IEEE TRANSACTIONS ON MAGNETICS, VOL. 54, NO.

1, JANUARY 2018 4000207

Characterization of Au/Fe/Au and Au/Co/Au Magneto-Plasmonic

Multilayers as an Ethanol Vapor Sensor
Mina Afsharnia and Seyedeh Mehri Hamidi
Magneto-plasmonic Lab, Laser and Plasma Research Institute, Shahid Beheshti University, Tehran 1983969114, Iran
In this paper, we investigate the sensing performance of Au/Fe/Au and Au/Co/Au magneto-plasmonic nanostructures as transducers
as well as the performance of TiO2 thin film and TiO2 NPs as sensing layers. A comparison between sensing performance of the
traditional surface plasmon resonance (SPR) and the magneto-optic (MO) SPR (MOSPR) transducing techniques is presented here.
The surface plasmon wave vector in these transducers which are consisted of metallic and magnetic materials is modulated by
external magnetic field in the transverse configuration. Magneto-plasmonic structures show a great enhancement of an MO Kerr
effect when the SPR condition is satisfied. As such enhancement strongly depends on the excitation conditions of the surface plasmon
polariton (SPP) and, therefore, on the refractive index of the dielectric in contact with the metal layer, we use this enhanced MO
signal as the sensing magnitude for investigating molecular interactions between ethanol vapor and TiO2 nanostructures onto the
transducers. Besides, when the SPP is excited, applied magnetic field would modulate the SPP wave vector. The modulated nature
of MOSPR signal would lead to a higher sensing performance in terms of sensitivity and signal-to-noise ratio with respect to the
traditional SPR signal. Moreover, our results show that using TiO2 NPs in the vicinity of multilayer transducers creates a better
sensing performance which is caused by porosity and enhancement in the surface area of absorbent layer.
Index Terms— Gas sensor, laser ablation, magneto plasmonic, surface plasmon resonance (SPR).

I. I NTRODUCTION performance of the surface plasmon resonance (SPR) sensor

V OLATILE organic compounds (VOCs) are organic chem-

ical compounds that have low boiling points. This would
cause evaporation and release of a significant number of mole-
cules in the air. These compounds, which can be natural or
artificial, are widely used in the chemical industry, household
products, etc. Although, most of these compounds are not
toxic, being exposed to them for a long time would cause
some health problems such as severe headaches, allergies,
respiratory problems, and nausea. Some of them such as
formaldehyde, benzene, toluene, and xylenes are highly toxic
and carcinogenic. Formaldehyde and acrylonitrile are used as
basic raw material in the resin industry [1]. Recently, the
presence of VOC compounds in exhaled breath is a biological
sign of some diseases. For example, ethanol, alkanes, and
benzene indicate lung cancer [2], and also acetone indicates
diabetes [3]. Despite the fact that these compounds are danger-
ous, they are still used as intermediates for production of other
chemicals in the industry and also as solvents in research labo-
ratories. Therefore, accurate detection of the abovementioned
compounds is important to diagnose the diseases, industrial
hygienists, and also for occupational safety.
There are different procedures for VOC sensing as gas
chromatographically [4], electrochemical [1], acoustical [5],
and optical methods [6]. Among them, optical methods have
higher sensitivity, selectivity, stability, faster response, and
also longer life time. However, the need for a sensor with
higher performance, cheaper price, and lower production time
is still a big challenge for researchers. In this paper, the
Manuscript received May 15, 2017; revised August 11, 2017; accepted
September 27, 2017. Date of publication December 4, 2017; date of current
version December 20, 2017. Corresponding author: S. M. Hamidi (e-mail:
m_hamidi@sbu.ac.ir).
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/TMAG.2017.2761754
0018-9464 © 2017 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
that is a kind of opto-chemical sensor with high sensitivity
and fast response has been investigated. As SPR is a powerful
technique for investigation of physical and chemical processes
that occur close to the interface between a metal and a
dielectric, Nylander et al. [7] used it in gas and biosensors
in 1982. In SPR sensors, coupling with prism is more common
because it is easy, available, and also compatible with all kinds
of modulations.
Surface plasmon polaritons (SPPs) are collective oscillations
of the free-electron gas density at the boundary of a metal and
a dielectric. The wave vector of these electromagnetic surface
waves (kSpp = k0 × nmetal × nd /(n2metal + n2d )1/2 ) depends
on the refractive index of the dielectric. Variations of the
refractive index will change the SPP wave vector and the
coupling conditions (i.e., angle, wavelength, intensity, and
phase). This feature serves as the foundation for development
of the SPR sensors [8], [9].
Although, SPR-based sensor provides high sensitivity, it is
not a suitable candidate for detecting low concentrations and
small molecules. Therefore, modulation techniques can be
used to improve the sensing performance and enhance the sen-
sitivity. The addition of new features in order to control the sur-
face plasmon properties opened a new field of research known
as “active plasmonics.” Different control agents have been
proposed in the literature: temperature [10], electric field [11],
electromagnetic waves [12], or magnetic fields [13], [14]. Very
recently, the combination of magnetooptic (MO) effects and
SPR, which is called MO SPR (MOSPR) [15], has been
reported in order to enhance the sensitivity of gas sensors.
As ferromagnetic metals are magneto-optically active, they
are good candidates for active plasmonics. However, they
have high absorption coefficient which results in high loss
and broad resonance curve. On the other hand, noble metals
show great plasmonic properties. Thus, for achieving optimum
4000207
performance and less reduction, combining noble and fer-
romagnetic metals would be a suitable procedure. These
structures, which are called magneto-plasmonic structures,
would increase MO effects [16]. For the first time in 2006,
Sepúlveda et al. [17] combined magneto-optical properties of
magnetic materials with SPR and introduced magneto-optical
SPR sensor. In addition to high sensitivity, these sensors have
high signal-to-noise ratio and low limit of detection [17].
In 2010, Regatos et al. [18] investigated the capability of
Au/Fe/Au structure for sensing. In 2011, sensing of VOCs
including methanol, ethanol, and isopropanol with two types
of plasmonic and magneto-plasmonic configurations was done
by Manera et al. [19]. In their research, TiO2 porous layer
was sensing layer which was deposited by Glancing Angle
deposition method. Next year, TiO2 nanorods as sensing layer
were used in order to improve sensing performance [20].
Amine vapors were detected using the magneto-plasmonic
method in 2013 [21]. In 2014, Manera et al. [22] used
Au/Co/Au transducer in the vicinity of Zn porphyrin dimers
which was deposited by the Langmuir–Schäfer technique as
sensing layer for Amine vapors detecting and they also studied
interactions between the molecules in the liquid phase for the
application of biosensing. This method had a better stability,
reversibility, performance, and also offered a linear range
of analyte concentration [22]. In 2014, Kübler et al. [23]
examined the properties of Au/IrMn/Co/Au multilayer in
order to use it in sensors. In 2015, David et al. [24] used
Au–Co alloy in multilayered nanostructures for achieving a
more sensitive and stable sensor.
In this paper, we prepared Au/Fe/Au and Au/Co/Au
magneto-plasmonic nanostructures. Then, their performances
as sensor transducers have been investigated. Due to the fact
that gold does not react with gases, it cannot be used directly
for gas sensing, so a sensing layer is required to be placed
on the structure. When this layer is exposed to analyte, its
optical constants would alter and a change in the reflective
SPR curve occurs. Since, we wanted to sense ethanol vapors,
TiO2 thin film, and TiO2 NPs were used as sensing layers.
Chemical stability, high refractive index, and high dielectric
constant make TiO2 the basic component in the sensors [25].
Subsequently, we have plotted the calibration curves for a
sample with the best sensing performance.
II. E XPERIMENTAL P ROCEDURE
A. Preparation of Magneto-Plasmonic Transducers
In order to determine optimum thicknesses for magneto-
plasmonic multilayers which are composed of ferromagnetic
and noble metals, the transverse matrix method (TMM) was
used [16]. In this way, we introduced Imin /ω parameter
[minimum intensity to full-width at half-maximum (FWHM)
of resonance ratio] and calculated it for different thicknesses.
Among the investigated thicknesses, the one with the maxi-
mum amount of Imin /ω was chosen. The optimum thickness
obtained for Au/Co/Au structure was 20/5/17 nm and for
Au/Fe/Au structure was 25/5/25 nm. These two transducers
were placed on chromium-deposited glass substrate by the
sputtering method.
IEEE TRANSACTIONS ON MAGNETICS, VOL. 54, NO. 1, JANUARY 2018
TABLE I
S AMPLES W HOSE S ENSING P ERFORMANCES W ERE I NVESTIGATED
B. Preparation of TiO2 Thin Film and NPs as Sensing Layer
Similar to nanolayers and NPs, TiO2 sensing layer has been
prepared via two different procedures comprising sputtering
and laser ablation in liquid (LAL) methods. TiO2 target
was irradiated with pulsed Q-switched Nd:YAG laser with
the wavelength 532 nm, the pulse duration of 7 ns, and the
repetition rate of 10 Hz for 2 min via the LAL method. For the
deposition of prepared TiO2 NPs, 10 μL of the final solution
was deposited onto the transducers that were being rotated in
a vacuum chamber for 9 min by the speed of 25 round per
minute.
On the other hand, 4 nm of TiO2 thin film was deposited
by the sputtering method on the rest of the transducers as
sensing layer. Thickness of the sensing layer is a key point
in the sensing process which is calculated by the TMM
method. When its thickness is appropriate, the evanescent
electromagnetic wave of SPP at the gold/air interface would
be allowed to detect the small changes in the optical constants
faster.
C. Ethanol Vapor Sensors
Abovementioned two different sensors have been illustrated
in Fig. 1 as Au/[Co/Fe]/Au/TiO2 multilayers, Au/[Co/Fe]/Au/
TiO2 (NPs).
These magneto-plasmonic nanostructures are summarized
and listed in four different samples (Table I).
D. Sensing Characterization
In order to monitor molecular interactions at the interface
between sensing layer and ethanol vapors, the variations
of reflectivity were measured using SPR and MOSPR in
Kretschmann configuration (Fig. 2). In the MOSPR measure-
ments, a pair of magnets was used in transverse configuration
for producing significant enhancement in the MO effects. The
magnetic field of these magnets was set to 11.5 mT, and the
modulation of the magnetic field is carried out by the rotation
of magnets. By approaching the magnets to the sample as
much as possible, the applied magnetic field to a multilayer
structure could be approximated to the applied magnetic field
to a homogenous structure. Using an appropriate magnetic
field led to saturated magnetic domains of ferromagnetic metal.
Therefore, the magnetization vector (M) would be parallel to
the sample surface and perpendicular to the incident plane.
When an external magnetic field was applied in the transver-
sal configuration to explore the modulation of the surface
plasmon wave vector, MO element was coupled with a com-
ponent of magnetic field that was placed in the incident plane.
This meant that only the P-component of light was influenced
AFSHARNIA AND HAMIDI: CHARACTERIZATION OF AU/FE/AU AND Au/Co/Au MAGNETO-PLASMONIC MULTILAYERS
Fig. 1. Schematics of different kinds of magneto-plasmonic nanostructures
as ethanol vapor sensors.
by magnetic field while S-component experienced no changes.
Thus, this configuration did not alter the polarization, but the
reflected intensity of P-polarized would vary as
Rpp Rpp (M) − Rpp (−M)
= . (1)
Rpp 2Rpp (0)
Rpp /Rpp was defined as the ratio of the reflectivity change
that happened when the external magnetic field was applied
in opposite directions to the reflectivity before applying the
magnetic field. Applying the magnetic field in the transversal
configuration changed the dispersion relation of SPP mode
in a way that it would be dependent on the wave vector
direction. Rpp /Rpp implied the change in the wave vector
due to the variation of field direction. In order to examine
the sensing performance of SPR and MOSPR methods, R
and Rpp /Rpp signals have been recorded when the sample
surface was exposed to the ethanol vapor.
As we wanted to expose samples to the vapors, we have
prepared a suitable cell. For entering ethanol vapors to the
cell with the aim of sensing in the room temperature, bubbling
method was used. In this method, dry air was being sent into
250 mL ethanol by the flow of 1 L/min for 1 min. Two
paths were provided from dry air cylinder to the cell; the
first one was for entering ethanol vapors to the cell and the
second one was used for cleaning the cell and the sample.
The prism/sample/cell combination was placed onto a rotation
stage and surface plasmons were excited by a p-polarized laser
beam at a wavelength of 635 nm, then the reflected light was
detected by a wide range silicon pin photodiode and a digital
oscilloscope.
III. R ESULTS AND D ISCUSSION
TiO2 NPs which were prepared by the LAL method have
been examined by UV-visible spectroscopy.
4000207
Fig. 2. Schematic of magneto-optic SPR experimental setup.
Fig. 3. Optical absorption spectra of TiO2 NPs prepared by the LAL method.
This spectroscopy indicated main absorption peak at 305 nm
which was expected (Fig. 3). The theoretical and experimen-
tal angular modulation of reflectance curve for samples 1
(Au/Co/Au/TiO2 multilayer) and 3 (Au/Fe/Au/TiO2 multi-
layer) are illustrated in Fig. 4. It indicates the theoretical and
experimental enhancement of the transverse MO Kerr effect
for those samples.
The enhancement coefficient of magnetic field (HEn), which
was defined as the ratio of output field from the last layer to
the input field into the first layer was obtained via the TMM
method as explained in [16]. This quantity (2) refers to the
localization of electromagnetic field in the magneto-plasmonic
multilayered structures
 
 HN 2
HEn(magnetic-field-enhancement) =    . (2)
H1 
As we expected, the maximum enhancement of the MO
effect and also the maximum localization in the ferromagnetic
layer has occurred at the angle that SPR happened. Since sur-
face plasmons are localized oscillations, electric and magnetic
fields of the incident light have been increased. Thus, this
increase would result in Kerr effect enhancement which is
related to magneto-optical modulation of the SPP wave vector.
There is a mismatch between experimental and theoretical
results which can be explained by the roughness of the
surface. This roughness made an area that included both gold
4000207 IEEE TRANSACTIONS ON MAGNETICS, VOL. 54, NO. 1, JANUARY 2018

Fig. 5. Comparison between SPR and MOSPR signals for sample 1,

Au/Co/Au/TiO2 multilayer.

flatter surfaces. For testing the ability of SPR and MOSPR

sensing methods, we have recorded the R and R/2R signals
for all prepared samples. Fig. 5 demonstrates these two signals
for sample 1.
Exploring the angular dependence of Rpp /R has shown
that when no SPP was excited, Rpp /R would have smooth
angular variations. These variations are due to the changes
in the electromagnetic field which were caused by the non-
diagonal elements of the ferromagnetic dielectric tensor. How-
ever, when SPPs were excited, a significant increase would
be observed in Rpp /R. The curve demonstrated that beside
the effect of non-diagonal elements, there was another reason
for changing the reflectance. Indeed, applying the magnetic
field perpendicular to the propagation direction of SPPs would
modulate SPP wave vector. This modulation played an impor-
tant role in the variations of reflectance. Rpp /R implied the
wave vector variations which were caused by the changes
of field direction. Maximum of the Rpp /R was related to
the minimum of the reflectance and also to the optimum
coupling.
It can be seen that the slope of the Rpp /R signal is larger
than the R signal [Fig. 6(a)] and it has a narrower dip. In
addition, the dip in the Rpp /R curve experiences a larger
shift due to the exposure to ethanol vapors [Fig. 6(b)]. All
of these characteristics would lead to a high-sensitive sensor.
One can conclude that using magneto-plasmonic structures and
controlling their properties by an external magnetic field result
in the increase of gas sensor sensitivity.
In transverse configuration, the magnetic field would change
the SPP wave vector and modify the dispersion relation of the
SPP mode in such a way that dispersion relation depended on
k direction [i.e., ω(k) = ω(−k)]. Thus, this magnetic field
induced non-reciprocity. In this case, the SPP wave vector
would be expressed as

Fig. 4. (a) Theoretical and experimental angular modulation of reflectance ksp (B) = ksp
0
+ ksp (B). (3)
for (a) Au/Co/Au/TiO2 multilayer and (c) Au/Fe/Au/TiO2 multilayer and also
0 indicates the SPP wave vector of the single interface
ksp
enhancement of magneto-optic effect in (b) Au/Co/Au/TiO2 multilayer and
(d) Au/Fe/Au/TiO2 multilayer. when no magnetic field is applied.ksp(B) is related to the
wave vector variations which is caused by applied magnetic
and ferromagnetic metals. Magneto-optical properties of these field. These variations were reported for an interface between
areas differed from the properties of ferromagnetic layers. a dielectric and a ferromagnetic metal [26] and also for
Therefore, we would approach the theoretical values by using Au/Co/Au multilayer [27].
AFSHARNIA AND HAMIDI: CHARACTERIZATION OF AU/FE/AU AND Au/Co/Au MAGNETO-PLASMONIC MULTILAYERS 4000207

Fig. 7. R/R versus angle of incidence for (a) sample 4

(Au/Fe/Au/TiO2(NPs). (b) Sample 3(Au/Fe/Au/TiO2) under ethanol vapor
Fig. 6. (a) SPR signal for sample 1 (Au/Co/Au/TiO2) under ethanol vapor exposure.
exposure. (b) MOSPR signal for sample 1 (Au/Co/Au/TiO2) under ethanol
vapor exposure.
TABLE II
A NGULAR S HIFTS W HEN S AMPLES W ERE B EING
MOSPR sensors employ the transversal MO kerr signal as E XPOSED TO E THANOL VAPORS
the sensing magnitude instead of the reflecting intensity. The
MO effects are very localized and show a very sharp curve.
As a consequence, small variations of the refractive index
would induce large changes in the MO response. In other
words, the modulated nature of the signal is expected to
ensure a high signal-to-noise ratio with higher sensitivity
performance.
In order to compare the ability of TiO2 NPs and TiO2 thin
films as sensing layers of the magneto-plasmonic multilayered
transducers, reflectivity variations were recorded when both of
them were exposed to ethanol alcohol vapor (Fig. 7).
TiO2 NPs made a porous layer which was more suitable for
interactions between vapors and sensing layer. This procedure
provided a larger surface area of absorbent layer which led to This was due to the fact that the thickness of top Au in
better penetration of gaseous molecules into the nanostructures Au/Co/Au structures was smaller than Au/Fe/Au ones, so a
and produced detectable changes in dielectric constant of the stronger SPP evanescent wave would observe the interface and
system. Even when we used TiO2 NPs as sensing layer, the sensing performance would be better.
magneto-optical signal has still shown a narrower curve and All of the results have verified that ethanol vapor absorption
experienced a larger shift in comparison with optical signal. resulted in the changes of the refractive index and the thickness
For all of the results pertaining to samples 1–4, when we of the sensing layer which could be explained by adsorption
used Fe rather than Co as ferromagnetic layer, FWHM would between ethanol molecules and TiO2 surface.
decrease. On the other hand, the required magnetic field to Physical adsorption is a reversible process which makes
saturate the Fe film was lower than that for Co and its adhesion the sensing mechanisms reversible, too. If the attractive force
with Au was much better. between a solid and a gas is more than attractive force between
According to Table II, the magneto-plasmonic multilayer gas molecules, gas molecules would condense on the solid.
containing Co has experienced a larger shift. Adsorbate would not penetrate into solid crystal lattice or solve
4000207
Fig. 8. Calibration curves based on (a) optical and magneto-optical
parameters and (b) angular shift due to exposure of Au/Co/Au/TiO2(NPs)
to different flows.
in it. When the absorbent and adsorbate are in touch for an
adequate period of time, equilibrium would occur between the
amount of the adsorbate and the adsorpt.
Molecular ethanol is bonded to Ti atoms via a lone oxygen
pair, while dissociated ethanol bonds strongly to Ti through
covalent bonds. Dissociated ethanol adsorption on Ti4+ is
more favorable than molecular ethanol adsorption.
Ethanol adsorption includes molecule–molecule and
molecule–substrate interactions. Ethanol would lose an H
adatomon a neighbor Obr and the oxygen of the ethoxy group
fills the Ov
CH3 CH2 OH + Obr → CH3 CH2 OTi + Obr − Had . (4)
In the closest layer to the surface, the interaction with
Ti4+ is expected to be dominant, while it is much weaker in
higher layers. Ethanol molecules interact with each other via
H-bonding and cause the formation of multilayer above the
surface of the sensing layer.
In the layer which is in contact with the TiO2 surface,
both dissociated and molecular ethanol is existed. Molecular
ethanol bonds to the TiO2 surface via H-bonding whereas the
ethoxy groups form stronger σ -bonds. In the upper layers,
molecular ethanol bonds to each other and to the layer in
contact with TiO2 surface through hydrogen bonds [28].
In porous layers, the formation of the multilayers leads to
complete filling of pores and subsequently, the refractive index
of the sensing layer would be changed significantly which
in turn results in a more pronounced variation of the sensor
response.
IEEE TRANSACTIONS ON MAGNETICS, VOL. 54, NO. 1, JANUARY 2018
A. Calibration Curves of the Optimum Sample
As mentioned above, the sensing performance of Au/Fe/Au
and Au/Co/Au magneto-plasmonic transducers was investi-
gated. Then, we have chosen one sample which had the
largest angular shift while it was exposed to ethanol vapors:
Au/Co/Au/TiO2 (NPs).
In order to obtain calibration curves for this sample, dry air
was being sent into 250 mL ethanol by the flow of 1 L/min
for 1, 2, and 3.5 min. After each time interval, dry air was
being sent into the cell by the flow of 1 L/min for cleaning
the cell and the sensing layer. This phenomenon has proved
the reversibility of our sensors.
We have plotted two kinds of calibration curves: one
of which has shown the angular shift due to exposure to
different flows. For the second one, optical and magneto-
optical parameters at the SPR angle, [(Rn − R0 )/R0 ] and
[((R/R)n − (R/R)0 )/(R/R)0 ], respectively, introduced.
Zero index indicated that no ethanol vapors went into the
cell and n index was related to different flows which went
into the cell. Then, we have calculated these parameters for
different flows. These calibration curves are shown in Fig. 8
for Au/Co/Au/TiO2 (NPs).
The performance of the magneto-plasmonic transducers
with two types of ferromagnetic materials; Fe and Co, for
ethanol vapor sensing has been investigated, as well as the
performance of the two types of sensing layers; TiO2 NPs
and TiO2 thin film. For this purpose, the optimum thickness
for multilayer structures by the TMM method was calculated.
In addition, a comparison between the sensing performance of
the prepared samples in traditional SPR and MOSPR sensing
configurations was presented.
Sensing based on MOSPR has shown larger angular shift
than sensing based on SPR which verified the better sens-
ing performance of the MOSPR method. Moreover, using
TiO2 NPs in the vicinity of multilayer transducers has indi-
cated better sensing performance originated from the poros-
ity and the enhancement of the surface area of absorbent
layer.
Calibration curves for one sample which had the largest
angular shift while it was exposed to ethanol vapors:
Au/Co/Au/TiO2 (NPs) was plotted. These calibration curves
have demonstrated that MOSPR signal provided higher sensi-
tivity and signal-to-noise ratio than SPR signal.
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Mina Afsharnia received the M.S. degree in photonics from Shahid Beheshti
University, Tehran, Iran, in 2016.
She is currently a Photonics Researcher on magnetic sensors and their
applications.
Seyedeh Mehri Hamidi received the Ph.D. degree in photonics from Laser
and Plasma Research institute, Shahid Beheshti University, Tehran, Iran,
in 2009.
She is currently the Director of the magneto-plasmonic lab with the Laser
and Plasma Research Institute, Tehran. She was involved in the research fields
of magneto-plasmonic, nanophotonics, neurophotonics, piezotonics, photonic
and magnetophotonic crystals, surface plasmon resonance, dielectric and
magnetic waveguides, and pulsed laser deposition technique.