WO2014034489A1 - 分析用除電部材 - Google Patents
分析用除電部材 Download PDFInfo
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- WO2014034489A1 WO2014034489A1 PCT/JP2013/072287 JP2013072287W WO2014034489A1 WO 2014034489 A1 WO2014034489 A1 WO 2014034489A1 JP 2013072287 W JP2013072287 W JP 2013072287W WO 2014034489 A1 WO2014034489 A1 WO 2014034489A1
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- analysis
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- carbon nanotubes
- present
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/08—Means for establishing or regulating a desired environmental condition within a sample chamber
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/18—Means for protecting or isolating the interior of a sample chamber from external environmental conditions or influences, e.g. vibrations or electromagnetic fields
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- 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 static elimination member for analysis. More specifically, the present invention relates to a static eliminator for analysis that can effectively eliminate static charges around a sample to be analyzed in an analysis application using an atomic force microscope (AFM).
- AFM atomic force microscope
- An atomic force microscope is a microscope having atomic resolution, and can easily observe the fine shape of a sample surface (for example, refer to Patent Document 1).
- the atomic force microscope can observe not only conductive materials but also insulating materials such as polymer compounds. From these points, the atomic force microscope is very effective as a surface observation means for various samples.
- a probe with a sharp tip is scanned over the surface of the sample, and the surface force is observed by changing the atomic force felt by the probe into an electrical signal.
- the probe is attached to the tip of the cantilever, and the probe and the surface of the sample are brought into contact with each other with a minute force.
- control of the analysis environment is suppression of charging around the sample to be analyzed. If the periphery of the sample to be analyzed is charged, for example, an accurate analysis result cannot be obtained in an analysis using an electrical signal.
- a means for suppressing charging around the sample to be analyzed a method of sticking a conductive tape or conductive paste around the sample to be analyzed, a method of removing static electricity around the sample to be analyzed by an electrostatic blower, or charging is unlikely to occur.
- a method of performing measurement in a high humidity environment is employed (see, for example, Patent Documents 2 and 3).
- water components may adhere to the sample to be analyzed, and accurate analysis results may not be obtained. Further, in a high temperature environment or a vacuum environment, even if an attempt is made to realize a high humidity environment, the water component evaporates, causing a problem that the high humidity environment cannot be maintained.
- the sample be sufficiently attached around the sample to be analyzed. This is because if the charge removal member is not sufficiently attached around the sample to be analyzed, the charge removal member may be displaced due to the shape or inclination of the attachment location.
- the subject of the present invention is that, in precision analysis such as analysis using an atomic force microscope, the sample can be sufficiently attached around the sample to be analyzed, and the sample around the sample to be analyzed is charged without being contaminated. For analysis, there is no risk of sparking even if metal is present in the vicinity of the sample to be analyzed, and it can be covered with a chamber for analysis, and analysis can be performed in a high temperature or vacuum environment without problems.
- the object is to provide a static elimination member.
- the static eliminating member for analysis of the present invention includes a fibrous columnar structure including a plurality of fibrous columnar objects.
- the static eliminator for analysis of the present invention has a shear adhesive force on the glass surface at room temperature of 1 N / cm 2 or more.
- the fibrous columnar structure is a carbon nanotube aggregate including a plurality of carbon nanotubes.
- the static eliminating member for analysis of the present invention is in the form of a sheet.
- the analysis static eliminator of the present invention is in the form of a probe.
- the sample in precise analysis such as analysis using an atomic force microscope, the sample can be sufficiently attached around the sample to be analyzed, and the sample around the sample to be analyzed can be charged without being contaminated.
- the sample can be sufficiently attached around the sample to be analyzed, and the sample around the sample to be analyzed can be charged without being contaminated.
- a static elimination member can be provided.
- the static elimination member for analysis of the present invention includes a fibrous columnar structure including a plurality of fibrous columnar objects.
- the analysis static elimination member of the present invention may be a member composed of a fibrous columnar structure including a plurality of fibrous columnar materials, or a fibrous shape including a plurality of fibrous columnar materials as long as the effects of the present invention are not impaired. It may be a composite of a columnar structure and any other suitable material. Since the static elimination member for analysis of the present invention includes a fibrous columnar structure including a plurality of fibrous columnar objects, it can be sufficiently attached around the sample to be analyzed in a precision analysis such as an analysis using an atomic force microscope.
- Charging around the sample to be analyzed can be suppressed without causing contamination of the sample or the surrounding environment.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal is present around the sample to be analyzed, and the analysis can be performed by covering the sample with a chamber. Analysis can be done without problems.
- the fibrous columnar structure including a plurality of fibrous columnar objects is an aggregate including a plurality of fibrous columnar objects.
- Such a fibrous columnar structure is preferably an assembly including a plurality of fibrous columnar objects having a length L.
- FIG. 1 shows a schematic cross-sectional view of an example of a preferred embodiment of a fibrous columnar structure included in the static elimination member for analysis of the present invention.
- the fibrous columnar structure 100 includes a plurality of fibrous columnar objects 2 having a length L.
- the plurality of fibrous columnar objects 2 can exist as an aggregate with each other, for example, by van der Waals force.
- the size and shape of the analysis static eliminator of the present invention can be appropriately selected according to the type of analytical instrument.
- Examples of the shape that can be taken by the static eliminating member for analysis of the present invention include a sheet shape and a probe shape. Any appropriate size can be adopted as the size that can be taken by the static eliminator for analysis according to the present invention, depending on the location of use.
- FIG. 2 shows a schematic cross-sectional view of an example of the static eliminating member for analysis in a preferred embodiment of the present invention when the static eliminating member for analysis of the present invention is in a sheet form.
- the static elimination member 1000 for analysis of this invention contains the fibrous columnar structure 100 provided with two or more fibrous columnar objects 2 of length L.
- the thickness direction of the sheet-shaped analysis static elimination member corresponds to the length L direction of the fibrous columnar object 2.
- a preferable usage form sticks the sheet
- FIG. 3 shows a schematic cross-sectional view of an example of the static eliminating member for analysis in a preferred embodiment of the present invention when the static eliminating member for analysis of the present invention is in a probe shape.
- the static elimination member 1000 for analysis of the present invention includes a fibrous columnar structure 100 including a plurality of fibrous columnar objects 2 having a length L.
- the length direction (horizontal direction in FIG. 3) of the probe-shaped analysis static elimination member corresponds to the length L direction of the fibrous columnar object 2.
- a preferred usage is to stick the lengthwise side of the static eliminating member for analysis of the present invention around the sample to be analyzed.
- the analysis static elimination member of the present invention may include any appropriate base material.
- FIG. 4 shows a schematic cross-sectional view of an example of the static eliminating member for analysis in a preferred embodiment of the present invention provided with such a base material.
- the static elimination member for analysis of this invention is a sheet form.
- the static elimination member 1000 for analysis of the present invention includes a fibrous columnar structure 100 including a plurality of fibrous columnar objects 2 having a length L and a substrate 1. One end 2 a of the fibrous columnar object 2 is fixed to the substrate 1.
- the fibrous columnar body 2 is oriented in the direction of the length L.
- the fibrous columnar body 2 is preferably oriented in a substantially vertical direction with respect to the substrate 1.
- the “substantially perpendicular direction” means that the angle with respect to the surface of the substrate 1 is preferably 90 ° ⁇ 20 °, more preferably 90 ° ⁇ 15 °, and further preferably 90 ° ⁇ 10 °. And particularly preferably 90 ° ⁇ 5 °.
- the length L of the fibrous columnar material is preferably 10 ⁇ m or more, more preferably 10 ⁇ m to 2000 ⁇ m, still more preferably 15 ⁇ m to 1500 ⁇ m, particularly preferably 20 ⁇ m to 1000 ⁇ m, and most preferably 25 ⁇ m to 500 ⁇ m. It is.
- the static eliminating member for analysis of the present invention can be sufficiently adhered to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope. The charging around the sample to be analyzed can be further suppressed.
- the static eliminator for analysis of the present invention has a shear adhesive force to the glass surface at room temperature of preferably 1 N / cm 2 or more, more preferably 1 N / cm 2 to 200 N / cm 2 , and even more preferably 5 N / cm 2 to 200 N / cm 2 , particularly preferably 10 N / cm 2 to 200 N / cm 2 .
- the static eliminating member for analysis of the present invention can be sufficiently adhered to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope. .
- the static eliminating member for analysis of the present invention may be displaced due to the shape or inclination of the sticking place. If the shear adhesive force on the glass surface at room temperature is too large, peeling after use may be difficult.
- the shear adhesive strength of the analysis static eliminator of the present invention is such that the contact surface between the analysis static eliminator and the adhesion site becomes the largest when the analysis static eliminator is placed on the adhesion site.
- the shear adhesive strength of the analytical static eliminator of the present invention refers to the shear adhesive force on the sheet surface side of the static eliminator for analysis of the present invention.
- the shear adhesive force of the analytical static eliminator of the present invention refers to the shear adhesive force on the length direction side of the analytical static eliminator of the present invention.
- any appropriate material can be adopted as the material for the fibrous columnar material.
- 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.
- any appropriate base material can be adopted depending on the purpose.
- examples thereof include quartz glass, silicon (silicon wafer, etc.), engineering plastic, super engineering plastic, and the like.
- 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 that can be included in the static eliminating member for analysis of the present invention can be set to any appropriate value depending on the purpose.
- the surface of the substrate that can be included in the static eliminator for analysis of the present invention is a conventional surface treatment such as chromic acid treatment, ozone exposure, flame exposure, high pressure, in order to improve adhesion to adjacent layers, retention, etc.
- Chemical or physical treatment such as electric shock exposure or ionizing radiation treatment, or coating treatment with a primer (for example, the above-mentioned adhesive substance) may be applied.
- the base material that can be included in the static elimination member for analysis of the present invention may be a single layer or a multilayer.
- the diameter of the fibrous columnar material is preferably 0.3 nm to 2000 nm, more preferably 1 nm to 1000 nm, and further preferably 2 nm to 500 nm.
- the fibrous columnar structure included in the static eliminating member for analysis of the present invention is preferably a carbon nanotube aggregate including a plurality of carbon nanotubes.
- the fibrous columnar product is preferably a carbon nanotube.
- the static eliminating member for analysis of the present invention may consist of only a carbon nanotube aggregate including a plurality of carbon nanotubes, or may include a carbon nanotube aggregate including a plurality of carbon nanotubes and any appropriate member. .
- the static eliminating member for analysis of the present invention includes a carbon nanotube aggregate including a plurality of carbon nanotubes and further includes a base material
- one end of the carbon nanotube may be fixed to the base material.
- the static eliminating member for analysis of the present invention includes a carbon nanotube aggregate including a plurality of carbon nanotubes and further includes a base material
- any appropriate method is adopted as a method for fixing the carbon nanotubes to the base material.
- the substrate used for manufacturing the carbon nanotube aggregate may be used as it is as a base material.
- an adhesive layer may be provided on the base material and fixed to the carbon nanotube.
- 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.
- the base material is a thermoplastic resin or a metal
- the substrate after crimping one end of the fibrous columnar structure in a molten state, the substrate may be cooled and fixed to room temperature.
- the fibrous columnar structure is preferably a carbon nanotube aggregate.
- the static eliminator for analysis of the present invention includes an aggregate of carbon nanotubes
- the static eliminator for analytical of the present invention is an adhesive or adhesive containing a contaminant such as an organic component in precision analysis such as analysis using an atomic force microscope. Adhesion can be sufficiently performed around the sample to be analyzed without using an agent. In other words, in addition to the effect that the analysis target sample and the surrounding environment are not contaminated, the analysis static neutralization member of the present invention can be sufficiently attached around the analysis target sample without being influenced by the shape or inclination of the application location. Can be expressed.
- the static elimination member for analysis of the present invention contains a carbon nanotube aggregate
- the static neutralization member for analysis of the present invention can be used in precise analysis such as analysis using an atomic force microscope without using a conductive tape or conductive paste. Further, charging around the sample to be analyzed can be further suppressed without using an electrostatic blower.
- the static eliminator for analysis of the present invention is free from contaminants such as organic components adhering to the sample to be analyzed, there is no problem of contamination of the surrounding environment due to volatilization of the organic solvent, dust, There is no risk of dust rising and adhering to the sample to be analyzed, and there is no risk of sparking even if metal is present around the sample to be analyzed, and the effect of further suppressing the charging around the sample to be analyzed can be exhibited. .
- the analysis static eliminator of the present invention includes an aggregate of carbon nanotubes
- the analytical static eliminator of the present invention when used, it is physically covered with a chamber in a precise analysis such as an analysis using an atomic force microscope. The effect that it is possible easily can be expressed.
- the static eliminator for analysis of the present invention includes an aggregate of carbon nanotubes, if the static eliminator for analysis according to the present invention is used, in a precision analysis such as analysis using an atomic force microscope, analysis under a high temperature environment or a vacuum environment Can be produced without any problem.
- One preferred embodiment of the aggregate of carbon nanotubes that may be included in the static eliminating member for analysis of the present invention includes a plurality of carbon nanotubes, and the plurality of carbon nanotubes is provided.
- the carbon nanotube has a wall number distribution width of 10 or more, and the relative frequency of the mode value of the wall number distribution is 25% or less.
- the distribution width of the number distribution of 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 number distribution of carbon nanotubes refers to the difference between the maximum number and the minimum number of carbon nanotube layers.
- the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and further, the carbon nanotubes have excellent adhesive properties. It can be the carbon nanotube aggregate shown. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the number of layers and the number distribution of the carbon nanotubes may be measured by 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.
- SEM scanning electron microscope
- TEM transmission electron microscope
- 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 the carbon nanotube layers is preferably 1 to 10 layers, more preferably 1 to 5 layers.
- the carbon nanotube can have more excellent mechanical properties and a high specific surface area. Furthermore, the carbon nanotube Can be an aggregate of carbon nanotubes exhibiting more excellent adhesive properties. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- 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%.
- the carbon nanotubes can have excellent mechanical properties and a high specific surface area. It can be a carbon nanotube aggregate exhibiting characteristics. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the mode value of the layer number distribution is preferably from 2 to 10 layers, and more preferably from 3 to 10 layers.
- 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, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the cross section thereof has any appropriate shape.
- the cross section may be substantially circular, elliptical, n-gonal (n is an integer of 3 or more), and the like.
- the length of the carbon nanotube is preferably 1 ⁇ m or more, more preferably 5 ⁇ m to 5000 ⁇ m, still more preferably 10 ⁇ m to 2000 ⁇ m, still more preferably 15 ⁇ m to 1500 ⁇ m, and particularly preferably 20 ⁇ m to 1000 ⁇ m. Most preferably, it is 25 ⁇ m to 800 ⁇ m.
- the carbon nanotube can have excellent mechanical properties and a high specific surface area, and the carbon nanotube exhibits excellent adhesive properties. Can be an aggregate.
- the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed. Further, if the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the diameter of the carbon nanotube is preferably 0.3 nm to 2000 nm, more preferably 1 nm to 1000 nm, and further preferably 2 nm to 500 nm.
- 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 body. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the specific surface area and density of the carbon nanotube can be set to any appropriate value.
- ⁇ Second Preferred Embodiment> Another preferred embodiment (hereinafter sometimes referred to as a second preferred embodiment) of the carbon nanotube aggregate that can be included in the static eliminating member for analysis of the present invention includes a plurality of carbon nanotubes, and the carbon nanotubes Have a plurality of layers, the mode value of the number distribution of the carbon nanotubes is present in the number of layers of 10 or less, and the relative frequency of the mode value is 30% or more.
- the distribution width of the number distribution of the carbon nanotubes is preferably 9 or less, more preferably 1 to 9 layers, still more preferably 2 to 8 layers, and particularly preferably 3 to 8 layers. It is.
- the “distribution width” of the number distribution of carbon nanotubes refers to the difference between the maximum number and the minimum number of carbon nanotube layers.
- the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and further, the carbon nanotubes have excellent adhesive properties. It can be the carbon nanotube aggregate shown. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the number of layers and the number distribution of the carbon nanotubes may be measured by 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.
- SEM scanning electron microscope
- TEM transmission electron microscope
- 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 the carbon nanotube layers is preferably 1 to 10 layers, more preferably 1 to 5 layers.
- the carbon nanotube can have more excellent mechanical properties and a high specific surface area. Furthermore, the carbon nanotube Can be an aggregate of carbon nanotubes exhibiting more excellent adhesive properties. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- 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%.
- the carbon nanotubes can have excellent mechanical properties and a high specific surface area. It can be a carbon nanotube aggregate exhibiting characteristics. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- 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.
- the carbon nanotube can have both excellent mechanical properties and a high specific surface area by adjusting the mode value of the wall number distribution within the above range.
- the carbon nanotube is excellent. It can be a carbon nanotube aggregate exhibiting adhesive properties. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the cross section thereof has any appropriate shape.
- the cross section may be substantially circular, elliptical, n-gonal (n is an integer of 3 or more), and the like.
- the length of the carbon nanotube is preferably 1 ⁇ m or more, more preferably 5 ⁇ m to 5000 ⁇ m, still more preferably 10 ⁇ m to 2000 ⁇ m, still more preferably 15 ⁇ m to 1500 ⁇ m, and particularly preferably 20 ⁇ m to 1000 ⁇ m. Most preferably, it is 25 ⁇ m to 800 ⁇ m.
- the carbon nanotube can have excellent mechanical properties and a high specific surface area, and the carbon nanotube exhibits excellent adhesive properties. Can be an aggregate.
- the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed. Further, if the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the diameter of the carbon nanotube is preferably 0.3 nm to 2000 nm, more preferably 1 nm to 1000 nm, and further preferably 2 nm to 500 nm.
- 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 body. Therefore, the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed.
- the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- the specific surface area and density of the carbon nanotube can be set to any appropriate value.
- a catalyst layer is formed on a smooth substrate, and the carbon source is activated in a state where the catalyst is activated by heat, plasma, or the like.
- the method include a method of manufacturing a carbon nanotube aggregate oriented substantially vertically from a substrate by chemical vapor deposition (CVD method) in which filling is performed and carbon nanotubes are grown. In this case, for example, if the substrate is removed, an aggregate of carbon nanotubes oriented in the length direction can be obtained.
- CVD method chemical vapor deposition
- any appropriate substrate can be adopted as the substrate.
- 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.
- substrate can be used as it is as a base material with which the carbon nanotube aggregate
- any suitable device can be adopted as a device for producing a carbon nanotube aggregate that can be included in the static elimination member for analysis of the present invention.
- a thermal CVD apparatus as shown in FIG. 5, there is a hot wall type configured by surrounding a cylindrical reaction vessel with a resistance heating type electric tubular furnace.
- a heat-resistant quartz tube is preferably used as the reaction vessel.
- Any suitable catalyst can be used as a catalyst (catalyst layer material) that can be used in the production of an aggregate of carbon nanotubes that can be included in the static elimination member for analysis of the present invention.
- metal catalysts such as iron, cobalt, nickel, gold, platinum, silver, copper, are mentioned.
- 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.
- 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.
- 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.
- 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.
- 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 for producing the aggregate of carbon nanotubes that can be included in the static eliminating member for analysis 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. is there.
- the thickness of the catalyst layer that can be used in the production of the carbon nanotube aggregate that can be included in the static eliminating member for analysis of the present invention is within the above range, the carbon nanotube aggregate has excellent mechanical properties and a high specific surface area.
- the aggregate of carbon nanotubes can exhibit excellent adhesive properties.
- the static eliminating member for analysis using such an aggregate of carbon nanotubes can be sufficiently attached to the periphery of the sample to be analyzed in precision analysis such as analysis using an atomic force microscope, and the sample to be analyzed and the surrounding environment are contaminated. Therefore, charging around the sample to be analyzed can be further suppressed. Further, if the static eliminating member for analysis of the present invention is used, there is no risk of sparking even if metal exists around the sample to be analyzed, and it can be physically easily covered and analyzed in a high temperature environment. Analysis under vacuum or in a vacuum environment can be performed without any problems.
- Any appropriate method can be adopted as a method for forming the catalyst layer.
- 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 a carbon source that can be used for producing a carbon nanotube aggregate that can be included in the static elimination member for analysis of the present invention.
- 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 static eliminating member for analysis 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. .
- ⁇ Evaluation of the number and distribution of carbon nanotubes in a carbon nanotube aggregate The number of carbon nanotube layers and the number distribution of carbon nanotubes in the aggregate of carbon nanotubes 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.
- SEM scanning electron microscope
- TEM transmission electron microscope
- Example 1 An alumina thin film (thickness 20 nm) was formed on a silicon wafer (manufactured by Silicon Technology) as a substrate previously cut into 10 mm ⁇ 10 mm by a sputtering apparatus (manufactured by ULVAC, RFS-200). On this alumina thin film, an Fe thin film (thickness: 1.0 nm) was further vapor-deposited with a sputtering apparatus (ULVAC, RFS-200).
- this substrate was placed in a 30 mm ⁇ 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., the tube was filled with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) and left standing for 5 minutes 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 carbon nanotubes included in the carbon nanotube aggregate (1) had a length of 100 ⁇ m and a diameter of 4.8 nm. In the distribution of the number of carbon nanotubes provided in the carbon nanotube aggregate (1), the mode value was present in two layers, and the relative frequency was 75%.
- the carbon nanotube aggregate (1) was peeled off from the substrate with tweezers to obtain a sheet-shaped analysis static eliminator (1) having a length of 10 mm and a width of 10 mm. Various evaluation was performed about the obtained static elimination member for analysis (1). The results are summarized in Table 1.
- Example 2 An alumina thin film (thickness 20 nm) was formed on a silicon wafer (manufactured by Silicon Technology) as a substrate previously cut into 10 mm ⁇ 10 mm by a sputtering apparatus (manufactured by ULVAC, RFS-200). On this alumina thin film, an Fe thin film (thickness: 2.0 nm) was further vapor-deposited with a sputtering apparatus (ULVAC, RFS-200). Thereafter, this substrate was placed in a 30 mm ⁇ 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.
- a mixed gas of helium / hydrogen 90/50 sccm
- 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) is filled in the tube, and left for 10 minutes to grow carbon nanotubes on the substrate. As a result, an aggregate of carbon nanotubes (2) in which is oriented in the length direction was obtained.
- the carbon nanotubes included in the carbon nanotube aggregate (2) had a length of 300 ⁇ m and a diameter of 10.1 nm.
- the mode value was present in three layers, and the relative frequency was 72%.
- the carbon nanotube aggregate (2) was peeled off from the substrate with tweezers to obtain a sheet-shaped analysis static elimination member (2) having a length of 10 mm and a width of 20 mm.
- Various evaluation was performed about the obtained static elimination member (2) for analysis. The results are summarized in Table 1.
- Example 3 An alumina thin film (thickness 20 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 alumina thin film, an Fe thin film (thickness: 1.0 nm) was further vapor-deposited with a sputtering apparatus (ULVAC, RFS-200). Thereafter, the film was patterned to a diameter of 30 ⁇ m by photolithography.
- this substrate was placed in a 30 mm ⁇ 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., the tube was filled with a mixed gas of helium / hydrogen / ethylene (85/50/5 sccm, moisture content 600 ppm) and left for 2 minutes to grow carbon nanotubes on the substrate. As a result, an aggregate (3) of carbon nanotubes in which are aligned in the length direction was obtained.
- a mixed gas of helium / hydrogen 90/50 sccm maintained at 600 ppm in water
- the carbon nanotubes included in the carbon nanotube aggregate (3) had a length of 30 ⁇ m and a diameter of 4.8 nm. 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%.
- the carbon nanotube aggregate (3) was peeled off from the substrate with tweezers to obtain a probe-shaped analysis static elimination member (3) having a diameter of 30 ⁇ m. Various evaluation was performed about the obtained static elimination member for analysis (3). The results are summarized in Table 1.
- Example 4 An Al thin film (thickness 10 nm) was formed on a silicon substrate (made by KST, wafer with thermal oxide film, thickness 1000 ⁇ m) previously cut into 10 mm ⁇ 10 mm by a vacuum deposition apparatus (manufactured by JEOL, JEE-4X Vacuum Evaporator). Thereafter, oxidation treatment was performed at 450 ° C. for 1 hour. In this way, an Al 2 O 3 film was formed on the silicon substrate. On the Al 2 O 3 film, an Fe thin film (thickness: 2.0 nm) was further deposited by a sputtering apparatus (manufactured by ULVAC, RFS-200) to form a catalyst layer.
- a sputtering apparatus manufactured by ULVAC, RFS-200
- the obtained silicon substrate with a catalyst layer was cut and placed in a 30 mm ⁇ quartz tube, and a helium / hydrogen (120/80 sccm) mixed gas maintained at a moisture content of 350 ppm was allowed to flow into the quartz tube for 30 minutes. Was replaced. Thereafter, the inside of the tube was gradually raised to 765 ° C. in 35 minutes using an electric tubular furnace, and stabilized at 765 ° C. While maintaining the temperature at 765 ° C., the tube was filled with a mixed gas of helium / hydrogen / ethylene (105/80/15 sccm, moisture content 350 ppm) and left for 15 minutes to grow carbon nanotubes on the substrate.
- the carbon nanotubes included in the carbon nanotube aggregate (4) had a length of 400 ⁇ m and a diameter of 14.6 nm.
- the distribution width of the number distribution is 17 layers (4 to 20 layers), and the mode value is present in 4 layers and 8 layers, The frequencies were 20% and 20%, respectively.
- the carbon nanotube aggregate (4) was peeled off from the substrate with tweezers to obtain a sheet-shaped analysis static eliminator (4) having a length of 10 mm and a width of 10 mm.
- Various evaluation was performed about the obtained static elimination member for analysis (4). The results are summarized in Table 1.
- the static elimination member for analysis of the present invention can be suitably used for precision analysis such as analysis using an atomic force microscope.
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Abstract
Description
本発明の分析用除電部材は、繊維状柱状物を複数備える繊維状柱状構造体を含む。本発明の分析用除電部材は、繊維状柱状物を複数備える繊維状柱状構造体からなる部材であっても良いし、本発明の効果を損なわない範囲で、繊維状柱状物を複数備える繊維状柱状構造体と任意の適切な他の材料との複合体であっても良い。本発明の分析用除電部材は、繊維状柱状物を複数備える繊維状柱状構造体を含むので、原子間力顕微鏡を用いる分析などの精密分析において、分析対象試料周辺に十分に貼着でき、分析対象試料や周辺環境が汚染されることなく、分析対象試料周辺の帯電を抑制できる。また、本発明の分析用除電部材を用いれば、分析対象試料周辺に金属が存在していてもスパークのおそれがなく、チャンバーで覆って分析することも可能であり、高温環境下や真空環境下での分析も問題なく行える。
本発明の分析用除電部材が繊維状柱状構造体を含む場合、該繊維状柱状構造体は好ましくはカーボンナノチューブ集合体である。
本発明の分析用除電部材が含み得るカーボンナノチューブ集合体の好ましい実施形態の1つ(以下、第1の好ましい実施形態と称することがある)は、複数のカーボンナノチューブを備え、該カーボンナノチューブが複数層を有し、該カーボンナノチューブの層数分布の分布幅が10層以上であり、該層数分布の最頻値の相対頻度が25%以下である。
本発明の分析用除電部材が含み得るカーボンナノチューブ集合体の好ましい実施形態の別の1つ(以下、第2の好ましい実施形態と称することがある)は、複数のカーボンナノチューブを備え、該カーボンナノチューブが複数層を有し、該カーボンナノチューブの層数分布の最頻値が層数10層以下に存在し、該最頻値の相対頻度が30%以上である。
本発明の分析用除電部材が含み得るカーボンナノチューブ集合体の製造方法としては、任意の適切な方法を採用し得る。
繊維状柱状物の長さLは、走査型電子顕微鏡(SEM)によって測定した。
ガラス(MATSUNAMI スライドガラス27mm×56mm)に、1cm2単位面積に切り出した分析用除電部材の貼着面が接触するように載置し、5kgのローラーを一往復させて分析用除電部材の貼着面をガラスに圧着した。その後、30分間放置した。引張り試験機(Instron Tensile Tester)で引張速度50mm/minにて、室温(25℃)にてせん断試験を行い、得られたピークをせん断接着力とした。
カーボンナノチューブ集合体におけるカーボンナノチューブの層数および層数分布は、走査型電子顕微鏡(SEM)および/または透過電子顕微鏡(TEM)によって測定した。得られたカーボンナノチューブ集合体の中から少なくとも10本以上、好ましくは20本以上のカーボンナノチューブをSEMおよび/またはTEMにより観察し、各カーボンナノチューブの層数を調べ、層数分布を作成した。
原子間力顕微鏡(AFM)による分析における分析対象試料の測定箇所周辺の除電性を、温度25℃で常圧下での分析環境下、温度200℃で常圧下での分析環境下、温度200℃で真空下での分析環境下のそれぞれについて評価した。
すなわち、分析対象試料の測定箇所を2回測定し、1回目(Trace)と2回目(Retrace)の表面形状のピーク値を比較した。
評価基準は下記の通りとした。
○:測定した表面形状のピーク値が1回目(Trace)と2回目(Retrace)とで±60%未満
×(a):測定した表面形状のピーク値が1回目(Trace)と2回目(Retrace)とで±60%以上異なる。
×(b):装置の構造上、施策が困難。
×(c):水分が蒸発してしまい、除電を実現できず。
原子間力顕微鏡(AFM)による分析における分析対象試料の測定箇所の汚染性を、温度25℃で常圧下での分析環境下、温度200℃で常圧下での分析環境下、温度200℃で真空下での分析環境下のそれぞれについて評価した。
すなわち、電界放出型電子顕微鏡(FE-SEM)により分析対象試料の測定箇所を観察し、物理的な異物の有無を調べた。またX線光電子分光分析装置(ESCA)にて分析対象試料の測定箇所の有機物由来の炭素を検出し、化学的な汚染の有無について調べた。
評価基準は下記の通りとした。
○:FE-SEM、ESCAのいずれの分析によっても汚染が検出されない。
×(d):FE-SEMの分析によって汚染が検出。
×(e):ESCAの分析によって汚染が検出。
あらかじめ10mm×10mmにカットされた基板としてのシリコンウェハ(シリコンテクノロジー製)上に、スパッタ装置(ULVAC製、RFS-200)により、アルミナ薄膜(厚み20nm)を形成した。このアルミナ薄膜上に、さらにスパッタ装置(ULVAC製、RFS-200)にてFe薄膜(厚み1.0nm)を蒸着した。
その後、この基板を30mmφの石英管内に載置し、水分600ppmに保ったヘリウム/水素(90/50sccm)混合ガスを石英管内に30分間流して、管内を置換した。その後、電気管状炉を用いて管内を765℃まで昇温させ、765℃にて安定させた。765℃にて温度を保持したまま、ヘリウム/水素/エチレン(85/50/5sccm、水分率600ppm)混合ガスを管内に充填させ、5分間放置してカーボンナノチューブを基板上に成長させ、カーボンナノチューブが長さ方向に配向しているカーボンナノチューブ集合体(1)を得た。
カーボンナノチューブ集合体(1)が備えるカーボンナノチューブの長さは100μmであり、直径は4.8nmであった。
カーボンナノチューブ集合体(1)が備えるカーボンナノチューブの層数分布において、最頻値は2層に存在し、相対頻度は75%であった。
カーボンナノチューブ集合体(1)をピンセットによって基板から剥がし、縦10mm×横10mmのシート状の分析用除電部材(1)とした。
得られた分析用除電部材(1)について各種評価を行った。
結果を表1にまとめた。
あらかじめ10mm×10mmにカットされた基板としてのシリコンウェハ(シリコンテクノロジー製)上に、スパッタ装置(ULVAC製、RFS-200)により、アルミナ薄膜(厚み20nm)を形成した。このアルミナ薄膜上に、さらにスパッタ装置(ULVAC製、RFS-200)にてFe薄膜(厚み2.0nm)を蒸着した。
その後、この基板を30mmφの石英管内に載置し、水分600ppmに保ったヘリウム/水素(90/50sccm)混合ガスを石英管内に30分間流して、管内を置換した。その後、電気管状炉を用いて管内を765℃まで昇温させ、765℃にて安定させた。765℃にて温度を保持したまま、ヘリウム/水素/エチレン(85/50/5sccm、水分率600ppm)混合ガスを管内に充填させ、10分間放置してカーボンナノチューブを基板上に成長させ、カーボンナノチューブが長さ方向に配向しているカーボンナノチューブ集合体(2)を得た。
カーボンナノチューブ集合体(2)が備えるカーボンナノチューブの長さは300μmであり、直径は10.1nmであった。
カーボンナノチューブ集合体(2)が備えるカーボンナノチューブの層数分布において、最頻値は3層に存在し、相対頻度は72%であった。
カーボンナノチューブ集合体(2)をピンセットによって基板から剥がし、縦10mm×横20mmのシート状の分析用除電部材(2)とした。
得られた分析用除電部材(2)について各種評価を行った。
結果を表1にまとめた。
基板としてのシリコンウェハ(シリコンテクノロジー製)上に、スパッタ装置(ULVAC製、RFS-200)により、アルミナ薄膜(厚み20nm)を形成した。このアルミナ薄膜上に、さらにスパッタ装置(ULVAC製、RFS-200)にてFe薄膜(厚み1.0nm)を蒸着した。その後、フォトリソグラフィ加工により、直径30μmにパターン化した。
その後、この基板を30mmφの石英管内に載置し、水分600ppmに保ったヘリウム/水素(90/50sccm)混合ガスを石英管内に30分間流して、管内を置換した。その後、電気管状炉を用いて管内を765℃まで昇温させ、765℃にて安定させた。765℃にて温度を保持したまま、ヘリウム/水素/エチレン(85/50/5sccm、水分率600ppm)混合ガスを管内に充填させ、2分間放置してカーボンナノチューブを基板上に成長させ、カーボンナノチューブが長さ方向に配向しているカーボンナノチューブ集合体(3)を得た。
カーボンナノチューブ集合体(3)が備えるカーボンナノチューブの長さは30μmであり、直径は4.8nmであった。
カーボンナノチューブ集合体(3)が備えるカーボンナノチューブの層数分布において、最頻値は2層に存在し、相対頻度は75%であった。
カーボンナノチューブ集合体(3)をピンセットによって基板から剥がし、直径30μmのプローブ状の分析用除電部材(3)とした。
得られた分析用除電部材(3)について各種評価を行った。
結果を表1にまとめた。
あらかじめ10mm×10mmにカットされたシリコン基板(KST製、熱酸化膜付ウェハ、厚み1000μm)上に、真空蒸着装置(JEOL製、JEE-4X Vacuum Evaporator)により、Al薄膜(厚み10nm)を形成した後、450℃で1時間酸化処理を施した。このようにして、シリコン基板上にAl2O3膜を形成した。このAl2O3膜上に、さらにスパッタ装置(ULVAC製、RFS-200)にてFe薄膜(厚み2.0nm)を蒸着させて触媒層を形成した。
次に、得られた触媒層付シリコン基板をカットして、30mmφの石英管内に載置し、水分350ppmに保ったヘリウム/水素(120/80sccm)混合ガスを石英管内に30分間流して、管内を置換した。その後、電気管状炉を用いて管内を765℃まで35分間で段階的に昇温させ、765℃にて安定させた。765℃にて温度を保持したまま、ヘリウム/水素/エチレン(105/80/15sccm、水分率350ppm)混合ガスを管内に充填させ、15分間放置してカーボンナノチューブを基板上に成長させ、カーボンナノチューブが長さ方向に配向しているカーボンナノチューブ集合体(4)を得た。
カーボンナノチューブ集合体(4)が備えるカーボンナノチューブの長さは400μmであり、直径は14.6nmであった。
カーボンナノチューブ集合体(4)が備えるカーボンナノチューブの層数分布において、層数分布の分布幅は17層(4層~20層)であり、最頻値は4層と8層に存在し、相対頻度はそれぞれ20%と20%であった。
カーボンナノチューブ集合体(4)をピンセットによって基板から剥がし、縦10mm×横10mmのシート状の分析用除電部材(4)とした。
得られた分析用除電部材(4)について各種評価を行った。
結果を表1にまとめた。
分析用除電部材を用いずに、各種評価を行った。
結果を表1にまとめた。
分析用除電部材として、カーボンナノチューブの粉末(Nanocyl製、商品名:short-DWNT)0.1mgを用いて、各種評価を行った。
結果を表1にまとめた。
分析用除電部材を用いず、静電ブロワー(KEYENCE製、商品名:SJ-5020)を用いて、各種評価を行った。具体的には、静電ブロワーを用いて、サンプル表面に対して数秒間照射した。その後、サンプルをチャンバー内にセットし、測定を行った。
結果を表1にまとめた。
分析用除電部材を用いず、高湿度条件下(湿度65%)で各種評価を行った。具体的には、温度25℃、湿度50%RHに保たれたチャンバー内にサンプルおよび純水を入れたシャーレを静置した。その後、1時間程度放置した後、測定を行った。
結果を表1にまとめた。
100 繊維状柱状構造体
1 基材
2 繊維状柱状物
2a 繊維状柱状物の片端
Claims (5)
- 繊維状柱状物を複数備える繊維状柱状構造体を含む、分析用除電部材。
- 室温におけるガラス面に対するせん断接着力が1N/cm2以上である、請求項1に記載の分析用除電部材。
- 前記繊維状柱状構造体が、複数のカーボンナノチューブを備えるカーボンナノチューブ集合体である、請求項1に記載の分析用除電部材。
- シート状である、請求項1に記載の分析用除電部材。
- プローブ状である、請求項1に記載の分析用除電部材。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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KR1020157001730A KR20150050550A (ko) | 2012-08-31 | 2013-08-21 | 분석용 제전 부재 |
US14/408,582 US20150153386A1 (en) | 2012-08-31 | 2013-08-21 | Discharge member for analysis |
CN201380044879.3A CN104583781A (zh) | 2012-08-31 | 2013-08-21 | 分析用除电部件 |
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EP (1) | EP2891889A4 (ja) |
JP (1) | JP2014048165A (ja) |
KR (1) | KR20150050550A (ja) |
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CN111261479B (zh) * | 2018-11-30 | 2021-10-26 | 浙江大学 | 具有静电导出作用的多自由度样品杆 |
CN113141696A (zh) * | 2020-01-20 | 2021-07-20 | 北京富纳特创新科技有限公司 | 除静电的方法 |
CN113141697A (zh) * | 2020-01-20 | 2021-07-20 | 北京富纳特创新科技有限公司 | 聚合物薄膜制备系统 |
CN115458379A (zh) * | 2021-06-08 | 2022-12-09 | 清华大学 | 碳纳米管器件及其使用方法 |
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JP3425382B2 (ja) * | 1998-12-03 | 2003-07-14 | 株式会社島津製作所 | 表面検査装置 |
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2013
- 2013-08-21 KR KR1020157001730A patent/KR20150050550A/ko not_active Application Discontinuation
- 2013-08-21 US US14/408,582 patent/US20150153386A1/en not_active Abandoned
- 2013-08-21 WO PCT/JP2013/072287 patent/WO2014034489A1/ja active Application Filing
- 2013-08-21 EP EP13833055.0A patent/EP2891889A4/en not_active Withdrawn
- 2013-08-21 CN CN201380044879.3A patent/CN104583781A/zh active Pending
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CN104583781A (zh) | 2015-04-29 |
EP2891889A4 (en) | 2016-04-13 |
KR20150050550A (ko) | 2015-05-08 |
JP2014048165A (ja) | 2014-03-17 |
US20150153386A1 (en) | 2015-06-04 |
EP2891889A1 (en) | 2015-07-08 |
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