Term 20211: Section EPW10

ECE 379: Smart Sensors

ONLINE Assignment No.2.

Submitted by –
Chandana Satya Sai Phani Kumar P
11715813
A23

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Review of -

‘Microwave Sensors for Non-Invasive Monitoring of Industrial Processes.’

Introduction:
The use of the electromagnetic waves for sensing purposes is an actively researched
approach with considerable potential for commercialisation. In particular, real-time non-
invasive microwave sensing is a developing technology which has been successfully used as
a sensing method for various industrial applications including environmental monitoring of
water pollutant concentrations and treated wastewater quality monitoring , water level
measurements , material moisture content , carbon level emission, for continuous process
monitoring of biogas plants and of course in the healthcare industry, for purposes such as
non-invasive real-time monitoring of glucose in diabetic patients and for assessing the lipid
concentration of biological cells as a means of detecting malignant neoplasmic growth .
Moreover, microwave-assisted heavy oil production is also a developing area.

The principle of real-time monitoring using microwaves is based on the interaction of the
electromagnetic waves with the matter under test. The test object changes the velocity of the
signal, attenuates or reflects it. Due to this interaction, the permittivity of the material
changes and it manifests itself as a frequency change or attenuation of the incident
electromagnetic signal. By considering how transmitted and reflected microwave powers
vary at discrete frequency intervals, the change in the signal can be linked to the
composition of the object under test.
A microwave resonator is made of a section of transmission line with open or shorted ends.
Depending on the type of transmission line, the resonators are called, for example, coaxial,
microstrip, strapline, slot line, or cavity resonators.
When the resonator is used as a sensor, the object to be measured is brought into contact
with at least some part of the electromagnetic field in the resonator. As a consequence, the
resonant frequency and the quality factor will change in relation to the permittivity of the
object. Due to the large variety of possible structures, sensors can be designed for
measurement of properties of almost any object.
Microwave analysis can be applied to suit a broad range of requirements and has a number
of advantages over competing technologies for wastewater sensing applications, including:

. true real-time sensing, since an analyte material flows past or through the sensor and an
instantaneous measurement is acquired without the need for significant pre-processing; and

. direct sample measurement – a feature currently unavailable in many competing

technologies.

The major advantages of microwave sensors are the capabilities to measure non-
destructively, without contact from a short distance using penetrating waves. Of particular
interest also is the non-ionising nature of the technology, which removes significant health

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hazards introduced by other types of sensor, particularly in the healthcare industry.
Disadvantages are the usually high degree of specialization and the simultaneous existence
of several variables affecting the microwave measurement in material measurements.
The potential of microwave sensing as a real-time monitoring platform for a range of novel
systems developed by the authors, namely, for the monitoring of a multiphase fluid flow in a
dynamic oil pipeline, for sensing of bacteria presence and quantity, for real-time monitoring
of nutrients concentration in wastewater and for non-invasive glucose level determination.
Where appropriate, the technology developed in the microwave domain is critically assessed
in terms of its place amongst competing technologies. Furthermore, the general theoretical
principle behind the microwave sensing is discussed and experimental results of the tested
prototypes are presented.

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 1- Monitoring of a multiphase fluid flow in a dynamic oil pipeline:

The output of an oil and gas reservoir consists of an oil, gas, and water mixture. Gas and
water are produced, as a natural phenomenon, which occurs in the petroleum field, when oil
is extracted from a well. In addition to that, water and gas might be injected at various points
into the well to maximise the amount of oil that can be retrieved. Measuring and monitoring
the produced mixture are very important requirements, in order to enhance the quality
aspects of production, and optimise the process for both operation and transportation.
There are many methods used for instantaneous monitoring of the multiphase flow, but the
two most commonly used methods for measuring gas and water fractions are based on g-
ray attenuation and electrical impedance techniques.

An alternative method of monitoring the quality of oil mixtures in real time was developed
by the authors. The basic electromagnetic wave sensor consists of two horn antennas, a
transmitter and a receiver. The object to be measured is put between the antennas in such a
way that the microwaves pass through the object. The attenuation or the phase shift of the
resonant frequencies are measured. Importantly, this configuration does not disturb the flow
of the oil and it is also non-ionising thus allaying issues with safety and potential exposure of
workers to ionising radiation.
300mm x 100mm, which is fitted to an open-ended cylindrical cavity as a PVC pipeline which
is given initial dimensions of 300mm x 42mm. The system is shown in Figure 1.

Figure 1 Experimental EM cavity

This sensor technique is based upon measuring the dielectric constant of the combined oil,
gas and water phases. The complex dielectric constant (Ɛ) for a material is Ɛ= Ɛr +jƐn, where
Ɛr is the relative permittivity and jƐn is the complex permittivity. Water, because of its dipole
structure, has a large dielectric constant. Frequency spectra are captured so that the shift in
the frequency of the resonant peaks can be used to determine the change in the phase
fractions. The antennas used with the sensor do not intrude into the pipeline, so the shift in
the resonant peaks is dependent on the medium permittivity within the pipeline, as well as
the temperature, salinity and the pipeline dimensions.

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The experimental testing of the developed system was carried on the two-phase oil-gas
mixtures in full frequency range. The operating frequency in the EM wave sensor is varied
according to the oil pipe size. Accordingly, after thorough investigations it was found that
the fundamental resonance was sufficient to determine most of the fluid features including
the percentages of water/oil/gas in the pipe. The experimental values of the frequency and
amplitude parameters have been measured within the laboratory over the expected
environmental conditions of temperature and pressure to be found within the pipeline. All
this information has been stored in a dedicated database where a neural network technique
has been used to unravel the complexity of the system parameters.
Figure 2 shows the spectra captured during these experiments with the focus on the
resonant peak area. Notably, the microwave sensing system must be calibrated to account
for different materials that vary considerably in their dielectric constant values.

The sensor is proven to be particularly sensitive to water because of its relatively high
permittivity, so this sensor may be best applied to monitor breakthrough. Notably, the
results of the measurements are in good correlation with theoretical model simulated using
HFSS software.

Figure 2 The TE111 peak frequency shifts as the percentage of oil and gas in the mixture
varies

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 2- Real-time monitoring of wastewater quality using microwave cavity:

Water quality assessments are based on the analysis of the physical, chemical and
bacteriological parameters and require customised apparatus and trained staff. In daily use
there are up to 70,000 known and emerging chemicals that might be present in various
water resources, including for drinking water production.

Multi-parameter water quality monitors, or sensor panels, are mainly used in finished water,
i.e. in water which has been treated and is ready for consumption. To this end water supply
companies have developed quality management systems and monitoring strategies using
well-established but laboratory-based techniques that are becoming of limited scope and
usefulness. Most current methods of water pollutant detection are labour-intensive, either
lab based and/or require expensive chemicals, maintenance and degrade over time. Among
these systems are: standard UV-Vis measurements, amperometry sensors, ion-sensitive
electrodes, fibre optic sensors that are particularly suited for operation at harsh
environments, biosensors and lab-on-chip sensors.

However, the water treatment industries still struggle in the search for cost-effective real-
time monitoring equipment, especially to detect phosphate, nitrate and nitrite in water.
Taking into the account industry needs, the authors have developed a novel approach for
the Realtime monitoring of the wastewater composition, which in particular is aimed at
quantifying the amount of phosphate and nitrate present. Preliminary results for in situ
monitoring of phosphorus levels in the treated wastewater validate the potential of
microwave sensors for a real-time water quality monitoring.

The microwave resonant cavity developed for this application is illustrated in Figure 3. It is a
two-port microwave resonant cavity sensor with PTFE tubing passing through the centre of
the aluminium construction. This allows samples to be pumped through the cavity, thus
allowing real-time nutrient concentration measurements via interaction with the
electromagnetic field formed inside. The system is designed such that its fundamental mode
of operation occurs at approximately 1.67GHz when the central PTFE pipe is water filled.
When the water is evacuated the operating mode shifts to approximately 1.75GHz.
A quaternary pump is used in this work, allowing mixing of multiple samples with various
water contaminants simultaneously to determine the sensor response. This is connected to
the PTFE tubing that runs through the centre of the sensor and feeds to a waste vessel –
samples are not re-circulated to prevent algae build up in the piping and also to prevent
unwanted sample contamination or dilution. The method used here for acquiring data has
proven to give considerable measurement reliability, and along with the heating block, helps
to further negate external impacts on measurements to ensure that the system provides
both short- and long-term repeatability. Data acquired for phosphate concentrations are
shown in Figure 5.

The detection limit of the system has been proven to be 5mg/L for PO4, with a
demonstrated operation range of 5-160mg/L. The accuracy of the sensor is ±7.5 per cent
over this operating range. The industry leader for online detection of phosphate
concentrations, Hache Lange, have developed the Phosphax sc phosphate analyser system

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which is currently one of the few widely available options for waste water treatment plants in
terms of monitoring effluent phosphate levels. It has a detection limit of 0.05, but an
operational range of 0.05-15 mg/L and accuracy of ±2 per cent.
Thus, while these devices offer the ability to detect a small level of PO4, their operating
range precludes use in areas where phosphate concentration is elevated. Such areas could
include the initial treatment stages in waste water plants, where it would be useful to know
the amount of treatment required in order to optimise process efficiency. In addition, work
by Wimalasuriya to characterise leachate water quality at land fill sites suggests that PO4
concentrations can exceed 60 mg/L, a claim that this is supported by similar investigations by
Broschat and Gamage. In such instances, the developed sensor system shows promise due to
its wide range of operation, in addition to its ability to monitor directly sample composition,
rather than relying on an inferred measurement from chemical reagents.

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To this end, the authors have evaluated the performance of interdigitated electrode planar
EM wave designs excited at microwave frequencies. In addition, the viability of different
methods of introducing a sample to the sensor are investigated. The sensors and fluidic cell
system are designed by the authors, and are currently patent pending, and thus represents a
novel aspect of the work. In addition, further novelty is demonstrated in the application of
EM wave sensors, excited at microwave frequencies, to the detection of P. aeruginosa. The
experimental setup is shown in Figure 5, and results are shown in Figure 6.

Table I shows a comparison of the sensor in terms of operational range and detection limit
with sensors developed by other authors. Importantly, the sensor developed by the authors
is reusable and shows excellent repeatability; other sensors in this area rely upon substrates
or other materials which tend to either make the sensors single use, or significantly impact
their response for prolonged use.

in Figure 6, the correlation between bacteria optical density and shifting resonant frequency
at approx. 292MHz is excellent (R2 = 0.993) which means that implementation as part of a
broader automated system would be quite straight-forward.

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 3- Non-invasive glucose monitoring using microwaves:

Diabetes is a metabolic disorder, which results from insulin deficiency and hyperglycaemia
and is reflected by blood glucose concentrations higher or lower than the normal range of
80-120mg/dL (4.4-6.6mmol/L).

Self-monitoring and point-of-care monitoring of blood glucose levels is one of the

important technical advances in the management of diabetes in the last few decades. It has
provided patients and providers with remarkable insights into the day-to-day excursions of
blood glucose concentrations.
Optical techniques are commonly employed for biomedical applications to assist when time
is a critical factor. However, these methods can be bulky and expensive to implement and
often there is still the requirement for an experienced operator to take time to consider the
meaning of results obtained. The current devices on the market all require a sample of blood
from the patient and then quantification of glycated haemoglobin (HbA1c). The chemical
reaction between glucose and haemoglobin leads to an average blood sugar level and does
not show any spikes in blood sugar level. There are also chemical systems, which directly
measure the quantity of glucose, but these also require a sample of blood. Furthermore, the
majority of methods for detecting glucose levels in the blood rely on in vivo methods
utilising complex chemical processes and/or sophisticated equipment, for example,
impedance spectroscopy, mid-infrared spectroscopy and optical coherence tomography.
Notably, the spectroscopy methods utilise the interaction of the electromagnetic waves at
various frequencies with a substance under test and these interactions are of three kinds: the
absorption, the emission and the scattering. Glucose biosensors can also be based on
electrochemical principle of detection that employ enzymes for molecular recognition, as
well as the optical, piezoelectrical, thermal, and mechanical principles.

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An electromagnetic coupling approach for indirect measurement of glucose concentration in
sodium chloride and Ringer-lactate solutions, which have similar to blood properties, was
employed at the low frequency of 40 kHz. The sensor was able to detect the effect of glucose
variations over a wide range of concentrations, with a sensitivity of 0.22mV/(mg/dL).

However, special caution should be taken when exploiting medical devices emitting signals
at low frequencies, so as not to interfere with natural biological signals and other hospital
diagnostic equipment, such as ECG, EEG, EMG.

Previous work by the authors (Goh et al., 2011a, b, c) with surgeons at local National Health
Service hospitals has indicated that there is a need for simple but rapid sensing techniques
which can be used during surgical procedures to detect parameters in a variety of patient
bodily fluids. In the ideal case, surgeons would like tools which are either:

In addition, the current methods are inappropriate during a surgical procedure as time is
often critical from the perspectives of patient well-being and hospital efficiency. Thus, there
is a great desire for tools which can be used at the point of care to assist medical
practitioners in rapidly diagnosing patients.
The authors suggest using electromagnetic waves for real-time non-invasive evaluation of
glucose level, and so constructed a sensor based upon a co-planar waveguide design. As
before, the sensor allowed real-time measurement of analytes. The experimental setup and
procedure are described in more detail in previous work by the authors. Further work has
improved the sensor in terms of its sensitivity to small quantities of glucose, and these
results are shown in Figure 7 for the glucose range 0.5-50 mmol/L. In the typical
physiological range of blood glucose for humans, the sensor is capable of sensitivity to
changes as small as 0.2mmol/L, which therefore shows considerable promise for future
implementation and has resulted in an international patent (Al-Shamma’a et al., 2010) being
recently granted.

Conclusion:

The paper illustrated the potential of microwave sensing as a portable monitoring platform
for a broad spectrum of commercial applications, with a focus on system developed by the
authors, namely, for the monitoring of a multiphase fluid flow in a dynamic oil pipeline, for
sensing of bacteria, for real-time monitoring of nutrients concentration in wastewater and for
healthcare industry, in particular for instantaneous non-invasive determination of the glucose
levels.
In terms of performance, comparative to competing sensor technologies, microwave sensors
have also been shown to harbour promise. Microwave sensors were also able to reliably
detect the presence of water contaminants, for example PO4 in the 5-160 mmol/L range,
thus finding new market applications.

While this work discusses performance characteristics of microwave sensors wherever

possible, it is also important to remember the wide spread of application domains that have
been demonstrated, with these being only a brief glimpse at what is possible. Furthermore,

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the microwave sensors developed by the authors have been shown to operate without the
need for chemical reagents, which enhances their speed of operation in addition to reducing
the potential maintenance costs.
It is suggested that a novel approach to wastewater monitoring, namely using specially
designed microwave cavity sensors, could lead to a successful development of an advanced
platform capable of providing for a real-time detection of water content with superior
sensitivity.

References
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and Water Resources Congress, ASCE, Reston, VA, pp. 3379-3388, translated by I.R. Edward
Beighley andW.K. Mark, 354.

[2] Al-Dasoqi, N., Mason, A., Alkhaddar, R., Shaw, A. and Al-Shamma’a, A. (2011b), “Real-time
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[10] Choudhury, B., Shinar, R. and Shinar, J. (2004), “Glucose biosensors based on organic
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595-601.

[14] Mason, A., Wylie, S., Thomas, A., Keele, H., Shaw, A. and Al-Shamma’a, A. (2010), “HEPA
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Smart Sensing and Intelligent Systems, Vol. 3 No. 3, pp. 322-337.
[15] Nyfors, E. and Vainikainen, P. (1989), Industrial MicrowaveSensors, Artech House,
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[16] Nyfors, E. and Vainikainen, P. (1991), “Industrial microwave sensors”, IEEE MTT-S
International Microwave Symposium.

[17] Subramanian, A., Oden, P.I., Kennel, S.J., Jacobson, K.B., Warmack, R.J., Thundat, T. and
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Physics Letters, Vol. 81 No. 2, pp. 385-387.

[18] Thet, N.T., Hong, S.H.,Marshall, S., Laabei,M., Toby, A. and Jenkins, A. (2013), “Visible,
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Vol. 11 No. 6, pp. 1440-1447.

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Question2 - Make a list of different sensors made using surface, bulk or LIGA
micromachining. Also enlist the usage in different areas.

Sol:
Building a MEMS using Surface Micromachining

Surface micromachining is a process that uses thin film layers deposited on the surface of a

substrate to construct structural components for MEMS.

• A sacrificial (oxide) layer is first deposited on the substrate.

• The first polysilicon layer is deposited on top of the oxide layer.

• This polysilicon layer is patterned and etched and forms the first set of cantilevers.

• A second oxide layer is deposited on top of the etched polysilicon layer.

• The second structural layer or polysilicon layer is deposited, patterned and etched. This
form the second set of cantilevers.

• The third oxide layer (sacrificial layer) is deposited.

• At this point, the surface has become extremely bumpy; therefore, this oxide deposition is
followed by a CMP.
• Two holes are etched through the top oxide layer providing an opening to the polysilicon
layer below it. These holes are needed to begin forming the posts which support the
cantilevers and allow rotation.

• To continue fabricating the posts, holes are etched into the second polysilicon layer.
• Another layer of oxide is deposited on the surface and into the two holes. This is the last
sacrificial layer.
• The third polysilicon layer is now deposited, patterned and etched. This layer forms the top
set of cantilevers.

• The oxide films below each structural layer provide the necessary space for the middle
cantilever to move after all of the oxide layers have been removed and the cantilevers
released.

• The last step of this process is to remove the oxide layers from between the structural
layers using a wet etch process of a hydrofluoric acid (HF) solution.
• Once the sacrificial layers are removed, the middle cantilever is free to rotate.

These steps - 1) oxide deposition, 2) structural layer deposition, pattern, etch, 3) sacrificial
etch – can be repeated several times when fabricating a complex moving structure such as
the linkage system, a gear transmission, an accelerometer, pressure sensor, Humidity sensor,
and other MEMS devices.

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Building a MEMS using Bulk Micromachining

Bulk etch is a subtractive process in which the silicon substrate is selectively removed.
Specific etchants are chosen that remove substrate material either isotropically (the same in
all directions) or anisotropically (not the same in all direction). The anisotropic wet etching of
silicon takes advantage of the crystalline structure of the silicon wafer to remove select
material following the planes of the silicon crystal. This selectivity is possible due to the
knowledge that certain plane orientations etch much faster than other planes (e.g., the (100)
plane etches approximately 400 times faster than the (111) plane).
An example of bulk etching in MEMS fabrication is in the construction of a MEMS pressure
sensor. A MEMS pressure sensor (right) consists of a silicon nitride thin film deposited onto
the surface of a silicon substrate. This layer of silicon nitride acts as the diaphragm or
membrane of the pressure sensor. A thin film of gold is deposited on top of the silicon
nitride, then patterned and etched to form a Wheatstone bridge sensing circuit. In order for
the membrane to move up and down with changes in pressure, it must be “released”. To
release the membrane, the silicon substrate beneath the membrane is removed by etching
the backside of the wafer.

The picture to the right shows the backside of a MEMS pressure sensor and the result of a
bulk etch using a solution of potassium hydroxide (KOH) and water. The KOH etchant
solution selectively etches the crystalline silicon along a specific plane. In the picture you can
see that the etchant preferentially etched the (100) plane of the silicon (the wafer surface in
this case) while simultaneously etching the (111) plane. The (111) plane etches about 400
times slower than the (100) plane. This allows for a controlled etch in which an inverted
pyramid shaped opening of a specific size is created. The etch of the (100) plane stops when
it hits the silicon nitride which is impervious to the KOH. For the purpose of this etch, the
silicon nitride layer is the etch stop layer. For the purpose of the pressure sensor, the silicon
nitride serves as the membrane or diaphragm on which the sensing circuit is constructed.

Fig 1- Pressure Sensor- Bulk Etching Fig 2- etching silicon nitride with KOH

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Building a MEMS using LIGA Micromachining

LIGA is an additive, lithographic process which allows for the fabrication of complex, three
dimensional structures with very high aspect ratios exceeding 100:1. 6 These structures can
have sub-micron size features with heights of several millimeters and widths of only a few
microns (e.g., probes, pin, electrodes, gears, waveguides, and molds). LIGA is also a type of
HARMST process – High Aspect Ratio Micro-Structure Technology. LIGA molds allow for
mass-production of microsized HARMST components. These components as well as other
LIGA components can be fabricated using polymers, metals and moldable materials.
The LIGA process consists of the following basic steps:
• Expose

• Develop

• Electroform (Electroplate)

• Strip

• Replicate or Release
Sensors made using this technique are
* Capacitive sensor

* Differential acceleration sensor

* Passive g-sensor

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Question 3- Make a list of different tests and checks to be done on smart sensors for
ensuring their reliability.

Sol:
a) Thermal Shock: It evaluates the resistivity of products to radical temperature changes.
Usually, this test is conducted under the following conditions: Ta: 0ᵒ C to 100ᵒ C (liquid bath).

b) Temperature Cycle: This is done to evaluate the low and high temperature resistivity of
products. The sensor is kept under its lowest and highest capable range of temperature to
check its durability and reliability.
c) Terminal Strength: This test is done to evaluate the resistivity of the terminals of the
product to the force imposed on the terminals while the products Are mounted, wired or
operated.

d) Shock Resistance: This test judges the structural resistivity and mechanical, resistivity of
products. The conditions of this test vary with the product structure. Usually, this test is
conducted under the impact acceleration and pulse width.

e) Tension Test: On each terminal of products. a specified load is imposed for 10 ±1s in the
direction of the terminal.

f) Bending Test: On the tip of each terminal of products, a specified load is imposed to bend
the terminal by 90 degrees and to change it back.

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