WO2009110157A1 - 走査プローブ顕微鏡およびこれを用いた試料の観察方法 - Google Patents

走査プローブ顕微鏡およびこれを用いた試料の観察方法 Download PDF

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Publication number
WO2009110157A1
WO2009110157A1 PCT/JP2008/073074 JP2008073074W WO2009110157A1 WO 2009110157 A1 WO2009110157 A1 WO 2009110157A1 JP 2008073074 W JP2008073074 W JP 2008073074W WO 2009110157 A1 WO2009110157 A1 WO 2009110157A1
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Prior art keywords
sample
field light
light
nanotube
measurement probe
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English (en)
French (fr)
Japanese (ja)
Inventor
中田　俊彦
渡辺　正浩
井上　隆史
日高　貴志夫
岡井　誠
俊章 守田
誠之 廣岡
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Hitachi Ltd
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Hitachi Ltd
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Priority to US12/864,196 priority Critical patent/US8181268B2/en
Priority to EP08873098A priority patent/EP2267428A4/en
Publication of WO2009110157A1 publication Critical patent/WO2009110157A1/ja
Anticipated expiration legal-status Critical
Priority to US13/446,279 priority patent/US8635710B2/en
Ceased legal-status Critical Current

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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]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/02—Multiple-type SPM, i.e. involving more than one SPM techniques
    • G01Q60/06—SNOM [Scanning Near-field Optical Microscopy] combined with AFM [Atomic Force Microscopy]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y35/00—Methods or apparatus for measurement or analysis of nanostructures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/645—Specially adapted constructive features of fluorimeters
    • G01N21/648—Specially adapted constructive features of fluorimeters using evanescent coupling or surface plasmon coupling for the excitation of fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/18—SNOM [Scanning Near-Field Optical Microscopy] or apparatus therefor, e.g. SNOM probes
    • G01Q60/22—Probes, their manufacture, or their related instrumentation, e.g. holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
    • G01Q70/08—Probe characteristics
    • G01Q70/10—Shape or taper
    • G01Q70/12—Nanotube tips

Definitions

  • the present invention relates to a scanning probe microscope technique and a sample observation method using the same.
  • a scanning probe microscope as a measuring technique of the fine three-dimensional shape (SPM: S canning P robe M icroscope) is known.
  • SPM S canning P robe M icroscope
  • AFM A tomic F orce M icroscope
  • This atomic force microscope cannot measure optical properties such as reflectance distribution and refractive index distribution on the sample surface.
  • the near-field scanning microscope S canning N ear- field O ptical M icroscope
  • this microscope scans near-field light leaking from a small aperture of several tens of nm while keeping the gap between the aperture and the sample at several tens of nm (opening).
  • Probe which measures optical properties such as reflectance distribution and refractive index distribution on the sample surface with a resolution of several tens of nanometers, which is the same size as the aperture, exceeding the diffraction limit of light.
  • Non-Patent Document 2 scans near-field light having a size of several tens of nanometers that is scattered from a minute tip of a probe by irradiating a metal probe with light from the outside (scattering probe). A method is also disclosed.
  • Non-Patent Document 3 describes that surface plasmons excited on a metal surface by a minute spot light propagate on the metal surface.
  • Patent Document 1 discloses a method of forming a minute spot light by forming a minute spherical lens at the fiber tip.
  • Patent Document 2 discloses that a carbon nanotube is filled with metal carbides such as V, Y, Ta, and Sb that express photoluminescence and electroluminescence, a ZnS phosphor, and a CaS phosphor. Is disclosed.
  • Patent Document 1 JP 2006-515682 A Patent Document 2: JP 2002-267590 A Non-Patent Document 1: Japan Journal of Applied Physics, Vol. 31, pp. L1302-L1304 (1992) Non-Patent Document 2: Optics Letters, Vol. 19, pp. 159-161 (1994) Non-Patent Document 3: Spectroscopic Research, Vol. 54, No. 4, pp. 225-237 (2005)
  • the above-mentioned near-field scanning microscope has a measurement resolution on the order of several tens of nanometers, and lacks the resolution by an order of magnitude or more compared to an atomic force microscope or an electron microscope having a resolution of the order of nm. It also has a fatal problem for industrial applications where measurement reproducibility is extremely low. That is, among the above methods, in the method using the aperture probe, it is extremely difficult to stably form the aperture, and the practical limit is several tens of nm. Further, when the sample is scanned, the probe collides with the sample and the opening is damaged or worn, so that the opening gradually widens and the reproducibility of the measurement image is lowered.
  • a scatter probe using a metal probe is said to have higher resolution than an aperture probe, but external illumination light may scatter at the base of the probe or the sample surface, resulting in background noise.
  • the probe collides with the sample and the tip is damaged or worn, resulting in a problem that the measurement resolution is lowered and sufficient reproducibility cannot be obtained.
  • the method of forming a minute spherical lens at the end of the fiber also has a resolution of the order of several tens of nanometers or more in principle, and when the sample is scanned, the spherical lens collides with the sample and becomes damaged or worn. The spot light becomes large and its shape deteriorates, so that the reproducibility of the measurement image is lowered.
  • the method of filling the inside of the carbon nanotube with the light emitting particles that express photoluminescence and electroluminescence also decreases the luminous efficiency when the particle diameter is on the order of nanometers, and the near-field light image with a high S / N ratio can be obtained. It is difficult to obtain.
  • Another object of the present invention is to measure physical property information such as stress distribution and impurity distribution of a semiconductor sample, optical information and concavo-convex information contributing to the classification of foreign matters and defects with a resolution of nanometer order, and manufacturing process conditions This is to realize high yield production of highly reliable semiconductor devices.
  • a scanning probe microscope includes a measurement probe in which a metal structure is embedded, a cantilever that supports the measurement probe, and the measurement probe that is driven by driving the cantilever.
  • a cantilever driving means for three-dimensionally scanning the sample to be inspected, a displacement detecting means for detecting deformation of the cantilever, and a measurement probe in which a metal structure is embedded and the surface of the sample to be inspected
  • a near-field light image acquisition means for generating a near-field light to acquire a near-field light image of the sample surface to be inspected.
  • an AFM image creating means for creating an atomic force microscope image (AFM image) of the sample surface to be inspected by processing a signal obtained by detecting the deformation of the cantilever by the displacement detecting means is provided.
  • the measurement probe is driven relative to the sample to be inspected by driving a cantilever that supports the measurement probe in which the metal structure is embedded.
  • the three-dimensional scanning is optically detected, the deformation of the cantilever due to the three-dimensional scanning is optically detected, and a near-field light image of the surface of the specimen to be inspected is obtained using a measuring probe embedded with a metal structure. I did it.
  • the signal obtained by detecting the deformation of the cantilever is processed to create an atomic force microscope image (AFM image) of the sample surface to be inspected.
  • AFM image atomic force microscope image
  • the present invention it is possible to measure optical information and unevenness information on the sample surface with nanometer resolution and high reproducibility without damaging both the probe and the sample.
  • physical property information such as stress distribution and impurity distribution of the semiconductor sample can be measured, and optical information and concavo-convex information contributing to the classification of foreign matter and defects can be measured, so that foreign matter / defect classification performance is improved.
  • optical information and concavo-convex information contributing to the classification of foreign matter and defects can be measured, so that foreign matter / defect classification performance is improved.
  • Irradiation of light to metal particles generates surface plasmons in which free electrons in the metal collectively vibrate, and the evanescent light generated on the surface of the metal particles by the irradiated light couples with the surface plasmons to cause plasmon resonance. It is known to wake up, absorb light and generate a locally enhanced electric field.
  • the present invention creates a probe that generates this locally remarkably enhanced electric field (near-field light) at its tip, and observes or measures the optical state of the sample surface using this probe. .
  • FIG. 1 A first embodiment of the present invention will be described with reference to FIG. 1, FIG. 9 to FIG. 12, and FIG.
  • Au gold
  • the method of filling the gold nanoparticles is, for example, by applying a capillary phenomenon by putting the nanotube 1 and the gold nanoparticles 2 that are open at both ends by applying a high-voltage current or heating into a vacuum chamber and reacting them by heating. Nanoparticles 2 can be included inside nanotubes 1.
  • this capillary phenomenon for example, applying a technology disclosed on the web (http://www1.accsnet.ne.jp/ ⁇ kentaro/yuuki/nanotube/nanotube2.html) Can do.
  • the outer diameter of the nanotube was 20 nm, and the inner diameter of the hollow portion was 4 nm.
  • the diameter of the gold nanoparticles 2a and 2b is 4 nm.
  • the limit metal particle diameter for generating plasmons is 1 nm or more, and the object of the present invention can be achieved if the diameter of the gold nanoparticles is 1 nm or more.
  • the limit of the diameter of the gold nanoparticle that can be manufactured relatively stably was 4 nm.
  • the diameter of the gold nanoparticles is not limited to 4 nm, and the object of the present invention can be achieved if the diameter is in the range of about 1 nm to 20 nm.
  • This probe is fused and fixed to the insulator holding portions 6a and 6b by using, for example, tungsten (W) as a binder by electron beam irradiation. Then, the laser beams 5a and 5b having a wavelength of 532 nm are condensed and irradiated by the objective lens 320 from above the insulator holding portions 6a and 6b and the light guide portion 200 composed of the gold nanoparticles 2a exposed at the upper ends of the nanotubes. Fine spot light is induced by plasmon resonance excited in the gold nanoparticle 2a.
  • W tungsten
  • the minute spot light excites a surface plasmon on the nanotube 1, and the surface plasmon propagates the nanotube 1 from the upper end to the lower end as indicated by broken arrows 7a and 7b. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1. The localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light.
  • the plasmon reflected in the opposite direction to the plasmon heading from the upper end to the lower end of the light guide part 200, that is, the nanotube 1 interferes to generate a standing wave, and the standing wave node (the weak part) and the antinode (Strong part) exists.
  • the positions of the nodes and the belly depend on the wavelength of the laser light applied to the light guide unit 200. Therefore, the length L of the nanotube 1 is desirably adjusted so that the antinode of the standing wave coincides with the lower end portion of the nanotube 1 according to the wavelength of the laser light.
  • FIG. 9 shows the configuration of a scanning probe microscope equipped with this probe.
  • the scanning probe microscope has a stage unit 1000 on which a sample can be placed and moved in a three-dimensional direction of XYZ, and a measurement unit that drives the nanotube 1 to measure the sample and processes the obtained signal to generate an image.
  • 2000 an illumination optical system 3000 that irradiates light for generating near-field light between the tip of the nanotube 1 and the sample, and a detection optical system 4000 that collects and detects the propagated light by detecting the near-field light.
  • a sample monitor optical system 5000 for observing and positioning a part to be measured on the sample and a control unit 6000 for controlling the whole.
  • the stage unit 1000 includes an XYZ stage 100 and a driver 101 that can place a sample and move in a three-dimensional direction of XYZ.
  • the sample 10 is placed on the XYZ stage 100, driven by the driver 101, and positioned at a desired measurement position while observing the surface of the sample 10 with the sample monitor optical system 5000 via the detection optical system 4000.
  • the measuring unit 2000 is a semiconductor laser that irradiates a laser beam (wavelength 405 nm) 208 to the back surface of the light guide unit 200 and the cantilever 201, the piezoelectric element actuator 202, the XYZ piezoelectric element actuator 204, and the cantilever 201 that guide the laser beam to the nanotube 1. 206, a four-divided position sensor 209 that detects reflected light from the cantilever 201, and a drive circuit 207 that controls the semiconductor laser.
  • the sample monitor optical system 5000 captures an image of light that passes through the imaging lens 330 and is reflected by the mirror 500, and a mirror 500 that can be taken in and out of the optical path of the detection optical system 4000 by a driving unit (not shown).
  • a camera 501 is provided.
  • the mirror 500 is driven by a driving means (not shown) and the detection optical system 4000 is driven.
  • the optical path of the reflected light from the sample is bent in the direction of the imaging camera 501, and the optical image of the sample surface is observed by the imaging camera 501.
  • the mirror 500 is driven by a driving means (not shown) and retracted from the optical path of the detection optical system 4000.
  • the nanotube 1 is fixed to the cantilever 201 together with the light guide part 200 including the insulator holding parts 4a and 4b and the gold nanoparticles 2a shown in FIG.
  • the cantilever 201 is fixed to a piezoelectric element actuator 202 for minutely vibrating in the Z direction, and further fixed to an XYZ piezoelectric element actuator 204 for finely scanning in the XYZ directions.
  • the This signal is sent to the overall control unit 420 in the control unit 6000 and is used for monitoring the intensity fluctuation of the emitted light from the individual laser light source 300.
  • the solid laser light source 300 Control the output to keep the intensity constant.
  • the illumination optical system 3000 includes a laser light source 300, a beam monitor optical system 3100, a beam shaping optical system 305, a polarizing plate 307, a beam splitter 315, and an objective lens 320.
  • light 301 emitted from the laser light source 300 and transmitted through the beam splitter 302 of the beam monitor optical system 3100 is converted into parallel light 306 having a circular beam shape by the beam shaping optical system 305, and the polarizing plate 307 is further passed through. After being transmitted, it enters the beam splitter 315, is reflected by the circular reflection region 316b, and irradiates the upper end of the nanotube 1 through the light guide 200 as the focused light 5a, 5b by the objective lens 320.
  • plasmon resonance is excited in the gold nanoparticle 2a by the convergent lights 5a and 5b incident on the gold nanoparticle 2a, and a minute spot light is induced.
  • the minute spot light excites surface plasmons on the nanotube 1, and the surface plasmons propagate the nanotube 1 from the upper end to the lower end. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the reflected light from the near-field light 8 that has interacted with the surface structure of the sample 10 is converted into propagating light 9a and 9b.
  • the polarizing plate 307 has a polarizing axis 308 formed radially (in the radial direction), and the polarization direction of the convergent lights 5 a and 5 b incident on the light guide unit 200 is parallel to the longitudinal direction of the nanotube 1.
  • the plasmon excitation efficiency and propagation efficiency are improved.
  • the detection optical system 4000 for detecting the propagation lights 9a and 9b reflected from the sample includes an objective lens 320, a beam splitter 315, an imaging lens 330, and a photoelectric conversion element 340.
  • the propagation lights 9a and 9b are condensed by the objective lens 320 into parallel light, and then transmitted through the annular transmission region 316a of the beam splitter 315, and the transmitted lights 90a and 90b are transmitted to the imaging lens 330. Then, the light is condensed on the light receiving surface of the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube, and photoelectrically converted.
  • the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube
  • the image forming unit 410 of the measurement unit 2000 generates a detection signal from the photoelectric conversion element 340 as a control signal for the driver 203 that drives the piezoelectric element actuator 202 and a control signal for the driver 205 that drives the XYZ piezoelectric element actuator 204.
  • a driver 203 for driving the piezoelectric element actuator 202 and the XYZ piezoelectric element actuator 204 with the output from the four-division position sensor 209 is generated by processing using the control signal from the scanning control unit 400.
  • , 205 is used to generate an AFM image.
  • the two-dimensional near-field light image and the AFM image generated by the image forming unit 410 are sent to the overall control unit 420 in the control unit 6000, and each image is displayed on a separate screen on the output screen of the output unit 430 such as a display. Or they are displayed on the same screen.
  • the back surface of the cantilever 201 is irradiated with laser light (wavelength 405 nm) 208 from the semiconductor laser 206 driven by the drive circuit 207, and the reflected light is received by the 4-split position sensor 209.
  • the XYZ piezoelectric element actuator 204 is driven by the driver 205 to lower the cantilever 201, and the nanotube 1 fixed to the tip is brought into contact with the sample 10.
  • the cantilever 201 is further lowered in this state, the inclination of the cantilever 201 changes, the reflection direction of the laser irradiated on the back surface of the cantilever 201 changes, and the incident position of the laser on the four-division position sensor 209 changes.
  • the output signal from the quadrant position sensor 209 changes.
  • the contact force can be obtained by comparing the changed signal with the contact force data based on the relationship between the output signal from the four-division position sensor 209 and the inclination of the cantilever 201 obtained in advance.
  • the XYZ stage 100 is driven to position the measurement region of the sample 10 below the nanotube 1 attached to the tip of the cantilever 201 (S2001).
  • the cantilever 201 is moved to the XYZ while monitoring the contact state (contact force) between the nanotube 1 and the sample surface with the output signal from the quadrant position sensor 209.
  • the piezoelectric element actuator 204 is lowered (Z-direction scanning 501) (S2002), and the descent is stopped when a predetermined set contact force is reached (S2003).
  • the cantilever 201 After measuring the near-field light at the descending point 502 (S2004), the cantilever 201 is raised (Z-direction scanning 503) (S2005). Based on the output signal from the quadrant position sensor 209, the nanotube 1 is completely If it is detached from the sample 10 (S2006), it is determined whether or not measurement of the measurement region is completed (S2607). If not, the XYZ piezoelectric element actuator 204 is driven to move the cantilever 201 to the next measurement. The point is moved (X scan 504) (S2009). The amount of movement (feed pitch) in X scanning is determined according to the resolution required for observation. At the next measurement point, the cantilever 201 is lowered again to measure near-field light (S2002 to S2006).
  • the above step-in operation is repeatedly performed over the two-dimensional measurement region (XY region) by the XYZ piezoelectric element actuator 204, and then the measurement is completed (S2007).
  • the method of measuring the two-dimensional measurement area is scanned in the same manner as a raster scan in a television.
  • the feed pitch (adjacent scanning interval) in the Y direction at this time is determined according to the resolution required for observation.
  • the scanning control unit 400 of the measuring unit 2000 controls the XYZ direction scanning of the XYZ piezoelectric element actuator 204 driven by the driver 205, the vibration control of the piezoelectric element actuator 202 driven by the driver 203, and the positioning of the sample 10 by the XYZ stage 100. Control of the contact force between the nanotube 1 and the sample 10 and measurement of near-field light are all controlled by the overall control unit 420 in the control unit 6000. An XYZ scanning signal of the XYZ piezoelectric element actuator 204 from the scanning control unit 400 and a near-field light measurement signal from the overall control unit 420 are respectively sent to the image forming unit 410 to generate a two-dimensional near-field light image and an AFM image. Then, the data is output to the output unit 430 such as a display via the overall control unit 420 (S2008).
  • Fig. 12 shows the relationship between the nanotube-sample contact force and the near-field light measurement timing.
  • the contact force change curve 510 of FIG. 12A As the nanotube 1 rises and retreats from the sample 10, the contact force changes from the push-in direction to the pull-in direction, and at the moment of separation from the sample, the pull-in force is Maximum. After detachment, the contact force is not received at all while moving to the next measurement point and approaching the sample again.
  • the force in the pushing direction is applied at the moment when the nanotube 1 comes into contact with the sample 10, and when the set contact force is reached, the cantilever 1 stops descending.
  • the reflectance distribution on the sample surface in the two-dimensional region can be measured with almost the same optical resolution as the gold nanoparticle diameter of 4 nm. It is desirable that the set contact force is 1 nN or less, preferably sub nN to pN.
  • the cantilever 201 is not vibrated in the Z direction, and only the lowering and raising operations for setting contact force are performed.
  • the detection of the contact force is not limited to the above-mentioned optical lever method, and the piezoelectric element actuator 202 causes the cantilever to vibrate in the Z direction with a sub-nanometer order amplitude and MHz order frequency, and the vibration amplitude or vibration frequency. It is also possible to detect from the change of.
  • the near-field light 8 having a spot diameter of 4 nm can be constantly generated between the two and the nanotube 1, and the nanotube 1 is brought into contact with the sample 10 with a low contact force, that is, the moment when the gold nanoparticle 2b contacts the sample 10.
  • the near-field light can be stably detected.
  • the resolution of the two-dimensional near-field light image is improved, and the image reproducibility can be dramatically improved.
  • FIG. 2 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the configuration and function of the nanotube are the same as in the example shown in FIG.
  • laser beams 5a and 5b having a wavelength of 532 nm are collected and irradiated from above the gold nanoparticles 2a exposed at the upper end of the nanotube 1, and plasmon resonance excited by the gold nanoparticles 2a Surface plasmons were excited on the nanotube 1.
  • a gold wedge 3 is brought close to the gold nanoparticle 2a exposed at the upper end of the nanotube 1, and laser beams 5a and 5b having a wavelength of 532 nm are collected from above. Irradiate with light.
  • a minute spot light is induced by plasmon resonance excited between the tip 3p of the gold wedge 3 and the gold nanoparticle 2a. This minute spot light excites surface plasmons on the gold nanoparticles 2a exposed at the upper end portion of the nanotube 1, and the surface plasmons propagate the nanotube 1 from the upper end portion to the lower end portion as indicated by broken arrows 7a and 7b. To go.
  • the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the nanotube 1 is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • FIG. 3 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the configuration and function of the nanotube are the same as in the example shown in FIG.
  • a gold wedge 3 is brought close to the gold nanoparticle 2a exposed at the upper end of the nanotube 1, and laser beams 5a and 5b having a wavelength of 532 nm are condensed and irradiated from above the gold wedge 3. Plasmon resonance was excited between the tip 3p of the gold and the gold nanoparticle 2a.
  • this modification as shown in FIG.
  • a gold wedge 3 is brought close to the gold nanoparticles 2a exposed at the upper end of the nanotube 1 from the lateral direction, and laser beams 5a and 5b having a wavelength of 532 nm are emitted from above. Condensed and irradiated to excite plasmon resonance between the tip 3p of the gold wedge 3 and the gold nanoparticle 2a. Small spot light is induced by plasmon resonance. This minute spot light excites surface plasmons on the gold nanoparticles 2a exposed at the upper end portion of the nanotube 1, and the surface plasmons propagate the nanotube 1 from the upper end portion to the lower end portion as indicated by broken arrows 7a and 7b. To go.
  • the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the nanotube 1 is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • FIG. 13 shows the configuration of the scanning probe microscope in this embodiment.
  • the basic configuration and function of this scanning probe microscope are the same as those of the scanning probe microscope in the embodiment shown in FIG. 9, except that a spectroscope 611 is arranged in the near-field light detection portion. That is, the near-field light 8 emitted from the lower end portion of the nanotube 1 and reflected by the sample 10 is converted into propagating light 9a and 9b to become parallel light 90a and 90b by the objective lens 320, and the spectroscope 611 by the imaging lens 330. Is collected through a mirror 610.
  • light having a desired wavelength is selected from the propagation light based on the control signal from the overall control unit 420, and condensed on the light receiving surface of the photoelectric conversion element 612 such as a photodiode or a photomultiplier tube. And photoelectrically converted.
  • This detection signal is sent to the overall control unit 420, and a two-dimensional near-field light image having a specific wavelength is formed.
  • the same wavelength as that of the incident laser beam is detected, whereas in this modification, near-field light that is wavelength-shifted from the incident laser beam is detected. Is possible.
  • the contact force between the nanotube 1 and the sample 10 is set to the order of sub nN to pN or less so that the sample itself is not deformed by contact with the nanotube 1 and Raman shift does not occur.
  • a light source such as an LED having a broad wavelength band
  • the spectroscope 611 is changed to the all-wavelength collective detection type using an array sensor such as a CCD one-dimensional sensor, a two-dimensional near-field spectroscopic image can be obtained, and spectroscopic analysis of the sample 10 with nanometer resolution. Is possible.
  • a white laser 620 that emits light of three colors having wavelengths of 630 nm, 520 nm, and 430 nm is used as the light source 620, and color separation filters 625r, 625g, and 624b are disposed in the near-field light detection portion.
  • the near-field light 8 is generated between the nanotube 1 and the sample 10 by the laser light emitted from the light source 620, and the reflected light passes through the objective lens 320 and the beam splitter 315 as propagating light 9 a and 9 b to form the imaging lens 330.
  • the process is the same as that described with reference to FIG.
  • the parallel lights 90a and 90b that have reached the objective lens 330 are collected by the imaging lens 330 via the mirror 610, and then become parallel light by the relay lens 615. Further, the dichroic mirror 621 (wavelength of 600 nm or more is transmitted and less) Is reflected) and the interference filter 625r (transmission center wavelength 630 nm) extracts light having a wavelength of 630 nm. This light is condensed by a condenser lens 631 onto a light receiving surface of a photoelectric conversion element 641 such as a photodiode or a photomultiplier tube, and is subjected to photoelectric conversion.
  • a photoelectric conversion element 641 such as a photodiode or a photomultiplier tube
  • the light reflected by the dichroic mirror 621 is extracted as light having a wavelength of 520 nm by a dichroic mirror 622 (reflecting at a wavelength of 480 nm or more and transmitting at a wavelength of 480 nm or less) and an interference filter 625g (transmission center wavelength 520 nm).
  • This light is condensed by a condenser lens 632 onto a light receiving surface of a photoelectric conversion element 642 such as a photodiode or a photomultiplier tube, and subjected to photoelectric conversion.
  • the three-wavelength detection signal is sent to the overall control unit 420, and a three-wavelength two-dimensional near-field light image is formed. It is also possible to generate a color image with nanometer resolution by synthesizing these three-wavelength signals. According to the present embodiment, for example, it is possible to execute a defect review for a semiconductor that is currently performing defect classification only from a monochrome image using an SEM, using an AFM image and a color image with nanometer resolution, and defect classification accuracy Is significantly improved. According to this modified example, not only the AFM image and the near-field light image can be simultaneously acquired, but also the near-field light 8 can be constantly generated stably, and the near-field light can be stably detected. . As a result, the resolution of the two-dimensional near-field light image is improved, and the image reproducibility can be dramatically improved.
  • FIG. 15 shows a changed part of the measurement unit 2000 in the present embodiment.
  • the material constituting the sample 10 can be determined with a nanometer spatial resolution.
  • the wavelength is not limited to 3 wavelengths, and the material analysis accuracy is improved by increasing the wavelength to 4 wavelengths and 5 wavelengths.
  • FIG. 17 shows an example in which the scanning probe microscope in this modification is applied to detection of a residual film at the bottom of a deep hole such as a contact hole.
  • the nanotube 1 is inserted into the contact hole 501 having a diameter of about 30 nm, the spectral signal at the moment when the nanotube 1 is brought into contact with the bottom of the hole with a low contact force, the spectral signal is stored in the memory unit 440 in advance. By checking the relationship with the spectral intensity, the presence / absence of the remaining film 502 and the material information thereof can be obtained.
  • the near-field light 8 can be constantly generated stably, and the near-field light can be stably detected. .
  • the resolution of the two-dimensional near-field light image is improved, and the image reproducibility can be dramatically improved.
  • FIG. 18 shows a configuration of a scanning probe microscope in the present embodiment.
  • the basic configuration and function of this scanning probe microscope are the same as those of the scanning probe microscope in the embodiment shown in FIG. 9, except that the cantilever 201 is minutely vibrated in the Z direction.
  • the piezoelectric element actuator 202 is driven by the driver 203, the cantilever 201 is minutely vibrated at a constant frequency f in the Z direction, and the near-field light 8 is intensity-modulated.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • FIG. 4 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the nanotube is the multi-layered carbon nanotube 1 or the metal nanotube 1 as in the first embodiment and its modifications, and has a configuration in which the lower end is sharpened conically.
  • the upper and lower ends of the internal cavity were filled with gold (Au) spherical nanoparticles 2a and 2b, but in this embodiment, as shown in FIG.
  • the light guide unit 200 is configured by mounting fluorescent particles 25 such as an outer shell.
  • FIG. 19 shows the configuration of a scanning probe microscope equipped with this probe.
  • the basic configuration and function of this scanning probe microscope are the same as those of the scanning probe microscope in the embodiment shown in FIG. 9, but immediately before a photoelectric conversion element 340 such as a photodiode or a photomultiplier tube that detects near-field light.
  • a wavelength selection filter 355 having a transmission band of fluorescence wavelength ⁇ 10 nm emitted by the fluorescent particles 25 is disposed. That is, as shown in FIG. 4, when the laser beams 5a and 5b emitted from the solid-state laser 300 are condensed and irradiated onto the fluorescent particles 25, fluorescence having a wavelength different from that of the laser beams 5a and 5b is generated.
  • plasmon resonance occurs in the gold nanoparticle 2a, and a minute spot light having the same wavelength as the fluorescence is induced.
  • the minute spot light excites a surface plasmon on the nanotube 1, and the surface plasmon propagates the nanotube 1 from the upper end to the lower end as indicated by broken arrows 7a and 7b. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1. This localized plasmon interacts with the surface structure of the sample 10 to cause a strong resonance phenomenon, and generates a minute near-field light 8 having the same wavelength as the fluorescence.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel lights 90a and 90b pass through the annular transmission region 316a of the beam splitter 315, and the transmitted light is extracted through the imaging lens 330, and only the fluorescence wavelength component 318 is extracted by the wavelength selection filter 355, and a photodiode or photomultiplier tube is extracted.
  • the photoelectric conversion element 340 is photoelectrically converted. The subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the fluorescent particles 25 are used for the light guide unit 200.
  • the present invention is not limited to this.
  • a nonlinear optical crystal or the like is used to generate near-field light having a wavelength half that of the incident light. It is also possible to do.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • the present embodiment it is possible to greatly reduce background noise such as an optical path in the middle of the laser beams 5a and 5b emitted from the solid-state laser 300 and scattered light from the nanotube itself, and the proximity with a high SN ratio. A field light image can be obtained.
  • FIG. 5 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the nanotubes are the multi-layered carbon nanotubes 1 or the metal nanotubes 1 as in the first embodiment and its modifications, and the lower ends are sharpened conically, and the upper and lower ends of the internal cavity are gold ( Au) spherical nanoparticles 2a and 2b are filled.
  • the gold nanoparticles 2a exposed at the upper end of the nanotube 1 have been configured to be focused and irradiated from above, but this embodiment
  • the light guide unit 200 that condenses and irradiates the linearly polarized laser light 16 in the direction 17 parallel to the longitudinal direction of the nanotube 1 from the lateral direction by the condenser lens 5 is used. Different.
  • FIG. 20 shows the configuration of a scanning probe microscope equipped with this probe.
  • the basic configuration and function of this scanning probe microscope are substantially the same as those of the scanning probe microscope in the embodiment shown in FIG. 9, but the laser beam is focused on gold nanoparticles 2a exposed at the upper end of the nanotube 1 from above.
  • an illumination optical system 700 having a built-in laser light source for condensing and irradiating the laser beam from the lateral direction to the nanotube 1 is mounted as shown in FIG. .
  • the illumination optical system 700 further sends a laser beam monitor signal to the overall control unit 420, and when the intensity of the laser light fluctuates, controls the output of the laser light source to make the intensity constant.
  • Fine spot light is induced by plasmon resonance excited by the gold nanoparticle 2a.
  • the minute spot light excites a surface plasmon on the nanotube 1, and the surface plasmon propagates the nanotube 1 from the upper end to the lower end as indicated by broken arrows 7a and 7b. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel lights 90 a and 90 b are transmitted through the annular transmission region 316 a of the beam splitter 315, and the transmitted light is photoelectrically converted by the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube via the imaging lens 330.
  • the subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • FIG. 6 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the configuration and function of the nanotube 1 are the same as in the example shown in FIG.
  • linearly polarized laser light 16 in a direction 17 parallel to the longitudinal direction of the nanotube 1 is condensed from the lateral direction by the condenser lens 5 with respect to the gold nanoparticles 2 a exposed at the upper end of the nanotube 1.
  • the light guide unit 200 to be irradiated is configured.
  • this modified example as shown in FIG.
  • the nanotube holding portions 21 a and 21 b are constituted by cylindrical gold or silver rods, which are referred to as a light guide portion 200.
  • a linearly polarized laser beam 16 in a direction 17 parallel to the longitudinal direction of the nanotube 1 is condensed and irradiated from the lateral direction to the nanotube holding portions 21 a and 21 b by the condenser lens 5.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8. It is also possible to omit the gold nanoparticles 2a and to excite and propagate plasmons directly from the cylindrical nanotube holding portions 21a and 21b to the nanotubes 1.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel lights 90 a and 90 b are transmitted through the annular transmission region 316 a of the beam splitter 315, and the transmitted light is photoelectrically converted by the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube via the imaging lens 330.
  • the subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • FIG. 7 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the nanotubes are the multi-layered carbon nanotubes 1 or the metal nanotubes 1 as in the first embodiment and its modifications, and the lower ends are sharpened conically, and the upper and lower ends of the internal cavity are gold ( Au) spherical nanoparticles 2a and 2b are filled.
  • the illumination optical system 3000 is completely eliminated, and a laser light source 27 such as a semiconductor laser (for example, a wavelength of 405 nm) is mounted on the gold nanoparticle 2a at the upper end of the nanotube 1.
  • a laser light source 27 such as a semiconductor laser (for example, a wavelength of 405 nm) is mounted on the gold nanoparticle 2a at the upper end of the nanotube 1.
  • a laser light source 27 such as a semiconductor laser (for example, a wavelength of 405 nm) is mounted on the gold nanoparticle 2a at the upper end of the nanotube 1.
  • FIG. 21 shows the configuration of a scanning probe microscope equipped with this probe.
  • the basic configuration of the present scanning probe microscope is the same as that of the present scanning probe microscope except that the illumination optical system 3000 is completely eliminated and the light guide unit 200 on which the laser light source 27 such as a semiconductor laser is mounted on the gold nanoparticle 2a at the upper end of the nanotube 1
  • the function is substantially the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the laser light source 27 is driven by a drive signal 720 from the drive circuit 710, and also sends a laser light monitor signal to the overall control unit 420. When the intensity of the laser light fluctuates, the output of the laser light source is controlled to control the intensity. To be constant.
  • Plasmons are excited in the gold nanoparticles 2a illuminated by the laser light source 27, and minute spot light is induced.
  • the minute spot light excites a surface plasmon on the nanotube 1, and the surface plasmon propagates the nanotube 1 from the upper end to the lower end as indicated by broken arrows 7a and 7b. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel lights 90 a and 90 b are transmitted through the annular transmission region 316 a of the beam splitter 315, and the transmitted light is photoelectrically converted by the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube via the imaging lens 330.
  • the subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • the illumination optical system 3000 is not required, so that the configuration of the scanning probe microscope is simplified, and at the same time, the plasmon excitation / propagation efficiency is improved by the adjacent laser light source, and the SN ratio is high. A near-field light image can be obtained.
  • FIG. 8 shows the configuration of the plasmon intensifying near-field probe in the present embodiment.
  • the nanotubes are the multi-layered carbon nanotubes 1 or the metal nanotubes 1 as in the first embodiment and its modifications, and the lower ends are sharpened conically, and the upper and lower ends of the internal cavity are gold ( Au) spherical nanoparticles 2a and 2b are filled.
  • the illumination optical system 3000 is completely eliminated, the laser light from the semiconductor laser (for example, wavelength 405 nm) 730 and the solid-state laser 730 is guided by the optical fiber 30, and the polarizing plate 307.
  • An optical system for illuminating the gold nanoparticles 2 a at the upper end of the nanotube 1 with the condensing lens 31 is configured as a light guide unit 200.
  • FIG. 22 shows the configuration of a scanning probe microscope equipped with this probe. Except for the point that the illumination optical system 3000 is completely eliminated and the light guide unit 200 including the laser light source 730, the optical fiber 30, the condensing lens 31, and the polarizing plate 307 is provided, the basic configuration and functions of the scanning probe microscope are as follows. 9 is substantially the same as the scanning probe microscope in the embodiment shown in FIG.
  • the laser light monitor signal of the laser light source 730 is sent to the overall control unit 420. When the intensity of the laser light fluctuates, the output of the laser light source 730 is controlled to make the intensity constant.
  • Plasmons are excited in the gold nanoparticles 2a illuminated by the laser light 32 from the optical fiber 30, and minute spot light is induced.
  • the minute spot light excites a surface plasmon on the nanotube 1, and the surface plasmon propagates the nanotube 1 from the upper end to the lower end as indicated by broken arrows 7a and 7b. Since the lower end of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and strong localized plasmons are excited in the gold nanoparticles 2b at the lower end of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained by this probe, and it becomes possible to identify, for example, regions 11 and 12 having different reflectivities of the sample 10 with this resolution. In the atomic force microscope, the regions 11 and 12 cannot be distinguished.
  • the reflected light of the near-field light 8 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel lights 90 a and 90 b are transmitted through the annular transmission region 316 a of the beam splitter 315, and the transmitted light is photoelectrically converted by the photoelectric conversion element 340 such as a photodiode or a photomultiplier tube via the imaging lens 330.
  • the subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the near-field light 8 having a spot diameter of 4 nm between the gold nanoparticle 2 b at the lower end of the nanotube 1 and the sample 10.
  • nanoparticles are used as the nanoparticles.
  • the present invention is not limited to this, and may be particles that are efficient from the viewpoint of plasmon excitation and plasmon propagation.
  • nanoparticles such as silver and aluminum are also applicable.
  • Nanotubes are not limited to multi-walled carbon nanotubes or metal nanotubes, but are single-walled carbon nanotubes, cylindrical structures with a nanometer order diameter such as metal-containing carbon nanotubes, or the like, and combinations with the above nanoparticles As long as the material and configuration are suitable for plasmon excitation and plasmon propagation, other materials and structures may be used.
  • the plasmon excitation wavelength is set to 532 nm or 405 nm.
  • the present invention is not limited to this, and from the viewpoint of plasmon excitation and plasmon propagation, the nanotube is made a resonator. It is desirable to use an efficient wavelength (resonance wavelength) for the nanotube length.
  • the near-field light is detected by detecting the propagation light from the sample surface at the bottom of the nanotube.
  • the present invention is not limited to this, and the bottom of the nanotube is not limited. It is obvious that a configuration may be used in which propagating light that propagates from the top to the bottom and scatters from the top is detected.
  • FIG. FIG. 24 shows the configuration of the light guide portion of the plasmon intensifying near-field probe in the present embodiment.
  • the light guide portion 200 that guides the excitation light to the nanotube 1 is provided on the back surface of the cantilever 201.
  • the cantilever 201 itself is used as the light guide portion.
  • a triangular pyramid-shaped tip 730 made of Si is similarly formed at the tip of a cantilever 201 made of Si, and the nanotube 1 is fixed to the tip.
  • the back light 201s of the cantilever 1 is focused and irradiated with excitation light 5a and 5b as propagating light.
  • the excitation light 5a, 5b for example using a near-infrared laser light having a wavelength of 830nm, NA (N umerical A perture : numerical aperture) of the cantilever 201 and focused by 0.2 Irradiates the back surface 201s.
  • the polarization direction 5p is P-polarized light, and the focusing angle 735 is about 23 °.
  • the incident angle 736 is desirably around 75 °, which is the Brewster angle, in order to suppress light loss due to surface reflection.
  • the incident excitation light is refracted and focused on the ridge line 730w of the triangular pyramid-shaped chip 730.
  • the focusing angle 737 is about 6 °.
  • the incident angle 738 with respect to the ridge line 730w is desirably set to about 16 ° or more which is a critical angle.
  • the surface of the chip 730 is coated with gold thin films 730f and 730r. In consideration of the plasmon generation efficiency, it is desirable that the thickness of the gold thin film 730f along the ridge line 730w is about 50 nm, and the thickness of the two slopes sandwiching the ridge line 730w is smaller than that.
  • Excited TM mode plasmon 740 includes gold nanoparticles 2a, 2c, and 2b filled in the surface and inside of nanotube 1 fixed to the tip of tip 730, as indicated by broken arrows 7a and 7b in FIG.
  • the nanotube is the multi-layered carbon nanotube 1 or the metal nanotube 1 as in the first embodiment and its modifications, and has a configuration in which the lower end is sharpened conically. As shown in FIG. 27, since the lower end portion of the nanotube 1 is sharpened in a conical shape, the electric field strength is locally increased, and a strong localized plasmon is excited in the gold nanoparticle 2b at the lower end portion of the nanotube 1. The The localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the outer diameter of the nanotube was 20 nm, and the inner diameter of the hollow portion was 4 nm.
  • the diameter of the gold nanoparticles 2a, 2b, 2c is 4 nm.
  • the limit metal particle diameter for generating plasmons is 1 nm or more, and the object of the present invention can be achieved if the diameter of the gold nanoparticles is 1 nm or more.
  • the limit of the diameter of the gold nanoparticle that can be manufactured relatively stably was 4 nm.
  • the diameter of the gold nanoparticles is not limited to 4 nm, and the object of the present invention can be achieved if the diameter is in the range of about 1 nm to 20 nm. In this case, it is necessary to change the outer diameter of the nanotube in accordance with the diameter of the gold nanoparticle.
  • money is used as a metal particle is demonstrated in a following example, the same effect can be acquired even if it is another kind of metal, for example, silver nanoparticle.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained with this probe.
  • the gold nanoparticle array is shown as the metal structure filled in the nanotube 1, but the present invention is not limited to this.
  • the gold nanorod 702 is filled.
  • the same effect can be obtained.
  • the nanorod material is another kind of metal, for example, a silver nanorod, the same effect can be obtained.
  • the same effect can be obtained even in a structure in which only the upper end and the lower end of the nanotube 1 are filled with the gold nanoparticles 2a and 2b.
  • the cantilever 201 and the chip 730 are made of Si.
  • the present invention is not limited to this.
  • the cantilever 201 and the chip 730 made of Si 3 N 4 are also applicable.
  • visible light having a wavelength of 532 nm can be used as the excitation light.
  • the polarization direction 5p is P-polarized light, and the focusing angle 735 is about 11.5 °.
  • the incident angle 736 is preferably around 63 ° which is a Brewster angle in order to suppress light loss due to surface reflection.
  • the incident excitation light is refracted and focused on the ridge line 730w of the triangular pyramid-shaped chip 730.
  • the convergence angle 737 is about 5.7 °. It is desirable that the incident angle 738 with respect to the ridge line 730w is set to about 30 ° or more which is a critical angle.
  • a plasmon reflected in the opposite direction from a plasmon heading from the upper end portion to the lower end portion of the nanotube 1 interferes to generate a standing wave, and a standing wave node (a weak portion) and an antinode (a strong portion).
  • the positions of the nodes and the belly depend on the wavelength of the laser light applied to the light guide unit 200. Therefore, the length L of the nanotube 1 is desirably adjusted so that the antinode of the standing wave coincides with the lower end portion of the nanotube 1 according to the wavelength of the laser light.
  • FIG. 30 shows the configuration of a scanning probe microscope equipped with this probe.
  • the configuration and functions of the scanning probe microscope are the same as those in the first embodiment shown in FIG.
  • the light guide 200 that guides the excitation light to the nanotube 1 is provided on the back surface of the cantilever 201.
  • the cantilever 201 itself is used as the light guide, so that the light guide 200 is guided as shown in FIG.
  • the optical unit 200 is configured to be excluded. Further, since the excitation lights 5a and 5b are P-polarized with respect to the back surface of the cantilever 201, the polarizing plate 307 is also excluded.
  • the wavelengths of the excitation light 5a and 5b are not fixed at 830 nm, but are preferably finely adjusted to a wavelength at which the excited TM mode plasmon 740 propagates to the nanotube 1 without loss, that is, with high coupling efficiency.
  • a white laser an optimum coupling wavelength is selected and used as excitation light, or a white laser light is used as excitation light, and only the optimum coupling wavelength is installed immediately before the photoelectric conversion element 340. It is desirable to detect selectively by a selection filter.
  • the TM mode plasmon 740 that has not been coupled to the nanotube 1 becomes near-field light at the tip of the chip 730, and this becomes background noise for the near-field light 8 generated at the tip of the nanotube 1.
  • the distance 745 between the tip of the tip 730 and the tip of the nanotube 1 be at least the size of the tip of the tip, for example, several tens to several hundreds of nm. Further, as shown in FIG.
  • the AFM image and the near-field light image can be simultaneously acquired, but also the gold nanoparticle 2b exposed at the lower end portion of the nanotube 1 and the sample 10 can be obtained.
  • the near-field light 8 having a spot diameter of 4 nm can be constantly generated between them, and the nanotube 1 is brought into contact with the sample 10 with a low contact force, that is, the proximity at the moment when the gold nanoparticle 2 b contacts the sample 10.
  • the near-field light can be stably detected.
  • the resolution of the two-dimensional near-field light image is improved, and the image reproducibility can be dramatically improved.
  • FIG. 26 shows the configuration of the light guide portion of the plasmon intensifying near-field probe in this modification.
  • the structures and functions of the cantilever 201, the tip 730, and the nanotube 1 are the same as those shown in FIG.
  • the incident angle of the excitation light 5a, 5b to the back surface 201s of the cantilever 201 is set to 0 °, that is, vertical incidence. is there.
  • the excitation light 5a, 5b for example using a near-infrared laser light having a wavelength of 830nm, NA (N umerical A perture : numerical aperture) of the cantilever 201 and focused by 0.2 Irradiates the back surface 201s perpendicularly.
  • the polarization direction 5p is P-polarized light, and the focusing angle 735 is about 23 °.
  • the incident excitation light is focused on the ridge line 730w of the triangular pyramid-shaped chip 730.
  • the focusing angle 737 is about 6 °. It is desirable that the tip 730 is formed in a state where the angle of the ridge line 730w with respect to the cantilever 201 is adjusted in advance so that the incident angle 738 with respect to the ridge line 730w is about 16 ° or more which is a critical angle.
  • the surface of the chip 730 is coated with gold thin films 730f and 730r.
  • the thickness of the gold thin film 730f along the ridge line 730w is about 50 nm, and the thickness of the two slopes sandwiching the ridge line 730w is smaller than that.
  • the irradiation of the P polarized light of the excitation light to the ridge 730w, along the thin gold film 730f surface TM (T ransverse M agnetic) mode plasmon 740 is excited and propagates toward the end of the tip 730. Since the allowable range of the resonance dip incident angle 738 at which the plasmon is excited is at most 2 to 3 °, the range of the focusing angle 737 of the excitation light is preferably about 6 °, which is twice that as described above.
  • Excited TM mode plasmon 740 includes gold nanoparticles 2a, 2c, and 2b filled in the surface and inside of nanotube 1 fixed to the tip of tip 730, as indicated by broken arrows 7a and 7b in FIG. Propagation from the upper end to the lower end.
  • the electric field strength is locally increased, and a strong localized plasmon is excited in the gold nanoparticle 2b at the lower end portion of the nanotube 1.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 8.
  • the cantilever 201 and the tip 730 made of Si 3 N 4 are also applicable.
  • the spot diameter of the near-field light 8 is 4 nm, which is almost the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained with this probe.
  • a gold nanoparticle array is shown as the metal structure filled in the nanotube 1, but the present invention is not limited to this.
  • the gold nanorod 702 is filled.
  • the nanorod material is another kind of metal, for example, a silver nanorod, the same effect can be obtained.
  • the near-field light image can be simultaneously acquired, but also the near-field having a spot diameter of 4 nm between the gold nanoparticle 2b exposed at the lower end of the nanotube 1 and the sample 10 is obtained.
  • the near-field light 8 By detecting the near-field light 8 at the moment when the nanotube 1 is brought into contact with the sample 10 with a low contact force, that is, when the gold nanoparticle 2b comes into contact with the sample 10, the light 8 can be generated stably at all times. , Stable detection of near-field light becomes possible. As a result, the resolution of the two-dimensional near-field light image is improved, and the image reproducibility can be dramatically improved.
  • FIG. 29 shows a configuration of a plasmon intensifying near-field probe in this modification.
  • the nanotube is the multi-layered carbon nanotube 1 or the metal nanotube 1 as in the first embodiment and its modifications, and has a configuration in which the lower end is sharpened conically.
  • the structures and functions of the cantilever 201 and the chip 730 are the same as those shown in FIG. 25 or FIG.
  • metal carbides such as V, Y, Ta, and Sb that express photoluminescence and electroluminescence instead of gold nanoparticles at the upper end of the nanotube 1
  • ZnS A fluorescent particle 770 such as a phosphor, a CaS phosphor, CdSe (core) / ZnS (outer shell) or the like is filled, and a gold nanoparticle 2b is filled at the lower end as in the other embodiments.
  • gold nanoparticles or nanorods may be filled in the nanotube 1.
  • FIG. 32 shows the configuration of a scanning probe microscope equipped with this probe.
  • the basic configuration and function of this scanning probe microscope are the same as those of the scanning probe microscope in the first embodiment shown in FIG. 9, but a photoelectric conversion element 340 such as a photodiode or a photomultiplier for detecting near-field light.
  • a wavelength selection filter 755 having a transmission band with a fluorescence wavelength of ⁇ 10 nm emitted from the fluorescent particles 770 is arranged immediately before the point. That is, as shown in FIG. 25, the TM mode plasmon 740 excited by the excitation lights 5a and 5b propagates toward the tip of the chip 730. This TM mode plasmon 740 excites the fluorescent particles 770 filled in the upper end portion of the nanotube 1 shown in FIG.
  • the localized plasmon interacts with the surface structure of the sample 10 to generate a strong resonance phenomenon, and generates a minute near-field light 790 having the same wavelength as the fluorescence.
  • the spot diameter of the near-field light 790 is 4 nm, which is substantially the same size as the gold nanoparticle 2b when the gold nanoparticle 2b is closest to the sample 10. That is, an optical resolution of 4 nm can be obtained with this probe.
  • the reflected light of the near-field light 790 is condensed by the objective lens 320 as propagating light 9a and 9b and becomes parallel light 90a and 90b.
  • the parallel light 90a and 90b are transmitted through the annular transmission region 316a of the beam splitter 315, and the transmitted light is extracted through the imaging lens 330, and only the fluorescence wavelength component 760 is extracted by the wavelength selection filter 755, and a photodiode or a photomultiplier tube is extracted.
  • the photoelectric conversion element 340 is photoelectrically converted. The subsequent processing is the same as that of the scanning probe microscope in the embodiment shown in FIG.
  • the fluorescent particles 770 are used.
  • the present invention is not limited to this, and it is also possible to generate near-field light having a wavelength half that of incident light by using, for example, a nonlinear optical crystal. is there.
  • the near-field light 790 having a spot diameter of 4 nm between the gold nanoparticle 2b at the lower end of the nanotube 1 and the sample 10.
  • the near-field light generated at the tip of the tip 730 by the TM mode plasmon 740 not coupled to the nanotube 1 is the wavelength of the excitation light 5a, 5b itself.
  • the near-field light 790 generated at the lower end of the nanotube 1 has a different fluorescence wavelength. That is, the near-field light generated at the tip of the chip 730, which becomes background noise, is wavelength-separated, and only the near-field light 790 generated at the lower end of the nanotube 1 can be detected, thereby obtaining a near-field light image with a high S / N ratio. It becomes possible.
  • the present invention it is possible to realize a scanning probe microscope having an optical resolution of nanometer order in combination with AFM.
  • physical property information such as stress distribution and impurity distribution of the semiconductor sample can be measured, and optical information and concavo-convex information contributing to the classification of foreign matter and defects can be measured, so that foreign matter / defect classification performance is improved.
  • by feeding back these measurement results to the semiconductor manufacturing process conditions it becomes possible to produce a highly reliable semiconductor device with a high yield.
  • FIG. 2 is a front sectional view of a plasmon intensifying near-field probe in Embodiment 1.
  • FIG. FIG. 6 is a front sectional view of a probe in Modification 1 of the plasmon intensifying near-field probe light guide section 200 in Embodiment 1.
  • FIG. 6 is a front sectional view of a probe in a second modification of the plasmon intensifying near-field probe light guide section 200 in the first embodiment.
  • 6 is a front sectional view of a plasmon intensifying near-field probe according to Embodiment 2.
  • FIG. 6 is a front sectional view of a plasmon intensifying near-field probe according to Embodiment 3.
  • FIG. 10 is a front sectional view of a probe in a modification of the plasmon intensifying near-field probe light guide section 200 in the third embodiment.
  • 6 is a front sectional view of a plasmon intensifying near-field probe in Embodiment 4.
  • FIG. 10 is a front sectional view of a plasmon intensifying near-field probe in Embodiment 5.
  • FIG. 1 is a block diagram illustrating a schematic configuration of a scanning probe microscope according to Embodiment 1.
  • FIG. It is the schematic which shows the polarizing axis of a polarizing plate.
  • It is the sample cross section which shows the step-in scanning of a nanotube, and a perspective view of a cantilever.
  • FIG. 6 is a block diagram illustrating a schematic configuration of a scanning probe microscope in Modification 1 of the detection optical system 4000 of Embodiment 1.
  • FIG. 10 is a block diagram illustrating a schematic configuration of a scanning probe microscope in Modification Example 2 of the detection optical system 4000 of Example 1.
  • FIG. 10 is a block diagram illustrating a schematic configuration of a scanning probe microscope in a first modification of the measurement unit 2000 according to the first embodiment. It is the schematic which shows the combination data of the reflected light intensity with respect to each material and each light source wavelength.
  • FIG. 10 is a block diagram illustrating a schematic configuration of a scanning probe microscope in a second modification of the measurement unit 2000 according to the first embodiment.
  • 6 is a block diagram illustrating a schematic configuration of a scanning probe microscope in Embodiment 2.
  • FIG. 6 is a block diagram illustrating a schematic configuration of a scanning probe microscope in Embodiment 3.
  • FIG. 10 is a block diagram showing a schematic configuration of a scanning probe microscope in Example 4.
  • FIG. 10 is a block diagram illustrating a schematic configuration of a scanning probe microscope according to a fifth embodiment. It is a flowchart which shows the procedure which measures the sample surface in Example 1 thru
  • FIG. 10 is a side sectional view of a plasmon intensifying near-field probe light guide cantilever 201 in Example 6. It is sectional drawing of the side surface of the plasmon augmentation near field probe light guide part cantilever 201 modification in Example 6.
  • FIG. 10 is a front sectional view of a gold nanoparticle-filled plasmon enhanced near-field probe in Example 6.
  • 10 is a front sectional view of a gold nanorod-filled plasmon enhanced near-field probe in Example 6.
  • FIG. It is sectional drawing of the front of the plasmon augmentation near-field probe modification in Example 6.
  • 10 is a block diagram showing a schematic configuration of a scanning probe microscope in Example 6.

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WO2014097886A1 (ja) * 2012-12-18 2014-06-26 学校法人早稲田大学 光学デバイスおよび分析装置
JPWO2014097886A1 (ja) * 2012-12-18 2017-01-12 学校法人早稲田大学 光学デバイスおよび分析装置
CN115343835A (zh) * 2022-08-17 2022-11-15 华南师范大学 一种基于镜面干涉场激发非线性荧光的三维各向同性超分辨成像方法及装置

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