Optical Fiber Technology 41 (2018) 109–117

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Optical Fiber Technology

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Quasi-distributed sol-gel coated fiber optic oxygen sensing probe T

a,⁎ b a a
Maizatul Zolkapli , Suhairi Saharudin , Sukreen Hana Herman , Wan Fazlida Hanim Abdullah
a
Faculty of Electrical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
b
Department of Photonics, MIMOS Berhad, 57000 Technology Park Malaysia, Kuala Lumpur, Malaysia

A R T I C L E I N F O A B S T R A C T

Keywords: In the field of aquaculture, optical sensor technology is beginning to provide alternatives to the conventional
Optical fiber oxygen sensor electrical sensor. Hence, the development and characterization of a multipoint quasi-distributed optical fiber
Quasi-distributed sensor sensor for oxygen measurement is reported. The system is based on 1 mm core diameter plastic optical fiber
Sol-gel where sections of cladding have been removed and replaced with three metal complexes sol-gel films to form
PdTFPP
sensing points. The sensing locations utilize luminophores that have emission peaks at 385 nm, 405 nm and
PtOEP
465 nm which associated with each of the sensing points. Interrogation of the optical sensor system is through a
Ru(dpp)32+
fiber optic spectrometer incorporating narrow bandpass emission optical filter. The sensors showed comparable
sensitivity and repeatability, as well as fast response and recovery towards oxygen.

1. Introduction minimal. Our goal in this work is to demonstrate that by capitalizing

In the past few decades, significant efforts have taken place to en-
hance the performance of oxygen sensors based on optical fiber via
incorporating oxygen sensitive nano-materials into their structure
[1–10]. At present, the majority of work in the field of optical oxygen
sensors has been devoted to coating the luminescent nanomaterials on
the tip of optical fiber [2,5,11–15], whilst the number of reports on the
sensing properties of quasi-distributed optical oxygen sensor based on
evanescent wave, are significantly lower [16–19]. This may be due to
the fact that the preparation of quasi-distributed or multipoint sensor
involves tedious and complicated fabrication techniques. Moreover,
such configuration requires sensing region to be arranged at different
points along an optical fiber.
A variety of techniques have been reported such as tapering the
optical fiber [20], etching the optical fiber to form a D-shape fiber
[21,22], bending the fiber into U-shape fiber [23,24], and stripping to
remove a region of cladding from the fiber [16,25,26]. In most cases, a
reduction of the cladding thickness is required to provide effective
evanescent field interaction, especially if short wavelengths are planned
to be used for sensor excitation. Hence, resulting in a very fragile fila-
ment that requires additional care as compared to single point sensing
where the luminescent material is immobilized on the tip of the optical
fiber. Despite of the difficulty, such arrangement is favored for si-
multaneous measurement of two or more parameters in complex media
and processes. Substantial research has reported various evanescent
wave sensing scheme [27–29] for oxygen measurement [30–34], but
sensing element arranged in quasi-distributed configuration is very
the evanescent wave phenomenon, a multi-position oxygen sensing
element can be fabricated in a single optical fiber for real-time and
simultaneous measurements. This is particularly important especially in
aquaculture for example where dissolved oxygen concentration varies
at different depth and location in the water. By having a quasi-dis-
tributed optical fiber dissolved oxygen sensor a large area of the pond
can be covered and can be monitored within a single system. The
measurement of dissolved oxygen at diverse locations and depths can
be made possible depending on how the sensor is placed. If the fiber
optic is deployed horizontally, it can measure the dissolved oxygen
levels at various locations. If it is deployed vertically, it can measure the
oxygen levels at different depths of the pond. Optical sensor technology
addresses the weaknesses of the conventional electrical sensor as it is
capable of measuring the parameter for a long period of time with
minimal measurement drift and without cleaning the sensing head
regularly as in the electrochemical based sensor [35–37]. These attri-
butes combined with less maintenance and calibration requirement in
optical dissolved oxygen technique has appealed more and more usage
of such sensor in the aquaculture sensor.
In this paper, the development of a quasi-distributed sol-gel coated
fiber optic oxygen sensor based on direct measurement of luminescence
intensity is demonstrated. To achieve this, a simple, low cost technique
to fabricate a plastic optical fiber sensor for the sensing of oxygen is
presented. A narrow bandpass emission optical filter is utilized to
capture the emission signal from the three sensing points. Each point
consists of a section of sol-gel coated uncladded fiber with a selected
length as mentioned in the previous publication [38]. The performance

⁎
Corresponding author.
E-mail address: maizatul544@salam.uitm.edu.my (M. Zolkapli).

https://doi.org/10.1016/j.yofte.2017.12.016
Received 26 October 2017; Received in revised form 19 December 2017; Accepted 19 December 2017
1068-5200/ © 2017 Elsevier Inc. All rights reserved.
M. Zolkapli et al.
characteristics, such as quenching behavior, sensitivity, repeatability
and response time of the sensing system are reported.
2. Experimental work
2.1. Preparation of the oxygen sensing fiber
A multimode plastic optical fiber (Mitsubishi Rayon Co. Ltd.) with a
core diameter of 1 mm was used in the experiment. The large core size
makes it easy to couple lots of light from the light source and con-
nectors do not need to be high precision [39]. In an attempt to make a
quasi-distributed sensor, the multiple sensing region needs to be created
along the optical fiber line and placed 15 cm apart from each other.
Hence, using sol-gel technique the oxygen sensitive material will be
coated at the pre-determined middle sections of the fiber. With the aid
of a retractable blade utility knife, a small section about 5 mm length of
the POF jacket was removed exposing the core-cladding. This is the
optimum size for the sensitive sections that gives high sensitivity as
reported in earlier study [38]. The cladding was then chemically etched
with acetone leaving the core region to be coated with sol-gel. To access
whether the cladding was completely removed, the diameter of the
fiber was measured using a digital Vernier caliper (Mitutoyo). Fig. 1
shows the FESEM images of the POF core-cladding surface before and
after chemical etching. This is to inspect that the cladding has been
completely removed prior to sol-gel dip coating step. Prior to the dip
coating process, the POF was wiped with EtOH and rinsed with copious
amounts of de-ionized water and left to dry at room temperature for one
hour. In order to verify the reproducibility of the sensor performance,
three samples were fabricated for each dye and the average values were
obtained.
2.2. Preparation of film coatings
The synthesis of sol-gel was done by adapting the procedure used by
Yeh et al. [11] with some modification. The optimized recipe used in
this work is based on characterization work performed by the team
[40,41]. For this study three types of oxygen sensitive luminescence
dyes namely Tris (4,7-diphenyl-1,10-phenanthroline) ruthenium (II)
dichloride (Ru(dpp)3Cl2)/Ru(dpp)32+), platinum octaethylporphyrin
(PtOEP) and 5,10,15,20-tetrakis (pentafluorophenyl) 21H,23H-por-
phine palladium (II) (PdTFPP) were used. These dyes which upon ex-
citation, responds to different spectral wavelength unique to each ma-
terial has been widely used as a probe for luminescent detection and
quantification of oxygen [3,11,13,42–44]. Silica sol was prepared by
mixing tetraethylorthosilicate (TEOS, 99.999% Aldrich) and octyl-
triEOS together to form precursor solutions. Ethanol (EtOH) was then
added to the sol solution to form a homogeneous solution. Then HCl
Fig. 1. The structure and the dimension of SK-4001 POF at 50× magnification (a) before etching and (b) after etching with acetone at two different locations along the sample.
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Optical Fiber Technology 41 (2018) 109–117
Table 1
Composition of the prepared sol and dye solution.
Sol solution TEOS (ml) EtOH (ml) Octyl- HCl (µl) Triton X-
triEOS (μl) 100 (µl)
4 1.25 40 400 40
Dye solution PtOEP (mg) PdTFPP (mg) Ru(dpp)32+ EtOH (ml) THF (ml)
(mg)
2 2 2 5 10
and triton X-100 were added with constant stirring to accelerate hy-
drolysis and prevent cracks in the sol-gel film. This mixture was mag-
netically stirred for 1 h at ambient temperature to get a stable silica sol.
To prepare the dye solution, each dye was dissolved separately with its
solvent and the solutions were stirred under ambient temperature for
1 h. EtOH was the solvent for Ru(dpp)32+, while THF was the solvent
for PtOEP and PdTFPP. Eventually, to prepare the luminophore-doped
sol-gel, the prepared sol solution was mixed with the dye solution. The
sol mixtures were capped and stirred for another 2 h at room tem-
perature to ensure the formation of a homogeneous sol-gel. The process
was repeated for all dyes. The composition of the prepared solution is
tabulated in Table 1.The sol-gel was coated on the core POF using a
computer-controlled dip coating apparatus at a speed of 120 mm/min.
This will result in about 10 nm thickness of sol-gel which has been
characterized earlier [40]. These fibers were dried in the oven at 70 °C
for 24 h for stabilization of dyes in the host matrix as shown in Fig. 2.
The dried coatings were then washed with de-ionized water to remove
the excess and unbound dye.
2.3. Experimental setup
Figs. 3 and 4 illustrate the experimental setup used to characterize
the performance of the quasi-distributed fiber optic oxygen sensor in
gas and aqueous media. The same optical setup was used for both gas
and aqueous except that the test chamber was different for each con-
dition. The sensor was characterized in two different salinity which are
0.1 ppt and 35 ppt (salinity of water and salt water respectively) at
three different temperatures; 10 °C, 25 °C and 40 °C. One end of the
sensor probe was fed to the fluorescence mini cube (FMC) filter. Ex-
citation energy was provided by the Doric LED3C_SMA (385 nm,
405 nm and 465 nm wavelength) which each wavelength was the ex-
citation suitable for each luminescent indicator. The excitation light
was transmitted to the sensors through a fiber optic cable. When the
excitation light from the source reached the luminescence materials on
the sensor, a molecular excitation occurred and a new colour was
emitted. This emission was then carried back to the FMC filter. The FMC
filter was used to split the emission of the indicator so that it can be
analyzed separately. The remaining 3 ports from the FMC filter were
M. Zolkapli et al.
connected to the spectrometer. Each channel filtered specific range of
spectrum which corresponds to the emission of the indicator. The lu-
minescence indicators were sensitive to levels of oxygen. Eleven dif-
ferent oxygen concentrations were obtained by mixing oxygen and ni-
trogen gas, which process was controlled by gas flowmeters. The
emission intensity was measured using Avaspec multichannel fiber
optic spectrometer (Avantes) which was then displayed on the com-
puter. Air pump and stone were placed in the water bath to oxygenate
the water, as surface water movement causes the contact to have more
contact with the air hence more oxygen gets into the water. A com-
mercial oxygen and temperature probe from Ocean Optics were placed
in the test chamber as reference.
3. Results and discussion
3.1. Oxygen sensing properties of the quasi-distributed optical sensor
The absorption spectra of PtOEP, PdTFPP and Ru(dpp)32+ which
obtained from UV–VIS spectrometer (Perkin Elmer Lambda 35) peaks at
385 nm, 405 nm and 465 nm respectively are illustrated in Fig. 5. Thus,
these are the LED wavelength for the exciting light source. PtOEP,
PdTFPP and Ru(dpp)32+ emit luminescence at roughly three different
wavelength, 590 nm, 640 nm and 670 nm respectively. Fig. 6 shows the
emission spectra of each dye from the fluorescence mini cube (FMC)
filter. Based on our studies, the emission can still be obtained at max-
imum of 1000 m length of quasi-distributed sensor. The three filter
ports corresponds to the exact wavelength of the oxygen sensitive lu-
minescence dyes so that each of the filter port allows the filtered lu-
minescence light waves to alternately pass to the spectrometer.
Fig. 3. Experimental setup for testing the quasi-distributed fiber optic oxygen sensor in gas media.
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Optical Fiber Technology 41 (2018) 109–117
Fig. 2. POF fiber after 24 h oven bake at 70 °C with each
fiber coated with PtOEP, PdTFPP and Ru(dpp)32+ sol-gel
respectively.
Fig. 7 shows the emission spectral response of the quasi-distributed
sensor measured using spectrometer at eleven different oxygen con-
centrations (0%–100%). It is evident from the emission spectra that the
response of the quasi-distributed optical oxygen sensor can be detected
and in accordance with their respective wavelengths. It is also apparent
that the relative emission intensity for each sensor reduced significantly
on increasing oxygen concentration. This result is in agreement with the
work done by X. Xiong et al. and C.S. Chu [14,45]. As oxygen crosses
the sol-gel film, the luminophores collide with the oxygen molecules
during their excited state lifetime, hence quenching the intensity of the
luminophores. The intensity count is directly relatable to the amount of
oxygen in the chamber. However, the quenching of luminescence is
better expressed by the Stern-Volmer equation in order to analyze the
sensor sensitivity:
I0 τ
= 0 = 1 + K SV [O2]
I τ (1)
K SV = k τ0 (2)
where I and I0 are the quenched and unquenched emission intensities, τ
and τ0 are the quenched and unquenched excited state lifetimes, K SV is
the Stern-Volmer quenching constant, k is the bimolecular diffusion
dependent quenching constant and [O2] is the concentration of
quencher. From equation 1, a plot of I0/ I or τ0/ τ versus [O2] is expected
to be linearly dependent upon the concentration of quencher, with a
slope equal to K SV and an intercept of unity. However, if both static and
dynamic quenching are present, Eq. (1) may be rewritten as
I0
= 1 + (K SV + K eq)[O2] + K eq K SV [O2]2
I (3)
M. Zolkapli et al.
Fig. 4. Experimental setup for testing the quasi-distributed fiber optic oxygen sensor in aqueous media.
where Keq is the dissociation constant for the binding of the quencher to
the luminescent species [46]. If the I0/ I and τ0/ τ plots versus [O2] are
linear and coincide, quenching is purely collisional i.e. Keq = 0. How-
ever, if I0/ I is everywhere greater than τ0/ τ , static quenching is present
[47].
Based on Fig. 8, it can be seen that all three sensors showing higher
slope in gas media, indicating that they are more sensitive to sense
oxygen in gas than in aqueous. This can be attributed to the increase
transmission of light at the core/water boundary since the normalized
index difference is lower than when it is in aqueous environment [48].
However, in aqueous media, there is a higher sensitivity observed with
higher salinity for Pd-doped and Pt-doped sensor which suggest that
there is a greater sensitivity to the luminophores with decreased
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Optical Fiber Technology 41 (2018) 109–117
quencher solubility. This is due to the fact that solubility of oxygen
decreases as salinity increases [49,50]. The Pt and Pd-doped sensors
also show the straight-line variation of Io/I versus oxygen concentration
for all conditions suggesting that the sensors experiences high sensi-
tivity. However, the Stern-Volmer plot for Ru-doped sensor is curved
and less steep, indicating that it is generally less sensitive than Pt and
Pd-doped sensors. But this fact have to be discounted as it is not the
objective of this study to compare sensitivity of the sensors. Three
different dyes were chosen to form the quasi-distributed arrangement
so that the emission wavelengths do not overlap. Moreover, such result
is not due to the variation in the natural lifetime of the probe, but it is
due to a combination of a lower solubility of oxygen and a lower bi-
molecular quenching rate constant as explained by Mills [6].
Fig. 5. UV–VIS absorption spectra of PtOEP, PdTFPP and Ru
(dpp)32+ which peaks at 385 nm, 405 nm and 465 nm re-
spectively.
M. Zolkapli et al.
Fig. 7. Emission spectra of the quasi-distributed optical fiber oxygen sensor as function of oxygen concentration. The emission of (a) CH1, (b) CH2 and (c) CH3 are at 670 nm, 640 nm and
590 nm respectively using a FMC filter.
Interestingly, the Pd and Pt-doped sensors do not display non-linear,
downward curving Stern-Volmer plots implying the platinum and pal-
ladium porphyrins are uniformly distributed in the hydrophobic parts
of the matrix, while ruthenium complexes can be found in different
region of the silica gel film with different accessibility to the oxygen
molecules [51,52]. This phenomenon is quite common in many silica
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Optical Fiber Technology 41 (2018) 109–117
Fig. 6. Emission spectra of the three oxygen sensitive lu-
minescence dye (Ru(dpp)32+, PtOEP, and PdTFPP) being
filtered by the FMC filter.
gel-based oxygen sensors especially for high oxygen concentrations
[2,5,24,53,54].
Table 2 summarizes the sensitivity slope and R-squared value for all
the sensors in all experiment conditions. As can be seen from the table,
almost all the linear regression coefficients were approximately 0.9,
which suggest a high linear correlation which is in accordance to the
M. Zolkapli et al. Optical Fiber Technology 41 (2018) 109–117

Fig. 8. Stern-Volmer plot for quasi-distributed fiber optic oxygen sensor in (a–c) gas and aqueous environment and (d–f) 0.1 ppt and 35 ppt water.

Table 2
Responses of the three sensing films to gaseous oxygen and dissolved oxygen.

Condition Sensitivity slope R squared

PdTFPP PtOEP Ru(dpp)32+ PdTFPP PtOEP Ru(dpp)32+

Oxygen gas 0.6381 0.105 0.0194 0.989 0.9916 0.9946

DO in 0.1 ppt water at 10 °C 0.0492 0.0319 0.0034 0.9952 0.997 0.9975
DO in 0.1 ppt water at 25 °C 0.0278 0.0176 0.0018 0.9973 0.9805 0.9534
DO in 0.1 ppt water at 40 °C 0.0535 0.0245 0.0023 0.9963 0.9675 0.9831
DO in 35 ppt water at 10 °C 0.0404 0.0346 0.0034 0.9939 0.9934 0.981
DO in 35 ppt water at 25 °C 0.0783 0.0362 0.0015 0.9831 0.9939 0.997
DO in 35 ppt water at 40 °C 0.12 0.0554 0.0015 0.9972 0.9845 0.9632

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M. Zolkapli et al.
Stern-Volmer equation 1. It is apparent from this table that by cali-
brating the reduction in intensity using a Stern-Volmer plot, it is pos-
sible to estimate the concentration (partial pressure) of oxygen in the
system as the Stern-Volmer constants changed with the quencher con-
centration.
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Optical Fiber Technology 41 (2018) 109–117
Fig. 9. Response characteristics of the quasi-dis-
tributed fiber optic oxygen sensor to gaseous
oxygen when switching alternately between
100% nitrogen and 100% oxygen.
3.2. Response time
Fig. 9 presents the response time and operation stability of the
quasi-distributed optical fiber oxygen sensor to oxygen when switching
between fully oxygenated and fully deoxygenated environments. In
M. Zolkapli et al. Optical Fiber Technology 41 (2018) 109–117

Table 3
Comparison of performance characteristics of the proposed quasi-distributed oxygen sensor with those of existing optical oxygen sensors.

O2-sensitive dye Support matrix Response time (t95), N2 to O2 (s) Recovery time (t95), O2 to N2, (s) Intensity ratios of I0/I100 Ref.

PdTCPP Octyl-triEOS/TEOS sol 2 43 153 [57]

PtTFPP Octyl-triEOS/TEOS sol 0.6 5 22 [11]
PtOEP Octyl-triEOS/TEOS sol 0.7 14 47 [11]
PtPorphyrin TEOS 12 190 70 [52]
PtTFPP Octyl-triEOS/TEOS sol 6.7 46.6 – [12]
PdTFPP n-Propyl-TriMOS/TEOS/Octyl-triEOS 2 43 65 [58]
Ru(dpp)32+ Silica-Ni-P composite coating 200 300 2.49 [45]
Ru(dpp)32+ Ormosil microbeads 30 20 – [59]
PdTFPP Octyl-triEOS/TEOS sol gel 10 45 63.85 This study
PtOEP Octyl-triEOS/TEOS sol gel 11 33 11.77 This study
Ru(dpp)32+ Octyl-triEOS/TEOS sol gel 10 40 3.07 This study

general, the response time of optical oxygen sensor is defined as the
time required for 95% of the total change in luminescence intensity to
occur [52,11]. It is found that the response time of PdTFPP-doped
oxygen sensor is 10 s when switching from nitrogen to oxygen gas and
the recovery time is 45 s when switching from oxygen to nitrogen. For
PtOEP-doped oxygen sensor, the response time is 11 s and the recovery
time is 33 s, while the response time of the Ru(dpp)32+-doped oxygen
sensor is 10 s and the recovery time is 40 s. The measurement of the
oxygen level by the sensors is validated by the Ocean Optics oxygen
probe.
As illustrated in Fig. 9, it is apparent that the optical sensors provide
stable and reproducible signals as the environment alternates between
oxygenated and deoxygenated condition. The fast response time is a
result of the microporous structure of the sol-gel matrix. The response
times obtained in this study are comparable to or better than that of the
existing oxygen sensors based on different fluorophores immobilized in
a sol-gel matrix [2,55,56] as tabulated in Table 3. I0/I100 among the
three films for both gaseous (GO) and dissolved oxygen (DO) were Ru
(dpp)32+ < PtOEP < PdTFPP (Table 3).
4. Conclusions
We have successfully demonstrated the feasibility of fabricating a
quasi-distributed fiber optic sensor for oxygen sensing. The quasi-dis-
tributed optical oxygen sensor based on luminescence intensity is
constructed by immobilizing the oxygen sensitive indicators namely
PtOEP, PdTFPP and Ru(dpp)32+ in Octyl-triEOS/ TEOS sol-gel matrix at
three locations on a fiber and employ a narrow bandpass emission
optical filter in the system. The experimental results in both gas and
aqueous media have shown that the proposed sensors exhibit good
sensitivity, linearity and comparable response time with existing single
optical oxygen sensors. The advantages of employing such sensors are
the simplicity of the measurement system, added to the low manu-
facturing, interrogation and maintenance costs to monitor oxygen
concentration at several position in real time simultaneously.
Acknowledgements
The authors wish to thank the Ministry of Education (MOE),
Malaysia for funding the research project through the Niche Research
Grant Scheme [Ref. No. 600-RMI/NRGS 5/3 (2013)], as well as MIMOS
Berhad and Institute of Research Management and Innovation (IRMI)
Universiti Teknologi MARA (UiTM) for the facilities and administrative
support.
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Maizatul Zolkapli received her Bachelor of Engineering (Electrical and Electronic) with
Honours from Universiti Tenaga Nasional, Malaysia (2001) and Master of Science
(Microelectronic Engineering) from Universiti Malaysia Perlis, Malaysia (2010). She is
currently pursuing her PhD degree at Universiti Teknologi MARA, Malaysia where she is
working on the synthesis and characterization of sol-gel coatings for fiber optic chemical
sensors.
Suhairi Saharudin is a senior staff researcher at Photonics R&D Laboratory in MIMOS
Berhad, Malaysia with more than 20 years’ experience in optical fibre research. He es-
tablished his career in Photonics after graduating with a master degree in Optical
Electronics from Strathclyde University, United Kingdom in 1993. During his tenure as
researcher, he was involved in several research projects ranging from Optical Fiber
Quantum Key Distribution to optical fibre chemical and physical sensors. He obtained his
Ph.D in 2006 from University Putra Malaysia in the field of Computer and
Communication System Engineering with project focus in Multiwavelength fiber laser
system. His research interest includes optical fibre communication, optical fibre sensor
and Quantum cryptography.
Sukreen Hana Herman received her PhD in Materials Science at the Japan Advanced
Institute of Science and Technology (JAIST) in 2009. She specialized in semiconductor
thin films fabrication and growth for various devices. Although her focused during her
studies for B. Eng and M. Eng in Kanazawa University, Japan was on physical vapor
deposition methods, Sukreen Hana explored to a wider variety of deposition methods to
include nanostructure materials and particles synthesis on various substrates, including
optical fibers. She is now a senior lecturer in the Faculty of Electrical Engineering,
Universiti Teknologi MARA, Malaysia.
Wan Fazlida Hanim Abdullah is a senior lecturer in the Faculty of Electrical Engineering
at the Universiti Teknologi MARA, Malaysia. Her research interests include microelec-
tronic devices, IC design and fabrication, nanoelectronics, sensors and systems and analog
circuits. She received her BE in Electronics Engineering from University of Southampton
(1993), MSc in electronic engineering from Universiti Putra Malaysia (2002) and PhD in
microengineering and nanoelectronics from Universiti Kebangsaan Malaysia (2010).