WO2000054030A2 - Spectrometre calorimetrique integre - Google Patents

Spectrometre calorimetrique integre Download PDF

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Publication number
WO2000054030A2
WO2000054030A2 PCT/US2000/006075 US0006075W WO0054030A2 WO 2000054030 A2 WO2000054030 A2 WO 2000054030A2 US 0006075 W US0006075 W US 0006075W WO 0054030 A2 WO0054030 A2 WO 0054030A2
Authority
WO
WIPO (PCT)
Prior art keywords
micro
instrument
substrate
semiconductor layer
groove
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/US2000/006075
Other languages
English (en)
Other versions
WO2000054030A3 (fr
Inventor
Slobodan Rajic
Panagiotis George Datskos
Marybeth Egert
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.)
UT Battelle LLC
Lockheed Martin Energy Research Corp
Original Assignee
UT Battelle LLC
Lockheed Martin Energy Research Corp
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 UT Battelle LLC, Lockheed Martin Energy Research Corp filed Critical UT Battelle LLC
Priority to AU51219/00A priority Critical patent/AU5121900A/en
Publication of WO2000054030A2 publication Critical patent/WO2000054030A2/fr
Publication of WO2000054030A3 publication Critical patent/WO2000054030A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • G01J3/30—Measuring the intensity of spectral lines directly on the spectrum itself
    • G01J3/36—Investigating two or more bands of a spectrum by separate detectors
    • 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
    • G01J3/02—Details
    • G01J3/0256—Compact construction
    • G01J3/0259—Monolithic
    • 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
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/38—Radiation pyrometry, e.g. infrared or optical thermometry using extension or expansion of solids or fluids
    • G01J5/40—Radiation pyrometry, e.g. infrared or optical thermometry using extension or expansion of solids or fluids using bimaterial elements
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/171—Systems in which incident light is modified in accordance with the properties of the material investigated with calorimetric detection, e.g. with thermal lens detection
    • 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
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/60—Radiation pyrometry, e.g. infrared or optical thermometry using determination of colour temperature
    • G01J5/601—Radiation pyrometry, e.g. infrared or optical thermometry using determination of colour temperature using spectral scanning

Definitions

  • This invention relates to the field of calo ⁇ met ⁇ c spectroscopy, and m particular, to an integrated calo ⁇ met ⁇ c spectrometer embodied as a micro-instrument integrated on a semiconductor substrate
  • Gravimet ⁇ c that is mass based, sensor technologies such as surface acoustic wa ⁇ e devices, quartz crystal micro-balances, micro-cantilever chemical detectors, and the like, sometimes
  • Chemical analysis has been undertaken in a number of different ways, including spectral analysis and thermal analysis.
  • An apparatus used in spectral analysis is the
  • a monochromator is a device for isolating a narrow portion of a spectrum.
  • Apparatus which can be used as thermal detectors in thermal analysis include, for example,
  • bolometers thermopiles, pyroelectrics and micro-cantilevers.
  • a bolometer for example, is a very sensitive thermometer whose electrical resistance varies with temperature and which is used in the detection and measurement of feeble thermal radiation.
  • Bolometers have been especially useful in the study of infrared spectra.
  • a monochromator and a thermal infrared detector array, for example, a micro-
  • Such a chemical sensor can detect the presence of minute amounts of chemical analytes, for example less than parts per trillion (ppt), with increased selectivity by allowing a simultaneous determination of the
  • a thermal detector surface is provided with an active detector surface of individual sensing elements coated with an appropriate chemical layer having an affinity for a family or
  • thermal detector for example, its electrical resistance will change during the measurement
  • wavelength region with the aid of a monochromator or other tunable sources including, for
  • the passive sampling is not selective and can be measured only in real time, the passive sampling can act as a trigger for the active sampling.
  • the thermal detector surface can be regenerated after the test, for example by ohmic
  • a two dimensional waveguide micro-instrument has all of the necessary components integrated on the same semiconductor substrate, namely: an
  • IR infrared
  • Control circuitry can also be integrated on the substrate, for example onto the side opposite
  • the IR source can be an IR receiving channel for an IR source off of the substrate or direct source on the substrate.
  • Micro-cantilevers, micro-bolometers and micro- balances can be integrally formed on the substrate or can be formed separately and bonded to
  • the substrate for example adhesively bonded.
  • adhesively bonded is the solution to
  • a micro-instrument for detecting a chemical comprises: a semiconductor substrate; a waveguide formed by a
  • the waveguide semiconductor layer disposed on the substrate, the waveguide semiconductor layer having an
  • thermal detectors attached to the substrate, each of the thermal detectors having a measurable characteristic physical parameter and each of the thermal detectors having a characteristic chemistry exhibiting a preferential adsorption of at least one chemical to be sensed; and, a
  • each of the thermal detectors receiving different wavelengths of the monochromatic spectrum.
  • the micro-instrument can further comprise control circuitry formed integrally with
  • the substrate on a side of the substrate opposite the waveguide semiconductor layer
  • At least the waveguide semiconductor layer can have a groove, one end of the groove
  • Another end of the groove is open for receiving the polychromatic radiation from a source external to the instrument.
  • the micro-instrument can further comprise a source of the polychromatic radiation disposed in the groove.
  • a micro-bridge can extend across the
  • the micro-bridge having a coating, for example tungsten, which emits the
  • the micro-instrument can further comprise a thermal barrier, for example a coating, between the waveguide semiconductor layer and the source of the polychromatic radiation
  • the array of micro-mechanical thermal detectors can be formed integrally with the substrate or can be formed from at least one different substrate material and bonded in position.
  • the self focusing dispersion element can comprise a self focusing reflection grating.
  • Figure 1 is a perspective view of a chemical detection micro-instrument in accordance
  • Figures 2 and 3 illustrate alternative embodiments for forming and integrating micro-
  • FIGS 4 and 5 illustrate respective micro-mechanical thermal detectors which can be
  • Figure 6 is a diagrammatic representation of a chemical detector, useful for
  • a chemical detector which is not a micro-instrument in accordance with the inventive
  • numeral 10 comprises a broad band light source 12, a monochromator 14 and an array 16 of
  • thermo sensing elements for example thermal sensing elements.
  • Broad band is defined as
  • the array forms a thermal infrared detector array and can be embodied as a
  • Chemical detector 10 can detect the presence of minute amounts of chemical analytes, for example less than parts per trillion (ppt), with increased selectivity by allowing a simultaneous determination of the identity of the unknown species.
  • ppt parts per trillion
  • the thermal detector array 16 comprises a plurality of individual sensing elements 18, 20, 22, . . . , 24.
  • the individual sensing elements are provided with respective active detector surfaces 26, 28, 30, . . . , 32 coated with an appropriate chemical layer having an affinity for the family or group of the target chemical or chemicals.
  • a layer of gold for a first example,
  • silica or platinum or other gas chromatograph coating for a second example, can be utilized for detecting trinitrotoluene (TNT).
  • TNT trinitrotoluene
  • the use of highly selective chemical coatings is not required.
  • the application of the chemical layer corresponds to a first step of a method.
  • the sensing elements have respective read out terminals 34, 36, 38, . . . , 40, but are
  • the sensing elements have a characteristic physical parameter which can be measured. In the case of a bolometer, for example, this parameter is electrical resistance. In the case of a micro-cantilever, for
  • this parameter is the amount of bending.
  • the read out terminals provide respective electrical signals representative of the physical parameter of the individual sensing elements.
  • the array 16 can be placed into a chamber 46, into which a sample is drawn through an inlet or opening 48 defined by a valve 50, shown diagrammatically by a conical ring.
  • thermal detectors If a micro-bolometer is used as the thermal detector, for example, its electrical resistance will change during the adso ⁇ tion. If a micro-cantilever is used as the
  • thermopile array for example, its bending characteristics will change during the adso ⁇ tion. If a thermopile array is used as the thermal detector, for example, its voltage will change
  • thermo detector for example, its
  • Exposing the sensing elements to the sample, in a chamber as described, or otherwise, is a further method step.
  • a photothermal spectrum can be obtained for the chemicals adsorbed on the surfaces of the sensing elements by scanning a broad band wavelength region with the aid of the broad band light source 12 and the
  • the monochromator 14 directs different directions
  • the monochromator generates a monochromatic spectrum responsive to te polychromatic source.
  • the array 16 can be removed from the chamber 46 or the chamber 46 can be
  • light of wavelength ⁇ 2 is directed from the monochromator 14 to detector 20 and light of
  • wavelength ⁇ 3 is directed from the monochromator 14 to detector 18.
  • the temperature of those particular detector pixels will rise proportionally to the
  • this spectrum is based on the respective resistance changes of the individual sensing elements. If the sensor utilizes micro-cantilevers, for example, this spectrum is based on the respective bending characteristics of the individual sensing elements.
  • the detection resolution depends on the quality of the optical system and the density and number of thermal
  • the thermal detector surface formed by the sensing elements, can be regenerated by heating the array 16.
  • One alternative, for example, is by focusing the
  • a micro-instrument 100 based on the underlying principles explained in connection with Figure 6, but in accordance with the inventive arrangements taught herein, is shown in
  • the instrument 100 is embodied on a silicon semiconductor chip or substrate 102.
  • the chip is illustrated as substantially square, but can be other shapes.
  • the chip is coin-sized,
  • the dimensions can be expected to decrease as integration technology improves.
  • the instrument comprises a plurality of components, which are formed integrally on the chip 102. These components include a source 104 of polychromatic light, a dispersive
  • the source 104 of polychromatic light is preferably an infrared (IR) source.
  • the source 104 is formed in part by a groove 112, for example a v-shaped groove, which extends
  • portion 116 of the side edge of the waveguide layer 106 to define an input aperture to the
  • a free standing micro-bridge 118 can be etched into a thermal barrier 120 can be the structural component of an IR micro-source. The thermal barrier is preferably applied
  • the IR source and waveguide monochromator will be located on the IR source and waveguide monochromator.
  • the IR source and waveguide monochromator will be located on the IR source and waveguide monochromator.
  • Polychromatic light that enters the waveguide through aperture 116 will be dispersed by the self focusing reflection grating into a monochromatic spectrum falling onto the array of micro-mechanical detectors, each of the detectors receiving radiation
  • micro-mechanical thermal detectors can include, for example, micro-cantilevers, micro-bolometers and micro-balances.
  • the array 108 of micro-mechanical thermal detectors can include, for example, micro-cantilevers, micro-bolometers and micro-balances.
  • micro-mechanical detectors can be integrally
  • the detectors are so thin, for example as thin as 0.5 microns, that
  • Suitable substrates for the thermal detectors in the array can include, for example, Ge, GaAs, InAs, InP, InSb, InGaAs, HgCdTe, SiC and GaN.
  • the dispersive self focusing waveguide 106 can comprise a self focusing reflection
  • Control circuitry 109 can be disposed on the same substrate 102, but on the opposite side of the components noted above.
  • the micro-instrument will be capable of detecting many
  • micro-instrument is similar to the operation of the calorimetric spectrometer 1_0 explained in connection with Figure 6. If silicon is used as the propagation medium for forming the waveguide layer, photons above 1.1 ⁇ m in wave length will be transmitted through the thin waveguide layer, which is
  • the control circuitry 109 is coupled to the thermal detectors for measuring changes in the characteristic physical parameter after adso ⁇ tion of at least one chemical to be detected and responsive to the monochromatic spectrum.
  • a V-shaped thermal detector 110A is formed on substrate 132.
  • a thermal detector HOB has a se ⁇ entine legs to provide greater movement and thus greater

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Photometry And Measurement Of Optical Pulse Characteristics (AREA)

Abstract

Selon cette invention, un micro-instrument destiné à la détection d'un composé chimique est formé sur un substrat de semi-conducteur de la taille d'une pièce de monnaie. Un guide d'ondes est formé par une couche semi-conductrice disposée sur le substrat. Le guide d'onde sur couche semi-conductrice possède une encoche formant une ouverture d'entrée dans laquelle pénètre le rayonnement polychromatique. Un émetteur infrarouge disposé dans l'encoche sert à générer le rayonnement polychromatique. Un réseau de détecteurs thermiques micromécaniques peut être formé intégralement avec le substrat. Chacun des détecteurs thermiques possède un paramètre physique caractéristique mesurable et comporte un revêtement manifestant une adsorption préférentielle pour au moins un composant chimique à détecter. Un réseau de réflexion autofocalisé est formé intégralement avec la couche semi-conductrice de guide d'onde; il sert à diriger un spectre monochromatique sur le réseau en réponse au rayonnement polychromatique, et ce de manière à ce que chaque détecteur thermique reçoive des longueurs d'ondes différentes du spectre monochromatique.
PCT/US2000/006075 1999-03-12 2000-03-09 Spectrometre calorimetrique integre Ceased WO2000054030A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU51219/00A AU5121900A (en) 1999-03-12 2000-03-09 Integrated calorimetric spectrometer

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US26729299A 1999-03-12 1999-03-12
US09/267,292 1999-03-12

Publications (2)

Publication Number Publication Date
WO2000054030A2 true WO2000054030A2 (fr) 2000-09-14
WO2000054030A3 WO2000054030A3 (fr) 2001-02-15

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PCT/US2000/006075 Ceased WO2000054030A2 (fr) 1999-03-12 2000-03-09 Spectrometre calorimetrique integre

Country Status (2)

Country Link
AU (1) AU5121900A (fr)
WO (1) WO2000054030A2 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100492074C (zh) * 2006-12-01 2009-05-27 中国科学院半导体研究所 绝缘体上硅背腐蚀全反射的垂直耦合结构及制作方法
WO2011134156A1 (fr) * 2010-04-29 2011-11-03 晶兆科技股份有限公司 Module opto-mécanique de micro-spectromètre comprenant une fente conique et structure de fente associée
US9273997B2 (en) 2012-11-16 2016-03-01 Oto Photonics, Inc. Spectrometer, assembling method thereof, and assembling system

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3625490A1 (de) * 1986-07-28 1988-02-04 Kernforschungsz Karlsruhe Multikomponenten-prozessanalysensystem
JPH0619079Y2 (ja) * 1988-04-28 1994-05-18 オリンパス光学工業株式会社 自動分析装置における分光装置
US5784507A (en) * 1991-04-05 1998-07-21 Holm-Kennedy; James W. Integrated optical wavelength discrimination devices and methods for fabricating same
US5512490A (en) * 1994-08-11 1996-04-30 Trustees Of Tufts College Optical sensor, optical sensing apparatus, and methods for detecting an analyte of interest using spectral recognition patterns
US5623561A (en) * 1995-09-29 1997-04-22 Georgia Tech Research Corporation Integrated optic interferometric sensor
US5923421A (en) * 1997-07-24 1999-07-13 Lockheed Martin Energy Research Corporation Chemical detection using calorimetric spectroscopy

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100492074C (zh) * 2006-12-01 2009-05-27 中国科学院半导体研究所 绝缘体上硅背腐蚀全反射的垂直耦合结构及制作方法
WO2011134156A1 (fr) * 2010-04-29 2011-11-03 晶兆科技股份有限公司 Module opto-mécanique de micro-spectromètre comprenant une fente conique et structure de fente associée
CN102762966A (zh) * 2010-04-29 2012-10-31 台湾超微光学股份有限公司 具有锥状狭缝的微型光谱仪的光机模块及其狭缝结构
US9746616B2 (en) 2010-04-29 2017-08-29 Oto Photonics Inc. Optical module of micro spectrometer with tapered slit and slit structure thereof
US9273997B2 (en) 2012-11-16 2016-03-01 Oto Photonics, Inc. Spectrometer, assembling method thereof, and assembling system

Also Published As

Publication number Publication date
WO2000054030A3 (fr) 2001-02-15
AU5121900A (en) 2000-09-28

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