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WO2002097409A1 - Procede de reconnaissance automatique et d'analyse et d'identification spectroscopiques de particules - Google Patents

Procede de reconnaissance automatique et d'analyse et d'identification spectroscopiques de particules Download PDF

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Publication number
WO2002097409A1
WO2002097409A1 PCT/EP2002/005779 EP0205779W WO02097409A1 WO 2002097409 A1 WO2002097409 A1 WO 2002097409A1 EP 0205779 W EP0205779 W EP 0205779W WO 02097409 A1 WO02097409 A1 WO 02097409A1
Authority
WO
WIPO (PCT)
Prior art keywords
particle
scattered light
particles
identification
analysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2002/005779
Other languages
German (de)
English (en)
Inventor
Heiko Leonhardt
Ludwig Pohlmann
Lothar Holz
Markus Lankers
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
rap ID Particle Systems GmbH
Original Assignee
rap ID Particle Systems GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by rap ID Particle Systems GmbH filed Critical rap ID Particle Systems GmbH
Priority to DE10292357T priority Critical patent/DE10292357D2/de
Publication of WO2002097409A1 publication Critical patent/WO2002097409A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • G01N21/65—Raman scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/94—Investigating contamination, e.g. dust
    • 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
    • G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
    • G01J3/4412—Scattering spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1468—Optical investigation techniques, e.g. flow cytometry with spatial resolution of the texture or inner structure of the particle
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1434—Optical arrangements
    • G01N2015/1452—Adjustment of focus; Alignment
    • 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
    • G01N21/6456—Spatial resolved fluorescence measurements; Imaging
    • G01N2021/646—Detecting fluorescent inhomogeneities at a position, e.g. for detecting defects
    • 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
    • G01N21/65—Raman scattering
    • G01N2021/653—Coherent methods [CARS]
    • G01N2021/656—Raman microprobe
    • 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
    • G01N21/6456—Spatial resolved fluorescence measurements; Imaging
    • G01N21/6458—Fluorescence microscopy
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/8806—Specially adapted optical and illumination features
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/10—Scanning
    • G01N2201/103—Scanning by mechanical motion of stage
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/10—Scanning
    • G01N2201/108—Miscellaneous
    • G01N2201/1087—Focussed scan beam, e.g. laser

Definitions

  • the present invention relates to a method for the automated detection and spectroscopic identification of particles, in particular particulate contaminants.
  • Charged particles can be electrostatically deposited on surfaces the.
  • Another possibility is the use of impactors with which, in addition to the separation, classification of the particles in size classes is possible, as specified in US Pat. No. 5,343,767 "Low Particle Loss Cascade Impactor".
  • DE 41 11 903 C2 describes a method and a device which is capable of automatically capturing entire areas by Raman spectroscopy.
  • the method disclosed herein it is possible to obtain the simultaneous or sequential recording of a confocal, light microscopic, optical sectional image and a set of spectroscopic intensity distributions, so that on the basis of this information the assigned mean spectrum of the spectroscopic method used can then be specified for each suitably selected section of the optical sectional image.
  • fully automated detection, spectroscopic analysis and identification of particles is not possible with this method.
  • the object of the present invention is to provide a suitable technology for the automated detection and spectroscopic identification of microparticles, in particular in the size range from 0.1 ⁇ m to 100 ⁇ m, which are deposited on smooth surfaces and which is particularly suitable for the use of Raman spectroscopy and the analysis and identification of the particles in a significantly shorter time.
  • the object is achieved by a method according to claim 1.
  • Advantageous embodiments of the invention are specified in the subclaims.
  • a laser beam is scanned over the surface of a sample carrier on which particles have been deposited.
  • the scanning is preferably carried out by a relative movement in the x-y direction between the laser beam and the sample carrier, more preferably by the movement of the sample carrier in the x-y plane with respect to the laser beam.
  • the sample carrier is preferably moved with the aid of stepper motors.
  • a change in the scattered light intensity is detected by at least one scattered light sensor in a defined angular range relative to the filter surface. The intensity of this selectively detected light is characteristic of particles of a certain size. This selectivity can be further increased by using several sensors in different angular positions.
  • This particle-sensitive scattered light triggers an impulse to a software control, which interrupts the scanning process and causes the stepper motors, which perform the described movement, to come to an immediate standstill in order to position the laser focus exactly on the particle and / or the position for an automatic analysis after the completion of the scanning process, in order to first end the scanning process completely and then to control the positions again in order to carry out the signal registration of the light inelastically scattered by the particle for the subsequent spectral analysis.
  • readjustment can be carried out by moving the sample carrier and / or a lens in the y direction until the particle is precisely in the focus of the laser beam.
  • Another signal which is triggered by the change in the scattered light, starts the signal registration of the light inelastically scattered by the particle.
  • This light is freed of its elastic scattered light component with the aid of a filter, spectrally broken down in a spectrometer, preferably a Raman spectrometer, and detected with a detector, for example a CCD camera.
  • the software control sends a signal to the stepper motor control to restart the scanning process.
  • the data obtained during the spectral analysis are automatically sent to a control computer. There the data is automatically smoothed and corrected on the background. Then the experimental data is compared with that of a database and the result is output.
  • sought-after particulate contaminants can be distinguished relatively reliably from surface irregularities of the sample carrier.
  • Figure 1 shows the flow diagram of a measuring process according to the inventive method
  • FIG. 1 b shows the exemplary calculation of the correlation between particle size and signal intensity in an angular range on an aluminum-coated sample carrier
  • FIG. 2 shows the optical detailed structure of a measuring system for carrying out the method according to the invention
  • FIG. 3a shows the relative position of particles on a sample carrier
  • FIG. 3b shows the measuring positions at which a particle measurement has taken place
  • FIG. 4 shows a spectrum of a 4 ⁇ m diamond chip automatically generated by the method according to the invention.
  • FIG. 1 The flow diagram of a measuring process is shown in FIG. 1, the detailed optical structure described is shown in FIG. 2.
  • Laser with a wavelength of 785 nm is used for this experiment.
  • a surface loaded with particles is irradiated with a laser beam 1 and, at the same time, is moved step by step in the xy plane in 0.5 ⁇ m steps using a displacement unit (not shown).
  • the laser light 1 is coupled into a microscope 5 by means of a bandpass filter 2 with the aid of a mirror 3 and a beam splitter 4 and is focused on the surface of the sample carrier 6 with an SLWD objective 5 '.
  • the scattered light is picked up with a probe 7 in approximately 45 ° with an angular range of approximately 16 ° to 74 ° and recorded with a photodiode 8.
  • a change in the scattered light intensity indicates the presence of a searched particle P.
  • the further movement of the displacement unit is interrupted.
  • the objective 5 ' is positioned in the y direction with the aid of a further displacement table, the reflected light being detected by a diode 9. If the position of the maximum intensity is reached, the particle P is in the optimal focus range.
  • the backscattered light from the sample carrier 6 is collected by the same objective 5 ′, coupled into a fiber 10, and the excitation wavelength is filtered out with a notch filter 11.
  • the inelastically scattered light is spectrally split in a Raman spectrometer 12 and the Raman lines are recorded with a detector (not shown).
  • a signal is sent via RS232 to start the Raman measurement of particle P. For this purpose, the dark current is measured.
  • the laser is faded out by a shutter and faded in after the selected integration time and the receiver is initialized.
  • the spectrum obtained is preprocessed in a control computer 16, then compared with the spectra present in the database, and the result, the substance from which the particle is made, is displayed.
  • the device is released for a new measuring cycle.
  • the corresponding solid angle is 0.77 sr.
  • the strength of the scatter signal increases from 0.5 to 5.0 ⁇ m by a factor of 25, which corresponds approximately to a quadratic dependence and is sufficient for differentiating different particle sizes based on the scattered light intensity in the specified angular range.
  • FIGS. 3a, 3b show the result of the particle analysis of an approximately 25 ⁇ 50 ⁇ m area which is loaded with 3-5 ⁇ m diamond chips.
  • the relative position of the particles to one another can be seen in the photo in FIG. 3a.
  • the measurement positions at which a particle measurement took place designate the white squares in FIG. 3b.
  • the measurement time per particle was approx. 5 s.
  • An example of a diamond spectrum can be seen in FIG. 4. From this measurement it can be deduced that the particle recognition registers the particles lying on the surface and records them very quickly spectroscopically.
  • the pure scanning time for the surface under consideration was approx. 10 s.
  • the measurement time for the 27 measurement points was 2 min 15 s.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un procédé de reconnaissance automatique et d'analyse et d'identification spectroscopiques de particules, en particulier d'impuretés particulaires. Selon ce procédé, la surface d'un support d'échantillon sur lequel des particules ont été déposées est balayée à l'aide d'un faisceau laser et l'intensité de la lumière diffusée est continuellement mesurée. Ledit procédé est caractérisé en ce que pour l'analyse et l'identification spectroscopiques de particules, seule la lumière diffusée présentant une sensibilité particulaire et/ou dimensionnelle est détectée dans une zone angulaire prédéfinie par rapport à la surface du support.
PCT/EP2002/005779 2001-05-31 2002-05-24 Procede de reconnaissance automatique et d'analyse et d'identification spectroscopiques de particules Ceased WO2002097409A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE10292357T DE10292357D2 (de) 2001-05-31 2002-05-24 Verfahren zur automatisierten Erkennung, spektroskopischen Analyse und Identifizierung von Partikeln

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10127538.2 2001-05-31
DE10127538 2001-05-31

Publications (1)

Publication Number Publication Date
WO2002097409A1 true WO2002097409A1 (fr) 2002-12-05

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PCT/EP2002/005779 Ceased WO2002097409A1 (fr) 2001-05-31 2002-05-24 Procede de reconnaissance automatique et d'analyse et d'identification spectroscopiques de particules

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DE (1) DE10292357D2 (fr)
WO (1) WO2002097409A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004008762A1 (de) * 2004-02-23 2005-09-08 Erwin Kayser-Threde Gmbh Verfahren und Vorrichtung zur Detektion und zum Identifizieren von Biopartikeln
WO2008020343A3 (fr) * 2006-08-18 2008-04-24 Primus Special Projects Pty Lt Trieuse
NL1039263C2 (nl) * 2011-12-23 2013-06-26 Zevenaar Elektronica & Sensoren B V Apparaat en werkwijze voor het tellen en bemeten van deeltjes.
EP1904826B1 (fr) * 2005-07-14 2019-02-20 Battelle Memorial Institute Systèmes et procédés de détection biologique et chimique
CN110346042A (zh) * 2019-08-01 2019-10-18 南京邮电大学 一种多传感器杂散光消除光谱仪

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0056426A2 (fr) * 1980-10-08 1982-07-28 Firma Carl Zeiss Dispositif pour la représentation de paramètres d'un échantillon
US4766324A (en) * 1987-08-07 1988-08-23 Tencor Instruments Particle detection method including comparison between sequential scans
DE4111903A1 (de) * 1991-04-12 1992-10-15 Bayer Ag Spektroskopiekorrelierte licht-rastermikroskopie
EP0685731A1 (fr) * 1994-06-02 1995-12-06 Mitsubishi Denki Kabushiki Kaisha Méthode et appareil pour déterminer la position et analyser des particules contaminantes
DE19946110C1 (de) * 1999-09-17 2001-02-01 Apsys Advanced Particle System Optisches Verfahren zur Charakterisierung von Partikeln in einem System, z.B. einem Reinraum, und Vorrichtung zur Durchführung des Verfahrens

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0056426A2 (fr) * 1980-10-08 1982-07-28 Firma Carl Zeiss Dispositif pour la représentation de paramètres d'un échantillon
US4766324A (en) * 1987-08-07 1988-08-23 Tencor Instruments Particle detection method including comparison between sequential scans
DE4111903A1 (de) * 1991-04-12 1992-10-15 Bayer Ag Spektroskopiekorrelierte licht-rastermikroskopie
EP0685731A1 (fr) * 1994-06-02 1995-12-06 Mitsubishi Denki Kabushiki Kaisha Méthode et appareil pour déterminer la position et analyser des particules contaminantes
DE19946110C1 (de) * 1999-09-17 2001-02-01 Apsys Advanced Particle System Optisches Verfahren zur Charakterisierung von Partikeln in einem System, z.B. einem Reinraum, und Vorrichtung zur Durchführung des Verfahrens

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004008762A1 (de) * 2004-02-23 2005-09-08 Erwin Kayser-Threde Gmbh Verfahren und Vorrichtung zur Detektion und zum Identifizieren von Biopartikeln
DE102004008762B4 (de) * 2004-02-23 2006-10-12 Erwin Kayser-Threde Gmbh Verfahren und Vorrichtung zur Detektion und zum Identifizieren von Biopartikeln
EP1904826B1 (fr) * 2005-07-14 2019-02-20 Battelle Memorial Institute Systèmes et procédés de détection biologique et chimique
WO2008020343A3 (fr) * 2006-08-18 2008-04-24 Primus Special Projects Pty Lt Trieuse
NL1039263C2 (nl) * 2011-12-23 2013-06-26 Zevenaar Elektronica & Sensoren B V Apparaat en werkwijze voor het tellen en bemeten van deeltjes.
CN110346042A (zh) * 2019-08-01 2019-10-18 南京邮电大学 一种多传感器杂散光消除光谱仪
CN110346042B (zh) * 2019-08-01 2022-03-08 南京邮电大学 一种多传感器杂散光消除光谱仪

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