon nanotubes; and high modulus resins such as engineering plastics and super engineering plastics. Specific examples of the resin include polystyrene, polyethylene, polypropylene, polyethylene terephthalate, acetyl cellulose, polycarbonate, polyimide, polyamide, and the like. Any appropriate physical properties can be adopted as the physical properties such as the molecular weight of the resin as long as the object of the present invention can be achieved.

  The length of the fibrous columnar structure is preferably 1 μm to 10000 μm, more preferably 10 μm to 5000 μm, still more preferably 30 μm to 3000 μm, particularly preferably 50 μm to 2000 μm, and most preferably 100 μm. ˜2000 μm. When the length of the fibrous columnar structure is within the above range, it is possible to provide a viscoelastic body that has a small tack, excellent handling properties, and generates a small amount of outgas even under high temperature conditions.

  The diameter of the fibrous columnar structure is preferably 0.3 nm to 2000 nm, more preferably 1 nm to 1000 nm, and still more preferably 2 nm to 500 nm. When the diameter of the fibrous columnar structure falls within the above range, it is possible to provide a viscoelastic body that has a small tack, excellent handling properties, and generates a small amount of outgas even under high temperature conditions.

  In the present invention, the fibrous columnar structure is preferably a carbon nanotube aggregate including a plurality of carbon nanotubes.

  The viscoelastic body of the present invention may be composed only of a carbon nanotube aggregate, or may be composed of a carbon nanotube aggregate and any appropriate member.

  The viscoelastic body of the present invention may contain a substrate. At this time, when the viscoelastic body of the present invention includes a carbon nanotube aggregate including a plurality of carbon nanotubes, one end of the carbon nanotube may be fixed to the base material.

  Any appropriate base material can be adopted as the base material depending on the purpose. Examples thereof include quartz glass, silicon (silicon wafer, etc.), engineering plastic, super engineering plastic, and the like. Specific examples of engineering plastics and super engineering plastics include polyimide, polyethylene, polyethylene terephthalate, acetyl cellulose, polycarbonate, polypropylene, and polyamide. Any appropriate physical properties can be adopted as the physical properties such as molecular weight of these base materials within a range in which the object of the present invention can be achieved.

  The thickness of the base material can be set to any appropriate value depending on the purpose. For example, in the case of a silicon substrate, it is preferably 100 μm to 10000 μm, more preferably 100 μm to 5000 μm, and further preferably 100 μm to 2000 μm. For example, in the case of a polypropylene substrate, it is preferably 1 μm to 1000 μm, more preferably 1 μm to 500 μm, and further preferably 5 μm to 100 μm.

  The surface of the base material is chemically treated by conventional surface treatments such as chromic acid treatment, ozone exposure, flame exposure, high-voltage impact exposure, ionizing radiation treatment, etc. in order to improve adhesion and retention with adjacent layers. Or a physical treatment or a coating treatment with a primer (for example, the above-mentioned adhesive substance) may be applied.

  The substrate may be a single layer or a multilayer body.

  When the viscoelastic body of the present invention includes a carbon nanotube aggregate including a plurality of carbon nanotubes and includes a base material, any appropriate method is adopted as a method of fixing the carbon nanotube to the base material. Can do. For example, the substrate used for manufacturing the carbon nanotube aggregate may be used as it is as a base material. Further, an adhesive layer may be provided on the base material and fixed to the carbon nanotube. Furthermore, when the substrate is a thermosetting resin, a thin film is prepared in a state before the reaction, and one end of the carbon nanotube is bonded to the thin film layer, and then cured and fixed. In addition, when the base material is a thermoplastic resin or a metal, after crimping one end of the fibrous columnar structure in a molten state, the substrate may be cooled and fixed to room temperature.

≪Carbon nanotube aggregate≫
When the viscoelastic body of the present invention includes a fibrous columnar structure, the fibrous columnar structure is preferably a carbon nanotube aggregate. When the viscoelastic body of the present invention includes an aggregate of carbon nanotubes, the viscoelastic body of the present invention has a small tack and a better handling property, and generates a smaller amount of outgas even under high temperature conditions.

  FIG. 1 is a schematic cross-sectional view of an example in which the viscoelastic body according to a preferred embodiment of the present invention is a carbon nanotube aggregate (the scale is not accurately described in order to clarify each component). The carbon nanotube aggregate 10 includes a base material 1 and carbon nanotubes 2. One end 2 a of the carbon nanotube 2 is fixed to the substrate 1. The carbon nanotubes 2 are oriented in the length direction L. The carbon nanotubes 2 are preferably oriented in a direction substantially perpendicular to the substrate 1. Unlike the illustrated example, even if the carbon nanotubes do not have a base material, the carbon nanotubes can exist as an aggregate by van der Waals forces with each other. It may be an aggregate not equipped.

  When the carbon nanotube includes a base material in the carbon nanotube aggregate, any appropriate base material can be adopted as the base material depending on the purpose. As such a base material, what was demonstrated above is mentioned as a base material which the viscoelastic body of this invention can contain, for example.

<First Preferred Embodiment>
One preferred embodiment of the aggregate of carbon nanotubes that can be included in the viscoelastic body of the present invention (hereinafter sometimes referred to as the first preferred embodiment) includes a plurality of carbon nanotubes, and the carbon nanotubes are in multiple layers. The distribution width of the wall number distribution of the carbon nanotubes is 10 or more, the relative frequency of the mode of the wall number distribution is 25% or less, and the length of the carbon nanotubes is greater than 10 μm.

  The distribution width of the number distribution of the carbon nanotubes is 10 or more, preferably 10 to 30 layers, more preferably 10 to 25 layers, and further preferably 10 to 20 layers.

  The “distribution width” of the carbon nanotube layer number distribution refers to a difference between the maximum number of carbon nanotubes and the minimum number of layers. When the distribution width of the number distribution of carbon nanotubes is within the above range, the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and the carbon nanotubes exhibit excellent adhesive properties. It can be a carbon nanotube aggregate. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The number of layers and the number distribution of the carbon nanotubes may be measured with any appropriate apparatus. Preferably, it is measured by a scanning electron microscope (SEM) or a transmission electron microscope (TEM). For example, at least 10, preferably 20 or more carbon nanotubes may be taken out from the aggregate of carbon nanotubes and measured by SEM or TEM to evaluate the number of layers and the number distribution of the layers.

  The maximum number of the carbon nanotubes is preferably 5 to 30 layers, more preferably 10 to 30 layers, still more preferably 15 to 30 layers, and particularly preferably 15 layers to 30 layers. There are 25 layers.

  The minimum number of layers of the carbon nanotube is preferably 1 to 10 layers, more preferably 1 to 5 layers.

  When the maximum number and the minimum number of layers of the carbon nanotubes are within the above range, the carbon nanotubes can have more excellent mechanical properties and a high specific surface area. It can be an aggregate of carbon nanotubes that exhibits more excellent adhesive properties. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The relative frequency of the mode value of the layer number distribution is 25% or less, preferably 1% to 25%, more preferably 5% to 25%, and further preferably 10% to 25%. Particularly preferably, it is 15% to 25%. When the relative frequency of the mode value of the wall number distribution is within the above range, the carbon nanotube can have excellent mechanical properties and a high specific surface area, and further, the carbon nanotube has excellent adhesive properties. It can become the carbon nanotube aggregate which shows. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The mode value of the layer number distribution is preferably from 2 layers to 10 layers, and more preferably from 3 layers to 10 layers. When the mode value of the wall number distribution is within the above range, the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and the carbon nanotubes can exhibit excellent adhesion properties. It can be a nanotube aggregate. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  As the shape of the carbon nanotube, it is sufficient that its cross section has any appropriate shape. For example, the cross section may be substantially circular, elliptical, n-gonal (n is an integer of 3 or more), and the like.

  The specific surface area and density of the carbon nanotube can be set to any appropriate value.

<Second Preferred Embodiment>
Another preferred embodiment of the aggregate of carbon nanotubes that can be included in the viscoelastic body of the present invention (hereinafter sometimes referred to as a second preferred embodiment) includes a plurality of carbon nanotubes, The mode of the number distribution of the carbon nanotubes is present in the number of layers of 10 or less, the relative frequency of the mode is 30% or more, and the length of the carbon nanotube is 10 μm. It is less than 500 μm.

  The distribution width of the number distribution of the carbon nanotubes is preferably 9 or less, more preferably 1 to 9 layers, further preferably 2 to 8 layers, and particularly preferably 3 to 8 layers. It is.

  The “distribution width” of the carbon nanotube layer number distribution refers to a difference between the maximum number of carbon nanotubes and the minimum number of layers. When the distribution width of the number distribution of carbon nanotubes is within the above range, the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and the carbon nanotubes exhibit excellent adhesive properties. It can be a carbon nanotube aggregate. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The number of layers and the number distribution of the carbon nanotubes may be measured with any appropriate apparatus. Preferably, it is measured by a scanning electron microscope (SEM) or a transmission electron microscope (TEM). For example, at least 10, preferably 20 or more carbon nanotubes may be taken out from the aggregate of carbon nanotubes and measured by SEM or TEM to evaluate the number of layers and the number distribution of the layers.

  The maximum number of the carbon nanotubes is preferably 1 to 20 layers, more preferably 2 to 15 layers, and further preferably 3 to 10 layers.

  The minimum number of layers of the carbon nanotube is preferably 1 to 10 layers, more preferably 1 to 5 layers.

  When the maximum number and the minimum number of layers of the carbon nanotubes are within the above range, the carbon nanotubes can have more excellent mechanical properties and a high specific surface area. It can be an aggregate of carbon nanotubes that exhibits more excellent adhesive properties. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The relative frequency of the mode value of the layer number distribution is 30% or more, preferably 30% to 100%, more preferably 30% to 90%, and further preferably 30% to 80%. Particularly preferably, it is 30% to 70%. When the relative frequency of the mode value of the wall number distribution is within the above range, the carbon nanotube can have excellent mechanical properties and a high specific surface area, and further, the carbon nanotube has excellent adhesive properties. It can become the carbon nanotube aggregate which shows. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  The mode value of the layer number distribution is present in 10 layers or less, preferably in 1 layer to 10 layers, more preferably in 2 layers to 8 layers, More preferably, it exists in 2 to 6 layers. In the present invention, when the mode value of the wall number distribution is within the above range, the carbon nanotubes can have excellent mechanical properties and a high specific surface area. It can be a carbon nanotube aggregate exhibiting characteristics. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate.

  As the shape of the carbon nanotube, it is sufficient that its cross section has any appropriate shape. For example, the cross section may be substantially circular, elliptical, n-gonal (n is an integer of 3 or more), and the like.

  The specific surface area and density of the carbon nanotube can be set to any appropriate value.

≪Method for producing aggregate of carbon nanotubes≫
Any appropriate method can be adopted as a method for producing a carbon nanotube aggregate that can be included in the viscoelastic body of the present invention.

  As a method for producing an aggregate of carbon nanotubes that can be included in the viscoelastic body of the present invention, for example, a catalyst layer is formed on a smooth substrate, and a carbon source is filled in a state where the catalyst is activated by heat, plasma, or the like. In addition, there is a method of manufacturing a carbon nanotube aggregate that is oriented substantially vertically from a substrate by chemical vapor deposition (CVD) method, in which carbon nanotubes are grown. In this case, if the substrate is removed, a carbon nanotube aggregate oriented in the length direction can be obtained.

  Any appropriate substrate can be adopted as the substrate. For example, the material which has smoothness and the high temperature heat resistance which can endure manufacture of a carbon nanotube is mentioned. Examples of such materials include quartz glass, silicon (such as a silicon wafer), and a metal plate such as aluminum. The said board | substrate can be used as a base material which the carbon nanotube aggregate | assembly which can contain the viscoelastic body of this invention is provided as it is.

  Any appropriate apparatus can be adopted as an apparatus for producing a carbon nanotube aggregate that can be included in the viscoelastic body of the present invention. For example, as a thermal CVD apparatus, as shown in FIG. 2, a hot wall type configured by surrounding a cylindrical reaction vessel with a resistance heating type electric tubular furnace can be cited. In that case, for example, a heat-resistant quartz tube is preferably used as the reaction vessel.

  Any appropriate catalyst can be used as a catalyst (catalyst layer material) that can be used for producing a carbon nanotube aggregate that can be included in the viscoelastic body of the present invention. For example, metal catalysts, such as iron, cobalt, nickel, gold, platinum, silver, copper, are mentioned.

  When producing an aggregate of carbon nanotubes that can be included in the viscoelastic body of the present invention, an alumina / hydrophilic film may be provided between the substrate and the catalyst layer as necessary.

Any appropriate method can be adopted as a method for producing the alumina / hydrophilic film. For example, it can be obtained by forming a SiO ₂ film on a substrate, depositing Al, and then oxidizing it by raising the temperature to 450 ° C. According to such a manufacturing method, _Al 2 _{O 3} interacts with the SiO ₂ film hydrophilic, different _Al 2 _{O 3} surface particle diameters than those deposited _Al 2 _{O 3} directly formed. Even if Al is deposited and heated to 450 ° C. and oxidized without forming a hydrophilic film on the substrate, Al ₂ O ₃ surfaces having different particle diameters may not be formed easily. Moreover, even if a hydrophilic film is prepared on a substrate and Al ₂ O ₃ is directly deposited, it is difficult to form Al ₂ O ₃ surfaces having different particle diameters.

  The thickness of the catalyst layer that can be used in the production of the carbon nanotube aggregate that can be included in the viscoelastic body of the present invention is preferably 0.01 nm to 20 nm, more preferably 0.1 nm to 10 nm in order to form fine particles. . When the thickness of the catalyst layer that can be used in the production of the carbon nanotube aggregate that can be included in the viscoelastic body of the present invention is within the above range, the carbon nanotube aggregate may have excellent mechanical properties and a high specific surface area. In addition, the aggregate of carbon nanotubes can exhibit excellent adhesive properties. Therefore, a viscoelastic body that can exhibit excellent viscoelasticity can be provided by using such a carbon nanotube aggregate. Arbitrary appropriate methods can be employ | adopted for the formation method of a catalyst layer. For example, a method of depositing a metal catalyst by EB (electron beam), sputtering, or the like, a method of applying a suspension of metal catalyst fine particles on a substrate, and the like can be mentioned.

  Any appropriate carbon source can be used as the carbon source that can be used for producing the aggregate of carbon nanotubes that can be included in the viscoelastic body of the present invention. For example, hydrocarbons such as methane, ethylene, acetylene, and benzene; alcohols such as methanol and ethanol;

  Any appropriate temperature can be adopted as the production temperature in the production of the carbon nanotube aggregate that can be included in the viscoelastic body of the present invention. For example, in order to form catalyst particles that can sufficiently exhibit the effects of the present invention, the temperature is preferably 400 ° C to 1000 ° C, more preferably 500 ° C to 900 ° C, and further preferably 600 ° C to 800 ° C. .

≪Use of viscoelastic body≫
The viscoelastic body of the present invention can be used for various applications. In particular, the viscoelastic body of the present invention has a small tack and excellent handleability, and generates a small amount of outgas under high temperature conditions, reduced pressure conditions or vacuum conditions. For this reason, the viscoelastic body of the present invention can be preferably used in the analytical field, the superconducting field, and the like.

  Hereinafter, although the present invention is explained based on an example, the present invention is not limited to these. Various evaluations and measurements were performed by the following methods.

<Evaluation of the number and distribution of carbon nanotubes in a carbon nanotube aggregate>
The number and the distribution of the number of carbon nanotubes in the aggregate of carbon nanotubes of the present invention were measured by a scanning electron microscope (SEM) and / or a transmission electron microscope (TEM). From the obtained carbon nanotube aggregate, at least 10 or more, preferably 20 or more carbon nanotubes were observed by SEM and / or TEM, the number of layers of each carbon nanotube was examined, and a layer number distribution was created.

<Probe tack test>
A probe tack test was performed under the following conditions, and the maximum value of the adhesive strength was measured.
Equipment: Tacking tester (made by RESCA)
Probe: SUS5mmφ
Preload: 500gf
Press Speed: 1mm / min
Press Time: 5s
Test Speed: 2.5mm / min

<Outgas amount measurement>
The viscoelastic body was put into a sample cup, and heated and extracted at 400 ° C. for 1 hour in a pseudo air atmosphere using a heating furnace type pyrolyzer (DSP). The gas generated at that time was concentrated and collected on a part of the GC column with liquid nitrogen using a microjet cryotrap, and then GC / MS measurement was performed to calculate the amount of outgas per cm ³ .
(Analyzer: GC / MS)
DSP: PY-2020iD made by Frontier Lab
GC: Agilent Technologies, manufactured by Agilent Technologies, 6890
MSD: Agilent Technologies, made by Agilent Technologies, Agilent 5973N
(Measurement condition)
・ DSP (Double Shot Pyrolyzer)
Sample cup: Eco Cup LF
Heating temperature: 400 ° C x 1 hour / GC (gas chromatograph)
Column: Frontier Lab, Ultra ALLOY + 5 (0.25 μm, 0.25 mmφ × 30 m)
Column temperature: 40 ° C. (hold for 3 minutes) → temperature rise at 15 ° C./minute → 300 ° C. (hold for 10 minutes)
Carrier-gas: He (1 ml / min) (constant flow mode)
Inlet: Split mode (split ratio = 10: 1, total flow rate = 13 ml / min, temperature 300 ° C.)
・ MS (mass spectrometer)
Ionization method: EI
Ionization voltage: 70 eV
Interface temperature: 300 ° C
Ion source temperature: 230 ° C
Detector temperature: 150 ° C
Measurement mass range: m / z = 10-800
TIC mass range: 29-800

[Example 1]
An Al thin film (thickness 10 nm) was formed on a silicon wafer (manufactured by Silicon Technology) as a substrate by a sputtering apparatus (manufactured by ULVAC, RFS-200). On this Al thin film, a Fe thin film (thickness 0.35 nm) was further deposited by a sputtering apparatus (ULVAC, RFS-200).
Thereafter, this substrate was placed in a 30 mmφ quartz tube, and a mixed gas of helium / hydrogen (90/50 sccm) maintained at 600 ppm in water was allowed to flow through the quartz tube for 30 minutes to replace the inside of the tube. Thereafter, the inside of the tube was heated to 765 ° C. using an electric tubular furnace and stabilized at 765 ° C. While maintaining the temperature at 765 ° C., a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) was filled in the tube, and left for 1 minute to grow carbon nanotubes on the substrate. As a result, an aggregate of carbon nanotubes (1) in which is oriented in the length direction was obtained.
The length of the carbon nanotube provided in the carbon nanotube aggregate (1) was 30 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (1), the mode value was present in one layer, and the relative frequency was 61%.
Various evaluations were performed using the obtained carbon nanotube aggregate (1) as a viscoelastic body (1), and the results are summarized in Table 1.

[Example 2]
Except that the thickness of the Fe thin film was 1 nm, the same procedure as in Example 1 was performed to obtain a carbon nanotube aggregate (2) in which the carbon nanotubes were aligned in the length direction.
The carbon nanotubes included in the carbon nanotube aggregate (2) had a length of 30 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (2), the mode value was present in two layers, and the relative frequency was 75%.
Various evaluations were performed using the obtained carbon nanotube aggregate (2) as a viscoelastic body (2), and the results are summarized in Table 1.

[Example 3]
The carbon nanotubes are aligned in the length direction in the same manner as in Example 2 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) is 3 minutes. As a result, an aggregate (3) of carbon nanotubes oriented in the direction was obtained.
The length of the carbon nanotubes included in the carbon nanotube aggregate (3) was 50 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (3), the mode value was present in two layers, and the relative frequency was 75%.
Various evaluations were performed using the obtained carbon nanotube aggregate (3) as a viscoelastic body (3), and the results are summarized in Table 1.

[Example 4]
Similar to Example 1, except that the thickness of the Fe thin film was set to 2 nm and the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) was 5 minutes. The carbon nanotube aggregate (4) in which the carbon nanotubes were aligned in the length direction was obtained.
The carbon nanotubes included in the carbon nanotube aggregate (4) had a length of 70 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (4), the mode value was present in 7-8 layers, and the relative frequency was 66%.
Various evaluations were performed using the obtained carbon nanotube aggregate (4) as a viscoelastic body (4), and the results are summarized in Table 1.

[Example 5]
Example 1 except that acetylene was used instead of ethylene and the standing time after filling the tube with a mixed gas of helium / hydrogen / acetylene (85/50/5 sccm, moisture content 600 ppm) was 7 minutes. The carbon nanotube aggregate (5) in which the carbon nanotubes were aligned in the length direction was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (5) is provided was 100 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (5), the mode value was present in 7-8 layers, and the relative frequency was 66%.
Various evaluations were performed using the obtained carbon nanotube aggregate (5) as a viscoelastic body (5), and the results are summarized in Table 1.

[Example 6]
The carbon nanotubes are aligned in the length direction in the same manner as in Example 2 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) is 10 minutes. As a result, an aggregate (6) of carbon nanotubes oriented in the direction was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (6) is provided was 200 μm.
In the number distribution of the carbon nanotubes provided in the carbon nanotube aggregate (6), the mode value was present in two layers, and the relative frequency was 75%.
Various evaluations were performed using the obtained carbon nanotube aggregate (6) as a viscoelastic body (6), and the results are summarized in Table 1.

[Example 7]
The carbon nanotubes were measured in the length direction in the same manner as in Example 1 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) was 20 minutes. Thus, an aggregate (7) of carbon nanotubes oriented in the direction of was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (7) is provided was 400 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (7), the mode value was present in one layer, and the relative frequency was 61%.
Various evaluations were performed using the obtained carbon nanotube aggregate (7) as a viscoelastic body (7), and the results are summarized in Table 1.

[Example 8]
The carbon nanotubes are aligned in the length direction in the same manner as in Example 2 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) is 20 minutes. Thus, an aggregate (8) of carbon nanotubes oriented in the direction of was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (8) is provided was 500 μm.
In the number distribution of the carbon nanotubes provided in the carbon nanotube aggregate (8), the mode value was present in two layers, and the relative frequency was 75%.
Various evaluations were performed using the obtained carbon nanotube aggregate (8) as a viscoelastic body (8), and the results are summarized in Table 1.

[Example 9]
The carbon nanotubes are aligned in the length direction in the same manner as in Example 4 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) is 40 minutes. As a result, an aggregate (9) of carbon nanotubes oriented in the direction was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (9) is provided was 800 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (9), the mode value was present in three layers, and the relative frequency was 72%.
Various evaluations were performed using the obtained carbon nanotube aggregate (9) as a viscoelastic body (9), and the results are summarized in Table 1.

[Example 10]
The carbon nanotubes are aligned in the length direction in the same manner as in Example 2 except that the standing time after filling the tube with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) is 60 minutes. Thus, an aggregate (10) of carbon nanotubes oriented in the direction of was obtained.
The length of the carbon nanotube with which the carbon nanotube aggregate (10) is provided was 1200 μm.
In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (10), the mode value was present in two layers, and the relative frequency was 75%.
Various evaluations were conducted using the obtained carbon nanotube aggregate (10) as a viscoelastic body (10), and the results are summarized in Table 1.

[Comparative Example 1]
Various evaluations were performed using a double-sided adhesive tape (Nitto Denko Corporation, No. 5000N) as a viscoelastic body (C1), and the results are summarized in Table 1.

[Comparative Example 2]
Various evaluations were performed using a 3M polyimide double-sided tape (manufactured by Sumitomo 3M, 4390) as a viscoelastic body (C2), and the results are summarized in Table 1.

[Comparative Example 3]
Various evaluations were made using a 3M polyimide double-sided tape (manufactured by Sumitomo 3M, 4390) previously aged at 200 ° C. for 10 hours as a viscoelastic body (C3), and the results are summarized in Table 1.

  In particular, the viscoelastic body of the present invention has a small tack and excellent handleability, and generates a small amount of outgas under high temperature conditions, reduced pressure conditions or vacuum conditions. For this reason, the viscoelastic body of the present invention can be preferably used in the analytical field, the superconducting field, and the like.

10 Carbon nanotube aggregate 1 Base material 2 Carbon nanotube 2a One end of carbon nanotube

Claims (7)

A viscoelastic body having an outgas amount of 20 mg / cm ³ or less when stored at 400 ° C. for 1 hour.   The viscoelastic body according to claim 1, wherein the probe tack in the probe tack test is 200 gf or less at 25 ° C.   The viscoelastic body according to claim 1, comprising a fibrous columnar structure.   The viscoelastic body according to claim 3, wherein the fibrous columnar structure is a carbon nanotube aggregate including a plurality of carbon nanotubes.   The viscoelastic body according to claim 4, wherein the carbon nanotube has a length of 50 μm or more.   The viscoelastic body according to any one of claims 1 to 5, comprising a base material. The viscoelastic body according to any one of claims 1 to 6, which is used for an analytical instrument.

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