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DE20113591U1 - Combined quartz crystal microbalance and plasmon spectrometer - Google Patents

Combined quartz crystal microbalance and plasmon spectrometer

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Publication number
DE20113591U1
DE20113591U1 DE20113591U DE20113591U DE20113591U1 DE 20113591 U1 DE20113591 U1 DE 20113591U1 DE 20113591 U DE20113591 U DE 20113591U DE 20113591 U DE20113591 U DE 20113591U DE 20113591 U1 DE20113591 U1 DE 20113591U1
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DE
Germany
Prior art keywords
quartz crystal
quartz
crystal microbalance
prism
surface plasmon
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Expired - Lifetime
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DE20113591U
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German (de)
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RESONANT PROBES GmbH
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RESONANT PROBES GmbH
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Priority to DE20113591U priority Critical patent/DE20113591U1/en
Publication of DE20113591U1 publication Critical patent/DE20113591U1/en
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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/02Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
    • G01B7/06Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness
    • G01B7/063Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness using piezoelectric resonators
    • G01B7/066Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness using piezoelectric resonators for measuring thickness of coating
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01GWEIGHING
    • G01G3/00Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances
    • G01G3/12Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing
    • G01G3/16Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing measuring variations of frequency of oscillations of the body

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Length Measuring Devices Characterised By Use Of Acoustic Means (AREA)
  • Length Measuring Devices By Optical Means (AREA)

Description

Resonant Probes GmbH Il ! * i Il 1*1 I JResonant Probes GmbH II ! * i Il 1*1 I J

Kombinierte Schwingquarzmikrowaage und PiasmonenspeJctrombter *" '*' Combined quartz crystal microbalance and pyasmonium spectrometer *"'*'

BeschreibungDescription

Schwingquarz-MikrowaagenQuartz crystal microbalances

Schwingquarz-Mikrowaagen üblicher Bauart bestehen aus einem piezoelektrischen Quarz-Kristall in der geometrischen Gestalt einer Münze (1). Durch eine elektrische Wechselspannung, die über aufgedampfte Elektroden (3,6) angelegt wird, wird der Kristall zu einer Dicken-Scherschwingung angeregt. Wird die akustische Resonanzfrequenz (typisch im MHz-Bereich) getroffen, so erreichen die Schwingungsamplitude und die Wechselstrom-Leitfähigkeit ein scharfes Maximum. Dieses wird zur Messung der Resonanzfrequenz auf elektrischem Wege genutzt. Befindet sich auf der Oberfläche des Resonators ein dünner Film, so erhöht dieser die schwingende Masse und erniedrigt dadurch die Resonanzfrequenz. Aus der Messung der Verschiebung der Resonanzfrequenz nach Aufbringen eines Films kann die aufgebrachte Masse sehr genau bestimmt werden.1'2 Quartz crystal microbalances of the usual design consist of a piezoelectric quartz crystal in the geometric shape of a coin (1). The crystal is excited to a thickness shear oscillation by an alternating electrical voltage applied via vapor-deposited electrodes (3,6). If the acoustic resonance frequency (typically in the MHz range) is reached, the oscillation amplitude and the alternating current conductivity reach a sharp maximum. This is used to measure the resonance frequency electrically. If there is a thin film on the surface of the resonator, this increases the oscillating mass and thus lowers the resonance frequency. The applied mass can be determined very precisely by measuring the shift in the resonance frequency after a film has been applied. 1 ' 2

Schwingquarz-Mikrowäägung ist grundsätzlich in beliebigen Medien möglich. Bei Messungen in Flüssigkeiten stellt sich jedoch das Problem, daß der Film im Medium aufquellen kann. Da das quellende Medium an der Schwingung teilnimmt, erscheint die Masse des Films um den entsprechenden Wert erhöht.Quartz crystal microweighing is basically possible in any medium. However, when measuring in liquids, the problem arises that the film in the medium can swell. Since the swelling medium participates in the oscillation, the mass of the film appears to increase by the corresponding amount.

Oberflächenplasmonen-SpektroskopieSurface plasmon spectroscopy

Die Oberflächenplasmonen-Spektroskopie ein verbreitetes Verfahren zur Bestimmung von Schichtdicken (etwa eines adsorbierten Analyten) in der flüssigen Phase.3'4 An einer Grenzfläche zwischen einem Metall und einer Flüssigkeit haben die Maxwell-Gleichungen eine Lösung, die sowohl ins Metall als auch in die Flüssigkeit hinein exponentiell abfällt. Da diese Mode (das Oberflächenplasmon) an die Grenzfläche gebunden ist, hängt ihre Wellenlänge extrem empfindlich vom Brechungsindex an der Grenzfläche, und damit von der Adsorbatmenge, ab. Die Wellenlänge läßt sich bequem aus der Koppelbedingung (z.B. dem Einfallswinkel, bei dem das charakteristische Minimum der Reflektivität auftritt) erschließen. Sub-Monolagen-Empfindlichkeit wird problemlos erreicht. Die Kopplung der Plasmonen an den externen Lichtstrahl kann entweder von der Rückseite über ein Prisma in Verbindung mit einer semi-transparenten Metallschicht („Kretschmann-Konfiguration") oder aber von der Vorderseite über ein Beugungsgitter auf der Metall-Oberfläche erfolgen. Oberflächenplasmonen-Spektroskopie ist von dem Problem der Quellung in flüssigen Medien weniger betroffen als Schwingquarz-Mikrowäägung.Surface plasmon spectroscopy is a widely used method for determining layer thicknesses (for example of an adsorbed analyte) in the liquid phase. 3 ' 4 At an interface between a metal and a liquid, Maxwell's equations have a solution that decays exponentially into both the metal and the liquid. Since this mode (the surface plasmon) is bound to the interface, its wavelength is extremely sensitive to the refractive index at the interface and thus to the amount of adsorbate. The wavelength can be easily deduced from the coupling condition (e.g. the angle of incidence at which the characteristic minimum of the reflectivity occurs). Sub-monolayer sensitivity is easily achieved. The coupling of the plasmons to the external light beam can occur either from the back side via a prism in combination with a semi-transparent metal layer ("Kretschmann configuration") or from the front side via a diffraction grating on the metal surface. Surface plasmon spectroscopy is less affected by the problem of swelling in liquid media than quartz crystal microweighing.

Resonant Probes GmbH '"''JJJI'! I!Resonant Probes GmbH '"''JJJI'! I!

Kombinierte Schwingquarzmikrowaage unJ Plasmonenspektrometer · · · · ·Combined quartz crystal microbalance and plasmon spectrometer · · · · ·

Parallele Messungen von optischer und akustischer Messung durch parallele Schwingquarz-Mikrowäägung und Oberflächenplasmonen-SpektroskopieParallel measurements of optical and acoustic measurements by parallel quartz crystal microweighing and surface plasmon spectroscopy

Das unterschiedliche Verhalten und Schwingquarz-Mikrowäägung und Oberflächenplasmonen-Spektroskopie bei Quellung im flüssigen Medium läßt es attraktiv erscheinen, beide Methoden parallel zum Einsatz zu bringen. Aus dem Unterschied in der akustischen Dicke, die mit dem Quarz-Resonator gemessen wird, und der optischen Dicke, die über Oberflächenplasmonen-Spektroskopie bestimmt wird, läßt sich auf den Quellgrad schließen. Über die Realisierung dieser Kombination mittels Gitterkopplung auf der Quarzvorderseite ist in den Referenzen 5 und 6 berichtet.The different behavior of quartz microweighing and surface plasmon spectroscopy during swelling in a liquid medium makes it attractive to use both methods in parallel. The degree of swelling can be determined from the difference in the acoustic thickness measured with the quartz resonator and the optical thickness determined by surface plasmon spectroscopy. The realization of this combination by means of grating coupling on the quartz front side is reported in references 5 and 6.

Einkopplung von Oberflächenplasmonen auf Quarz-Resonatoren mittels Kretschmann-Geometrie mit einer flüssigen ZwischenschichtCoupling of surface plasmons onto quartz resonators using Kretschmann geometry with a liquid intermediate layer

Der Quarz-Resonator (1) kann grundsätzlich nicht direkt auf ein Prisma (2) aufgeklebt werden - wie dies die Kretschmann-Geometrie verlangen würde - weil das Prisma die akustische Resonanz zum Erliegen bringen würde. Mit der hier vorgelegten Erfindung wird dies Problem umgangen, indem Quarz und Prisma über eine hochbrechende Flüssigkeit (3) akustisch entkoppelt werden. Die Rückelektrode des Quarzes (4) hat weiterhin ein Loch, durch das der Lichtstrahl (5) bis zur Vorderelektrode (6) vordringen kann. Die Vorderelektrode ist gemäß der Kretschmann-Konfiguration semi-transparent ausgeführt. Die Erfüllung der Koppelbedingung wird wie üblich anhand der reduzierten reflektierten Intensität am Detektor (7) detektiert.The quartz resonator (1) cannot be glued directly onto a prism (2) - as the Kretschmann geometry would require - because the prism would bring the acoustic resonance to a standstill. The invention presented here circumvents this problem by acoustically decoupling the quartz and prism using a highly refractive liquid (3). The back electrode of the quartz (4) also has a hole through which the light beam (5) can penetrate to the front electrode (6). The front electrode is semi-transparent in accordance with the Kretschmann configuration. The fulfillment of the coupling condition is detected as usual based on the reduced reflected intensity at the detector (7).

Eine vorteilhafte Ausgestaltung der Erfindung ist im Schutzanspruch 2 angegeben. Hier werden als Abstandshalter zwischen Prisma und Schwingquarz elektrisch leitfähige O-Ringe (8) verwendet. Dies löst das Problem der elektrischen Kontaktierung des Schwingquarzes.An advantageous embodiment of the invention is specified in claim 2. Here, electrically conductive O-rings (8) are used as spacers between the prism and the quartz oscillator. This solves the problem of electrical contact with the quartz oscillator.

• ··· » · «· Resonant Probes GmbH * • ··· » · «· Resonant Probes GmbH *

Kombinierte Schwingquarzmikrowaage und Plasmonenspektrometer Referenzen Combined quartz crystal microbalance and plasmon spectrometer References

A. Janshoff, HJ. Galla, C. Steinern, Piezoelectric mass-sensing devices as biosensors - An alternative to optical biosensors? Angew. Chem. Intern. Ed. 39, 4004 (2000).A. Janshoff, HJ. Galla, C. Steinern, Piezoelectric mass-sensing devices as biosensors - An alternative to optical biosensors? Angew. Chem. Intern. Ed. 39, 4004 (2000).

D. Johannsmann,D.Johannsmann,

Viscoelastic analysis of organic thin films on quartz resonators, Macromol. Chem. Phys. 200, 501 (1999). Viscoelastic analysis of organic thin films on quartz resonators, Macromol. Chem. Phys. 200, 501 (1999).

W.M. Mullett, E.P.C.Lai, J.M. Yeung, Surface plasmon resonance-based immunoassays, Methods (Duluth). 22, 77, (2000).WM Mullett, EPCLai, JM Yeung, Surface plasmon resonance-based immunoassays, Methods (Duluth). 22, 77, (2000).

W. Knoll,W. Knoll,

Interfaces and thin films as seen by bound electromagnetic waves, Ann. Rev. Phys. Chem. 49, 569 (1998). Interfaces and thin films as seen by bound electromagnetic waves, Ann. Rev. Phys. Chem. 49, 569 (1998).

D. Johannsmann, A. Laschitsch, B. Menges, Patentschrift, Gerät zur Bestimmung von Schichtdicken, eingereicht beim Deutschen PatentamtD. Johannsmann, A. Laschitsch, B. Menges, patent specification, device for determining layer thicknesses, filed with the German Patent Office

A. Laschitsch, B. Menges, D. Johannsmann Simultaneous determination of optical and acoustic thickness of protein layers using surface plasmon resonance spectroscopy and quartz crystal microweighing Appl. Phys. Lett. 77, 2252 (2000)A. Laschitsch, B. Menges, D. Johannsmann Simultaneous determination of optical and acoustic thickness of protein layers using surface plasmon resonance spectroscopy and quartz crystal microweighing Appl. Phys. Lett. 77, 2252 (2000)

Claims (2)

1. Gerät zur Bestimmung von Schichtdicken, dadurch gekennzeichnet, daß eine Schwingquarz-Mikrowaage über eine Flüssigkeit mit einem Prisma im Kontakt steht, daß weiterhin die Rückelektrode ein Loch aufweist und die Vorderelektrode semitransparent ausgeführt ist, und daß auf diesem Wege auf der Schwingquarz-Oberfläche ein Oberflächenplasmon angeregt werden kann, das es erlaubt, neben der akustischen auch die optische Schichtdicke zu bestimmen. 1. Device for determining layer thicknesses, characterized in that a quartz crystal microbalance is in contact with a prism via a liquid, that the rear electrode further has a hole and the front electrode is semi-transparent, and that in this way a surface plasmon can be excited on the quartz crystal surface, which allows the optical layer thickness to be determined in addition to the acoustic layer thickness. 2. Gerät zur Bestimmung von Schichtdicken nach Schutzanspruch 1, dadurch gekennzeichnet, daß der mechanische Kontakt zwischen Schwingquarz und Prisma durch elektrisch leitende O-Ringe hergestellt wird und daß damit das Problem der elektrischen Kontaktierung gelöst wird. 2. Device for determining layer thicknesses according to claim 1, characterized in that the mechanical contact between the quartz oscillator and the prism is established by electrically conductive O-rings and that the problem of electrical contact is thus solved.
DE20113591U 2001-08-16 2001-08-16 Combined quartz crystal microbalance and plasmon spectrometer Expired - Lifetime DE20113591U1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG119167A1 (en) * 2002-12-31 2006-02-28 Agency Science Tech & Res A multi-parameter microchip
WO2006031198A1 (en) * 2004-09-15 2006-03-23 Agency For Science, Technology And Research Surface plasmon resonance and quartz crystal microbalance sensor

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG119167A1 (en) * 2002-12-31 2006-02-28 Agency Science Tech & Res A multi-parameter microchip
WO2006031198A1 (en) * 2004-09-15 2006-03-23 Agency For Science, Technology And Research Surface plasmon resonance and quartz crystal microbalance sensor
JP2008513772A (en) * 2004-09-15 2008-05-01 エイジェンシー フォー サイエンス, テクノロジー アンド リサーチ Surface plasmon resonance and quartz crystal microbalance sensor
EP1794574A4 (en) * 2004-09-15 2009-09-23 Agency Science Tech & Res SURFACE PLASMON RESONANCE AND QUARTZ CRYSTAL MICRO BALANCE SENSOR
US7869013B2 (en) 2004-09-15 2011-01-11 Agency For Science, Technology And Research Surface plasmon resonance and quartz crystal microbalance sensor
CN101163957B (en) * 2004-09-15 2011-07-13 新加坡科技研究局 Surface plasma resonance and quartz crystal microscale sensor

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