ACOUSTIC WAVE SENSORS

I. II. III.

Types and Principles of Operation Markets and Applications Technical Examples

This presentation is divided into three sections. The first section describes the construction and operation of the various types of acoustic wave sensing elements. The second section explains some of the sensor markets and applications. The final section is the bulk of the presentation and presents four sensor examples in detail.

ACOUSTIC WAVE SENSORS Part I

Types and Principles of Operation

This first section presents the basic operation of BAW and SAW sensors in detail and briefly describes surface transverse wave, love mode, and acoustic plate mode sensors.

Acoustic Wave Sensors

Definition of a Sensor:

A device that responds to a physical, chemical, biological, or electrical stimulus by producing an electrical output signal that is a function of the input stimulus For acoustic wave devices, we monitor the change in oscillation frequency when the device responds to the input stimulus

ACOUSTIC WAVE SENSOR

INPUT STIMULUS PHYSICAL, CHEMICAL, BIOLOGICAL, ELECTRICAL

TRANSDUCTION OF THE INPUT STIMULUS TO THE ACOUSTIC WAVE DEVICE

OUTPUT SIGNAL CHANGE IN RESONANT FREQUENCY

Definition of a Sensor: A device that responds to a physical, chemical, biological, or electrical stimulus by producing an electrical output signal that is a function of the input stimulus. For acoustic wave devices, we monitor the change in oscillation frequency when the device responds to the input stimulus. The input stimulus could be physical such as a changing pressure, temperature, or stress. It could be chemical such as a particular gas concentration or simply the presence of a chemical agent. It could also be biological. Examples of which could be the concentration of particular type of bacteria, the presence of a biological agent, or even the concentration of antibodies for a particular type of disease. Finally, it could also be electrical such as the strength of a electric or magnetic field or a changing conductivity. The transduction of the input stimulus to the acoustic wave device allows the acoustic wave device to respond by changing its resonant frequency.

Acoustic Wave Sensors

AT-CUT BAW Thickness Shear Mode (TSM) Device
Film Thickness (Angstroms)

Fine Tune Spot

We all know from our own experiences with manufacturing acoustic wave based products that they can be very sensitive to a variety of environmental factors such as variations in temperature, pressure, and packaging stress. We also know that the amount of metallization on the surface of a Quartz Bulk Acoustic Wave (BAW) device can dramatically shift the resonant frequency. We actually utilize this property to fine tune the resonant frequency to within some window of tolerance. This process is called mass loading. For a Surface Acoustic Wave (SAW) delay line, metal deposited in the delay path of the device will result in an increase in delay. When combined with a feedback amplifier to create an oscillator, the result is a decrease in the oscillation frequency. Knowing how sensitive these devices are to changes occurring on their surfaces, how can we utilize acoustic wave devices to sense or detect something of interest.

f (ppm)

Acoustic Wave Sensors

Vertically polarized displacement occurs within one wavelength of the surface Can only be used for gas sensing applications Sensitive to mechanical and electrical perturbations mass loading, visco-elastic properties, and electro-acoustic interactions

Maximum shear displacement occurs on the crystal faces in the plane of the crystal plate Can be used for both gas and liquid sensing applications Sensitive to mechanical and electrical perturbations mass loading, visco-elastic properties, and electro-acoustic interactions

To answer this, we should take a look at the basic operation of these devices. Starting with the surface acoustic wave (SAW) delay line, we can see that propagating wave is confined to the top surface of the substrate. Because of this, the SAW is a very sensitive probe for measuring mechanical and electrical properties on its surface. We also note that since there is a vertically polarized displacement, the SAW can only be used for gas sensing applications. Putting the SAW in an aqueous environment will result in the SAW being completely damped out. For the BAW device, or more specifically an AT cut Thickness Shear Mode (TSM) device, we can see that the thickness shear vibration is in the plane of the crystal plate with the maximum displacements occurring on the crystal faces. This is ideal for sensing application and because there is no vertical component of displacement, the BAW device can be used for liquid-based applications without experiencing excessive damping. Both the SAW and BAW devices are sensitive to mechanical and electrical properties occurring on their surfaces. For mechanical properties, they are sensitive to mass loading and visco-elastic changes like stiffening and softening. For electrical properties, the devices can be sensitive to any property that interacts with the electrical field that is coupled to the propagating acoustic wave. This effect has been given the term electro-acoustic interactions.

Acoustic Wave Sensors

BAW (TSM) and SAW Gas-Based Sensors:
Top Electrode AT Quartz
ST Quartz SAW Delay Line

Sensing Film
Sensing Film Input IDT Output IDT

Bottom Electrode

Application as a gas sensor is achieved by placing a gas specific sensing film on the surface of the device When the sensing film gets exposed to a gas, mechanical and electrical perturbations in the sensing film will cause a corresponding change in the oscillation frequency of the acoustic wave device oscillator. The sensing films can be metal, metal oxide, metal nitride, polymer, or biological material (antigens, bacterial biofilms, or cell cultures)

Application of the SAW or BAW device is achieved by placing a gas specific sensing film on the surface of the device. When the sensing film gets exposed to the target gas, mechanical and electrical perturbations in the sensing film will cause a corresponding change in the oscillation frequency of the acoustic wave device oscillator. Mechanical examples: 1. Mass loading as a concentration of gas adsorbs (sticks onto) onto the surface of the sensing film will result in a decrease in oscillation frequency. 2. Changes in a sensing film as a concentration of gas diffuses into the bulk of the sensing film can result in elastic stiffening or softening. Elastic stiffening will result in an increase in the oscillation frequency, while elastic softening or swelling of the sensing film will result in a decrease in the oscillation frequency. Electrical examples: 1. Conductivity changes in the sensing film as it gets exposed to a concentration of gas can result in either an increase or decrease in oscillation frequency depending on whether the gas causes the conductivity of the sensing film to increase or decrease. Note that in some cases where the sensing film is metal, the device electrodes themselves can become the sensing material. Also note that when you have a metal sensing film, you will not be able to observe any electrical properties because the metal film will short out any electric field that is coupled to the propagating acoustic wave.

Acoustic Wave Sensors

BAW (TSM) Liquid-Based Sensors:
Fluid Cell Fluid Cell

Liquid Sensing Film o-ring AT Quartz o-ring o-ring

Liquid under test AT Quartz o-ring

Application as a liquid sensor can be achieved with a sensing film or by direct contact of the liquid onto the surface of the BAW device Sensing film case - Attachment of the chemical or biological stimulus results in mechanical perturbations causing a corresponding change in resonant frequency Direct contacting case - Mechanical properties of the fluid causes perturbations on the surface of the BAW (TSM) device resulting in resonant frequency changes

Application as a liquid sensor can be achieved with a sensing film or by direct contact of the liquid onto the surface of the BAW device. For the sensing film case, attachment of the chemical or biological stimulus results in mechanical perturbations causing a corresponding change in the resonant frequency. Mechanical examples: 1. Mass loading as a concentration of chemical adsorbs onto the surface of the sensing film or when a bio-molecule attaches to some selective surface chemistry. Mass loading results in a decrease in resonant frequency. 2. Visco-elastic changes of the sensing film as a concentration of chemical diffuses into the bulk of the sensing film. Elastic stiffening of a sensing film will result in an increase in the resonant frequency, while elastic softening or swelling of the sensing film will result in a decrease in the resonant frequency. For the directly contacting case, the mechanical properties of the fluid causes perturbations on the surface of the BAW device resulting in resonant frequency changes. Mechanical examples: 1. Viscous loading of the BAW: The density and viscosity of the fluid will strongly affect the BAW equivalent circuit parameters and resonant frequency. Electrical Properties: Note that for a sensing film placed on top of a metal electrode, the BAW device will not detect any electrical properties because the metal film will short out the electric field that is coupled to the propagating acoustic wave. 7

Acoustic Wave Sensors

Surface Transverse Wave (STW):
Metal Trapping Grating Surface Displacement Output IDT

Input IDT

Similar to the SAW, the Surface Transverse Wave (STM) device uses input and output transducers to launch and receive the propagating acoustic surface wave. However, the differences are two-fold. First, the STW device uses a metal trapping grating structure to trap the propagating wave to the surface of the substrate. Without the grating, the wave propagates at a slight angle into the bulk of the substrate resulting in attenuation of the wave. Secondly, the displacement of the propagating STW is in the plane of the substrate without any vertical component of displacement. Since there is no vertical component of displacement, the STW could theoretically be used for liquid-based applications. In a practical sense, use as a liquid-based sensor is unachievable. Placing water on the surface of the device will short out the IDT electrodes preventing the excitation of the STW before it even has a chance to propagate. Isolation of the IDTs from the liquid has been tried with various types of packaging, but this usually results in significant losses in the device characteristics. For this reason, the STW is typically only used for gas sensing.
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R.L. Baer, C.A. Flory, M. Tom-Moy, and D.S. Solomon, STW Chemical Sensors, Proceedings IEEE Ultrasonics Symposium, pp. 293-298, 1992.

Acoustic Wave Sensors

Love Mode:
Input IDT Thin Film Trapping Layer Surface Displacement Output IDT

Similar to the SAW and STW, the Love Mode device uses input and output transducers to launch and receive the propagating acoustic surface wave. Also similar to the STW, the displacement of the propagating love mode is in the plane of the substrate without any vertical component of displacement. The love mode device, however, uses a thin trapping layer to trap the propagating wave to the surface of the substrate instead of a metal grating. For the love mode device, the same argument regarding liquid-sensing application applies. The love mode device is typically used for gas sensing.
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J.C. Andle and J.F. Vetelino, Acoustic Wave Biosensors, Proceedings IEEE Ultrasonics Symposium, pp. 451-460, 1995.

Acoustic Wave Sensors

Shear Horizontal Acoustic Plate Mode (SHAPM) :

The shear horizontal acoustic plate mode (SH-APM) device combines the best properties of both the BAW and SAW devices. It employs separate input and output transducers in order to allow differential signal measurements like the SAW structures but also allows the sensor crystal to be employed as a physical barrier between the electronics and the sensing medium. The wave is a waveguide mode with energy throughout the bulk of the crystal and is dependent on the thickness of the substrate. Like all the previous surface launched acoustic wave devices, the SH-APM device uses input and output IDTs to launch and receive the acoustic wave. Similar to the BAW thickness shear mode device, the maximum displacements occur on the top and bottom surfaces of the plate. Similar to the STW and Love Mode devices, the surface displacement is shear and in the plane of the plate so it can be used for liquid-based applications. The waveguide modes have energy distributed between the two surfaces as a standing wave as in the BAW sensor but traveling along the surface as in a SAW. The continuous exchange of energy between the two surfaces allows the signal between the IDTs to be influenced by changes on the opposite surface.. Since the wave interacts with both surfaces of the plate, either surface can be used as the sensing surface. For liquid sensing applications and for corrosive or explosive gases, this is a great advantage over the STW and Love Mode device because you can isolate the sensing medium from the electrodes by making the bottom surface of the SH-APM device the sensing surface.
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S.J. Martin, A.J. Ricco, and G.C. Frye, Sensing in Liquids with SH Plate Mode Devices, Proceedings IEEE Ultrasonics Symposium, pp. 607-611, 1988.

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ACOUSTIC WAVE SENSORS Part II

Markets and Applications

This section discusses some of the markets and applications for sensors in general. Most of these applications could be achieved by using acoustic wave sensors.

11

Potential Markets and Applications

Major Markets
Military Automotive Industrial and Environmental Food Industry Medical

Types of Sensors
Chemical Biological Physical

The major markets are military, automotive, industrial and environmental, food industry, and medical. The sensors are based on chemical, biological, and physical sensing properties.

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Potential Markets and Applications

Military Applications

Chemical Agent Detectors

Blister - Mustard, Lewisite, etc. Blood - Hydrogen Cyanide, Cyanogen Chloride, etc. Choking/Lung - Chlorine, Cyanide, etc. Incapacitating Canniboids, Phenothiazines, etc. Nerve Sarin, Soman, etc. Anthrax, Botulism, Plague, Smallpox, Q-fever, etc. Army Research Laboratory (ARL), Office of Naval Research (ONR), Air Force Research Laboratory (AFRL), Department of Defense (DOD), and Defense Advanced Research Projects Agency (DARPA)

Bio-Agent Detectors

Funding Agencies

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Potential Markets and Applications

Automotive

Combustion Control

Hydrocarbons (HC) Carbon monoxide (CO) Nitric Oxides (NO and NO2) Oxygen (O2) Particulates Air/Fuel ratio Oil quality/viscosity

Engine Performance Control

Other Physical Sensors Tire pressure, torque, and acceleration

Funding Agencies

Department of Energy (DOE), Department of Transportation (DOT), and the National Science Foundation (NSF)

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Potential Markets and Applications

Industrial and Environmental

Combustion Emissions Monitoring

Water Quality

NOx, SOx, CO, CFCs, Lead, and Mercury Electrical Power Generation (Coal-Fired Combustion) Municipal, Medical, and Low Level Nuclear Waste Incineration Aquaculture, Coastal, Inland, Drinking Water Reserves, and Ground Water Oxygen, Conductivity/Salt/pH, Chlorophyll Process or byproduct gases Chemical fumes Department of Energy (DOE), Environmental Protection Agency (EPA), and the National Science Foundation (NSF)

Work Place Monitoring

Funding Agencies

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Potential Markets and Applications

Food Industry

Process Control

Moisture Content Viscosity and Texture pH and Conductivity (acidity and Salt Content) Sugar Content (Glucose and Sucrose) Microbial Detection (E. Coli, Salmonella, etc.) Microbial Toxin Detection (liquid and gas) Ingredient Freshness (Milk, Meat, etc.) Frying Oil (Viscosity and Chemical)

Food Freshness

Food Quality : Taste (Electronic Nose)

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Potential Markets and Applications

Medical

Point-of-care Diagnostics
Emergency Room Diagnostics Neonatal and Critical Care Monitoring

Bio-chemical screening Detection and identification of bacterial infection

Nitric Oxide Treatment with Nitric Oxide Oxygen Carbon Dioxide Drug Discovery and Development

Detection of biomolecular interactions

Attachment of candidate drug molecules with proteins Identifying specificity of proteins with other drugs

Funding Agencies

National Institutes of Health (NIH), the National Science Foundation (NSF), and the U.S. Army Medical Research and Materiel Command (USAMRMC)

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ACOUSTIC WAVE SENSORS Part III

Technical Examples

The following section will give four sensor examples in a fair amount of detail. Some general references on acoustic wave sensors are:
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D.S. Ballantine, R.M. White, S.J. Martin, A.J. Ricco, E.T. Zellers, G.C. Frye, and H. Wohltjen, Acoustic Wave Sensors : Theory, Design, and Pysico-chemical Applications, Academic Press, 1997. J.C. Andle and J.F. Vetelino, Acoustic Wave Biosensors, Proceedings IEEE Ultrasonics Symposium, pp. 451-460, 1995. E. P. EerNisse, R. W. Ward, and R. B. Wiggins, Survey of Quartz Bulk Resonator Sensor Technologies, IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, vol. 35, no. 3, pp. 323-330, May 1998. E. Benes, M. Groschl, F. Seifert, A. Pohl, Comparison Between SAW and BAW Sensor Principles, Proceedings IEEE International Frequency Control Symposium, pp. 5-20, 1997.

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Acoustic Wave Sensors

Examples:

SAW GAS SENSOR

Mass Loading of a SAW Mercury Sensor Electrical Changes of a Metal Oxide Coated NO Monitor

BAW (TSM) LIQUID SENSOR

Viscous Liquid Loading of a BAW (TSM) Viscometer Liquid Conductivity Measurements using a Modified BAW (TSM) Device

There are four examples covered in this next section. The first example demonstrates the SAW devices ability to detect changes in mass of a sensing film placed on the surface of a delay line. The second example demonstrates the SAW devices ability to detect changes in conductivity of a sensing film placed on the surface of a delay line. The third example demonstrates how the BAW device can be used to detect changes in viscosity of a liquid. The fourth example demonstrates how one can modify the electrode structure of a BAW device to enhance its sensitivity to electrical effects of a solution or sensing film.

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Acoustic Wave Sensors

Dual Delay Line SAW Mercury Sensor:
Passivation

Glass Layer
Gold Sensing Film

Quartz Substrate

Sensor Delay Line

Temperature Sensors

Passivated Reference Gold Film

Reference Delay Line

The figure above demonstrates the construction of a dual delay line SAW Mercury sensor. One delay line is used as the sensor, while the other delay line is used as a reference to cancel out environmental fluctuations such as variations in temperature and pressure. To achieve matched temperature-frequency characteristics for both delay lines, the same material and thickness film is used. The reference film is placed underneath a passivation layer (glass) preventing it from reacting to mercury, while the sensing film is placed on top of the passivation layer allowing it to respond to the gaseous mercury. The difference between the two delay lines is the mercury response independent of temperature and pressure fluctuations. The sensors ability to detect mercury is due to the strong interaction between gold and mercury, known as amalgamation. Upon sorption of mercury onto the surface of the gold, changes in film mass induce corresponding changes in the propagation of the SAW which results in changes in the oscillation frequency. The rate of frequency change is a function of the mercury concentration.
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R. Haskell, J. Caron, M. Duplisea, J. Ouellette and J. Vetelino, Effects of Film Thickness on Sensitivity of SAW Mercury Sensors, Proceedings IEEE Ultrasonics Symposium, pp. 429-434, 1999. R.B. Haskell, J.J. Caron, Temperature Compensated Surface-Launched Acoustic Wave Sensor, U.S. Patent 6,378,370, April, 2002.

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Acoustic Wave Sensors

Perturbation Theory For Mechanical Effects
f 4 + = fh k1 ( ) + k 2 + k3 2 + 2 f v0
- fractional coverage of the gold film over the IDT center-to-center distance - nominal operating frequency h - film thickness Ki - normalized particle velocities in the xi direction film density nominal saw velocity and Lam constants of the film Predicted Mass Loading Due to a Monolayer of Hg For a 261 MHz ST-quartz SAW delay line with a sensing film with dimensions of 1mm x 1.25mm, the expected shift in frequency due to one monolayer of mercury is 8600 Hz

The fractional change in oscillation frequency due to mass and elasticity perturbations can be expressed using the Tiersten formula shown above. Examining the equation closely, one can see that the mass-induced frequency variations are embodied in the terms, while the elasticity-induced changes are embodied in the terms containing and . It is apparent from the equation above that increases in film mass result in a decrease in oscillation frequency, while increases in mechanical stiffness result in increases in oscillation frequency. In the case of mercury amalgamation to a gold film, both of these situations arise. By choosing a gold film that is just continuous (75 to 100) mass loading is optimized as described in the referenced works below.
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H.F. Tiersten, B.K. Sinha, Journal of Applied Physics, 49(1), pp. 87-95 (1978). R. Haskell, J. Caron, M. Duplisea, J. Ouellette and J. Vetelino, Effects of Film Thickness on Sensitivity of SAW Mercury Sensors, Proceedings IEEE Ultrasonics Symposium, pp. 429-434, 1999. R. B. Haskell, A Surface Acoustic Wave Mercury Vapor Sensor, Masters Thesis, Univ. of Maine, 2002. J.J. Caron, R.B. Haskell, C.J. Freeman, J.F. Vetelino, Surface Acoustic Wave Mercury Vapor Sensors, U.S. Patent 5,992,215, November, 1999.

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Acoustic Wave Sensors

75 Gold Film Hg SAW Sensor Response 10 ppb Hg @ room temperature

25 Slope 0

0.1

0.0

-25 Frequency -50 Hg Off 60 90 120 Hg On 150 180 Hg Off 210

-0.1

-0.2

-75

-0.3 240

time (min)

The response of the SAW mercury sensor to a 10 ppb mercury exposure is shown above. When operated at room temperature, the amalgamation process is essentially irreversible. Almost all of the mercury that comes into contact with the film sticks to it indefinitely until it is removed by heating to 150C. The rate of adsorption onto the surface of the gold film is a function of the mercury concentration.

Freq. Slope (kHz/min)

f (ppm)

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Acoustic Wave Sensors

75 Gold Film Hg SAW Sensor Response 20, 40, 60, 80, and 100ppb Hg @ 50C

10 5 0 -5 -10 -15 -20 -25 -30 -35 -40 55

f (ppm)

20 40 60 80 100

Hg Off

Hg On

60

65 time (min)

70

75

The figure above shows the response magnitudes for concentrations of 20, 40, 60, 80, and 100 ppb mercury at an operating temperature of 50C. You can see that the initial slope of the response changes significantly as a function of mercury concentration.

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Acoustic Wave Sensors

75 Gold Film Hg SAW Sensor Response Frequency Slope vs. Mercury Concentration 0

Frequency Slope (kHz/min)

-0.2 -0.4 -0.6 -0.8 -1 -1.2 0 20 40

y = -0.0083x - 0.1108 R2 = 0.9693

60

80

100

120

Concentration (ppb Hg)

By taking the derivative (calculating slope) of the initial part of the response of the previous set of plots, you can plot the frequency slope as a function of the mercury concentration as shown above. The plot shows that the mercury sensor is extremely linear with respect to mercury concentration. The equation above can be stored in a microprocessor and used to calculate mercury concentration when it encounters a measured frequency slope.

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Acoustic Wave Sensors

Dual Delay Line SAW NO Sensor:
Sensor Delay Line

WO3:Ru SMO Sensing Film Aluminum Reference Matching Film

Quartz Substrate

Reference Delay Line

The figure above demonstrates the construction of a dual delay line SAW Nitric Oxide (NO) sensor. The sensor delay line uses an RF sputtered ruthenium-doped tungsten trioxide (WO3:Ru) film as the sensing element, while the reference delay line is used to cancel out environmental fluctuations such as variations in temperature and pressure. The reference delay line uses an aluminum film to match the temperature-frequency characteristics of the sensing delay line. The sensor utilizes the electroacoustic effect to detect changes in the conductivity of the WO3:Ru film caused by interactions with NO. In the electroacoustic effect, the electric fields associated with the SAW penetrate into the adjacent semi-conducting metal oxide (SMO) film. Because the electric fields interact with the charge carriers in the film, they are effected by changes in the film conductivity. The net effect of this interaction is an alteration of the SAW properties (i.e. phase velocity).
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J.J. Caron, T.D. Kenny, L.J. LeGore, D.G. Libby, C.J. Freeman, and J.F. Vetelino, A Surface Acoustic Wave Nitric Oxide Sensor, Proceedings IEEE International Frequency Control Symposium, pp. 156-162, 1997. J.J. Caron, R.B. Haskell, J.C. Andle, J.F. Vetelino, Temperature Stable Piezoelectric Substrates for SAW Gas Sensors, Sensors and Actuators, B:Chemical v B35 n 1-3 pt 1, pp. 141-145 (1996).

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Acoustic Wave Sensors

Perturbation Theory for Electroacoustic Interactions:

2 f = k 2 f

v sc ( 0 + s ) 1+ f

- fractional coverage of the film over the IDT center-to-center distance

k2 - piezoelectric coupling coefficient for the substrate

- short circuit SAW velocity

0 - dielectric constant of free space s - dielectric constant of the substrate f sheet conductivity of the sensing film
A closed-form expression can be derived for the relationship between SAW oscillation frequency changes and film conductivity changes using simplified perturbation theory. Ignoring mechanical perturbations to the film (which have a minor effect compared with electrical perturbations for this particular gas-film system), the relationship is shown above.
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B.A. Auld, Acoustic Fields and Waves in Solids, Vol II, Wiley Interscience Publication, 1973. R. Lec, R.S. Falconer, Z. Xu and J.F. Vetelino, Macroscopic Theory of Surface Acoustic Wave Gas Microsensors, Proceedings IEEE Ultrasonics Symposium, pp. 585-589, 1988. J.D. Galipeau, An Experimental Study of a Surface Acoustic Wave Hydrogen Sulfide Microsensor, Masters Thesis, Univ. of Maine, 1996.

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Acoustic Wave Sensors

Frequency Shift as a Function of Film Sheet Conductivity

50 0 -50 -100 -150 -200 -250 1E-9

27 RYC Quartz : =0.4

f (ppm)

1E-8

1E-7

1E-6

1E-5

Sheet Conductivity (Seimens)

The perturbation equation for electroacoustic interactions is plotted above for a 27 rotated y-cut quartz substrate. In order to optimize the electroacoustic interaction for sensing applications, the SMO film conductivity must fall within the range where the curve of the above figure has a significant slope. The film conductivity is tailored to fall within this range by precisely controlling parameters such as film thickness, operating temperature, and deposition and annealing procedures.
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J.J. Caron, T.D. Kenny, L.J. LeGore, D.G. Libby, C.J. Freeman, and J.F. Vetelino, A Surface Acoustic Wave Nitric Oxide Sensor, Proceedings IEEE International Frequency Control Symposium, pp. 156-162, 1997.

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Acoustic Wave Sensors

400 WO3:Ru Coated SAW Sensor Response 3ppm Nitric Oxide @ 250C

200 180 160 140

f (ppm)

120 100 80 60 40 20 0 0

Response Magnitude

10

Time (min)

This plot demonstrates the NO sensors response to 3ppm Nitric Oxide. The sensing film was a 400 WO3 film doped with Ru and the operating temperature was 250C. Since the SAW nitric oxide sensor is operated at an elevated temperature (250C), the conductivity induced SAW response is driven by the diffusion of nitric oxide into the bulk of the WO3 film instead of adsorption of nitric oxide onto the surface of the WO3 film. Because of this, the response shape is very different than the SAW mercury sensor response. The amount of response magnitude, instead of the initial response slope, is determined by the nitric oxide concetration.
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J.J. Caron, T.D. Kenny, L.J. LeGore, D.G. Libby, C.J. Freeman, and J.F. Vetelino, A Surface Acoustic Wave Nitric Oxide Sensor, Proceedings IEEE International Frequency Control Symposium, pp. 156-162, 1997.

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Acoustic Wave Sensors

400 WO3:Ru Coated SAW Sensor Response Varied Concentrations of Nitric Oxide @ 250C

250 200
3 ppm 4 ppm 2 ppm 5 ppm

Df (ppm)

150
1 ppm

100
800 ppb 700 ppb

900 ppb

50
400 ppb 500 ppb

600 ppb

0 0 20 40 60 80 100 120

Time (min)

The figure above shows the sensors response to exposures of NO ranging from 400 ppb to 5 ppm. The data shows that the sensor responds in a very linear fashion up to about 3 ppm. Concentrations above 3ppm NO cannot be measured due to the fact that high concentrations of NO reduce the film conductivity to the point that it is no longer in the range for which the SAW device is sensitive.
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J.J. Caron, T.D. Kenny, L.J. LeGore, D.G. Libby, C.J. Freeman, and J.F. Vetelino, A Surface Acoustic Wave Nitric Oxide Sensor, Proceedings IEEE International Frequency Control Symposium, pp. 156-162, 1997.

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Acoustic Wave Sensors

400 WO3:Ru Coated SAW Sensor Response Response Magnitude vs. NO Concentration

250 200

Df (ppm)

150 100 50 0 0 0.5

y = 67.767x - 0.520 R2 = 0.996

1.5

2.5

NO Concentration (ppm)

Taking the response magnitudes of the previous plot and plotting them as a function of NO concentration results in the figure above. It is obvious that the sensor behaves in a very linear fashion, and is ultimately capable of measuring extremely low concentrations of NO.

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J.J. Caron, T.D. Kenny, L.J. LeGore, D.G. Libby, C.J. Freeman, and J.F. Vetelino, A Surface Acoustic Wave Nitric Oxide Sensor, Proceedings IEEE International Frequency Control Symposium, pp. 156-162, 1997.

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Acoustic Wave Sensors

BAW (TSM) Liquid Viscometer:
y
Liquid

Viscously-Entrained Liquid

Top Electrode AT Quartz

x
Displacement ux(y)

q,q

When a thickness shear mode (TSM) resonator is placed in contact with a liquid, the resonant frequency and series resistance is dependent on the density and viscosity of the contacting liquid. The illustration above shows the cross-sectional displacement profile for a TSM ATcut resonator contacted by a viscous liquid. As shown, the oscillating surface generates plane-parallel laminar flow in the contacting liquid. The viscouslyentrained liquid undergoes a phase lag that increases from the distance from the surface of the TSM device.
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S.J. Martin, K.O. Wessendorf, C.T. Gebert, G.C. Frye, R.W. Cernosek, L. Casaus, and M.A. Mitchell, Measuring Liquid Properties with Smooth and Textured Surface Resonators, Proceedings IEEE International Frequency Control Symposium, pp. 603-608, 1993. K.K. Kanazawa and C.E. Reed, Study of Liquids in Shear Using a Quartz Resonator, Proceedings IEEE International Frequency Control Symposium, pp. 350, 1987.

31

Acoustic Wave Sensors

Viscous Liquid Loading for BAW (TSM) Resonators:

fs

fs

3/ 2

q
q

density of the liquid under test viscosity of the liquid under test
q quartz shear stiffness q quartz mass density

The change in resonant frequency is proportional to the square-root of the density/viscosity product as shown above.

32

Acoustic Wave Sensors

5MHz Fundamental AT Quartz Impedance Magnitude %wt Solutions of Glycerol
2000.00

Impedance Magnitude (W)

1800.00 1600.00 1400.00 1200.00 1000.00 800.00 600.00 400.00 200.00 0.00 4985000 4990000 4995000 5000000 5005000 5010000
DI water M 5% M 10% M 20% M 40% M 60% M 80% M Air M

Frequency (Hz)

The plot above demonstrates the series impedance dependence on the viscosity of various glycerol solutions.

33

Acoustic Wave Sensors

Change in Series Resonant Frequency 5MHz Fundamental AT Cut Quartz %wt Solutions of Glycerol in Water 0

-500

Df (ppm)

-1000

-1500

-2000 0 10 20 30 40 50 60 70 80

Glycerol (% Weight)

Plotting the series resonant frequency as a function of the percent weight of glycerol generates the plot above.

34

Acoustic Wave Sensors

Change in Series Resonant Frequency vs. (r *)1/2 5MHz AT Cut Quartz %wt Solutions of Glycerol in Water 0 -200 -400 -600
y = -224.73x R2 = 0.9984

Df (ppm)

-800 -1000 -1200 -1400 -1600 -1800 -2000 0 1 2 3 4

1/2

(r *)

(g cm-2 s-1/2)

And finally, plotting the shift in frequency as a function of the square-root of the density-viscosity product for the various concentrations of glycerol creates the plot shown above. You can see that the shift in frequency is directly proportional to the square-root of the density-viscosity product.

35

Acoustic Wave Sensors

BAW Sensors for Measuring Solution Conductivity:
Conductive Ionic Solution , AT Quartz q,q Fringing Electric Field Ground Electrode

C0

For a commercial AT resonator, the C0 value is mostly a function of the quartz thickness and the area of the electrodes and to a lesser extent the interaction of the fringing electric fields in the quartz and the air surrounding the resonator. This C0 value determines a large part of the anti-resonant frequency of the device. When one side of the resonator is placed in a conductive ionic solution, the part of C0 caused by the fringing fields will cause a corresponding change in the anti-resonant frequency and equivalent circuit parameters as a function of the solution concentration

A bulk acoustic wave TSM device can be used to measure the conductivity of nonviscous solutions. For a TSM device with equivalent electrodes (shown above), the interaction with the conductive solution is not electro-acoustic in nature, but is mainly a function of the fringing electric fields. Because the top electrode is metal, it will short out any electric field that is coupled to the propagating bulk acoustic wave. For this reason, the acoustic wave device does not interact with the solution via the propagating BAW. Instead, the fringing fields interacting with the conductive solution directly influences the C0 of the resonator causing the anti-resonant frequency of the device to be dependent on conductivity of the solution.
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M. Yang and M. Thompson, Perturbations of the Electrified Interface and the Response of the Thickness Shear Mode Acoustic Wave Sensor Under Conductive Liquid Loading, Anal. Chem., vol. 66, pp. 3591-3597, 1993. F. Josse, Acoustic Wave Liquid-Phase-Based Microsensors, Sens. Actuators A, vol. 44, pp. 199-208, 1994. Z.A. Shana and F. Josse, Quartz Crystal Resonators as Sensors in Liquids Using the Acoustoelectric Effect, Anal. Chem., vol. 66, pp. 1955-1964, 1994. F. Josse, Z.A. Shana, and H. Zong, Quartz Resonators as Effective Detectors for Dilute Conductive Liquids, Proceedings IEEE Ultrasonics Symposium, pp. 425430, 1993.

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Acoustic Wave Sensors

5MHz AT Quartz TSM Sensor Response Impedance Magnitude for Varying NaCl Solutions Equivalent Top and Bottom Electrodes (diam. 0.25") 12000.00 10000.00 DI water M 1x10-4 M 5x10-4 M 1x10-3 M 5x10-3 M 1x10-2 M 5x10-2 M 1x10-1 M 5x10-1 M 1mol M
Parallel Anti-resonant Frequency

Magnitude (Ohms)

8000.00 6000.00 4000.00 2000.00 0.00 4994000

Series Resonant Frequency

4996000

4998000

5000000

5002000

5004000

Frequency (Hz)

The plot above demonstrates how a 5MHz AT-cut (equivalent electrodes: 0.25) resonator responds to varying concentrations of conductive salt solution. Notice how the series resonant frequency (minimum impedance) is unaffected by varying concentrations of salt, while the anti-resonant (maximum impedance) frequency is severely affected by the changing salt concentration.

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Acoustic Wave Sensors

5 MHz AT Quartz TSM Sensor Response Series and Parallel Resonant Frequency Change vs. Molarity NaCl in Water
0 -50 -100
Series

Df (ppm)

-150 -200
Parallel

-250 -300 -350 0.00001

0.0001

0.001

0.01

0.1

NaCl Concentration (moles/L)

Plotting the frequency values for the minimum and maximum impedances for all the various salt concentrations results in the plot shown above. As can be seen, the antiresonant frequency is very sensitive to conductive solutions. The fact that the anti-resonant frequency changes considerably, while the series resonant frequency is virtually unaffected eludes to a C0 change instead of an electro-acoustic interaction. If the effect was electro-acoustic, then the series resonant frequency would be very sensitive to the conductivity of salt solution.

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Acoustic Wave Sensors

5 MHz AT Quartz TSM Sensor Response Series and Parallel Resonant Impedances vs. Molarity NaCl in Water
0 -1000 -2000

DR ( )

-3000 -4000 -5000 -6000 0.00001

0.0001

0.001

0.01

0.1

NaCl Concentration (moles/L)

Plotting the impedance values obtained at the series and parallel resonant frequency results in the plot shown above. This plot demonstrates how sensitive the antiresonant frequency is to the conductivity of the bulk solution. It should be noted, however, that this sensor configuration can only be sensitive to the conductivity of the bulk solution due to the fringing electric fields at the electrode edges. It will not be sensitive to electrical changes of a sensing film placed on top of the sensors electrode surface.

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Acoustic Wave Sensors

Lossy Electrode for electroacoustic interactions:
Conductive Ionic Solution , AT Quartz q,q Ring Electrode Lossy Electrode

C0
Mode Shape

The bulk wave sensor shown previously is useful for measuring liquid conductivity, but is difficult to implement. Ideally we would prefer to measure the series resonant frequency using a standard oscillator circuit. The ring electrode structure shown above was designed to enhance the electro-acoustic interaction (series resonant frequency change) with a conductive solution or a sensing film placed on the surface. The plot shown above illustrates the strength of the acoustic mode as a function of position across the surface of the resonator. As can be seen, the acoustic activity in the center of the resonator is not very strong, but is still somewhat present. The acoustic wave in the center (no metal) does have an electric field that is coupled to the propagating acoustic wave that can interact with a conductive solution or a sensing film placed on the surface. Additionally, the liquid or sensing film in the center non-electrode region will behave as a lossy electrode coupling more acoustic energy into the TSM device as a function of conductivity of the solution or sensing film on its surface. So as the conductivity increases, the series resonant frequency, series resistance, and overall Q of the resonator will dramatically change and can be easily measured using a standard oscillator circuit.
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C. Zhang and J. Vetelino, Bulk Acoustic Wave Sensors for Sensing MeasurandInduced Electrical Property Changes in Solutions, IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, vol. 48, no. 3, pp. 773-778, May 2001.

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Acoustic Wave Sensors

5MHz AT Quartz TSM Sensor Response Impedance Magnitude for Varying NaCl Solutions Ring Structure (o.d. 0.45", i.d. 0.30") Bottom Electrode (o.d. 0.25") 8000.00 7000.00 6000.00 DI water M 1x10-4 M 5x10-4 M 1x10-3 M 5x10-3 M 1x10-2 M 5x10-2 M 1x10-1 M 5x10-1 M 1mol M

Magnitude (W)

5000.00 4000.00 3000.00 2000.00 1000.00 0.00 5011000

5013000

5015000

5017000

5019000

5021000

Frequency (Hz)

The figure above shows the impedance plots for a 5MHz AT-Cut ring structure (o.d. 0.45, i.d. 0.30, bottom o.d. 0.25) for various concentrations of salt solution. As can be seen, the series resonant frequency is very dependent on the conductive solution concentration.

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Acoustic Wave Sensors

5MHz AT Quartz TSM Sensor Responses Series Resonant Frequency Change vs. Molarity NaCl in Water 0 -50 -100 Df (ppm) -150 -200 -250 -300 -350 -400 0.00001

0.0001

0.001

0.01

0.1

NaCl Concentration (moles/L)

The figure above plots the series resonant frequencies as a function of the salt concentration for a ring electrode and an identical structure with a solid electrode. The solid electrode structure has no electro-acoustic interaction with the conductive solution resulting in no frequency shift. The ring electrode structure is very sensitive to the concentration of salt in water. As the conductivity of the solution increases, the amount of acoustic coupling increases resulting in significant series resonant frequency changes. Notice how the shift in frequency occurs over a certain range of conductivity similar to the SAW device presented earlier.

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Acoustic Wave Sensors

5MHz AT Quartz TSM Sensor Responses Series Impedance Change vs. Molarity NaCl in Water 400 300 200
DRs (W)

100 0 -100 -200 -300 -400 0.00001 0.0001 0.001 0.01 0.1 1

NaCl Concentration (moles/L)

The figure above plots the series resonant resistance values as a function of salt concentration for the ring electrode structure and an identical structure with a solid electrode. There is no change observed for the solid electrode, while the ring electrode resistance is very dependent on the salt concentration.

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Acoustic Wave Sensors

Summary
Gas Sensing

SAW BAW STW and Love Mode SH-APM BAW SH-APM Mechanical Mass, Visco-elastic properties Electrical - Conductivity

Liquid Sensing

Mechanical and Electrical Sensitivity

A wide range of acoustic wave devices can be used for gas and liquid based sensing applications. For gas sensing, SAW, BAW, STW, Love Mode, and SH-APM make excellent platforms for a wide range of sensing applications. For liquid-based sensing, BAW and SH-APM can be utilized. All acoustic wave devices are sensitive to mechanical and electrical perturbations on their surfaces. For mechanic effects, they are sensitive to mass loading and viscoelastic changes. For electrical effects they are sensitive to any effect that interacts with the electric field that is coupled to the propagating acoustic wave. In general, acoustic wave devices are very sensitive and make excellent platforms for a variety of sensing applications.

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