WO2015146614A1 - Procédé d'analyse sims et dispositif d'analyse sims - Google Patents

Procédé d'analyse sims et dispositif d'analyse sims Download PDF

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Publication number
WO2015146614A1
WO2015146614A1 PCT/JP2015/057400 JP2015057400W WO2015146614A1 WO 2015146614 A1 WO2015146614 A1 WO 2015146614A1 JP 2015057400 W JP2015057400 W JP 2015057400W WO 2015146614 A1 WO2015146614 A1 WO 2015146614A1
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WIPO (PCT)
Prior art keywords
solid sample
fixing member
carbon nanotubes
fibrous columnar
sims
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PCT/JP2015/057400
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English (en)
Japanese (ja)
Inventor
前野　洋平
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日東電工株式会社
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Publication of WO2015146614A1 publication Critical patent/WO2015146614A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/142—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised

Definitions

  • the present invention relates to a SIMS analysis method and a SIMS analysis apparatus. Specifically, the present invention relates to a method for analyzing a measurement target sample in SIMS (Secondary Ion Mass Spectrometry) and an apparatus for analyzing the measurement target sample in SIMS.
  • SIMS Single Ion Mass Spectrometry
  • SIMS Secondary Ion Mass Spectrometry: secondary ion mass spectrometry
  • components atoms, molecules
  • SIMS can be applied to elemental analysis of organic matter and inorganic matter, and isotope analysis is also possible (see, for example, Patent Document 1).
  • the SIMS analysis method of the present invention comprises: A method for analyzing a solid sample by SIMS, comprising: As a fixing member for fixing the solid sample, a fixing member having a fibrous columnar structure including a plurality of fibrous columnar objects having a length of 200 ⁇ m or more on the surface is used.
  • the shear adhesive force with respect to the glass surface in the room temperature of the said fibrous columnar structure is 10 N / cm ⁇ 2 > or more.
  • the fibrous columnar structure is a carbon nanotube aggregate including a plurality of carbon nanotubes.
  • the SIMS analyzer of the present invention is An apparatus for analyzing a solid sample by SIMS, A fixing member for fixing the solid sample;
  • the fixing member is a fixing member having a fibrous columnar structure including a plurality of fibrous columnar members having a length of 200 ⁇ m or more on the surface.
  • the shear adhesive force with respect to the glass surface in the room temperature of the said fibrous columnar structure is 10 N / cm ⁇ 2 > or more.
  • the fibrous columnar structure is a carbon nanotube aggregate including a plurality of carbon nanotubes.
  • the SIMS analyzer for analyzing a solid sample in such a SIMS analysis method can be provided.
  • FIG. 4 is a photographic diagram showing SIMS analysis results in Example 1.
  • the SIMS analysis method of the present invention is a method for analyzing a solid sample by SIMS, and a fibrous columnar structure including a plurality of fibrous columnar members having a length of 200 ⁇ m or more is provided on the surface as a fixing member for fixing the solid sample.
  • the fixing member which has is used.
  • a fixing member for fixing a solid sample by using a fixing member having a fibrous columnar structure having a plurality of fibrous columnar bodies having a length of 200 ⁇ m or more on the surface, a solid that is a measurement target Contamination of the sample can be prevented, the solid sample can be stably fixed, and good contrast can be expressed.
  • the SIMS analyzer of the present invention is an apparatus for analyzing a solid sample by SIMS, and includes a fixing member for fixing the solid sample, and the fixing member includes a fibrous column having a plurality of fibrous columnar members having a length of 200 ⁇ m or more.
  • the fixing member for fixing the solid sample is a fixing member having a fibrous columnar structure having a plurality of fibrous columnar bodies having a length of 200 ⁇ m or more on the surface, so that the solid to be measured Contamination of the sample can be prevented, the solid sample can be stably fixed, and good contrast can be expressed.
  • any configuration other than the fixed member in the SIMS analyzer of the present invention may be adopted depending on the purpose. That is, for example, a fixing member portion of a commercially available SIMS analyzer is changed to a special fixing member in the SIMS analyzer of the present invention, and various changes necessary for the change are made in the present invention. SIMS analyzer.
  • the fixing member is a member for fixing a solid sample, and its size and shape can be appropriately selected according to the type of SIMS analyzer to be used.
  • the fixing member is a fixing member having a fibrous columnar structure on the surface
  • the fixing member may be a fixing member made only of the fibrous columnar structure, or a fixing member made of the fibrous columnar structure and any appropriate member. It may be a member. Examples of such an appropriate member include a base material.
  • the fibrous columnar structure includes a plurality of fibrous columnar objects having a length of 200 ⁇ m or more.
  • the length of the fibrous columnar material is preferably 200 ⁇ m to 2000 ⁇ m, more preferably 300 ⁇ m to 1500 ⁇ m, still more preferably 400 ⁇ m to 1000 ⁇ m, particularly preferably 500 ⁇ m to 1000 ⁇ m, and most preferably 600 ⁇ m to 1000 ⁇ m. It is.
  • the length of the fibrous columnar body is within the above range, contamination of the solid sample to be measured can be prevented, the solid sample can be stably fixed, and good contrast can be expressed.
  • FIG. 1 shows a schematic cross-sectional view of an example of a fixing member used in a SIMS analysis method in a preferred embodiment of the present invention or provided in a SIMS analysis apparatus in a preferred embodiment of the present invention.
  • a fibrous columnar structure 10 includes a base material 1 and a plurality of fibrous columnar objects 2. 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 fibrous columnar structure 10 may be an aggregate including only the plurality of fibrous columns 2. That is, the fibrous columnar structure 10 may not include the base material 1.
  • the plurality of fibrous columnar objects 2 can exist as an aggregate with each other, for example, by van der Waals force.
  • the shear adhesive force of the fibrous columnar structure to the glass surface at room temperature is preferably 10 N / cm 2 or more, more preferably 10 N / cm 2 to 200 N / cm 2 , and further preferably 15 N / cm 2.
  • 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.
  • metals such as aluminum, quartz glass, silicon (silicon wafer, etc.), engineering plastic, super engineering plastic, and the like can be given.
  • 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 substrate can be set to any appropriate value depending on the purpose.
  • the surface of the substrate is chemically treated with conventional surface treatments such as chromic acid treatment, ozone exposure, flame exposure, high-voltage strike exposure, ionizing radiation treatment, etc., in order to improve adhesion and retention with adjacent layers.
  • conventional surface treatments such as chromic acid treatment, ozone exposure, flame exposure, high-voltage strike exposure, ionizing radiation treatment, etc.
  • a physical treatment or a coating treatment with a primer may be performed.
  • the substrate may be a single layer or a multilayer body.
  • the diameter of the fibrous columnar material is preferably 0.3 nm to 2000 nm, more preferably 1 nm to 1000 nm, still more preferably 2 nm to 500 nm, particularly preferably 2 nm to 200 nm, and most preferably 2 nm to 100 nm.
  • the diameter of the fibrous columnar body is within the above range, contamination of the solid sample to be measured can be further prevented, the solid sample can be fixed more stably, and a better contrast can be expressed.
  • the fibrous columnar structure is preferably a carbon nanotube aggregate including a plurality of carbon nanotubes.
  • the fibrous columnar product is preferably a carbon nanotube.
  • the fixing member is preferably a fixing member having a carbon nanotube aggregate including a plurality of carbon nanotubes having a length of 200 ⁇ m or more on the surface.
  • the fixing member is a fixing member having a carbon nanotube aggregate including a plurality of carbon nanotubes having a length of 200 ⁇ m or more on the surface, contamination of the solid sample to be measured can be further prevented, and the solid sample can be more stable. It can be fixed and better contrast can be expressed.
  • the fixing member is a fixing member having a carbon nanotube aggregate including a plurality of carbon nanotubes having a length of 200 ⁇ m or more on the surface
  • the fixing member is a fixing member having a carbon nanotube aggregate on the surface. It may be a fixing member made only of a body, or a fixing member made of a carbon nanotube aggregate and any appropriate member. Examples of such an appropriate member include a base material.
  • the fixing member is a fixing member made of a carbon nanotube aggregate and any appropriate member
  • one end of the carbon nanotube may be fixed to the arbitrary appropriate member.
  • a suitable member preferably includes a substrate.
  • the substrate used for the production of the carbon nanotube aggregate may be used as it is as a base material.
  • an adhesive layer may be provided on the substrate to bond and fix the carbon nanotubes.
  • the base material is a thermosetting resin
  • a thin film may be prepared in a state before the reaction, and one end of the carbon nanotube may be pressure-bonded to the thin film layer, and then cured and fixed.
  • the base material is a thermoplastic resin or metal
  • One preferred embodiment of the aggregate of carbon nanotubes includes a plurality of carbon nanotubes, the carbon nanotubes having a plurality of layers, and the carbon nanotube layer.
  • the distribution width of the number distribution is 10 layers or more, and the relative frequency of the mode value of the layer number distribution is 25% or less.
  • the distribution width of the number distribution of the carbon nanotubes is preferably 10 or more, more preferably 10 to 30 layers, still more preferably 10 to 25 layers, particularly
  • the number of layers is 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 fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the number of carbon nanotube 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 carbon nanotube layers is preferably 5 to 30 layers, more preferably 10 to 30 layers, and even more preferably 15 to 30 layers. Particularly preferred are 15 to 25 layers.
  • the minimum number of carbon nanotube layers is preferably 1 to 10 layers, and more preferably 1 to 5 layers.
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area, Furthermore, the carbon nanotube can be a carbon nanotube aggregate exhibiting excellent adhesive properties. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the relative frequency of the mode value of the number distribution of carbon nanotubes is preferably 25% or less, more preferably 1% to 25%, and even more preferably 5% to 25%. Particularly preferred is 10% to 25%, and most preferred is 15% to 25%.
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area. It can be an aggregate of carbon nanotubes exhibiting excellent adhesive properties. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the mode of the number distribution of the carbon nanotubes is preferably present from 2 layers to 10 layers, more preferably from 3 layers to 10 layers. .
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and the carbon nanotubes have excellent adhesive properties. It can become the carbon nanotube aggregate which shows. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the carbon nanotubes may have any appropriate shape in cross section.
  • 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 200 ⁇ m or more, more preferably 200 ⁇ m to 2000 ⁇ m, still more preferably 300 ⁇ m to 1500 ⁇ m, still more preferably 400 ⁇ m to 1000 ⁇ m, particularly
  • the thickness is preferably 500 ⁇ m to 1000 ⁇ m, and most preferably 600 ⁇ m to 1000 ⁇ m.
  • 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.
  • the carbon nanotube aggregates exhibit excellent adhesive properties. Can be. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the specific surface area and density of the carbon nanotubes can be set to any appropriate values.
  • Another preferred embodiment of the aggregate of carbon nanotubes includes a plurality of carbon nanotubes, the carbon nanotubes having a plurality of layers, and the carbon nanotubes.
  • the mode value of the number distribution of layers exists in 10 layers 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, further preferably 2 to 8 layers, particularly Three to eight layers are preferred.
  • 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 furthermore, the carbon nanotubes have excellent adhesive properties. It can be the carbon nanotube aggregate shown. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the number of carbon nanotube 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 carbon nanotube layers is preferably 1 to 20 layers, more preferably 2 to 15 layers, and further preferably 3 to 10 layers. .
  • the minimum number of carbon nanotube layers is preferably 1 to 10 layers, more preferably 1 to 5 layers.
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area, Furthermore, the carbon nanotube can be a carbon nanotube aggregate exhibiting excellent adhesive properties. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the relative frequency of the mode value of the number distribution of the carbon nanotubes is preferably 30% or more, more preferably 30% to 100%, and further preferably 30% to 90%. Particularly preferred is 30% to 80%, and most preferred is 30% to 70%.
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area. It can be an aggregate of carbon nanotubes exhibiting excellent adhesive properties. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the mode value of the number distribution of the carbon nanotubes is preferably present in the number of layers of 10 or less, more preferably in the number of layers from 1 to 10, and more preferably The number of layers is from 2 to 8 and particularly preferably from 2 to 6 layers.
  • the carbon nanotubes can have excellent mechanical properties and a high specific surface area, and the carbon nanotubes have excellent adhesive properties. It can become the carbon nanotube aggregate which shows. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the shape of the carbon nanotube it is sufficient that its cross section 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 nanotubes is preferably 200 ⁇ m or more, more preferably 200 ⁇ m to 2000 ⁇ m, even more preferably 300 ⁇ m to 1500 ⁇ m, even more preferably 400 ⁇ m to 1000 ⁇ m, and particularly
  • the thickness is preferably 500 ⁇ m to 1000 ⁇ m, and most preferably 600 ⁇ m to 1000 ⁇ m.
  • 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.
  • the carbon nanotube aggregates exhibit excellent adhesive properties. Can be. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • the specific surface area and density of the carbon nanotubes can be set to any appropriate values.
  • Any appropriate method can be adopted as a method for producing a carbon nanotube aggregate.
  • a method for producing a carbon nanotube aggregate for example, a catalyst layer is formed on a smooth substrate, a carbon source is filled in a state where the catalyst is activated by heat, plasma, etc., and carbon nanotubes are grown.
  • a method of producing an aggregate of carbon nanotubes oriented almost vertically from a substrate by a vapor deposition method (Chemical Vapor Deposition: CVD method).
  • CVD method Chemical Vapor Deposition: CVD method
  • any appropriate substrate can be adopted as the substrate that can be used in the method for producing a carbon nanotube aggregate.
  • 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 substrate can be used as it is in the SIMS analysis method of the present invention, or as a base material that can be included in a carbon nanotube aggregate that can be included in a fixing member included in the SIMS analysis device of the present invention.
  • any appropriate apparatus can be adopted as an apparatus for producing the carbon nanotube aggregate.
  • 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.
  • 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 the carbon nanotube aggregate.
  • 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 in the production of the carbon nanotube aggregate is preferably 0.01 nm to 20 nm, more preferably 0.1 nm to 10 nm in order to form fine particles.
  • the formed carbon nanotubes can have both excellent mechanical properties and a high specific surface area. It can be a carbon nanotube aggregate exhibiting excellent adhesive properties. Therefore, the fixing member having such an aggregate of carbon nanotubes can further prevent contamination of the solid sample to be measured, can fix the solid sample more stably, and can exhibit better contrast.
  • 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 the carbon source that can be used for the production of the carbon nanotube aggregate.
  • hydrocarbons such as methane, ethylene, acetylene, and benzene
  • alcohols such as methanol and ethanol
  • Arbitrary appropriate temperature can be employ
  • the temperature is preferably 400 ° C to 1000 ° C, more preferably 500 ° C to 900 ° C, and further preferably 600 ° C to 800 ° C. .
  • a fibrous columnar structure having a thickness of 700 ⁇ m is placed on a conductive aluminum sample stage (EM 301, G301), and compressed by a mirror surface of a silicon wafer so that the thickness becomes half (350 ⁇ m). It was. Particles obtained by pulverizing rock as an analysis sample are sprinkled on the surface of the fibrous columnar structure of the obtained fixing member (with the fibrous columnar structure disposed on the sample stage), and a silicon wafer is sprinkled from above the particles. The particles were brought into close contact with the surface of the fibrous columnar structure by the dead weight of the silicon wafer.
  • Example 1 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: 2.0 nm) was further vapor-deposited with a sputtering apparatus (ULVAC, RFS-200). Thereafter, the substrate was placed in a 30 mm ⁇ quartz tube, and a mixed gas of helium / hydrogen (105/80 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 105/80 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., the tube was filled with a mixed gas of helium / hydrogen / ethylene (90/80/15 sccm, moisture content 600 ppm) and left standing for 35 minutes to grow carbon nanotubes on the substrate.
  • a mixed gas of helium / hydrogen / ethylene 90/80/15 sccm, moisture content 600 ppm
  • the length of the carbon nanotubes provided in the carbon nanotube aggregate (1) was 700 ⁇ m.
  • Various evaluations were performed using the obtained carbon nanotube aggregate (1) as a sample fixing member (1) for a SIMS analyzer.
  • the shear bonding strength of the sample fixing member (1) for SIMS analyzer was 20.7 N / cm 2 .
  • the results of SIMS analysis are shown in FIG.
  • FIG. 3 according to the SIMS analysis method of the present invention and according to the SIMS analysis apparatus of the present invention, 16 O is confirmed only from particles without charging and drifting of the sample. It was found that the effect of obtaining an image having a clear interface can be expressed.
  • the analysis field of view was set to 25 ⁇ m per side, and an image was obtained with 16 O (oxygen). It should be noted that charging during measurement was not generated without neutralization by E-gun.
  • SIMS analysis method of the present invention By using the SIMS analysis method of the present invention or the SIMS analysis apparatus of the present invention, it is possible to prevent contamination of the solid sample to be measured, to stably fix the solid sample, and to exhibit good contrast. SIMS analysis Is possible.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

La présente invention porte sur un procédé d'analyse de spectrométrie de masse d'ions secondaires (SIMS) qui peut empêcher une contamination d'un échantillon solide à mesurer, fixer l'échantillon solide de manière stable, et présenter un bon contraste. L'invention porte en outre sur un dispositif d'analyse SIMS destiné à analyser un échantillon solide dans un tel procédé d'analyse SIMS. Dans ce procédé d'analyse SIMS destiné à analyser un échantillon solide à l'aide d'une SIMS, un élément de fixation ayant, sur la surface, une structure colonnaire fibreuse comprenant une pluralité d'objets colonnaires fibreux ayant une longueur d'au moins 200 µm est utilisé en tant qu'élément de fixation destiné à fixer l'échantillon solide. Ce dispositif d'analyse SIMS destiné à analyser un échantillon solide à l'aide d'une SIMS comprend un élément de fixation destiné à fixer l'échantillon solide, ledit élément de fixation ayant, sur la surface, une structure colonnaire fibreuse comprenant une pluralité d'objets colonnaires fibreux ayant une longueur d'au moins 200 µm.
PCT/JP2015/057400 2014-03-24 2015-03-13 Procédé d'analyse sims et dispositif d'analyse sims WO2015146614A1 (fr)

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JP2014059490A JP2015184084A (ja) 2014-03-24 2014-03-24 Ｓｉｍｓ分析方法およびｓｉｍｓ分析装置
JP2014-059490 2014-03-24

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JP2017175126A (ja) * 2016-03-18 2017-09-28 日東電工株式会社 搬送固定治具

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6281025B1 (en) * 1999-09-30 2001-08-28 Advanced Micro Devices, Inc. Substrate removal as a function of SIMS analysis
JP2005300502A (ja) * 2004-04-16 2005-10-27 Hitachi High-Technologies Corp 分析試料の作製方法
JP2013160588A (ja) * 2012-02-03 2013-08-19 Nitto Denko Corp 飛行時間型二次イオン質量分析装置用試料固定部材

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6281025B1 (en) * 1999-09-30 2001-08-28 Advanced Micro Devices, Inc. Substrate removal as a function of SIMS analysis
JP2005300502A (ja) * 2004-04-16 2005-10-27 Hitachi High-Technologies Corp 分析試料の作製方法
JP2013160588A (ja) * 2012-02-03 2013-08-19 Nitto Denko Corp 飛行時間型二次イオン質量分析装置用試料固定部材

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