WO2011136317A1 - Échantillon de référence pour l'étalonnage d'un spectromètre d'émission à ultraviolets sous vide à excitation par faisceau électronique - Google Patents

Échantillon de référence pour l'étalonnage d'un spectromètre d'émission à ultraviolets sous vide à excitation par faisceau électronique Download PDF

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Publication number
WO2011136317A1
WO2011136317A1 PCT/JP2011/060354 JP2011060354W WO2011136317A1 WO 2011136317 A1 WO2011136317 A1 WO 2011136317A1 JP 2011060354 W JP2011060354 W JP 2011060354W WO 2011136317 A1 WO2011136317 A1 WO 2011136317A1
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Prior art keywords
vacuum ultraviolet
emission
electron beam
sample
calibration
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PCT/JP2011/060354
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English (en)
Japanese (ja)
Inventor
知史 長見
伸仁 飯田
敏尚 須山
健太郎 福田
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株式会社トクヤマ
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Publication of WO2011136317A1 publication Critical patent/WO2011136317A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/244—Detectors; Associated components or circuits therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J2003/2866—Markers; Calibrating of scan
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/244—Detection characterized by the detecting means
    • H01J2237/2445—Photon detectors for X-rays, light, e.g. photomultipliers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H01J2237/2803—Scanning microscopes characterised by the imaging method
    • H01J2237/2808—Cathodoluminescence
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/282—Determination of microscope properties
    • H01J2237/2826—Calibration

Definitions

  • the present invention relates to a standard sample for calibration of a vacuum ultraviolet light emission measuring apparatus using low energy electron beam excitation.
  • UV light is generally referred to as UV light and is widely used for lighting, pest control, resin curing, and the like.
  • deep ultraviolet light having a wavelength of 200 to 350 nm
  • vacuum ultraviolet light having a wavelength of 200 nm or less.
  • Deep ultraviolet rays are expected to be used in fields such as sterilization and water purification, various medical fields, high-density recording fields, high color rendering light-emitting diode lighting fields, and decomposition fields of pollutants in combination with photocatalysts. ing.
  • vacuum ultraviolet rays are light with a shorter wavelength, they are said to be the core of the next-generation semiconductor manufacturing process and are also expected as light emitting materials.
  • Known materials that emit deep ultraviolet light include diamond, hexagonal boron nitride, and aluminum nitride that emit light by electron beam excitation.
  • a solid light emitting material such as deep ultraviolet light has not been developed as a material for emitting vacuum ultraviolet light, and a deuterium lamp, a laser using fluorine gas, or the like is used.
  • this type of light source has problems in life, stability, and economy, and development of solid light emitting materials has been expected as visible light has changed from incandescent bulbs to solid light emitting materials.
  • a typical method of emitting vacuum ultraviolet light with a solid light emitting material is a method of exciting with radiation such as X-rays or ⁇ rays having very high energy.
  • the emission wavelength is in the vacuum ultraviolet region.
  • the light emission conditions are almost the same as those at the time of sample measurement.
  • the physical properties are stable and there is no change in emission wavelength or intensity.
  • the rise of the emission spectrum is clear and the amount of emitted light can be easily integrated.
  • the shape of the spectrum of the emitted light is sharp and the emission wavelength can be easily specified. In particular, it is necessary to adjust the optical system because the emitted light passes through the same optical system as the sample and is used instead of the sample or together with the sample. is there.
  • the emission wavelength is in the vacuum ultraviolet region because the refractive index varies depending on the wavelength when a transparent window material or lens is used in the vacuum ultraviolet region in the optical system.
  • the present invention shows that the electron-beam-excited luminescence detection apparatus for the vacuum ultraviolet region is normal, and is a standard sample for calibration that serves as a reference for quantitative comparison of the luminescence intensity of samples and quantification of elements that contribute to luminescence.
  • the purpose is to provide.
  • the inventors of the present invention have intensively studied to solve such problems related to calibration of the vacuum ultraviolet SEM-CL.
  • the vacuum ultraviolet light is sufficiently emitted by electron beam excitation, satisfying the characteristics required for calibration standard samples for electron beam excited vacuum ultraviolet light emission measuring devices, such as no change due to electron beam irradiation or change over time.
  • the present inventors have completed the present invention.
  • the present invention relates to a calibration standard sample for an electron beam-excited vacuum ultraviolet light emission measuring device made of an oxide crystal having a band gap energy of 6.2 eV or more, and an electron beam-excited vacuum ultraviolet light emission intensity using the calibration standard sample. And a wavelength calibration method for an electron beam excited vacuum ultraviolet light emission measuring device.
  • the calibration standard sample for the electron beam-excited vacuum ultraviolet emission measuring device of the present invention sufficiently emits vacuum ultraviolet light by electron beam excitation, and there is no change due to electron beam irradiation or change over time.
  • a calibration standard sample for an excitation vacuum ultraviolet emission measuring device measurement of a vacuum ultraviolet spectrum by electron beam excitation emission and acquisition of an electron beam excitation emission image can be stably and reproducibly performed with a simple method.
  • the calibration standard sample for the electron beam excited vacuum ultraviolet emission measuring device of the present invention is not limited to the SEM-CL for vacuum ultraviolet region, but can be used as a calibration standard sample in the spectral analysis of all electron beam excited vacuum ultraviolet emission. can do.
  • This figure is a schematic diagram of an example of SEM-CL for vacuum ultraviolet region to which the present invention is applied.
  • This figure is an example of a CL spectrum of the calibration standard sample of the present invention.
  • This figure is an example of the change with time of the emission intensity when the magnesium oxide crystal is continuously irradiated with the electron beam.
  • This figure is an example of the daily fluctuation of the emission intensity of the magnesium oxide crystal.
  • This figure is an example of the change over time of the emission intensity when the aluminum oxide crystal is continuously irradiated with the electron beam.
  • This figure is an example of the daily fluctuation of the emission intensity of the aluminum oxide crystal.
  • This figure shows an example of a calibration curve based on emission intensity measured by changing the amount of Nd added to the LaF 3 crystal.
  • This figure is an example of the change over time of the light emission intensity when the silicon dioxide crystal is continuously irradiated with the electron beam.
  • This figure is an example of how to determine the peak position of a silicon dioxide crystal used for wavelength calibration.
  • FIG. 1 shows a schematic diagram of an SEM-CL for vacuum ultraviolet region as an example of an electron beam excited vacuum ultraviolet light emission measuring apparatus that calibrates by applying a calibration standard sample of the present invention.
  • the vacuum ultraviolet SEM-CL is composed of a scanning electron microscope section and a spectroscope chamber, and the scanning electron microscope section is provided with a condensing mirror.
  • a vacuum ultraviolet light emitting sample is held in a low vacuum atmosphere of 1 to 300 Pa in an electron microscope, and the sample is irradiated with a low energy electron beam of 1 to 30 kV and excited by the low energy electron beam to have a wavelength of 200 nm or less.
  • the light containing the vacuum ultraviolet light is emitted, and then the emitted light is transmitted to the spectroscope chamber by a condenser mirror.
  • the emitted light transmitted to the spectroscope chamber is condensed on the diffraction grating and is separated by wavelength by the diffraction grating.
  • the vacuum ultraviolet rays dispersed by the diffraction grating are detected by a detector such as a CCD.
  • the scanning electron microscope section and the spectroscope chamber are connected by a window material or a condenser lens made of a material transparent to vacuum ultraviolet rays such as pinholes and MgF 2 .
  • a window material or a condenser lens made of a material transparent to vacuum ultraviolet rays such as pinholes and MgF 2 .
  • the vacuum ultraviolet light generated in the sample is attenuated.
  • some fluorides are sensitive to electron beams, and hydrogen fluoride generated by electron beams may corrode a condensing mirror and the like, and gradually weaken vacuum ultraviolet light.
  • the relationship between the diffraction grating and the detector goes wrong, the emission wavelength will go wrong.
  • an oxide crystal having a band gap energy of 6.2 eV or more is used as a calibration standard sample.
  • Oxide crystals are ceramics and are stable solid compounds that are not altered during storage due to oxidation or decomposition reactions, and are damaged by electron beam irradiation, resulting in changes in composition and crystal structure, resulting in emission intensity and emission wavelength. Does not change. Further, the rise of the emission spectrum is clear and the amount of emitted light can be easily integrated, the shape of the spectrum of the emitted light beam is sharp, and the emission wavelength can be easily specified.
  • the emission wavelength by electron beam excitation is in the vacuum ultraviolet region, and it can be used under the same measurement conditions as the sample.
  • Examples of the oxide crystal having a band gap energy of 6.2 eV or more include a lithium oxide crystal, a beryllium oxide crystal, a boron oxide crystal, a magnesium oxide crystal, an aluminum oxide crystal, a silicon dioxide crystal, and a calcium oxide crystal. .
  • magnesium oxide crystals, aluminum oxide crystals, and silicon dioxide crystals are suitable as standard samples for calibration for electron beam-excited vacuum ultraviolet emission measuring devices because they are stable in air and high-quality single crystals are easily available.
  • These crystals are not particularly limited in shape, purity, and crystallinity in use, but are desirably high-purity single crystals because of their high emission intensity and easy handling.
  • the state of the electron beam excitation vacuum ultraviolet emission measuring device can be checked by measuring the spectrum of the vacuum ultraviolet emission light using the calibration standard sample of the present invention. For example, if there is a deviation in the emission wavelength due to an error in the relationship between the diffraction grating and the detector, the emission spectrum measured using the calibration standard sample of the present invention and the peak wavelength are shifted in a normal state, thereby detecting the abnormality. Can do. If the relationship between the diffraction grating and the detector is distorted as described above, the emission intensity can be calibrated by adjusting the relationship between the diffraction grating and the detector. Based on the peak wavelength of the emission spectrum of the sample, the wavelength of the electron beam excited vacuum ultraviolet light emission measuring device can be calibrated.
  • silicon oxide has two sharp peaks in the vacuum ultraviolet region among oxide crystals having a band gap energy of 6.2 eV or more.
  • the calibration standard sample of the present invention it is possible to calibrate the emission intensity of the electron beam excited vacuum ultraviolet light emission measuring device. For example, if the optical system goes wrong and the sensitivity is reduced, the photon count value of each wavelength of the emission spectrum measured under the same conditions as that measured using the calibration standard sample of the present invention under normal conditions, You can know the abnormality. In this way, when a deviation occurs in the optical system, the emission intensity can be calibrated by adjusting the optical system. In addition, when the optical system adjustment cannot be solved easily, such as when the collector mirror is corroded, the sensitivity of the device is corrected based on the emission intensity of the calibration standard sample of the present invention under normal conditions. You can also
  • the ratio I 0 / I C of the emission intensity I 0 of each wavelength of the vacuum ultraviolet emission spectrum at the normal time and the emission intensity I C of each wavelength of the vacuum ultraviolet emission spectrum at the time of calibration of the standard sample for calibration of the present invention Using this as a correction coefficient, the corrected emission intensity of the measurement sample can be obtained by multiplying the emission intensity of each wavelength of the vacuum emission spectrum of the measurement sample by the correction coefficient of each wavelength.
  • the calibration standard sample of the present invention as the emission intensity reference, it is possible to quantitatively measure the electron beam excited vacuum ultraviolet emission intensity between samples having different measurement conditions.
  • the measurement conditions such as the electron beam current value and measurement time are changed according to the measurement sample, excluding the measurement conditions such as acceleration voltage that are affected by the substance.
  • the calibration standard sample of the present invention is also measured under the measurement conditions of each measurement sample, and the ratio of the emission intensity between the measurement sample and each wavelength of the calibration standard sample of the present invention (emission intensity of the measurement sample / calibration standard).
  • the emission wavelength region of the calibration standard sample of the present invention preferably includes the emission wavelength of the sample.
  • the calibration standard sample is mounted on the sample stage together with the sample and measured under the same conditions before and after the sample is measured.
  • the calibration standard sample of the present invention it is possible to perform quantitative measurement of electron beam excited vacuum ultraviolet emission intensity between samples having different measurement conditions as described above, so that it is contained in the measurement sample. Quantification of the additive can be easily performed.
  • the electron beam excitation vacuum ultraviolet emission intensity and the element concentration added to contribute to electron beam excitation vacuum ultraviolet emission have a correlation. This makes it possible to quantify the amount of element added to the sample that contributes to a small amount of light emission.
  • a time-consuming operation for sample preparation such as wet analysis-ICP-emission analysis is required.
  • the ratio of the electron beam excitation vacuum ultraviolet emission intensity of the measurement sample and the calibration standard sample obtained by quantitative measurement by measuring the calibration standard sample with the measurement sample before and after the measurement (measurement sample).
  • FIG. 2 shows a vacuum ultraviolet emission spectrum of the magnesium oxide crystal by electron beam excitation, measured using the vacuum ultraviolet SEM-CL shown in FIG.
  • the magnesium oxide crystal a single crystal (manufactured by MTI) grown by electrofusion was mirror-polished. No conductive coating treatment was applied to the magnesium oxide crystals.
  • the SEM-CL for the vacuum ultraviolet region the scanning electron microscope body is SU-6600 scanning electron microscope manufactured by Hitachi High-Technologies Corporation, CCD is DU420-BN type manufactured by Andor Technology, and the diffraction grating is 1200 / mm. used.
  • the measurement conditions were an acceleration voltage of 20 kV, an irradiation current of 430 pA, a measurement time of 5 seconds, a temperature of 300 K, and a vacuum degree of the sample chamber of 80 Pa.
  • FIG. 3 shows the time-dependent change in emission intensity when the same magnesium oxide crystal as used in the vacuum ultraviolet emission spectrum measurement is used and the magnesium oxide crystal is continuously irradiated with an electron beam for 20 minutes under the same measurement conditions except for the measurement time. Indicated.
  • the integrated value of the count number of photons having a peak wavelength of 170 nm ⁇ 1 nm at which the emission intensity of the magnesium oxide crystal is maximized is taken as the emission intensity, and the emission intensity at the start of the measurement is taken as 100%.
  • the emission intensity of the magnesium oxide crystal when measured once a day for 5 days under the same measurement conditions as the vacuum ultraviolet emission spectrum measurement. The variation is shown in FIG. In FIG.
  • the integrated value of the count number of photons having a peak wavelength of 170 nm ⁇ 1 nm that maximizes the emission intensity of the magnesium oxide crystal is taken as the emission intensity, and the emission intensity on the first day is set as 100%. From the above examples, it can be said that the magnesium oxide crystal has a small variation in emission intensity and is suitable as a standard sample for calibration.
  • the magnesium oxide crystal emits light at a wavelength of 170 nm to 200 nm, and can be used as a reference for the emission intensity of 170 nm to 200 nm.
  • Example 2 The vacuum ultraviolet emission spectrum by electron beam excitation measured in the same manner as in Example 1 except that an aluminum oxide single crystal (manufactured by MTI) grown by the Czochralski method was used as the oxide crystal is shown in FIG.
  • FIG. 5 shows the time-dependent change of the luminescence intensity when the irradiation is continued
  • FIG. 6 shows the daily fluctuation of the luminescence intensity.
  • the integral value of the count number of photons having a peak wavelength of 170 nm ⁇ 1 nm at which the emission intensity of the aluminum oxide crystal is maximized is taken as the emission intensity, and the emission intensity at the start of the measurement is set to 100%.
  • FIG. 5 shows the time-dependent change of the luminescence intensity when the irradiation is continued
  • FIG. 6 shows the daily fluctuation of the luminescence intensity.
  • the integral value of the count number of photons having a peak wavelength of 170 nm ⁇ 1 nm at which the emission intensity of the aluminum oxide crystal is maximized is taken
  • the integrated value of the count number of photons having a peak wavelength of 170 nm ⁇ 1 nm that maximizes the emission intensity of the aluminum oxide crystal is taken as the emission intensity, and the emission intensity on the first day is set as 100%. From the above examples, it can be said that the aluminum oxide crystal has a small variation in emission intensity and is suitable as a calibration standard sample.
  • the aluminum oxide crystal emits light at 150 nm to 190 nm, and can be used as a reference for the emission intensity of 150 nm to 190 nm.
  • Example 3 Using calibration standard sample of the present invention shows quantitative example of Nd content in LaF 3.
  • the ratio of the electron beam excited vacuum ultraviolet emission intensity of the sample was determined.
  • the magnesium oxide crystal of Example 1 was used as the calibration standard sample.
  • the Nd concentration of the LaF 3 crystal containing Nd was quantified using the calibration curve method by wet analysis-ICP-emission analysis method after decomposing the same sample whose luminescence intensity was measured by the alkali melting method.
  • the vertical axis represents the emission intensity ratio of 173 nm electron-excited vacuum ultraviolet light emission between LaF 3 crystals containing different concentrations of Nd and the calibration standard sample
  • the horizontal axis represents the quantitative value of the Nd concentration of each sample.
  • the calibration curve obtained is shown in FIG. In other words, by quantitatively measuring the emission intensity ratio using a calibration standard sample, once the correlation between the element concentration contributing to the emission and the emission intensity ratio is obtained, the emission intensity ratio can be easily determined from the next. The Nd content of can be calculated.
  • Example 4 An electron beam measured in the same manner as in Example 1 except that a silicon dioxide single crystal (manufactured by MTI) grown by a hydrothermal method was used as the oxide crystal, and the irradiation current was 2 nA and the measurement time was 15 seconds as measurement conditions.
  • the vacuum ultraviolet emission spectrum by excitation is shown in FIG. FIG. 8 shows the change over time in the emission intensity when the electron beam is continuously irradiated for 20 minutes.
  • the emission intensity of the silicon dioxide crystal is the integrated value of the count number of photons having a peak wavelength of 150 nm ⁇ 1 nm and the integrated value of the count number of photons having a peak wavelength of 175 nm ⁇ 1 nm. Based on the emission intensity, it was set to 100%.
  • the emission peak wavelength was defined as the peak wavelength at the center of the two inflection points of each peak.
  • FIG. 8 and Table 1 show that silicon dioxide has a small variation in emission peak wavelength and is suitable as a standard sample for wavelength calibration.
  • wavelength calibration of an electron beam excited vacuum ultraviolet emission measuring device such as SEM-CL for vacuum ultraviolet region can be performed.

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Abstract

L'invention concerne un échantillon de référence pour l'étalonnage, qui indique qu'un détecteur d'émission à excitation par faisceau électronique pour la région à ultraviolets sous vide est normal et sert de référence dans la comparaison quantitative des intensités d'émission des échantillons ou la quantification d'un élément contribuant à l'émission. L'invention concerne un échantillon de référence pour l'étalonnage d'un spectromètre d'émission à ultraviolets sous vide à excitation par faisceau électronique, ledit échantillon de référence comprenant des cristaux d'oxyde ayant une énergie de bande interdite de 6,2 eV ou plus ; et un procédé pour mesurer quantitativement une intensité d'émission à ultraviolets sous vide à excitation par faisceau électronique, qui comprend la mesure des intensités des émissions à ultravioletss sous vide à excitation par faisceau électronique d'un échantillon d'essai et ledit échantillon de référence pour l'étalonnage dans les mêmes conditions de mesure, et déterminer le rapport d'intensité d'émission de l'échantillon d'essai sur l'échantillon de référence pour l'étalonnage (c'est-à-dire, intensité d'émission de l'échantillon d'essai/ d'intensité d'émission de l'échantillon de référence pour l'étalonnage).
PCT/JP2011/060354 2010-04-28 2011-04-28 Échantillon de référence pour l'étalonnage d'un spectromètre d'émission à ultraviolets sous vide à excitation par faisceau électronique WO2011136317A1 (fr)

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CN103175607A (zh) * 2013-02-28 2013-06-26 北京振兴计量测试研究所 一种真空紫外光谱辐照度标定方法及系统
EP3081921B1 (fr) * 2015-04-16 2019-08-14 Heraeus Electro-Nite International N.V. Procédé d'étalonnage de spectromètre

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Publication number Priority date Publication date Assignee Title
US9711255B2 (en) 2015-01-16 2017-07-18 Stanley Electric Co., Ltd Ultraviolet-emitting material and ultraviolet light source

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103175607A (zh) * 2013-02-28 2013-06-26 北京振兴计量测试研究所 一种真空紫外光谱辐照度标定方法及系统
EP3081921B1 (fr) * 2015-04-16 2019-08-14 Heraeus Electro-Nite International N.V. Procédé d'étalonnage de spectromètre

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