WO1999000855A1 - Method and system for detecting material using piezoelectric resonators - Google Patents
Method and system for detecting material using piezoelectric resonators Download PDFInfo
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- WO1999000855A1 WO1999000855A1 PCT/US1998/013535 US9813535W WO9900855A1 WO 1999000855 A1 WO1999000855 A1 WO 1999000855A1 US 9813535 W US9813535 W US 9813535W WO 9900855 A1 WO9900855 A1 WO 9900855A1
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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
- G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
-
- 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
- G01N2291/01—Indexing codes associated with the measuring variable
- G01N2291/012—Phase angle
-
- 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
- G01N2291/023—Solids
- G01N2291/0231—Composite or layered materials
-
- 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
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- 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
- G01N2291/04—Wave modes and trajectories
- G01N2291/042—Wave modes
- G01N2291/0421—Longitudinal 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
- G01N2291/04—Wave modes and trajectories
- G01N2291/042—Wave modes
- G01N2291/0422—Shear waves, transverse waves, horizontally polarised waves
Definitions
- This invention relates generally to sensors for detecting small quantities of materials, and more particularly to material sensors based on piezoelectric resonators .
- piezoelectric resonators based on piezoelectric properties of materials have been used in many important applications. For instance, quartz crystal resonators are widely used as frequency control elements in oscillator circuits found in many devices such as computers and watches. They are also used as bulk-acoustic wave filters in a variety of circuits for frequency selection purposes.
- piezoelectric resonators One important application of piezoelectric resonators is in detecting very small quantities of materials. Piezoelectric resonators used as sensors in such applications are sometimes called "micro-balances.”
- a piezoelectric resonator is typically constructed as a thin planar layer of crystalline piezoelectric material sandwiched between two electrode layers.
- the resonator When used as a sensor, the resonator is exposed to the material being detected to allow the material to bind on a surface of the resonator.
- the conventional way of detecting the amount of the material bound on the surface of a sensing resonator is to operate the resonator as an oscillator at its resonant frequency. As the material being detected binds on the resonator surface, the oscillation frequency of the resonator is reduced. The change in the oscillation frequency of the resonator, presumably caused by the binding of the material on the resonator surface, is measured and used to calculate the amount of the material bound on the resonator or the rate at which the material accumulates on the resonator surface.
- a piezoelectric resonator as a material sensor is typically proportional to its resonance frequency.
- the sensitivities of material sensors based on the popular quartz crystal resonators are limited by their relatively low oscillating frequencies, which typically range from several MHz to about 100 MHz.
- TFR thin-film resonator
- a thin-film resonator is formed by depositing a thin film of piezoelectric material, such as A1N or ZnO, on a substrate.
- the resonant frequency of the thin-film resonator is on the order of 1 GHz or higher.
- the high resonant frequencies and the corresponding high sensitivities make thin-film resonators useful for material sensing applications.
- the conventional method of detecting material by measuring a change in the oscillation frequency of the sensing resonator requires the incorporation of the sensing resonator in an oscillator circuit to drive the sensing resonator into oscillation. To obtain accurate measurement results, the oscillator circuit has to be stable and frequency matched to the resonant frequency of the sensing resonator.
- sensing resonators may have significantly different resonant characteristics. For instance, the non-uniformity in the deposition thickness of a piezoelectric layer deposited across a substrate can cause the resonance frequencies of thin-film resonators from the same production batch to vary significantly. As a result, a non-adjustable oscillator circuit is incapable of effectively driving all of the sensing resonators into oscillation.
- a method and system for detecting material using a sensing resonator that measures a change in insertion phase shift of the resonator caused by the binding of the material being detected on a surface of the resonator.
- An input electrical signal having a frequency within a resonance band of the piezoelectric resonator is coupled to and transmitted through the resonator to generate an output electrical signal which is phase-shifted from the input signal due to the insertion of the resonator in the signal path.
- the insertion phase shift is altered when the material being detected binds on the resonator surface.
- the output electrical signal received from the piezoelectric resonator is analyzed to determine the change in insertion phase shift caused by the binding of the material on the resonator surface.
- the measured change in insertion phase shift provides quantitative information regarding the material bound to the resonator surface.
- the need for tuned oscillator circuits is entirely eliminated, and therewith the problem of matching oscillator circuits with different sensing resonators.
- One of the important advantages of the phase shift detection according to the invention is that the input electrical signal is kept at a constant frequency during the measurement. The constant frequency of the input signal provides a baseline of the measurement, and there is no longer the need to follow an ever changing oscillation frequency as in the conventional method.
- phase detection is the simplification of the electronics for the sensing system. Because the input signal is kept constant during measurement, simple and inexpensive signal sources with adjustable output frequencies, such as frequency synthesizers, can be used. Another significant advantage of the phase detection approach is that one signal source can be used to provide input signals simultaneously to multiple resonators. As a result, a reference resonator may be used in conjunction with a sensing resonator to effectively separate environmental effects from the phase shift change caused by the binding of the material being detected on the sensing resonator.
- phase detection approach of the invention can be advantageously used with different types of sensing resonators in different configurations.
- both the conventional quartz crystal resonators and the newer thin-film resonators can be used as sensors, and the sensing resonator may be configured as a one-port or two-port device.
- the resonators in the sensor may operate in longitudinal or shear modes.
- a thin- film sensing device includes a reference resonator and at least one sensing resonator monolithically formed on a substrate.
- the input electrical signal is coupled to the electrodes of the reference and sensing resonators via a transmission line and a power divider.
- the close proximity of the reference and sensing resonators allows the resonators to be fabricated with closely matched resonant characteristics, which allow effective cancellation of environmental effects during material sensing operations.
- FIGURES IA and IB are schematic diagrams illustrating the operational principles of the invention.
- FIG. 2 is a schematic diagram of a material sensing system having a one-port resonator as a sensor
- FIG. 3 is a schematic diagram of a material sensing system having a one-port sensing resonator and a one- port reference resonator;
- FIG. 4 is a schematic diagram of a material sensing system with two-port sensing and reference resonators
- FIGS. 5A and 5B are schematic top and cross sectional views, respectively, of a three-port sensor having thin-film sensing and reference resonators monolithically formed on a substrate
- FIG. 6A shows measured insertion phase curves of a sensing resonator and a reference resonator before a material detection operation
- FIG. 6B shows measured insertion phase curves of the sensing and reference resonators of FIG. 6A after the material detection operation.
- a bulk-acoustic wave piezoelectric resonator 20 is used as a sensor to detect the existence of a given material.
- the resonator 20 typically includes a planar layer of piezoelectric material bounded on opposite sides by two respective metal layers which form the electrodes of the resonator.
- the two surfaces of the resonator are free to undergo vibrational movement when the resonator is driven by a signal within the resonance band of the resonator.
- at least one of its surfaces is adapted to provide binding sites for the material being detected.
- the binding of the material on the surface of the resonator alters the resonant characteristics of the resonator, and the changes in the resonant characteristics are detected and interpreted to provide quantitative information regarding the material being detected. It is a feature of the present invention to derive such quantitative information by detecting a change in the insertion phase shift of the resonator caused by the binding of the material being detected on the surface of the resonator.
- the present invention inserts the resonator in the path of a signal of a pre-selected constant frequency, and monitors the variation of the insertion phase shift caused by the binding of the material being detected on the resonator surface.
- FIG. IA shows the resonator 20 before the material being detected is bound to its surface 26.
- the resonator 20 is electrically coupled to a signal source 22, which provides an input electrical signal 21 having a frequency f within the resonance band of the resonator.
- the input electrical signal is coupled to the resonator 20 and transmitted through the resonator to provide an output electrical signal 23.
- the output electrical signal 23 is at the same frequency as the input signal 21, but differs in phase from the input signal by a phase shift ⁇ ⁇ , which depends on the piezoelectric properties and physical dimensions of the resonator.
- the output signal 23 is coupled to a phase detector 24 which provides a phase signal related to the insertion phase shift.
- IB shows the sensing resonator 20 with the material being detected bound on its surface 26.
- the same input signal is coupled to the resonator 20. Because the resonant characteristics of the resonator are altered by the binding of the material as a perturbation, the insertion phase shift of the output signal 25 is changed to ⁇ 2 . The change in insertion phase shift caused by the binding of the material is detected by the phase detector 24. The measured phase shift change is related to the amount of the material bound on the surface of the resonator.
- the sensing resonators may be conventional quartz resonators or the more recently developed thin- film resonators. Nevertheless, thin-film resonators are generally preferred because of their high resonance frequencies and the accompanying higher sensitivities.
- a thin-film resonator used as the sensing element may be formed to support either longitudinal or shear bulk-acoustic wave resonant modes. Longitudinal-mode TFR sensors can be effectively used in a vacuum or gaseous environment. On the other hand, shear-mode TFR sensors are more suitable for use in a liquid sample. This is because a longitudinal-mode resonance is severely damped by the presence of liquid at the surface, while a shear mode resonance is only partially damped.
- FIG. 2 shows a simple sensor system embodying the invention that has a one-port resonator 27 as the sensing element.
- a one-port resonator has one electrode that is used for both signal input and output. The other electrode of the one-port resonator is typically grounded.
- a signal source 28 provides an input signal which has a frequency within the resonant bandwidth of the sensing resonator 27.
- the input signal is coupled to a power divider 30, which splits the input signal into two portions.
- One portion of the input signal is sent through a coupler 32 to the input/output electrode 29 of the resonator 27.
- the input signal is transmitted across the resonator 27 and reflected back to the electrode 29.
- the output signal i.e., the reflected signal which has an insertion phase shift with respect to the input signal
- the coupler 32 is a directional device that is capable of separating the output signal from the input signal.
- the output signal is directed by the coupler 32 to a phase detector 36 as a sensor signal 35.
- the second portion of the input signal is also sent from the power divider 30 to the phase detector 36 as a reference signal 37.
- the phase detector 36 processes the sensor signal and the reference signal to provide a phase signal indicative of a phase difference between the sensor and reference signals.
- the sensing resonator In a sensing operation, the sensing resonator is exposed to the material being detected, and the insertion phase shift changes as a result of the binding of the material on the surface of the resonator 27.
- This change is reflected in the phase signal generated by the phase detector 36.
- phase detection approach of the invention is that the input signal is maintained at a pre-selected constant frequency during measurement.
- a stable signal source with an adjustable signal frequency is relatively simple and inexpensive to construct, in contrast to the rather complicated and expensive temperature-compensated high- frequency oscillator circuitry required by the conventional approach of tracking the changing oscillation frequency of the resonator.
- the signal source 28 may be a frequency synthesizer. Frequency synthesizers are relatively inexpensive and readily available.
- the phase detector 36 in the illustrated embodiment includes a double-balanced mixer 44 ( or a mathematical multiplier) which receives the sensor and reference signals.
- the sensor signal and the reference signal can be expressed respectively as A sen cos(fot) and A re fCOS (&>t-
- ⁇ is the phase difference between the sensor signal and the reference signal.
- the mixer 44 multiplies the sensor signal and the reference signal to produce a signal
- Adet ( t ) L (A S enA re f ) COS (kt ) COS (kt- ⁇ )
- L (A se nA re f) is a generic loss function.
- the loss function L(A sen A re f) is therefore a constant.
- the term L (A se nA re f) (1/2) cos ( ⁇ ) varies with the phase difference, ⁇ , but does not vary with time, i.e., it is a DC term.
- the output of the mixer 44 is passed through a low-pass filter 46 which eliminates the time dependent term in Aet and leaves only the DC term as the output of the phase detector 36. In this way, the phase detector provides a DC voltage signal indicative of a phase difference between the sensor signal and the reference signal.
- the measured phase shift change can be used to derive the total amount of the material bound on the surface of the sensing resonator.
- the DC voltage signal can be monitored as a function of time to determine the rate at which the insertion phase shift changes. This rate of change relates to the rate at which the material being detected binds to the surface of the sensing resonator 27. If the resonator is used in an aqueous environment, the rate of change provides an indication of the concentration or density of the material being detected in the liquid.
- the exposure of a sensing resonator to the material being detected involves subjecting the resonator to different environmental conditions which can also alter the resonant characteristics of the resonator.
- the resonator when used as a thickness monitor in an epitaxial deposition operation, the resonator is often subjected to heat which could shift the resonance frequency.
- the contact of the surface with the liquid also introduces certain viscosity loading effects that are separate from the effects caused by the binding of the molecules on the surface. Such environmental effects can mask the phase change caused by the material being detected and generate erroneous results.
- such environmental effects are effectively distinguished from the material binding effects by the use of a reference resonator.
- the reference resonator preferably has resonant characteristics sufficiently close to those of the sensing resonator so that the phase shifts of the two resonators caused by the environmental effects are very similar in magnitude.
- the sensing and reference resonators are subject to substantially identical environmental conditions. Nevertheless, the material to be detected is prevented from binding on the surface of the reference resonator. This can be achieved by blocking the surface of the reference resonator from the material being detected, or by coating only the sensing resonator to provide the needed binding sites for the material.
- the environmental conditions are expected to cause substantially the same insertion phase shift change in the two resonators. Since the material being detected does not bind on the reference resonator, the phase shift change of the reference resonator reflects mainly the environmental effects. The phase shift change of the reference resonator is subtracted from the total phase shift change of the sensing resonator to provide a difference signal which reflects mainly the material binding effects .
- FIG. 3 shows a sensing system which has a one-port sensing resonator 50 and a one-port reference resonator 52.
- the signal source, power divider, and phase detector used in this system are identical to those in the system of FIG. 2 and are therefore identically numbered.
- the sensing resonator 50 and the reference resonator 52 preferably have very similar resonant characteristics and substantially overlapping resonant bands.
- the signal source 28 provides an input signal of a frequency which is within the overlapping portion of the resonant bands of the resonators and preferably is set equal to the average of the resonance frequencies of the two resonators.
- the input electrical signal provided by the signal source 28 is split by a power divider 30 and the split signals are coupled through couplers 56, 58 to the respective sensing and reference resonators 50, 52.
- the output signals of the resonators are directed to the phase detector 36 by the respective couplers 56, 58 as sensor and reference signals.
- the phase detector 36 processes the sensor and reference signals to produce a phase signal indicative of a phase difference between the two signals. As described above, this phase difference is expected to be caused mainly by the binding of the material being detected on the surface of the sensing resonator 50.
- the phase detection according to the invention can also be advantageously implemented with two-port resonators.
- a two-port resonator has one electrode for receiving an input signal, and a second electrode for providing an output signal.
- FIG. 4 shows a sensing system which has a two-port sensing resonator 60 and a two-port reference resonator 62.
- the sensing and reference resonators preferably have very similar resonant characteristics, and the resonant bands of the two resonators substantially overlap with each other.
- a signal source 28 provides an input electrical signal which has a frequency within the overlapping portion of the resonant band of the two resonators.
- the input signal is split by a power divider 30, and the split signals are coupled to the respective input electrodes 64, 66 of the sensing and reference resonators 60, 62.
- the input signals are transmitted through the resonators to form output electrical signals at the respective output electrodes 68, 70 of the sensing and reference resonators.
- the output signals of the two resonators are coupled to the phase detector 36, which produces a phase signal indicative of a phase difference between the two output signals. Quantitative information of the material bound on the surface of the sensing resonator can then be derived from the phase signal.
- the two-port reference/sensing resonator combination described above is implemented as a monolithically fabricated three-port device which comprises basically two two-port thin-film resonators with their input electrodes connected to a common input.
- the two resonators 72, 74 are supported on a thin Si0 2 layer 76 which is thermally grown on a silicon substrate 78.
- the Si0 2 layer 76 has a thickness of about 1000 A.
- the Si substrate 78 has thickness of about 345 ⁇ , a width of 4 mm and a length of 12 mm.
- the portions of the Si substrate under the resonators are etched away to allow the resonators to undergo resonant movement.
- the bottom of the Si substrate 78 has a layer of silver paint 80 applied thereto which serves as a grounding plane.
- the resonator 72 has an epitaxially deposited A1N layer 82 grown to a thickness of about 2.35 ⁇ m to provide a shear mode resonance frequency of 900 MHz.
- the piezoelectric layer may be formed of ZnO.
- the A1N layer 82 is in the shape of a square of side width of 500 ⁇ m.
- a rectangular input electrode 86 and a rectangular output electrode 88 are formed on opposite sides of the piezoelectric layer 82.
- Each of the electrodes 86, 88 is a 0.5 ⁇ m thick Al layer.
- the width of the electrodes is about 200 ⁇ .
- the overlapping portion of the two electrodes 86, 88 defines a square active area of the resonator 72, which is about 200 ⁇ m by 200 ⁇ m.
- the size of the active area of the resonator is selected to keep the static capacitance of the resonator sufficiently small to avoid distortion of the phase response of the resonator around resonance. With the chosen size and thickness of the active area of the resonator, the static capacitance is about 0.64 pF.
- the other resonator 74 is generally a mirror image of the resonator 72, with an AIN layer 84 formed between an input electrode 90 and an output electrode 92. Due to the symmetry of the two resonators, either resonator can be prepared, such as by applying a proper coating, for use as the sensing resonator. The other resonator is then used as the reference resonator.
- the input electrical signal is coupled to the two resonators via a transmission line 96 formed on the substrate.
- the transmission line 96 is a deposited Al strip which has a width of 277 ⁇ m and a thickness of 0.5 ⁇ m. The dimensions of the transmission line are chosen to provide a 50 ⁇ impedance on the Si substrate.
- Similar transmission lines 97, 98 are connected to the output electrodes 88, 92 of the two resonators 72, 74, respectively, for coupling the respective output signals to a phase detector.
- the transmission line 96 conducts the input electrical signal to a power divider 91 which splits the input electrical signal into two portions.
- the split signals are conducted to the respective input electrodes 86, 90 of the two resonators by a deposited Al strip 94 which has the same width as the input electrodes.
- the power divider 91 is in the form of a T-junction of the transmission line 96 and the connecting strip 94.
- This T-junction power divider is simple in structure and easy to fabricate. Nevertheless, other types of power dividers may also be used.
- the T-junction may be replaced by a Wilkinson power divider which is only slightly more complicated in design but provides better isolation between the two resonators.
- the two resonators are disposed close to each other on the same substrate.
- the proximity ensures that the two resonators are subjected to substantially identical environmental conditions during a material sensing operation.
- sufficient distance should be provided to reduce cross talk between the two resonators.
- the centers of the two resonators are separated by about 2000 ⁇ m.
- Another important advantage of forming the sensing and reference sensors in close proximity on the same substrate is that the two resonators are likely to have closely matched resonant frequencies and phase responses. The matched phase responses allow accurate phase shift measurements and effective cancellation of environmental effects.
- the general structure of the monolithic sensing/reference resonator combination described above can be used to fabricate sensing devices with more than two resonators on a given substrate.
- two or more three-port TFR devices each having a sensing resonator and a reference resonator can be monolithically fabricated on one substrate.
- the output of the sensing resonator in each three-port device can be referenced to the output of the reference resonator in the same device.
- the sensor can be formed as a multiple- port device with one reference resonator and two or more sensing resonators, with the input electrodes of the resonators connected to a common signal input.
- each of the sensing resonators is referenced to the output of the reference resonator.
- TFR structures may be used to fabricate multiple-resonator sensors for use with the phase detection technique of the invention.
- a resonator network illustrated in FIG. 7A of U.S. Patent 5,231,327 to Ketcham includes two resonators which share a common input electrode.
- One of the resonators may be used as the reference resonator, and the other the sensing resonator.
- the '327 patent is hereby incorporated by reference.
- FIGS. 6A and 6B show measured results taken with a longitudinal-mode three-port TFR sensing device which has a sensing resonator and a reference resonator arranged in the general structure shown in FIGS. 5A and 5B.
- the sensor was used to detect Listeria bacteria in an aqueous sample.
- the surface of the sensing resonator was coated with the antibody for the Listeria bacteria.
- the antibody molecules provided strong binding sites for the bacteria.
- the surface of the reference sensor was coated with a different antibody which was not expected to have significant binding with the Listeria bacteria in the liquid sample.
- FIG. 6A shows the phase curves 102, 104 region for the sensing and reference resonators, respectively, taken before the sensing operation.
- the resonance frequency of the sensing resonator was 840.1 MHz, as indicated by the marker 106
- the resonance frequency of the reference resonator was 834.5 MHz, as indicated by the marker 108. It can be seen that the phase bands of the two resonators have significant overlap.
- the sensor was used in the phase detection system of FIG. 4.
- the frequency of the input electric signal for the two resonators was set close to 837.25 MHz (indicated by the marker 110) , which was about the medium of the resonant frequencies of the two resonators. At that frequency, the insertion phase difference between the sensing and reference resonators was about 41 degrees.
- FIG. 6B shows the measured phase curves 112, 114 of the two resonators after this binding procedure. It will be appreciated that the phase curves of the resonators are provided in FIGS. 6A and 6B only for the purpose of illustrating the operating principles of the invention. If the sensing system of FIG. 4 is used, it will not be necessary to scan over the entire resonance region.
- the input signal will be set at a constant frequency, such as 837.25 MHz, and the phase difference between the resonators at that frequency will be detected and indicated by the phase signal generated by the phase detector.
- a constant frequency such as 837.25 MHz
- the phase difference between the sensing resonator and the reference resonator was altered by the binding process.
- the phase difference between the two resonators was reduced to about 30 degrees.
- the binding of the material being detected on the surface of the sensing resonator changed the insertion phase difference by about 11 degrees at the selected input frequency of 837.25 MHz.
- the sensing and reference resonators are monolithically formed as a thin-film multiple-port sensing device. The monolithic construction ensures close matching of the resonant characteristics of the sensing and reference resonators, thereby allowing accurate measurement and effective cancellation of environmental effects.
Abstract
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EP98931725A EP1018173A1 (en) | 1997-06-30 | 1998-06-29 | Method and system for detecting material using piezoelectric resonators |
BR9810479-9A BR9810479A (en) | 1997-06-30 | 1998-06-29 | Method and system for detecting material using piezoelectric resonators |
CA002295225A CA2295225A1 (en) | 1997-06-30 | 1998-06-29 | Method and system for detecting material using piezoelectric resonators |
AU81768/98A AU8176898A (en) | 1997-06-30 | 1998-06-29 | Method and system for detecting material using piezoelectric resonators |
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US08/884,991 | 1997-06-30 | ||
US08/884,991 US5932953A (en) | 1997-06-30 | 1997-06-30 | Method and system for detecting material using piezoelectric resonators |
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EP (1) | EP1018173A1 (en) |
AU (1) | AU8176898A (en) |
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CA (1) | CA2295225A1 (en) |
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Also Published As
Publication number | Publication date |
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EP1018173A1 (en) | 2000-07-12 |
BR9810479A (en) | 2000-09-12 |
US5932953A (en) | 1999-08-03 |
AU8176898A (en) | 1999-01-19 |
CA2295225A1 (en) | 1999-01-07 |
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