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A review of characterization techniques for materials' properties measurement

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 Journal of Telecommunication, Electronic and Computer Engineering (JTEC)

A Review of Characterization Techniques for

Materials’ Properties Measurement Using Microwave
Resonant Sensor
Amyrul Azuan Mohd Bahar1, Zahriladha Zakaria1, Azmi Awang Md Isa1, Eliyana Ruslan2 and Rammah A. Alahnomi1
1
Microwave Research Group, Centre for Telecommunication Research and Innovation (CeTRI),
Faculty of Electronics and Computer Engineering, Universiti Teknikal Malaysia Melaka (UTeM),
76100 Durian Tunggal, Melaka, Malaysia.
2
Faculty of Engineering Technology, Universiti Teknikal Malaysia Melaka (UTeM),
76100 Durian Tunggal, Melaka, Malaysia.
amyrulazuan@yahoo.com

Abstract— This paper presents a compilation of important high frequency electric fields. Nevertheless, the subsurface
review in the development of microwave resonant sensor detection of samples will affect the properties of materials
technology used in previous years. The major research work for when exposed to extremely high electric field distribution [1].
each year is reviewed. Most of the resonators are designed for Other than that, the moisture content of the materials and its
material characterization in specific application areas such as
effect on the dielectric properties of materials also can be
food quality control, medical, bio-sensing and subsurface
detection. In the last few years, several resonant sensors based determined by using near-field sensors, which are highly
on the planar and non-planar structure are compared and sensitive. However, high lossy materials decrease the quality
examined in order to propose a new topology of microwave factor of the resonator drastically and at the same time reduce
sensors designed. The weaknesses of conventional sensors such as the measurement accuracy of microwave sensor [2]. On the
bulky size, high cost manufacturing and consume high volumes other hand, microwave techniques for drying food products
of detectable sample have been reviewed. Most significantly, this have also been very popular since the percentage moisture
new proposed structure must gain high quality factor to gain content of materials can be classified, although the
improvement in an accuracy of the sensing capability and can permittivity of the samples will change as well as the water
overcome previous design weaknesses. This device will
content of samples varies accordingly [3]. Those problems
discriminate the composition and properties of samples based on
scattering parameters in certain operating frequency. The have been studied extensively in order to gain some
proposed system outlined in this paper, featuring new innovation knowledge for future research works.
in resonator structure as well as providing advanced capability Basically, the material characterization structure designs use
design of future research works. The contribution of this study is mostly resonant methods, in which these methods can be
useful for various types of applications where the characterizing classified into resonator methods and resonant perturbation
of materials is very important, while improving its performance methods. Resonant methods offer the potential of
especially in terms of accuracy and sensitivity. The previous characterizing the properties of a material at a single
studies will be reviewed and critically compared in order to gain frequency or a discrete set of frequencies with high accuracy
a better understanding in microwave resonant sensors and new
in comparison to broadband methods. Conventionally,
ideas for further research improvement in application, which
require characterizing of materials. waveguide, dielectric and coaxial cavity resonators have been
used for characterizing materials but in different topologies.
Index Terms— Accuracy, Characterization, Capability, Most of the methods and techniques applied are based on the
Methods, Microwave, Resonators, Resonant, Sensitivity, Split- applications used by the industry. A wide category concerning
ring, Sensor, Techniques. the dielectric properties of materials can be characterized into
the resonator as transmission, reflection or absorption
I. INTRODUCTION elements. Wideband permittivity measurements are mostly
made of transmission sensors or reflection sensors, such as
Accurate measurement of material characterization has gained coaxial probes. However, this type of measurement is
significant importance over the last decade. The ability to frequently overly complicated for industrial applications [4].
analyze composition and properties of a material which In this case, planar resonant sensors are taking place as the
undergoes physical and chemical changes has led to many current complex permittivity measurements.
applications in the industry such as food quality control, bio- Sensors require a scalar measurement that allocates less cost
sensing and subsurface detection. In the food industry, the and more robust instrumentation to be employed; resonant
research interest in dielectric properties of food materials has sensors can be fully described in terms of scalar measurements
been growing, in which there has been an intensive research so that they provide themselves to industrial applications,
for predicting heating rates when the materials are subjected to whenever wideband characterization is not required. A typical

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 Journal of Telecommunication, Electronic and Computer Engineering (JTEC)

application of resonant sensors has been presented in the tough because it was a multilayer structure and can be easily
previous work [5]. In RF and microwave circuit design, the produced by less expensive printed circuit technology. The
dielectric permittivity of the substrate plays an important role relative error of the system was very small, which was less
and requires precise evaluation over a broad range of than 3% based on the test results in several samples [4]. Table
frequencies. Knowledge of these properties plays a crucial role 1 shows the comparison of the previous research works in
in the accurate design of a variety of circuit technologies. The solid materials characterization due to different types of
following sections aim to provide a general discussion of some methods and techniques.
well-established dielectric measurement techniques, primarily
applicable to moderate and high loss liquid samples and even Table 1
Comparison of previous research works in solid materials characterization
for solid and gas samples [6].
Moreover, by introducing an accurate equivalent circuit
model for the planar sensor, the experimental calibration No Title/Author/Year Remarks
procedure is avoided. The low cost and simplicity of The resonator was designed at
A Planar Resonant Sensor
manufacturing allows the use of the resonator in a disposable for the Complex
frequency 656.58 MHz. Solid
manner [7] and an effort has been made to present a recent samples were used. The
Permittivity
advantages are reducing costs,
technique on several phases of materials such as solid, liquid 1[1] Characterization of
improving robustness and have
and mixture. To satisfy the current demands of many Materials.
excellent accuracy. Low cost
Elisa Fratticcioli, 2002
applications especially the biological and chemical industries, manufacturing since it uses planar
a mixture technique can be implemented by using planar structure and easy to fabricate.
resonant sensors developed by various researchers. In this The resonator was designed at
paper, an effort has been made to describe and show the A Simple and Low-Cost
frequency 500-800 MHz. Solid
Measurement System for
interesting advances in microwave resonator sensor the Complex Permittivity
samples were used. The
developments. The structure to produce highly sensitive 2[3] advantages are less fabrication
Characterization of
cost, robustness improvement and
sensors is shown with some comparisons based on Materials.
can be disposable. Suitable for
frequencies, methods, techniques, and technologies used. It is Elisa Fratticcioli, 2004
measurement in compact areas.
expected that the information from this paper will help
researchers to have a broader perspective of resonator The resonator sensor was designed
at frequency 883 MHz. Solid
structure, and hopefully it can be considered as an alternative Microwave permittivity samples were used such as Teflon,
to produce a better technique design. measurements through R4003, FR4, RF35 and glass. The
3[4]
cross-shaped ring sensors. advantages are high accuracy and
II. TYPE OF MATERIAL SAMPLES Biffi Gentili, 2002 extremely compact. Since the size
is compact, the fabrication cost is
less expensive.
A. Characterization of Solid
Several studies have been conducted on solid samples for The resonator sensor was designed
materials characterization in order to introduce novel resonant at frequency 2.4 GHz. Solid
samples were used such as grain,
sensor design with the improvements in accuracy and sand and concrete. The advantages
sensitivity of the device [1, 3, 4 and 8]. For example, [1] Planar Resonator Sensor for are a highly sensitive detector of
produced microwave planar resonant sensor based on the 4[8] Moisture Measurements. moisture contents in solid. Other
adoption of a scalar two- port measurement method. There are Jerzy Skulski, 1998 than that, time measurement will
be very short and able to measure
similarities between both papers in term of frequency. The practically on-line. The fabrication
operating frequency is 500-800 MHz on 2004 and the first cost is cheaper since the resonator
paper produced on 2002 used 656.58 MHz as the operating is planar based.
frequency. The improvements in Q-factor, accuracy and
robustness have been made. The method used is suitable for
the detection of moisture content in wet powdered materials B. Characterization of Liquid
[1]. The characterization of materials does not only focus on the
[4] designed a Cross-Shaped microstrip ring sensor with full solid phase, but also all of the phases such as liquids, gases
planar microstrip technology. A scalar network analyzer was and mixtures. Several studies on liquid materials
used to compute the resonant frequency and the matching characterization have been conducted and have been discussed
amplitude of the transmission parameter for the fundamental in succeeding paragraphs [2, 7, 9, 10, 11, 12 and 28]. For
mode. The complex permittivity was estimated by inverting example, [2] designed a split-ring resonator by combining the
the measured parameters using an algorithm based on dielectric resonator coupling for accuracy enhancement. This
Artificial Neural Network (ANN). This design was modified resonator was designed in simulation software before coming
based on their research work in 2001 “full-wave modelling of up with fabrication process. The sensor was simulated using
microwave planar reflection sensors of material moisture the 3D full-wave solver Ansys High-Frequency Structure
testing”. The design structure has three layers of substrate Simulator (HFSS). The complex permittivity of water and
with different dimension specifications. The upper and second saline solutions was modeled using a first order Debye model.
layers used RO4003 substrate and the bottom layer used FR4 The advantage of this filter over the resonant sensor presented
materials. Each layer has its own function, which are input, by [1] was that its sensitivity was much better due to high Q-
hidden and output port of the sensors. The sensor was very factor. However, this design had limitations in bandwidth

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 Journal of Telecommunication, Electronic and Computer Engineering (JTEC)

which operates at 20-40 GHz frequency range. Moreover, the

Q-factor was still relatively low for a DR resonator, which was
due to radiation. The high performance resonant sensor could
be produced using this method with some modifications on its
basic design. Other parameters, such as bandwidth and
frequency ratio also varied accordingly [2].

Figure 3: Location of capillary and MUT inside the cavity [7]

[9] introduced a new idea for designing microwave sensor

for precise permittivity characterization of liquids used for
aqueous glucose detection in medical applications. This idea
was based on the planar half-wavelength microstrip line
(MSL) resonator. The resonator was a highly sensitive sensor
Figure 1: Geometrical parameters of the coupled DR-SRR sensor [2] for precise permittivity change detection of liquids present.
The resonant frequency was 2 GHz using near-field sensor. A
Another example is the integration of waveguide cavity very sensitive concentration less than 0.01% was detectable.
resonator designed by [7] presented for Pharmaceutical Even small mixture content can be detected for measuring
industry application. The simulation results were obtained purposes. The sensor was also applicable to other liquid
using the Full-wave finate-element method (FEM)-based High mixtures independent of small, medium or high loss. A simple
Frequency Structure Simulation (HFSS) commercial software and highly sensitive microstrip sensor structure has been
package. The resonant frequency of the sensor was 8 GHz and presented [9].
substrate material used in fabrication process was RT/Duroid [10] proposed a new method for wide range applications by
with dielectric constant 2.2 and loss tangent 0.00009. The designing a microwave microfluidic sensor using a microstrip
high-resonant construction was a modernization of well- split-ring resonator based on perturbation theory. The resonant
known measurement cells where the dielectric constant was frequency and Q-factor depends on dielectric properties of
deduced by cavity perturbation from the shift in resonant resonator, which was the operating frequency at 3 GHz. The
frequency and the change in the factor. The advantages of the design used Rogers Corporation RT/Duroid 5880 laminate
sensor are low cost and it can be easily integrated with many substrate for fabrication process, which had the permittivity at
other components. The error in the measured results was 2.2 and lost tangent at 0.00009. It was modified from [7]
within plus minus 0.5% and this proves that the resonant research work. COMSOL Multiphysics software has been
sensor is much better in terms of sensitivity and accuracy [7]. used to perform the simulation of electromagnetic properties
Figure 2 and 3 show the structure of resonator sensor for of the structure. Several common solvents were chosen for
liquid characterization. testing purposes such as hexane, chloroform, ethanol,
methanol and water. The resonator was compact and planar,
making it suitable for a lab-on-a chip approach and suitable
for evaluation of the material properties [10].
[12] presented the concept of microwave resonator using
micro fabricated sensor referring to liquids characterization.
The design was compatible with a future lab-on-a-chip
integration for convenience used. Some solvent has been
tested such as de-ionized water-ethanol mixtures, which had
the volume of ethanol ranging from 0% - 20%. The resonant
frequency used was 20 GHz and standard match impedance 50
ohm. The associated transmission coefficient and maximum
relative error were less than 0.1% and 6.5%, respectively,
which was a highly accurate permittivity characterization. The
dimensions of the design structure were presented in details,
including procedures fabrication process. The microfluidic
area was attached to the top surface of the structure to convey
Figure 2: Layout of substrate integrated waveguide cavity resonator with the liquid toward the sensing region. Simulated process for
microstrip feed section and hole within the cavity through which the MUT is determining frequency and attenuation was done using High
inserted [7] Frequency Structure Simulator (HFSS). The effective and
accurate complex permittivity characterization has been done
successfully in applications area [12].

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 Journal of Telecommunication, Electronic and Computer Engineering (JTEC)

[28] constructed a flow-type liquid sensor by using a 2 port C. Characterization of Mixture

SH-SAW resonator. SAW devices were used as sensor in a Mixtures sample is the materials, which have different states
variety of fields. The waves propagating in this method were of matter such as solids, liquids and gases. Since the phases
parallel between the surface and particle displacement, which are not fixed, the technique used for device structure must be
means the sensor was suitable for sensing the liquids applicable and have an ability to characterize variation of
characterization. There are a lot of advantages of this kind of samples. Several studies have been carried out on the mixture
sensor, which is very effective due to the small size, highly samples [6, 13, 22, 23 and 45]. For example, [6] developed the
stable operation, and high signal-to-noise ratio. The amounts complementary split-ring resonators (CSRRs). The design was
of liquid during measurement were very small. The sensitivity constructed such as high measurements in sensitivity and
of the sensor can be increased based on the operating accuracy, while at the same time eliminated the extensive
frequency of the sensor. The resonant frequency of the SAW sample preparation procedure needed. The sensors were
resonator was 40 MHz and insertion loss of the sensor was working on a 0.8 – 1.3 GHz band of frequency. Several
taken to be 60 dB with Q-factor 400 [28]. The summary of samples have been tested for performance results, which were
sensing techniques for liquid measurement is shown in Table on air, Teflon, RO3003 and FR4. The fabrication process was
2. less expensive and easy to process with a very low loss.
Table 2 Minimum transmission and minimum reflection were
Comparison of previous research works in liquid materials characterization
observed depending on the permittivity of the sample under
test. The structure was fabricated using printed circuit board
No Title/Author/Year Remarks technology [6].
[13] introduced a compact resonant near-field sensor for
The resonator sensor was designed liquid characterization. It had a very low fabrication cost and
at frequency 20-40 GHz. Liquid
Accuracy Enhancement of
samples were used such as water the technique was based on a folded substrate-integrated half-
a Split-Ring Resonator mode resonator with a planar sensing tip. Several samples
and saline solutions. This technique
Liquid Sensor Using
1[2]
Dielectric Resonator
will improve Q-factor of the design such as saline, ethanol, salt, sugar and water solutions can be
and enhances accuracy of the discriminated by the sensor with a change of concentration of
Coupling.
sensor. However, the fabrication
Nora Meyne, 2014
cost is quite expensive since the less than 1%. Besides lower cost, the advantages of the sensor
materials used are roger type. were the simplicity of the structure and easy access to the tip
from the top, which means that the construction of the sensor
Substrate Integrated The resonator sensor was designed can be done in a shorter time compared to other resonant
Waveguide Cavity at frequency 8 GHz. Liquid sensors, especially in biological and chemical application area.
Resonators for Complex samples were used such as The resonant frequency was 5 GHz for test process using
Permittivity ethanediol, acetone, methanol and HFSS software in the simulation process [13].
2[7]
Characterization of dimethyl sulphoxide. The
Materials. advantages are easily integrated [23] developed a gas-liquid separated micro-resonator for
Kashif Saeed, 2008 with many other components and measuring the multifunctional characteristics of biological
less expensive manufacturing cost. cells. Two resonator regions which are gas-phase and liquid-
phase areas were used to separate from water-shedding wall
The resonator sensor was designed and resonate the samples in the chamber at around 2.5 kHz. It
Microwave Sensor for
Precise Permittivity
at frequency 2 GHz. Liquid proved that water-shedding wall can avoid leakage between
samples were used such as water both separated areas, as shown in Figure 4.
Characterization of Liquids
and glucose solvents. The
Used for Aqueous Glucose
3[9] advantages are very sensitive to
Detection in Medical
concentration with less than 0.01%
Applications.
detectable sample. Other than that,
U. Schwerthoeffer, 2014
the structural design is simple and
highly sensitive sensor structure.

The resonator sensor was designed

at frequency 3 GHz. Liquid
Novel Microwave Micro
samples were used such as hexane,
fluidic Sensor Using a
chloroform, ethanol, methanol and
4[10] Microstrip Split-Ring
distilled water. The advantages are
Resonator.
suitable for a lab-on-a chip
Ali A. Abduljabar, 2014
approach and easily integrated with
other components.

The resonator sensor was designed

at frequency 20 GHz. Liquid Figure 4: Schematic view of gas-liquid separated resonator [23]
A Microwave and Micro
samples were used such as water
fluidic Planar Resonator
and ethanol mixtures. The The structure was developed using a micro
Efficient and Accurate
advantages are efficient techniques
5[12] Complex Permittivity
for high Q-factor resonator and
electromechanical system (MEMS) technology. Silicon-on-
Characterization of insulator (SOI) wafer was used for fabrication process and the
have high accuracy on permittivity
Aqueous Solutions.
Thomas Chretiennot, 2013
characterization of aqueous structures were formed using deep reactive ion etching (D-
solutions. It is also suited to a lab- RIE). Based on the experimental results, the performance of
on-a-chip approach
the sensor was very good and attempts were made to refine the

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 Journal of Telecommunication, Electronic and Computer Engineering (JTEC)

gas-liquid separated resonator [23]. Table 3 shows that the quality control, bio-sensing and chemical products. The
summary of previous studies in the mixture phase (solid, advantages and disadvantages of the various techniques have
liquid, gas) characterization of resonant sensors. been highlighted and thorough comparisons among various
techniques have been presented. The focus of the discussion
Table 3 has been on the performance of each technique to seek the best
Comparison of previous research works in mixture materials characterization
sensitivity and accuracy for better measurement. This analysis
presented in paper has been drawn from specific design sensor
No Title/Author/Year Remarks
details and measurement results of each of the sensors. This
The resonator sensor was has led to the tremendous development in both theoretical
designed at frequency 0.8-1.3 sensor design techniques and in the industry technology used.
Material Characterization GHz. Mixture samples were
Using Complementary Split- used such as air, Teflon, RO
As a result, the resonant cavity method is known as the precise
Ring Resonators. 3003 and FR4. The advantages technique in the resonator sensor design for materials
1[6]
are high measurement characterizing. However, the complexity of the manufacturing
Muhammed Said Boybay, sensitivity, less expensive process leads to the high cost of fabrication, even though the
2012 fabrication cost, easy process of
fabrication and very low loss
sensitivity could be higher. Thus, the planar resonator sensor
detection structure. is proposed in this study. This technology can be used to
enhance the weaknesses of conventional resonator design due
The resonator sensor was
designed at frequency 5 GHz. to the planar structure. Further, it can be easily integrated with
Mixture samples were used other components or devices. It is less expensive and
such as saline, ethanol, salt, consumes minimum volume of detectable samples. The design
Substrate-Integrated Half- sugar and water aqueous structures also are simple and easy to fabricate, although they
Mode Resonant Near-Field solution. The advantages are
2[13] Sensor for Liquid compact in size and act as can achieve higher Q-factor with certain techniques. The
Characterization. resonant near-field sensor and device can be expanded based on its achievement. Although
Nora Haase , 2013 have very low cost fabrication the research in this area is not at its infancy stage, the research
process. It is easy access to the is still ongoing. Hopefully, the challenges faced by the
tip from the top of sensor and
also have the simplicity of researchers can be overcome and improved in order to gain
structure. advancement and improvement in this technology.
The resonator sensor was
designed at frequency 4.8-8.7
ACKNOWLEDGMENT
A Circular Patch Resonator GHz. Mixture samples were
for the Measurement of used such as nematic liquid- Sincerely to express the appreciation to Universiti Teknikal
3[22] Microwave Permittivity of crystal mixture. The advantage Malaysia Melaka (UTeM) and Ministry of Higher Education
Nematic Liquid Crystal. of the design is simple resonator
Diminic E. Schaub, 2011 construction, but have quite
(MOHE) for funding this work under the research grant
expensive materials for the RAGS/1/2014/TK03/FTK/ B00078.
fabrication process.

The resonator sensor was

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