Chemical Sensor Arrays

Participant Guide
Description and Estimated Time to Complete

Chemical Sensor Arrays (CSAs) are MEMS devices that gather, detect, measure, and identify a
substance or several substances in a minute sample. That sample could be a few drops of blood, an
unknown gas or smell, or an unknown liquid. Many of these arrays are cantilever-based, using micro
and nano-sized cantilevers. This unit provides information about MEMS Chemical Sensor Arrays,
primarily the cantilever-based arrays. It covers how they work and where they are used.

It would be to your benefit to have reviewed SCME’s “How Does a Cantilever Work?” prior to
completing this unit.

Estimated Time to Complete

Allow approximately 20 minutes

Introduction

A Chemical Sensor Array (CSA) is an array of microtransducers and supporting integrated circuits
(see process flow diagram below). A CSA is designed to detect and measure the amount or
concentration of one or more substances contained in a sample environment. The substances,
referred to as target materials or analytes, could be specific gas molecules or atoms, antibodies or
proteins, mercury vapor or volatile organic compounds. One or more analytes in a sample are
detected and the quantity measured using microtransducers. The system electronics analyze and
identify the type and/or quantity of analytes.

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 The microtransducers of CSAs could be optical devices, electronic diodes, microcantilevers,
biological cells and molecules (biological, physical or chemical). The application and, more
specifically, the target material being analyzed, determine the type of transducer used. The most
common transducer used in CSAs is the microcantilever.

Chemical Sensor Array with Analytes

In a cantilever-based CSA, the target material is detected when it comes in contact with a chemically
sensitive material on a cantilever's surface (see figure above). The amount of target material is
measured by monitoring a change in one or more of the cantilever's mechanical or electrical
properties, such as displacement, resistance, or resonant frequency.

This unit will focus on the applications of chemical sensor arrays and the operation of cantilever-
based CSA operation. Many of the following applications are not cantilever-based, but rather an
array of electrodes, diodes, or biomolecules use to detect specific molecules.

Objectives

• State at least five applications of a MEMS CSA.

• Compare and contrast the operations of a static and dynamic cantilever-based CSA.
• Describe at least two operating characteristics of a CSA.

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 Key Terms (Definitions can be found in the Glossary at this end of this unit)

Analytes
Cantilever
Chemical Sensor Array
MEMS
Piezoresistive
Resonant frequency
Selectivity

Chemical Sensor Array Applications

The MEMS Chemical Sensor Array (CSA) is an analytical tool used in a variety of applications and
microenvironments. It is currently used to monitor glucose levels in diabetics, detect fuel leaks in a
space shuttle, identify toxic gases in an environment, identify various types of cells in a blood
sample, and analyze DNA hybridization. Common applications of MEMS CSAs are found in the
following fields:
• Medical
• Forensics
• Environmental control
• Aerospace
• Fragrance design
• Food production
• Security and defense

Within these fields, CSAs are used for the following applications (to name just a few):
• Detection of chemical vapors
• Detection of biological agents (medical as well as biowarfare agents)
• Vibration monitors
• Medical diagnostics and therapeutics
• Olfactory applications
• Sample analysis (gas or liquids)

Following are briefs descriptions of some chemical arrays that are already on the market or currently
being tested for the market.

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 Lab-on-a-Chip (LOC) Array

A lab-on-a-chip (LOC) is a MEMS that incorporates several laboratory functions on a single chip.
An LOC can consist of a chemical sensor array designed to sense one or more analytes, a micropump
to handle the flow of the sample to and from the array, and the electronics to control the device and
analyze the output of the CSA.

This Lab-on-a-chip (LOC) is a

miniaturized, portable version of a
blood-count machine that is being
tested by astronauts. One portion
of the LOC uses a CSA to analyze
blood samples in real-time to
diagnose infection, allergies,
anemia or deficiencies in the
immune system.1

Lab-on-a-chip – Blood Analysis Chemical Sensor Array

[Photo courtesy of Y. Tai, California Institute of Technology]

The Artificial Nose (or ENose)

For fragrance design, food production, and gas detection, the CSA is used as an artificial olfactory
system (an artificial nose). It analyzes a fragrance by separating the component particles that when
combined, provide an overall scent. In food production, MEMS CSAs are used to detect specific
compounds in a food's odor, such as the odor of a fish or meat. By analyzing the amount of the
compounds present, a CSA can determine the freshness of the meat or the presence of contaminants.2

The picture is the ENose developed by NASA

and tested on the International Space Station in
late 2008. The ENose Sensor Unit (the darker-
looking metal object) is housed in its Interface
Unit (white). The ruler, shown for size
comparison, is 12 inches (about 30.5 cm) long. 3

The ENose developed by NASA's Advanced

Environmental Monitoring and Control division
[Graphic source: NASA]

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 For gas detection, the artificial nose can detect a specific gas or the composition of a gas. The
artificial nose is currently used in the space station to detect ammonia.3 In counterterrorism CSAs
are being designed to detect toxic and hazardous gases in the field. Such devices could be
incorporated into the helmets or clothing of military personnel.

How Does the ENose Work?4

(a)

The ENose uses a collection of 16 different polymer films on a set of electrodes. The graphic (a)
illustrates six films/electrodes. These films are specially designed to conduct electricity based on
their resistance. A baseline resistance reading is established (a) with no odors (ambient air). When a
substance -- such as the stray molecules from an ammonia leak -- is absorbed into these films, the
films expand slightly (b), changing their resistivity. The amount of expansion of each film
determines the amount of its electrode current.

(b)

Because each film is made of a different polymer, each one reacts to a chemical compound in a
slightly different way. While the changes in resistivity in a single polymer film would not be enough
to identify a compound, the varied changes in 16 films produce a distinctive, identifiable pattern for a
specific compound. Graphic (c) shows a different compound being sensed.

(c)
[Graphics Courtesy of NASA's Advanced Environmental Monitoring and Control division]

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 Bio-Sensors

In medical diagnostics, CSAs are used as bio-sensors to analyze samples for substances such as
antibodies, proteins, antigens, and DNA. They are used for glucose monitors, pH sensors, protein
binding, DNA detection, and gene expression profiling.

DNA or gene microarrays are biosensors used to

analyze and measure the activity of genes. These
arrays enables scientists and doctors to analyze
complex biological problems:
• Identify the genetic variations that could play
a role in diseases such as Alzheimer's and
Parkinson's.
• Analyze and test for viruses that cause
diseases such as SARS (Severe Acute
Respiratory Syndrome), HIV, tuberculosis,
and other infectious diseases.
• Analyze a patient's blood to determine the
best drug and dosage for that patient's
particular disease.

Researchers can use microarrays and other

methods to measure changes in gene
expression (activity) and thereby learn how
cells respond to a disease or to some other challenge.5 Gene expression microarrays (image right)
measure tens of thousands of genes on a single GeneChip™ and provide scientists the data to
understand regulatory processes at the cellular level.

CSAs in Destructive Environments

Due to their small size, design and packaging, MEMS CSAs are used in environments that are
destructive to comparable macrosensors and where other types of sensors are ineffective. Such
environments include
• electric and magnetic fields,
• hazardous chemical vapors,
• nuclear radiation,
• radio frequency (RF) radiation, and
• contaminated and hazardous liquids.

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 The Cantilever-based CSA

The most common CSA transducer is the microcantilever. Its versatility and low construction costs
make it an ideal transducer for a variety of analytes. CSA microcantilevers are typically 10 – 500 µm
long, up to 100 µm wide, and up to 2 µm thick. The top or bottom surface or both surfaces are coated
with a chemically reactive material designed specifically for the analyte targeted. 2 For static CSA’s
in optical fiber array applications, the standard pitch of the microcantilevers is 250 mm, with a
typical spring constant of 0.02 N/m and resonance frequency of 4 kHz. 2

The scanning electron image below is of a microcantilever CSA developed by the Cantilever Array
Sensor Group at the Swiss Nanoscience Institute. Such cantilevers are being developed for
“applications in chemistry, physics, biochemistry and medicine”. They are ideal for such
applications because they “are miniaturized, ultrasensitive and fast-responding sensors.”13

Microcantilever Chemical Sensor Array

[Image courtesy of Dr. Christoph Gerber, Institute of Physics, University of Basel]

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 How does a Cantilever-Based CSA work?

Cantilever Construction

Chemically Reactive Probe Coating

The primary components of a CSA are the microcantilever transducers. The suspended end of each
microcantilever is coated with a probe material that has an attraction to specific molecules in the test
environment. For cantilever-based CSAs, the cantilevers can be constructed with different surface
materials on the top and the bottom. In some CSAs, the top surface is coated with a chemically
reactive coating (probe coating) which may exist at the suspended end of the cantilever or may cover
the entire top surface. In the fabrication process, the deposition of this selective coating is referred to
as "functionalizing the surface." By functionalizing the surface, the cantilever can be designed to
have the target material “stick to” or adsorbed to a specific portion of the cantilever's surface (e.g. the
tip, the middle, the full length of the cantilever or both the top and bottom surfaces). The fabrication
process can be designed to selectively coat only the desired portion of the cantilever's surface with
the chemically reactive coating.

On the bottom of the cantilever, the coating may be to be neutral so that it will not react with any of
the substances in the sample environment. However, some applications have the probe coating on
both the top and bottom surfaces of the cantilever.

Probe Coating and Analytes (Target Material)

The probe material is a chemically sensitive substance that experiences a chemical change when it
adsorbs a specific target material (analyte). By designing a CSA with a different probe coating on
each cantilever, a CSA can be used to detect several different substances within the same sample.
The figure (Probe Coating and Analytes) illustrates an array that can detect three different analytes
(green, purple and red). The fourth microcantilever is the reference cantilever.

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 How a CSA Works

(Refer to figure: "How a CSA works") When a target material in the sample adsorbs to the probe
coating on a cantilever's surface, it causes a minute, but measurable change in the cantilever's
mechanical or electrical properties. As more target material adsorb to the cantilever's surface, the
resulting change is measured. This change is processed by the integrated circuitry (Signal
Processing) of the MEMS into relative data. This data is analyzed and compared to reference data
for determining the type and amount of material (Analytes Identification).

One or more of the cantilever's properties are monitored. The properties monitored depend on the
design of the system. Some systems monitor a static property such as displacement or resistance.
Others monitor a dynamic property such as resonant frequency. (Note about resonant frequency:
Mechanical systems like to vibrate at a natural frequency which is a property of their geometric
design. The natural frequency is at or near the system's resonant frequency.)

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 An Interesting Fact

It is interesting to note, that prior to the onset of micron and nano-technology, these minute changes
in the mechanical properties of such small devices were considered negligible. However, current
technology provides innovative methods for measuring these negligible changes allowing microscale
components to be monitored and measured like their macroscopic equivalents.

Mass-Sensitive Transducer

Microtransducer affected by change in mass

Since cantilever transducers are very small (from a few nanometers to hundreds of microns in size),
their sensitivity is high compared to similar macrotransducers. The overall mass of a microcantilever
is measurably affected by the chemisorption or adsorption of a very small quantity or mass of
material (even a few molecules or atoms can be detected). A small change in mass causes a
measurable change in one or more of these cantilever's properties. For example, more mass causes a
greater displacement or a lower resonant frequency. This type of cantilever transducer is referred to
as a mass-sensitive transducer.

It is important to note that due to the micron size of the cantilever and the nano size of the analyte,
the cantilever's bend or displacement is due to a small amount of mass, not weight. Weight is mass
affected by the force of gravity. A diving board is a cantilever that bends due to the weight of a
person standing on its suspended end. The microcantilever has too little mass to be affected by the
force of gravity.

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 Stress-Induced Curvature

Stress-induced curvature

Mass-sensitive transducers are not as effective as the transducer and analytes get smaller. For
applications such as biomedical diagnostics and gas detection, the analytes can be nano-sized
particles (1 to 100 nm). For such applications, cantilever displacement is dependent upon a surface
stress caused by the chemisorption of the analytes on or within the probe coating. When the analytes
adsorb into the probe coating an expansion or contraction occurs (see figure). This cause the
cantilever to bend or flex. This is called "stress-induced curvature."

Static and Dynamic CSAs

There are two operational modes used to detect changes in the cantilever's mechanical or electrical
properties: Static and Dynamic.

The static mode measures the bending or flexing of the cantilever due to stress or a change in mass.
When the probe coating captures the target analytes, the cantilever bends due to an increase in mass
or stress of the probe coating. This bending is a measurable static response.

The dynamic mode measures a shift in the cantilever's resonant frequency due to an increase in
mass. When the probe coating captures the target analytes, the cantilever's resonant frequency shifts
to a lower frequency. This shift is due to an increase in mass which is seen as an increase in the
cantilever's overall mass.

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 Static Mode

In the static mode of operation, as the chemically

reactive surface selectively adsorbs the target
material, the cantilever bends due to an increase
in mass or surface stress caused by an increase of
analytes bonding to the probe coating's
molecules (see figure). The bending causes a
measurable cantilever displacement. This
displacement can be measured by sensing a
change in angular deflection (Δ angular
deflection) or change in resistance (ΔR).

Cantilever displacement due to surface stress

Static - ΔR

To measure a change in resistance, the microcantilevers are constructed with a piezoresistive layer.
This layer is usually a doped silicon layer fabricated into the cantilever during construction. As the
target material is adsorbed by the chemically reactive layer the cantilever bends. This creates a
measurable change in the resistance of the cantilever’s piezoresistive layer.

Static – Δ angular deflection

To measure a change in angular

deflection, a reflective layer consisting of
a material such as gold is coated onto the
surface of the cantilever prior to the
chemically reactive layer. A laser beam is
directed to and reflected from the
cantilever's surface creating a reference
angle. As the cantilever bends, the
change in the angular deflection is
detected by measuring the change in
position of the reflected beam.

With both measurements, the amount of

change in resistance or change in angular
deflection is related to the amount of
target material adsorbed in the probe
coating.
Measuring Displacement with a change in Angular Deflection

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 Dynamic Mode

In the dynamic CSA, the cantilevers are initially excited by a piezoelectric, magnetic, electrostatic or
thermal actuation. Target molecules in the sample environment attach to each of the cantilevers'
surfaces. As with the static mode, the selective probe material on the cantilevers' surfaces determines
which molecules adsorb to which surface. This adsorption changes the cantilever's mass resulting in
a change in resonant frequency. The amount of change in resonant frequency is a function of the
amount of mass loading. The change in mass is dependent upon the concentration of the target
material within the sample environment and the amount of time the cantilever is exposed to the
sample.

Watch this YouTube video to see a dynamic mode biosensor in action: Microcantilevers as
Biosensors [https://youtu.be/rPJa0QMxcbs]

Static or Dynamic?

CSA for Liquid Environment

The type of CSA (static or dynamic) used for a specific application is determined by the sample
environment. In liquid environments the damping effect of the liquid on the cantilever's movement
can make frequency measurements very difficult resulting in false readings. Therefore, static CSA's
are primarily used in liquid environments (see figure above). In gaseous environments, both static
and dynamic CSA's are used. In order to gather more information from the sample and ensure its
accuracy, some CSAs use a combination of static and dynamic modes.

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 Operating Characteristics of CSAs

A few of the operating characteristics considered in the design of CSA microcantilevers include
• sensitivity,
• selectivity,
• response time,
• size, and
• power consumption.

Cantilever-based CSAs have proven to be highly sensitive, highly selective, and to have fast response
times. Because each cantilever in an array can be coated with a different probe material, a single
cantilever array can be designed to detect a large number of different analytes. It can also be
designed to have redundancy (nominally identical sensors) in order to reduce false positives (greater
accuracy) and yield a better response. Such an array can analyze a broad spectrum of materials
within a single complex mixture. For example, rather than have to take several vials of bloods to test
for different analytes using various test processes, technicians could place a drop of blood on a CSA
and it could test for all of the different analytes simultaneously.

Mass Sensitivity

Cantilever transducers have an inherently high mass sensitivity due to the small mass of the
cantilever itself. The physical properties of the cantilever (width, thickness, length and material) are
used to further enhance its sensitivity to minute
changes in mass. For example, the physical
geometry of the cantilever affects its resonant
frequency. A long cantilever will have a lower
resonant frequency than a shorter cantilever of
the same material, thickness and width. A
thicker cantilever is inherently stiffer, yielding
a higher frequency. Therefore, the CSA
designer must know what detection electronics
are best suited for the operational frequencies
and match the cantilever design to the
electronics.

Cantilever length - short vs. long

Response Time

The response time for a microcantilever is the time it takes for the cantilever to respond to the target
material on its surface and produce a change in the output. The response time is affected by several
parameters, three of which are
• the concentration of the target material in the environment,
• the probe material itself, and
• the method used to interpret the change in a mechanical property.

For the best response time, the chemical reaction between the target material and the probe material

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 must be as fast as possible. The more time it takes for the adsorption to occur, the slower the
response time. Once the chemical reaction occurs, the change it creates in the frequency, resistance
or deflection must be sensed quickly in order to generate an immediate output. In a CSA this change
is measured by integrated circuits directly interfaced with the monitored characteristic of the
cantilever (i.e. the piezoresistance, resonant frequency, or angular deflection). This direct
measurement coupled with the time required for the chemical reaction to occur on the cantilever's
surface determine the sensor's response time.

Non-Cantilever Based CSAs

The type of CSA discussed in this unit is a cantilever-based CSA that uses mass or stress sensitive
transducers. There are variations of CSAs that use other types of transducers that may be better
suited for a specific application and its requirements. Following is a short description of other types
of non-cantilever based CSAs.

Optical Sensor Array

Partial output from a Colorimetric Optical Array.

In optical sensor arrays the chemical reaction between the probe coating and the target analytes
affects an optical property of the transducer. This results in a change in the optical signal such as
color (wavelength) or light intensity.

The graphic shows a partial output from a colorimetric optical array. A colorimetric sensor arrays
act as an "optoelectronic nose" by using an array of multiple dyes whose color changes are based on
the full range of intermolecular interactions. The four volatile organic compounds in the graphic have
four different patterns as identified by the sensor array. This particular array can sense up to 15
analytes simultaneously in the same sample.

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 Schottky Diode Array

In a Schottky Diode Sensor Array the target material

absorbs (diffuses) through the probe coating to a metal
layer. The metal layer serves as a gate for a diode. Any
change at the gate causes a change in the diode's electrical
characteristics.

Schottky Diode Sensor Array

[Image source: University of California, Santa Barbara,
Department of Chemical Engineering.]

Cell-based Sensor Array

The Cell-based Sensor Array uses biological cells as the transducers to detect the presence of specific
molecules (analytes) within the cells' environment. There are several types of molecular transducers
being developed and tested.

One type of molecular transducer uses cell amplification. When a cell interacts with the analytes a
chemical change occurs within the cell causing the production of many "so-called second messenger"
molecules. This is essentially a biological gain or cell signal amplification. A chemical change
within the cell or an electrical activity can be monitored to measure the amount of amplification. The
amount of amplification indicates the amount of analytes in the sample.6

CSAs Working Together

With the variety of sensor arrays available, a system can be developed to mimic the human senses.
Cantilever-based arrays distinguish between different smells and tastes, optical arrays react to
different wavelengths and intensities (sight), and acoustic arrays detect a change in acoustic
properties as a result of interacting with the environment (hearing).

A CSA can be used in combination with other sensors or as a stand-alone device. Its versatility,
reliability, selectivity and design flexibility make it an ideal sensor system for a variety of
applications, many of which are still being realized.

Summary

A Chemical Sensor Array is an array of microtransducers and supporting integrated circuits. A CSA
is designed to detect and measure the amount or concentration of one or more substances contained
in a sample environment.

The cantilever-based CSA uses an array of microcantilevers to detect and measure specific materials
within a sample environment. The micron size of the cantilevers results in higher selectivity,
improved sensitivity, faster response time and low construction costs. These characteristics make the
cantilever CSA a very popular sensor for a wide range of applications.

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 Food For Thought

What are some additional applications where CSA's could be used to detect a combination of gases,
scents or particles?

In the dynamic mode, which microcantilever would be more sensitive to mass loading – one 100
microns in length or 60 microns in length? (Assume the thickness, width and materials are the same
for both cantilevers).

In many applications, dynamic mode or static mode CSAs could be used. Below is a CSA used to
detect a specific virus in the bloodstream. Based on your knowledge of the microcantilever modes of
operation, which mode – dynamic or static – do you think would be best for this application and
why?

Nanocantilevers coated with antibodies* (blue-green) that

capture viruses (red spheres). As the cantilevers identify and
capture more virus molecules, one or more of the mechanical
or electrical characteristics of the cantilevers can change and
be detected by an electronic interface.
The size of the particle being detected and captured is one of
the factors affecting the size of the cantilever. [Image
generated and printed with permission by Seyet, LLC]

*Antibodies are proteins produced in the blood in response to

the presence of an antigen (e.g., virus, bacteria, toxin).

References

1
“Building a hand-held lab-on-a-chip to simply blood tests.” National Space Biomedical
Research Institute. April 11, 2006.
2
"Cantilever array sensors". Lang, Hegner, and Gerber. Materials Today. 2005.
3
"Electronic Nose". Science @ NASA. October 6, 2007.
4
"Instruments – Electronic Nose". Advanced Environmental Monitoring and Control. NASA.
"Gene chip". Genetics Encyclopedia. DNA microarrays. Answers.com.
5
"Sensors: Engineering structures and materials from Micro to Nano". Stetter, Hesketh and
Hunter. The Electrochemical Society Interface. Spring 2006.
6
"BioMedical Applications of MEMS". Jack W. Judy. University of California. Los Angeles.
7
"Cantilever Array for Proteomic and Genomic Applications". Gerber, Hegner and Lang. Institute
of Physics. University of Basel. Switzerland. (Swiss Nanoscience Institute).
8
"CMOS MEMS Oscillator for Chemical Gas Detection". Bedair. Carnegie Mellon University.
2004.

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 9
"Gradient residual stress induced elastic deformation of multilayer MEMS structures". Huany,
Zhang. Sensors and Actuators. 2006
10
"Microcantilever Transducers: A New Approach in Sensor Technology". Sepaniak, Datskos,
Lavrik, Tipple. Analytical Chemistry. 2002.
11
The MEMS Handbook, Edited by Mohamed Gad-el-Hak, CRC Press, 2002
12
Cantilever Arrays in as Nanomechanical Sensors. Cantilever Array Sensor Group. Swiss
Nanoscience Institute, Institute of Physics, University of Basel.
13
“Feature Selection for Chemical Sensor Arrays Using Mutual Information”. X.Rosalind Wang,
Lizier, Nowotny, Berna, Prokopenko, Trowell. PLOS | One. Tenth Anniversary. March 4, 2014.
( http://journals.plos.org/plosone/article?id=10.1371/journal.pone.0089840 )
14
Chemical gas sensor array dataset. Jordi Fonollosa, Rodriguez-Lujan, Huerta. ScienceDirect.
Volume 3, June 2015, pages 85 – 89.
(http://www.sciencedirect.com/science/article/pii/S2352340915000050 )

Glossary

Analytes: A substance or chemical constituent that is undergoing analysis or being measured.

Cantilever: A beam supported at one end and with the other end suspended freely outwards.

Chemical Sensor Array: An array of sensors that chemical reacts with a target material resulting in a
measurable change (i.e. resonant frequency or mass) with the sensor.

Chemisorption: The molecular bonding of gas to a solid.

Piezoresistive: The piezoresistive effect describes the changing electrical resistance of a material due
to applied mechanical stress.

Resonant frequency: The frequency at which a moving member or a circuit has a maximum output
for a given input.

Selectivity: The pumping speeds for specific gases. Pumps that are selective do not pump all gases
at the same rate.

Support for this work was provided by the National Science Foundation's Advanced Technological
Education (ATE) Program.

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