WO2007087936A2 - Dispositif et procédé de détection d'une substance dans un liquide - Google Patents

Dispositif et procédé de détection d'une substance dans un liquide Download PDF

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Publication number
WO2007087936A2
WO2007087936A2 PCT/EP2006/069827 EP2006069827W WO2007087936A2 WO 2007087936 A2 WO2007087936 A2 WO 2007087936A2 EP 2006069827 W EP2006069827 W EP 2006069827W WO 2007087936 A2 WO2007087936 A2 WO 2007087936A2
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WO
WIPO (PCT)
Prior art keywords
temperature
piezoelectric layer
mass
substance
resonant frequency
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PCT/EP2006/069827
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German (de)
English (en)
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WO2007087936A3 (fr
Inventor
Jan Weber
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Siemens Aktiengesellschaft
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Publication of WO2007087936A2 publication Critical patent/WO2007087936A2/fr
Publication of WO2007087936A3 publication Critical patent/WO2007087936A3/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0256—Adsorption, desorption, surface mass change, e.g. on biosensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/028—Material parameters
    • G01N2291/02881—Temperature

Definitions

  • the present invention relates to an apparatus and a method for detecting a substance in a liquid by means of at least one piezoacoustic resonator element, the at least one piezoelectric layer and two electrodes adjacent to the piezoelectric layer, and at least one surface portion suitable for the attachment of the substance to be detected from the Liquid is arranged, has and is such that by applying a voltage by means of the electrodes to the piezoelectric layer, a volume vibration of the piezoelectric layer is excited at resonance frequency and the resonance frequency of the piezoacoustic resonator element changes depending on the mass of the deposited substance to be detected.
  • the essential functional component is a piezoacoustic resonator element in which a thickness oscillation, i.e. a body volume oscillation of the piezoelectric layer, is excited by applying an alternating voltage.
  • FIGS. 1a and 1b schematically show two basic types of BAW resonators, as described in the review article by M. Dubois "Thin Film Bulk Acoustic Resonators: A Technology Overview", published on the occasion of the conference MEMSWAVE 03, Toulouse, France, JuIy 2-4, 2003.
  • 1A schematically shows an example of a so-called “thin film acoustic acoustic resonator (FBAR)."
  • FBAR thin film acoustic acoustic resonator
  • a piezoelectric AlN layer 300 is applied on a carrier substrate in the form of an Si wafer 400. On the underside and the upper side of the piezoelectric layer
  • Electrodes 100 and 200 attached.
  • an alternating electric field is applied to the piezoelectric layer 300 by the electrodes 100/200, conversion of the electrical energy into mechanical energy occurs due to the inverse piezoelectric effect.
  • the resulting bulk acoustic wave propagates within the piezoelectric layer with the advancing direction parallel to the electric field and reflecting the wave at the electrode / air interface.
  • the resonance vibration is achieved when the thickness of the
  • Layer structure of the resonator is equal to half the wavelength of the input signal amounts.
  • a cavity is provided on the underside of the piezoelectric layer, so that the acoustic waves can be reflected at the electrode / air interface.
  • FIG. 1B shows a construction of a BAW resonator as a so-called solidly mounted resonator (SMR).
  • SMR solidly mounted resonator
  • an acoustic mirror (Bragg reflector) 500 between the lower electrode 300 and the substrate 400 is provided.
  • This acoustic mirror consists of several layers with very different acoustic impedance, which are arranged in alternating sequence, for example, layers of W / SiO2 or A1 / A1N, etc.
  • the layer thickness is ⁇ / 4.
  • SAW Surface Acoustic Wave
  • the BAW resonators Surface Acoustic Wave resonators
  • Thick vibration (volume vibration) of the piezoelectric layer is excited, in contrast to surface waves in surface acoustic wave resonators.
  • the excitation of a volume oscillation takes place by means of a suitable electrode arrangement in combination with a suitable crystallographic orientation of the piezoelectric layer.
  • the excited volume oscillation of the piezoacoustic resonator element may be a longitudinal oscillation or a thickness shear oscillation.
  • WO 2004/017063 A2 of the Applicant describes a generic device which is designed as a biosensor for the attachment of a substance to the surface of the BAW resonator. In this way, for example, a specific substance can be identified. Addition can mean adsorption and / or absorption.
  • the resonator for this purpose has a sensitive coating, for example in the form of a polymer film, which is mounted on an electrode of the resonator.
  • a sensitive coating for example in the form of a polymer film, which is mounted on an electrode of the resonator.
  • Various substances to be detected for example hydrocarbons, can be absorbed on this polymer film.
  • the substance to be detected is present in a fluid (gas or liquid), which serves as a measuring medium.
  • the sensor is brought into contact with the measuring medium containing the substance that can attach to the sensitive coating.
  • a microfluidics with measuring cell is used, through which the measuring medium flows over the respective surface section of the sensor.
  • the surface portion of the sensor to which the substance in question attaches depends in many cases on the nature of the substance to be detected, in order to be able to detect a specific substance selectively from a mixture of several substances in this way.
  • the above patent application describes detection of DNA fragments by means of a sensor having on a surface portion of the electrode a coating with a selected DNA sequence, which allows attachment of suitable DNA sequences according to the key-lock principle.
  • This equilibrium state of desorption is determined by the conditions of the corresponding system, such as, for example, the type of coating, the concentration of the species involved, temperature, etc.
  • the resonance frequency changes depending on the mass of the deposited substance.
  • the characteristic value concerned is the mass sensitivity of the resonator, which is proportional to the square of the resonant frequency of the resonator.
  • devices for stabilizing the temperature of the device for detecting a substance in a liquid have been proposed. Due to the required temperature measurement, heating and optionally cooling, these devices are very expensive to produce and difficult to miniaturize.
  • devices have been proposed which combine the device for detecting a substance in a liquid with a temperature measuring resistor. With the help of this measuring resistor, the temperature of the device is determined.
  • a subsequent evaluation device has a calibration curve, which provides information about the influence of the temperature on the measurement results of the sensor for determining the mass accumulation. With the aid of this calibration curve, the evaluation device calculates a temperature-independent measured value for the mass addition, knowing the measured temperature.
  • the object of the invention is to provide a simplified device and a simplified method for the detection of a substance. Another object is to provide an apparatus and a method for detecting a substance with increased accuracy.
  • a device having the features of claim 1 and a method having the features of claim 17 are provided to solve the objects.
  • the invention provides an apparatus for detecting a substance in a liquid, which comprises at least one piezoacoustic resonator element with at least one piezoelectric layer, electrodes disposed on the piezoelectric layer and at least one surface portion adapted for the attachment of the substance to be detected from the liquid, wherein the piezoacoustic resonator element is such that a volume vibration by applying a voltage to the piezoelectric layer by means of the electrodes the piezoelectric layer is excited at the resonant frequency, which changes as a function of the mass of the deposited substance to be detected, and comprises an evaluation device for determining an attachment characteristic value from the measured resonance frequency.
  • the device additionally comprises a device for determining a temperature influence on the resonant frequency by measuring at least two different oscillations, of which a first oscillation of a mass and temperature dependence and a second oscillation is subject exclusively to a temperature dependence, wherein the evaluation device is set up for determining an accumulation characteristic value is to determine a temperature-independent appurtenance characteristic on the basis of the measured values of the at least two measurements.
  • an exclusive temperature dependency means that there is essentially no dependence of the oscillation on the mass accumulation.
  • the property of the exclusive temperature dependence or temperature and mass dependence of the different vibrations is based on the fact that they are different vibration modes. This requires that these vibrations be generated in a structure consisting of at least two layers, one layer not being too small over the other. Structures consisting of one layer allow only vibrations that are in the propagation direction (the direction perpendicular to the layer) take the form of a sine function. If one adds at least one layer, with an acoustic impedance that deviates from the first layer, then the oscillations can take on forms that deviate from the sine function.
  • These vibration modes can be described by a Fourier series. They are defined by their Fourier coefficients. In particular, different modes, that is to say oscillations with different Fourier coefficients, can be excited in one and the same layer stack. These different modes may have the property of being temperature and mass dependent or essentially only temperature dependent.
  • Such temperature-dependent and / or mass-dependent modes can be determined by modeling the acoustic layer stack.
  • a specific one-dimensional layer stack is to be modeled using one of the models well-known from the literature (Transmission Line Model, Mason Model, see eg KM Lakin, GRKline, K.T.Mc Carron, High-Q Microwave Acoustic Resonators and Filters, IEEE transactions on microwave theory and techniques, Vol.41, No.12, December 1993) and the resonant frequencies are to be determined.
  • the literature Transmission Line Model, Mason Model, see eg KM Lakin, GRKline, K.T.Mc Carron, High-Q Microwave Acoustic Resonators and Filters, IEEE transactions on microwave theory and techniques, Vol.41, No.12, December 1993
  • Resonant frequencies is now the mass sensitivity (that is, the frequency change per mass coating) to determine. This can be done, for example, by varying the thickness of the uppermost layer and, in turn, determining the resonant frequencies. From the mass change (due to the
  • Layer stack is obtained, which contains two resonances, one of which has a high mass sensitivity and the other a disappearing mass sensitivity (ie Essentially mass-independent). This can be further optimized by continuing the process with the variation of further layers.
  • the advantage of the inventive approach is that both measured variables can be detected with the same principle, namely the generation of a volume vibration of a piezoacoustic resonator.
  • the same sensor type can be used for both measurements. This results in a simple construction of the device and low
  • the measurement is performed by the device at at least two different resonant frequencies, of which a first resonant frequency of a mass and temperature dependence and a second resonant frequency is substantially exclusively subject to a temperature dependence.
  • the at least two different resonance frequencies can be generated in one and the same piezoelectric layer.
  • the resonance frequencies can be excited either simultaneously or alternately.
  • the mass- and temperature-dependent resonant frequency in a first piezoelectric layer and the exclusively temperature-dependent resonant frequency in a second piezoelectric layer can be excited, leading to a piezoacoustic resonator element in FIG
  • Stack design or may belong to several resonator elements. Different resonance frequencies can be achieved, for example, by virtue of the fact that the first piezoelectric layer and the second piezoelectric layer have different thicknesses.
  • the measurement can be carried out in at least two different vibration modes, of which a first vibration mode of a mass and
  • Temperaturabhangmaschine and a second vibration mode substantially exclusively subject to a temperature dependence.
  • Such temperature-dependent and / or mass-dependent vibration modes can also be determined by simulation, for example, as is well known to the person skilled in the art.
  • the transition line model can be used.
  • the at least two different vibration modes can also be produced in one and the same piezoelectric layer in this embodiment.
  • the above-mentioned advantage results that both the mass and temperature-dependent measurement and the exclusively temperature-dependent measurement are carried out at the same location.
  • the vibration modes can be excited either simultaneously or alternately.
  • the mass- and temperature-dependent vibration mode in a first piezoelectric layer and the exclusively temperature-dependent vibration mode in a second piezoelectric layer are excited.
  • the advantage can arise that both measurements can be carried out at substantially the same frequency.
  • the described device for detecting a substance is constructed on a carrier substrate, which consists of a semiconductor material.
  • the device can be designed as a Si-integrated measuring array with a plurality of resonator elements.
  • an acoustic mirror consisting of several layers can be arranged.
  • One or more piezoacoustic resonator elements may have a multilayer structure.
  • the device for detecting the temperature influence on the resonance frequency can be configured as a temperature measuring device.
  • Embodiment the advantage that it determines the temperature of the liquid and thus can provide additional valuable information about the reaction kinetics.
  • a correction device may be present for correcting the resonance frequency of the piezoacoustic resonator element on the basis of the value detected by the temperature detection device.
  • the mass-dependent vibration is generated at substantially 1.6 GHz and the mass-independent vibration at substantially 2.8 GHz.
  • the invention additionally encompasses a method for detecting a substance in a liquid, comprising the steps of bringing into contact a liquid containing the substance with at least one piezoacoustic resonator element having at least one piezoelectric layer, at least two electrodes adjoining the piezoelectric layer and at least one surface section , which is adapted to the attachment of the substance to be detected from the liquid, exciting a volume vibration of the piezoelectric layer having a resonant frequency, which changes depending on the mass of the deposited substance to be detected, by applying a voltage by means of the electrodes to the piezoelectric layer Measuring the resonant frequency of the piezoacoustic resonator element as a function of the accumulated mass and the temperature, and determining an accumulation characteristic value from the measured resonant frequency.
  • the method comprises the additional steps of exciting and measuring a first one
  • Vibration which is dependent on the accumulated mass and the temperature
  • stimulation and measurement of at least one second oscillation which depends exclusively on the temperature
  • the step of determining a temperature-independent accumulation characteristic value from the results of the first and second measurement can be determined from the measurements.
  • the device according to the invention and the method according to the invention permit a detection of a substance in a liquid with considerably improved measuring accuracy, since the influence of the temperature of the measuring medium on the measuring signal is detected.
  • FIG. 1A and 1B schematically show the structure of an FBAR and an SMR resonator as examples of BAW resonators known in the prior art, in cross-section.
  • 2 shows a functional block diagram of a first exemplary embodiment of the device according to the invention.
  • Fig. 3 shows an exemplary embodiment of
  • Fig. 4 shows a further exemplary embodiment of a
  • Data acquisition device of the device according to the invention which comprises a resonator element which can be excited with different oscillations.
  • FIG. 5 shows an exemplary embodiment of a method according to the invention for detecting a substance in a liquid.
  • FIG. 6 shows a more detailed exemplary embodiment of a method according to the invention for detecting a substance in a liquid.
  • FIG. 7 shows an example of the influence of the mass attachment on the resonance frequency with different vibrations.
  • the device 1 for detecting a substance in a liquid shown in FIG. 2 comprises a measured value detection device 2, an evaluation device 3 for determining an attachment characteristic value and a device 4 for determining the temperature dependence of the measured resonance frequency.
  • the measured value detection device 2 has a surface section 2a, which is set up for the attachment of the substance to be detected from the liquid. In the present example it is a chemically selective coating for the absorption of the protein streptavidin. The person skilled in the art is, however, aware that this is only an example of a functional layer that is beneficial to the attachment of the substance to be detected.
  • the evaluation device 3 serves to determine an attachment characteristic value on the basis of the measured resonance frequency change.
  • the device 4 for determining the temperature dependence in which the substance to be detected is present comprises a device 4 a for measuring the resonance frequency shift and a device 4 b for determining the temperature based on the measured displacement.
  • the measured value detection device 2 and the device 4 for determining the temperature dependence in the exemplary embodiment of FIG. 1 are shown as separate components, the invention is not limited to such an embodiment. Rather, the
  • Measured value detection device to be an integral part of the device for determining the temperature dependence.
  • Figure 3 shows an exemplary embodiment of a
  • the measured value acquisition device 30 comprises a first piezoacoustic resonator element 31 and a second piezoacoustic resonator element 32.
  • the first piezoacoustic resonator element comprises a piezoelectric layer 310 made of ZnO and electrodes 311, 312 on the lower surface and the upper surface of the piezoelectric layer made of platinum, respectively.
  • the second piezoacoustic resonator element 32 comprises a piezoelectric layer 320, which likewise consists of ZnO, as well as two electrodes 321, 322 on the underside and the upper side of the piezoelectric layer, which likewise consist of platinum. Both piezoacoustic resonator elements are arranged on an acoustic mirror 33 consisting of several layers of very different impedance.
  • the resonance detuning was achieved in a simple manner by different thicknesses of the resonator elements, in that the thickness of the piezoelectric ZnO layer of the resonator elements 31, 32 was dimensioned differently. This results in different resonance frequencies of the elements 31, 32, z.
  • the mass and temperature-dependent resonant frequency f r i is formed in the element 31, while the substantially exclusively temperature-dependent resonant frequency f r 2 is produced in the element 32, which is higher in this exemplary embodiment.
  • the resonance detuning was chosen such that it lies within the range of the acoustic mirror bandwidth. In this way, an acoustic mirror 33 can be used for both resonator elements 31, 32, whereby the production costs are limited.
  • the embodiment of a measured value detection device shown in FIG. 3 can be used particularly advantageously in a Si-integrated FBAR array in which a plurality of resonators are arranged in the smallest possible space so that almost identical ambient and reaction conditions are achieved and an almost equal mass occupancy is ensured ,
  • FIG. 4 shows a further exemplary embodiment of a measured value detection device according to the invention in which only one piezoacoustic resonator element is used.
  • the measured value detection device 40 shown in this illustration comprises a piezoacoustic resonator element 410, on whose upper side or lower side in each case one electrode 421, 422 is attached.
  • the piezoacoustic resonator element 41 of this exemplary embodiment is set up such that it can be excited simultaneously with two different oscillations 44, 45. However, the excitation of the two oscillations can also be carried out in alternation.
  • the Grundmode- and first upper-mode oscillation are shown schematically according to schematically.
  • the piezoacoustic resonator element 41 is arranged on an acoustic mirror 42.
  • the fundamental mode oscillation is mass and temperature dependent, while the upper mode oscillation is exclusively one
  • FIG. 5 shows an exemplary embodiment of the method according to the invention for the detection of a liquid.
  • the method comprises the step 51 of contacting a liquid containing the substance to be detected with a measured value acquisition device having two piezoacoustic resonator elements, as described above with reference to FIG.
  • a measured value acquisition device having two piezoacoustic resonator elements, as described above with reference to FIG.
  • step 52 by applying an AC voltage to the electrodes of the piezoelectric layers, a volume vibration of the piezoelectric layer having a resonance frequency is generated.
  • step 53 the resonance frequencies of the piezoacoustic resonator elements are first measured in air and then in the analyte. Several measurements can be performed as reference before and after attachment of the substance or measurements based on calibration curves.
  • step 54 the evaluation of the measured resonance frequencies as a function of the deposition of the substance to be detected is carried out to determine an attachment characteristic value.
  • FIG. 6 shows a more detailed exemplary embodiment of the method according to the invention for the detection of a liquid.
  • the method comprises the step 61 of contacting a liquid containing the substance to be detected with a measured value detection device having two piezoacoustic resonator elements, as described above with reference to FIG. However, it is also possible, for example, to use the measured-value acquisition device of FIG. 4 as well.
  • step 62 by applying an AC voltage to the electrodes of the piezoelectric layers, a mass and temperature-dependent volume vibration of the piezoelectric layer having a resonant frequency is generated.
  • step 63 the mass and temperature-dependent resonant frequency of the piezoacoustic resonator elements is measured. Several measurements can be performed as reference before and after attachment of the substance or measurements based on calibration curves.
  • step 64 by applying an alternating voltage to the electrodes of the piezoelectric layers, an exclusively temperature-dependent volume oscillation of the piezoelectric layer with resonance frequency is generated.
  • step 65 the exclusively temperature-dependent resonant frequency of the piezoacoustic resonator elements is measured. Several measurements can be performed as reference before and after attachment of the substance or measurements based on calibration curves.
  • a temperature may be determined from the measurement of step 65.
  • step 67 the evaluation of the measured resonance frequencies from the measurements from steps 63 and 65 is carried out to determine a temperature-independent deposit characteristic value.
  • FIG. 7 shows an example of the influence of the mass attachment on the resonance frequency with different vibrations. This influence was measured with a device according to the invention according to FIG. On the Y axis, the layer thickness of the top electrode is varied, which corresponds to a change in the mass coating, so that the displacement of the resonance is directly related to the mass sensitivity. Due to the Display method with the help of grayscale the amplitudes appear distorted. For example, the 1.6GHz resonance is much darker than the 2.8GHz resonance. From this no direct conclusions can be drawn on the actual good of the resonance.
  • the resonant frequency is subject to a significant mass dependence, whereas with an oscillation of essentially 2.8 GHz, the resonant frequency is largely independent of the mass accumulation.
  • the two oscillations can either be generated in one and the same piezoelectric layer (410) or the first oscillation can be excited in a first piezoelectric layer (310) and the second oscillation in a second piezoelectric layer (320).

Abstract

L'invention concerne un dispositif et un procédé de détection d'une substance dans un liquide. Le dispositif comporte au moins un élément résonant piézoacoustique (30, 40) présentant au moins une couche piézoélectrique (310, 320; 410), des électrodes (311, 312; 321, 322; 411, 412) s'appuyant contre la couche piézoélectrique, et au moins une section de surface (2a) destinée à la fixation de la substance à détecter et provenant du liquide. L'élément résonant piézoacoustique (30, 40) est conçu de telle manière que par application d'une tension à la couche piézoélectrique (310, 320; 410) au moyen des électrodes, la couche piézoélectrique entre en vibration de volume avec fréquence résonante, cette vibration variant en fonction de la masse de la substance à détecter fixée. Un dispositif d'évaluation (3) sert à déterminer une caractéristique de fixation sur la base de la fréquence de résonance mesurée. Le dispositif selon l'invention comporte également un système de détermination (4) de l'influence de la température sur la fréquence de résonance par mesure d'au moins deux vibrations différentes, une première vibration dépendant de la masse et de la température et une deuxième vibration dépendant essentiellement de la température. Le dispositif d'évaluation (3) servant à déterminer une caractéristique de dépôt est conçu pour déterminer une caractéristique de dépôt dépendant de la température sur la base des valeurs des mesures.
PCT/EP2006/069827 2006-01-31 2006-12-18 Dispositif et procédé de détection d'une substance dans un liquide WO2007087936A2 (fr)

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DE102006004449.5 2006-01-31
DE200610004449 DE102006004449A1 (de) 2006-01-31 2006-01-31 Vorrichtung und Verfahren zur Detektion einer Substanz in einer Flüssigkeit

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DE102007047153A1 (de) * 2007-10-02 2009-04-30 Siemens Ag Feuchtigkeitssensor mit Nanoröhren-Schicht, die an einen BAW-Resonator gekoppelt ist, und Verfahren zur Detektion von Wasser in einem Fluid unter Verwendung des Feuchtigkeitssensors
DE102007047156A1 (de) * 2007-10-02 2009-04-23 Siemens Ag Feuchtigkeitssensor mit hygroskopischer Keramikschicht und Verfahren zur Detektion von Wasser in einem Fluid unter Verwendung des Feuchtigkeitssensors
DE102007047155A1 (de) * 2007-10-02 2009-04-30 Siemens Ag Feuchtigkeitssensor mit hygroskopischer Keramikschicht, die an einen BAW-Resonator gekoppelt ist, und Verfahren zur Detektion von Wasser in einem Fluid unter Verwendung des Feuchtigkeitssensors
DE102011076193A1 (de) * 2010-10-01 2012-04-05 Siemens Aktiengesellschaft Bestimmen einer Materialeigenschaft einer Dünnschicht eines Materials
DE102015225470A1 (de) * 2015-12-16 2017-06-22 Siemens Aktiengesellschaft Verfahren zur Detektion und Substanzdetektor
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