WO2002097409A1 - Verfahren zur automatisierten erkennung, spektroskopischen analyse und identifizierung von partikeln - Google Patents
Verfahren zur automatisierten erkennung, spektroskopischen analyse und identifizierung von partikeln Download PDFInfo
- 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
Links
- 239000002245 particle Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000004611 spectroscopical analysis Methods 0.000 title claims abstract description 8
- 238000001514 detection method Methods 0.000 claims description 10
- 238000011109 contamination Methods 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 7
- 238000001069 Raman spectroscopy Methods 0.000 claims description 6
- 238000010183 spectrum analysis Methods 0.000 claims description 6
- 230000010354 integration Effects 0.000 claims description 3
- 230000001960 triggered effect Effects 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 abstract description 5
- 239000000523 sample Substances 0.000 description 14
- 238000005259 measurement Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 208000034809 Product contamination Diseases 0.000 description 1
- 238000003841 Raman measurement Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
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
Description
Claims
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 | 2001-05-31 | ||
DE10127538.2 | 2001-05-31 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002097409A1 true WO2002097409A1 (de) | 2002-12-05 |
Family
ID=7687430
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2002/005779 WO2002097409A1 (de) | 2001-05-31 | 2002-05-24 | Verfahren zur automatisierten erkennung, spektroskopischen analyse und identifizierung von partikeln |
Country Status (2)
Country | Link |
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DE (1) | DE10292357D2 (de) |
WO (1) | WO2002097409A1 (de) |
Cited By (5)
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 |
WO2008020343A2 (en) * | 2006-08-18 | 2008-02-21 | Primus Special Projects (Pty) Ltd | A sorter |
NL1039263C2 (nl) * | 2011-12-23 | 2013-06-26 | Zevenaar Elektronica & Sensoren B V | Apparaat en werkwijze voor het tellen en bemeten van deeltjes. |
EP1904826B1 (de) * | 2005-07-14 | 2019-02-20 | Battelle Memorial Institute | Systeme und verfahren für den biologischen und chemischen nachweis |
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)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0056426A2 (de) * | 1980-10-08 | 1982-07-28 | Firma Carl Zeiss | Vorrichtung zur Darstellung von Probenparametern |
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 (de) * | 1994-06-02 | 1995-12-06 | Mitsubishi Denki Kabushiki Kaisha | Methode und Gerät zur Lagebestimmung und Analyse von feinem Fremdmaterial |
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 |
-
2002
- 2002-05-24 WO PCT/EP2002/005779 patent/WO2002097409A1/de not_active Application Discontinuation
- 2002-05-24 DE DE10292357T patent/DE10292357D2/de not_active Ceased
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0056426A2 (de) * | 1980-10-08 | 1982-07-28 | Firma Carl Zeiss | Vorrichtung zur Darstellung von Probenparametern |
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 (de) * | 1994-06-02 | 1995-12-06 | Mitsubishi Denki Kabushiki Kaisha | Methode und Gerät zur Lagebestimmung und Analyse von feinem Fremdmaterial |
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 (8)
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 (de) * | 2005-07-14 | 2019-02-20 | Battelle Memorial Institute | Systeme und verfahren für den biologischen und chemischen nachweis |
WO2008020343A2 (en) * | 2006-08-18 | 2008-02-21 | Primus Special Projects (Pty) Ltd | A sorter |
WO2008020343A3 (en) * | 2006-08-18 | 2008-04-24 | Primus Special Projects Pty Lt | A sorter |
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 |
Also Published As
Publication number | Publication date |
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DE10292357D2 (de) | 2004-07-01 |
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