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WO2001001121A1 - Analyse plurimodale de structures micromecaniques destinee a la detection d'applications - Google Patents

Analyse plurimodale de structures micromecaniques destinee a la detection d'applications Download PDF

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Publication number
WO2001001121A1
WO2001001121A1 PCT/US2000/017379 US0017379W WO0101121A1 WO 2001001121 A1 WO2001001121 A1 WO 2001001121A1 US 0017379 W US0017379 W US 0017379W WO 0101121 A1 WO0101121 A1 WO 0101121A1
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Prior art keywords
frequency
detector
phase
mechanical
mode
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Ceased
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PCT/US2000/017379
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English (en)
Inventor
Patrick Ian Oden
Charles L. Britton, Jr.
Stephen F. Smith
Robert J. Warmack
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UT Battelle LLC
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UT Battelle LLC
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Priority to AU58871/00A priority Critical patent/AU5887100A/en
Publication of WO2001001121A1 publication Critical patent/WO2001001121A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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

Definitions

  • This invention relates to improved methods and apparatus for detecting and quantifying physical forces and chemical entities using micromechanical structures. More specifically, the invention is directed to the use of not only the fundamental resonance of the mechanical structure for sensing but also combining this signal with one or more higher order mechanical resonances to enhance the sensitivity (signaltonoise ratio). Furthermore, such a technique/apparatus may be used to determine various film properties of deposited structures on surfaces.
  • Thundat et al. teach the use of fundamental as well as second and third order mechanical resonances of a cantilever structure. This is achieved only through selective deposition of coating materials at particular locations on the structure. Each of the resulting coating schemes creates a different set of structural resonance characteristics. Species to be measured then interact at sites on the structure ' s mechanical nodes as determined by the selective coating scheme. The method requires a complicated selective coating and is not feasible for routine production at this time. Furthermore, such a coating scheme would work only for a specific mechanical mode of the resonating structure.
  • a device and a method for analyzing changes in micromechanical structure response utilizes the multi-resonant character of mechanical oscillators to enhance sensor response by simultaneously monitoring the location, in frequency, of one or more of the mechanical resonance modes and correlating the signal against the concentration of the detectable species in the appropriate space.
  • the method requires the identification of the shifts in frequency for different modes or overtones of the fundamental frequency.
  • Figure 1 is a schematic view of a piezoelectric transducer and mechanical resonator sensing apparatus before end loading of the mass to be sensed.
  • Figure 2 is a schematic view of the piezoelectric transducer and mechanical resonator apparatus illustrated in Figure 1 after end loading the mass.
  • Figure 3 is a schematic representation of the system used to control and monitor multi-mode sensor response.
  • Figure 4 is a graph of theoretical frequency shift as related to increased resonance mode, based on gravimetric measurements using the apparatus illustrated in Figure 1.
  • Figure 5 is a graph of mass induced frequency shifts vs. deposited mass for modes 1 through 8.
  • Figure 6 is a graph the relative sensitivity to mass induced frequency shifts at various modes using experimental data illustrated in Figure 4.
  • Figure 7 is a semi-log plot of an experimental versus theoretical comparison of the end-loaded sensitivity (gravimetric) of a silicon beam structure. Squares are experimental and circles are theoretical points.
  • Figure 8 is a simplified graph illustrating frequency shifts and separations as the mode number is increased.
  • Figure 9 is graph of frequency shifts resulting from deposition of a thin gold (Au) film on a silicon (Si) cantilever bar.
  • Figure 10 is a plot of frequency fluctuation vs. time over a two-minute interval.
  • Figure 11 is a block diagram showing a basic detector circuitry for monitoring the cantilever resonance response.
  • Figure 12 is a block diagram of a dual-channel compensation scheme for monitoring the cantilever resonance response.
  • Figure 13 is a block diagram of a dual-channel mixing compensation scheme for monitoring the cantilever resonance response.
  • FIG 14 is a block diagram of an instrument system according to this invention.
  • a multi-modal analysis of cantilever structures may be used to improve physical, chemical and biological sensing. This is generally accomplished by measuring the fundamental frequency in conjunction with a number of higher order modes of the mechanical structure and monitoring changes or shifts in these responses upon exposure to selected species to be detected in the environment of the detector.
  • the present invention provides a method and apparatus to dramatically enhance the sensitivity of these measurements to such mass or stress changes by using higher-order modes in particular.
  • the present invention provides enhanced knowledge of the dynamic character of a resonator based upon the relative changes of different modal resonances, it can further be used with a micro-centrifugal separator system by allowing differentiation between aerosols based on their mass as they distribute along the length of the resonator structure.
  • An additional use is process characterization of coating methods and structural uniformity for micromechanical systems.
  • MEMS microelectromechanical systems
  • One scheme will use cantilevered structures placed in a variety of locations along a wafer followed by monitoring the changes in modal resonance as a coating or processing step is performed.
  • a related scheme will involve observation of the uniformity of the coating over one resonator structure and monitor relative changes in modal resonance character of this individual structure.
  • the method of this invention may be useful in theoretical studies directed to a better understanding of the physical properties of cantilevers and coated cantilevers. Higher order resonances are useful for determining the density, mechanical dimensions and Youngs's modulus for fabricated structures. Such determinations may be used for quality control to determine structure thickness and length and the thickness of an applied coating.
  • Microcantilevers are typically made of materials such as silicon and silicon nitride, as well as fabricated ceramic, high performance ceramic, or other ceramic specifically composed of a number of substances and combinations of substances, including but not limited to elements of group 14 (IUPAC IVB, CAS IV A) and groups 13/15 (IUPAC IIIB, CAS IIIA/VB,VA). Though other methods exist, the oscillation of these structures is normally induced through the use of a piezoelectric transducer.
  • While oscillating, these structures also referred to inter alia as beams, resonators, cantilevers, microcantilevers, mechanical resonators, micromechanical resonators, mechanical beams, oscillating bars, and resonating microbars, are susceptible to changes (or shifts) in oscillation frequency (or resonance) brought on by effective changes in their geometry and/or structural characteristics or outside forces.
  • the microcantilever may respond to pressure (e.g. light, particles, etc) or changes induced by particles.
  • Coated microcantilevers may respond to selective adsorption of gasses and particles or reactions or other physical interaction modalities.
  • the present invention also comprehends the acquisition of multi-modal frequency shifts at different times but under the same stress or signal conditions, under the assumption that these frequency shifts remains relatively stable over time.
  • the present invention considers several higher modes of oscillation up to and including an excitation frequency around 2.8 MHz, the current limit of commercially available sensors. Theoretically, the measurements could be made at even higher frequencies.
  • FIG 1 is a schematic representation of device 1 , a microcantilever 3 mounted on a piezoelectric (PZT) device 5.
  • Cantilever 3 has a thickness t, a Young ' s modulus E and a density P.
  • Figure 2 is an illustration of the device of Figure 1 having an additional mass 7 deposited at the distal region of the bar. Under these conditions, the new thickness is t*, the Young's Modulus is E* and the density P*.
  • Figure 3 is a schematic representation of the system used to control and monitor multi-mode sensor response.
  • the sensor of Figure 1 with a suitable coating (Fig.2), is caused to vibrate by the PZT device.
  • the vibration is detected using a laser and a photodetector to monitor the vibration. Collectively they are shown as 11.
  • a modal response processing system 13 interfaces the detector to a data acquisition system 15 and is used to seek frequencies on the basis of projected locations or by manual tuning or by use of a software searching sequence.
  • n is the specific mode of oscillation
  • t E
  • t E
  • the symbol is a quantity dependent upon the geometry of the resonator and is determined by solving the equation:
  • sensing is accomplished by monitoring changes in response frequency of the device. These changes are induced either by alterations in the material properties of the device, such as through mass addition for gravimetric sensing (e.g. Fig.2) or exposure to chemical processes on the structure's active area, or through changes in the geometry of the active surface area.
  • S m becomes the definition of the sensitivity of the device.
  • Typical sensitivities of prior art devices are in the range of 10 cm 2 /gm to 200 cm 2 / gm. With this method device, sensitivities in the range of 2000-3000 cm 2 /gm have been observed.
  • Multiple or arrayed sensors may be used to detect different entities in the same sample by using different coatings. Alternatively, two or more different coatings might be applied to the same microcantilever. Examples of suitable coatings are numerous. Metals, especially noble metals, may be applied by sputtering. Coatings may be applied by microsyringe, brush, Q-tip®, spin casting, dipping, air-brush spraying, Langmuir-Blodgett film transfer, plasma deposition, evaporation, sublimation and self-assembled monolayers as described in U.S. patent 5,445,008. Biosensors may be attached by the methods disclosed in Bastiaans, U.S. patent 4,735,906 or Nakagawa, U.S. patent 5,363,697.
  • One variation of this concept is to use a frequency shift method (i.e.: frequency mixing) to fold higher-order mechanical mode resonances into a lower frequency band so as to enhance the signal-to-noise ratio for the device and therefore, enhance the sensitivity. In such manner, the errors inherent in measurements of higher frequencies can be minimized
  • the present invention enables not only acquisition of a signal from a single mode of response, but rather a system which provides a collective measure of many mechanical modes which in turn greatly enhances obtainable knowledge about a mechanical system as applied to sensing. Comparison of the shifts observed for each mode enables one to study the effects of changes in composition of the cantilever and of changes in coatings. Each sensor can be calibrated at the highest detectable mode even though used at a lower frequency.
  • the present invention quite surprisingly provides for dramatically superior sensitivity in the detection of barometric pressure (including very high vacuum) and analytes such as mercury vapor, hydrogen, chemical and biological warfare agents and other airborne entities for which early detection of parts-per-billion to parts-per-trillion amounts is considered critical.
  • barometric pressure including very high vacuum
  • analytes such as mercury vapor, hydrogen, chemical and biological warfare agents and other airborne entities for which early detection of parts-per-billion to parts-per-trillion amounts is considered critical.
  • the first was composed of polycrystalline silicon, with minimal dimensions of 397 ⁇ m, 29 ⁇ m, 2 ⁇ m (length, width, thickness) provided by Park Scientific Instruments, Inc. (Sunnyvale, CA) and used in force-constant calibrations of force-microscopy cantilever scanning styli.
  • the second structure is a silicon nitride (SiN x ) structure with nominal dimensions of 200 ⁇ m, 20 ⁇ m, 0.6 ⁇ m (length, width, thickness), commercially available for force-microscopy applications from Digital Instruments, Inc. (Santa Barbara, CA).
  • a standard laser-deflection apparatus with an integrated piezoelectric stage (PZT) for exciting the beam structure into resonance was used (Digital Instruments Nanoscope III Multi-mode laser-deflection head).
  • PZT piezoelectric stage
  • HP3589A network/spectrum analyzer was used to provide the drive signal-to-response measurements using the split-segment photodetector signal. Mechanical-resonance amplitude and phase responses were then exported to a computer for further processing.
  • the fundamental and several higher mode resonances for the beams were measured by exciting the structure through PZT crystal with a 0.5-V RMS sinusoidal signal and monitoring the amplitude and phase signal through the resonance point.
  • the cantilever holder assemblies then were transferred to a turbomolecular-pump-driven high- vacuum system with an integrated electro-beam evaporation system.
  • the beams were masked with a glass cover slip to expose only the extreme end to deposition in order to limit the measurement to mass-deposition processes only.
  • Deposition of a thin gold film through the shadow mask was performed in a 5 x 10 "5 Torr vacuum at a rate of 0.05-0.1 nm/sec. After removal from the chamber, the deposition area was determined by optical microscopy. In the case of the silicon bar, the area was 1.26 x 10 "9 m 2 ( 11 % of total structural area); for the SiN x structures, 6.3 x 10 '10 m 2 - (or 16% area).
  • Frequency-stability measurements ultimately determine a minimum-detectable mass (MDM) or mass density (MDMD) that the sensor can deliver. Therefore, to illustrate the full potential of the present invention, it was necessary to investigate the stability with which frequency measurements can be made for the different modes of oscillation.
  • MDM minimum-detectable mass
  • MDMD mass density
  • Frequency stability was used along with the mass sensitivity of each mode to determine a minimum-detectable mass or mass density.
  • the results of Figure 10 show the typical frequency fluctuation observed for these structures. Specifically, it shows the eighth-mode resonance of the 2 ⁇ m thick silicon structure. In all measures of the frequency stability made in the two- or four- minute time scale, a stability in the center frequency within 0.1 to 0.4 Hz was observed through all the observed resonance modes (as determined by the nominal one-standard-deviation spread). This, taken together with the enhanced mass sensitivity of the higher resonance modes, shows that these higher modes exhibit an inherently greater gravimetric sensitivity. As also illustrated in Figure 9, the standard deviation of the signal is 0.179 Hz.
  • the minimum detectable mass density for this mode is shown to be 0.57 ng/cm 3 , which equates to a minimum detectable mass of 7.2 fg for this test structure, or one part in 7.46 ( 10 6 when compared to the total mass of the cantilever.
  • Applying the same analysis to the corresponding data for the ninth mode of the SiN x structure yielded a standard deviation of 0.256 Hz around the center frequency, which represents a minimum-detectable mass density of 0.35 ng/cm 2 . This equates to a minimum-detectable mass of 2.2 fg on the sensor (one part in 13.38 ( 10 6 when compared to the entire cantilever).
  • the present invention provides a method of gravimetrically sensing mass on the order of femtograms.
  • the mechanical structure response must be appropriately converted to electrical signals which can be amplified or otherwise conditioned (e.g., filtered, frequency-shifted, or analyzed) by more-or-less conventional means, such as analog, digital, or mixed-mode integrated circuit (IC) devices.
  • IC integrated circuit
  • the electronic subsystem will be incorporated into a custom application-specific integrated-circuit (ASIC) chip for higher production levels.
  • ASIC application-specific integrated-circuit
  • FIG. 11 A block diagram of a basic readout circuit is shown in Figure 11 below.
  • the fundamental sensing mechanism for cantilever 21 is that of resonance-frequency locking, through a phase-locked loop (PLL) topology which samples the drive 23 and microsensor signals 25, compares their respective phases in the Phase Detector block 29, filters the error voltage in the Nonlinear Integrator 31 , and applies the smoothed adjustment signal to the control input of the Sine VCO (voltage-controlled oscillator) 33, which generates the variable-frequency/phase sinusoidal drive signal to excite the mechanical structure (e.g., cantilever).
  • PLL phase-locked loop
  • the diagram indicates the availability of both 0° and 90° phases of the drive signal from the VCO; this configuration is often useful for optimum phase-detector performance and affords tightest and most accurate PLL locking (and sensor reading), particularly in low signal-to-noise conditions.
  • Several advanced composite phase-detector circuits can be employed here to accomplish these goals in an inexpensive ASIC format.
  • the next two drawings ( Figures 12 and 13) provide the signal flows for differential measurement topologies which can further enhance the effective accuracy, repeatability, and stability of the basic mechanical-structure sensing scheme.
  • two identical, proximally mounted sensor devices one being coated (41) and one reference uncoated (43) are deployed with identical PLL drive/readout electronic channels 45 a and 45b.
  • Sensor#l is the primary measurement device and is coated to sense the selected species or other parameter of interest. It resonates at a nominal frequency/;.
  • the matching Sensor #2 is completely identical, except that it is not coated; it operates at/.
  • the outputs of both readout circuits are sent to a frequency comparator 47, which calculates the absolute value of the difference-frequency, l/;- l.
  • This offset value represents the change in the mechanical resonance (presumedly at any one or more of the higher-order modes) due to the desired parameter only; at least to a first order, the common-mode effects of pressure, temperature, vibration, power-supply voltage, time, etc. which affect both devices equally will be canceled out.
  • Figure 14 provides a suggested block-level diagram of a complete measurement system based on the present technology.
  • the main frequency-control (PLL) loop includes a low-noise composite phase detector, a following nonlinear integrator/low-pass filter to smooth the loop error voltage, and one or more sine-wave VCO modules, and an output-drive power amplifier to excite the cantilever (or other mechanical structure used for sensing).
  • PLL power amplifier
  • transient drive/readout waveforms e.g., pulse, wavelet
  • Multichannel architecture ideal for ASIC implementation - Multichannel architecture ideal for ASIC implementation; - Ability to store ensembles of mode-frequency sets as a signature (including amplitudes);
  • - IM measurements could be used to continually assess cantilever/mechanical system health (via appearance of nonlinearities); - Processing to permit tradeoffs of noise bandwidths vs. speed of measurement;

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  • Physics & Mathematics (AREA)
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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Measurement Of Mechanical Vibrations Or Ultrasonic Waves (AREA)

Abstract

L'invention concerne un dispositif et un procédé permettant de déterminer les concentrations d'espèces dans un environnement au moyen d'un résonateur mécanique. Le procédé repose sur l'utilisation d'au moins une structure en porte-à-faux dans lesquelles plusieurs résonances en mode mécanique sont déterminées pour la structure au cours des mesures, et utilisées pour déterminer les modifications de l'environnement autour du dispositif, ou pour mesurer les modifications des dimensions fondamentales ou les propriétés matérielles de la structure/de la couche supérieure de matière déposée sur la structure.
PCT/US2000/017379 1999-06-29 2000-06-23 Analyse plurimodale de structures micromecaniques destinee a la detection d'applications Ceased WO2001001121A1 (fr)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1452852A1 (fr) * 2003-02-28 2004-09-01 ANT Technology Co., Ltd. Biocapteur à haute résolution
WO2004095011A1 (fr) * 2003-04-17 2004-11-04 Akubio Limited Detection de capteurs de phenomenes de rupture
EP1607725A4 (fr) * 2003-03-25 2007-09-19 Seiko Epson Corp Procede et instrument de mesure de masse, et circuit d'excitation de piece vibratoire piezo-electrique pour mesure de masse
GB2473635A (en) * 2009-09-18 2011-03-23 Cambridge Entpr Ltd Detecting concentration of target species
US8288154B2 (en) * 2002-10-21 2012-10-16 Alegis Microsystems Nanomotion sensing system and method
EP2325630A3 (fr) * 2009-11-13 2013-02-13 Honeywell International Inc. Appareil différentiel à nanocapteurs résonants et procédé
AT514855A1 (de) * 2013-10-04 2015-04-15 Univ Wien Tech Vorrichtung zur Fraktionierung von in einer Flüssigkeit enthaltenen Partikeln
US9279792B2 (en) 2011-04-13 2016-03-08 3M Innovative Properties Company Method of using an absorptive sensor element
US9429537B2 (en) 2011-04-13 2016-08-30 3M Innovative Properties Company Method of detecting volatile organic compounds
US9506888B2 (en) 2011-04-13 2016-11-29 3M Innovative Properties Company Vapor sensor including sensor element with integral heating
US9658198B2 (en) 2011-12-13 2017-05-23 3M Innovative Properties Company Method for identification and quantitative determination of an unknown organic compound in a gaseous medium
EP3575784A1 (fr) * 2018-05-28 2019-12-04 Consejo Superior de Investigaciones Cientificas (CSIC) Procédé et système d'analyse d'analytes par transduction de résonance mécanique
US10782240B2 (en) * 2013-09-04 2020-09-22 Applied Invention, Llc Test mass compensation of mass measurement drift in a microcantilever resonator

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EP0072744A2 (fr) * 1981-08-17 1983-02-23 Allied Corporation Capteur chimique
EP0215669A2 (fr) * 1985-09-17 1987-03-25 Seiko Instruments Inc. Diagnostique et procédé d'analyse de composés biochimiques, microbes et cellules
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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8288154B2 (en) * 2002-10-21 2012-10-16 Alegis Microsystems Nanomotion sensing system and method
EP1452852A1 (fr) * 2003-02-28 2004-09-01 ANT Technology Co., Ltd. Biocapteur à haute résolution
EP1607725A4 (fr) * 2003-03-25 2007-09-19 Seiko Epson Corp Procede et instrument de mesure de masse, et circuit d'excitation de piece vibratoire piezo-electrique pour mesure de masse
WO2004095011A1 (fr) * 2003-04-17 2004-11-04 Akubio Limited Detection de capteurs de phenomenes de rupture
US7543476B2 (en) 2003-04-17 2009-06-09 Akubio Limited Rupture event sensors
GB2473635A (en) * 2009-09-18 2011-03-23 Cambridge Entpr Ltd Detecting concentration of target species
WO2011033285A1 (fr) * 2009-09-18 2011-03-24 Cambridge Enterprise Limited Appareil et procédé permettant de détecter des espèces cibles dans un analyte
EP2325630A3 (fr) * 2009-11-13 2013-02-13 Honeywell International Inc. Appareil différentiel à nanocapteurs résonants et procédé
US9506888B2 (en) 2011-04-13 2016-11-29 3M Innovative Properties Company Vapor sensor including sensor element with integral heating
US9279792B2 (en) 2011-04-13 2016-03-08 3M Innovative Properties Company Method of using an absorptive sensor element
US9429537B2 (en) 2011-04-13 2016-08-30 3M Innovative Properties Company Method of detecting volatile organic compounds
US9658198B2 (en) 2011-12-13 2017-05-23 3M Innovative Properties Company Method for identification and quantitative determination of an unknown organic compound in a gaseous medium
US10782240B2 (en) * 2013-09-04 2020-09-22 Applied Invention, Llc Test mass compensation of mass measurement drift in a microcantilever resonator
AT514855B1 (de) * 2013-10-04 2015-08-15 Univ Wien Tech Vorrichtung zur Fraktionierung von in einer Flüssigkeit enthaltenen Partikeln
AT514855A1 (de) * 2013-10-04 2015-04-15 Univ Wien Tech Vorrichtung zur Fraktionierung von in einer Flüssigkeit enthaltenen Partikeln
EP3575784A1 (fr) * 2018-05-28 2019-12-04 Consejo Superior de Investigaciones Cientificas (CSIC) Procédé et système d'analyse d'analytes par transduction de résonance mécanique
WO2019229000A1 (fr) 2018-05-28 2019-12-05 Consejo Superior De Investigaciones Cientificas (Csic) Procédé et système d'analyse d'analytes par transduction de résonance mécanique

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