Materials and Design 92 (2016) 906–910

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Characterization of Metglas/poly(vinylidene fluoride)/Metglas

magnetoelectric laminates for AC/DC magnetic sensor applications
S. Reis a,b,1, M.P. Silva a,1, N. Castro a,b, V. Correia a,b, P. Martins a,⁎, A. Lasheras c, J. Gutierrez c, J.M. Barandiarán c,d,
J.G. Rocha b, S. Lanceros-Mendez a,e
a
Centro/Departamento de Física, Universidade do Minho, 4710-057 Braga, Portugal
b
Centro Algoritmi, Universidade do Minho, 4800-058 Guimarães, Portugal
c
Departamento de Electricidad y Electrónica, Facultad de Ciencia y Tecnología, Universidad del País Vasco (UPV/EHU), P.O. Box 644, 48080 Bilbao, (Spain)
d
BCMaterials, Ibaizabal Bidea Bdng 500, Parque Científico y Tecnológico de Bizkaia, 48160, Derio, Spain
e
BCMaterials, Parque Científico y Tecnológico de Bizkaia, 48160-Derio, Spain

a r t i c l e i n f o a b s t r a c t

Article history: Polymer-based magnetoelectric materials show increasing interest for a large number of applications and, in par-
Received 28 October 2015 ticular, for the development of magnetic sensors. Nevertheless, relevant parameters such as sensitivity, accuracy,
Received in revised form 9 December 2015 linearity, hysteresis and resolution have been vaguely or never discussed. This work reports on those parameters
Accepted 14 December 2015
on a Metglas/poly(vinylidene fluoride)/Metglas magnetoelectric laminate.
Available online 17 December 2015
The sensitivity and resolution determined for the DC (30 mV·Oe−1 and 8 μOe) and AC magnetic field sensor
Keywords:
(992 mV·Oe−1 and 0.3 μOe) are favorably comparable with the most sensitive polymer-based ME sensors. Fur-
Magnetoelectric ther, the correlation coefficient, linearity and accuracy values are 0.995, 95.9% and 99.4% for the DC magnetic field
Magnetic sensor sensor and 0.9998, 99.4% and 99.2% for the AC magnetic field sensor. Therefore, the magnetoelectric materials re-
AC/DC ported in the present study can be used for innovative AC/DC magnetic field sensors.
Linearity © 2015 Elsevier Ltd. All rights reserved.
Sensitivity
Resolution
Accuracy
Hysteresis

1. Introduction highest ME response found in ceramic ME composites, their low electri-

The magnetoelectric (ME) effect is defined as the variation of the electric
polarization in the presence of an applied magnetic field (direct ME effect)
or as the variation of the magnetization in the presence of an applied electric
field (converse ME effect) [1–3]. This effect is present in materials through
different principles: by the coupling of magnetic moments and electric di-
poles in single-phase multiferroic materials [4] or by the elastic coupling be-
tween piezoelectric and magnetostrictive phases in composites [2,5–9].
Nevertheless, single-phase ME materials are not suitable for technological
applications due to their low ME response (≈1–20 mV·cm−1·Oe−1),
which typically appears at low temperatures (≈10 K) [6].
Among composite structures, laminated ME composites, comprising
bonded piezoelectric and magnetostrictive layers, are the ones with the
highest ME response, thus being the most suitable materials for techno-
logical applications [6,10,11]. The piezoelectric element in such com-
posite structures can be ceramic or polymeric [6,12]. Despite the
⁎ Corresponding author.
E-mail address: pmartins@fisica.uminho.pt (P. Martins).
1
Equal contribution.
cal resistivity, high dielectric losses, fragility and fatigue [6,13,14] are the
main drawbacks that impair their widespread applicability [6]. Polymer-
based ME materials do not reveal the aforementioned drawbacks of ce-
ramic composites, emerging as an appropriate solution for applications
due to their high ME coupling, easy fabrication, large scale production
ability, low-temperature processing into a variety of forms and, in some
cases, biocompatibility [6,15]. The ME coefficients found in polymer-
based ME laminates as well as the broad range of the magnetic fields at
which they respond, allow a large range of applications, in particular in
the fields of magnetic sensors and actuators [6,16–18].
Due to the limitations found in some of the conventional magnetic
field sensors, including low operational temperatures and high opera-
tional power [6,19], self-powered polymer-based ME sensors are of in-
creasing interest and applicability [6,20,21]. On the other hand, vital
characteristics of sensors which will determine their applicability,
such as sensitivity, linearity, hysteresis, accuracy and resolution
[22–25], have never been (or just partially addressed) for ME materials
[26–28]. Once, these parameters are properly reported, ME based mag-
netic field sensors will show application potential in compasses, naviga-
tion, location, magnetic anomaly detection and in the medical/biological
field [6,19,29], among others.

http://dx.doi.org/10.1016/j.matdes.2015.12.086
0264-1275/© 2015 Elsevier Ltd. All rights reserved.
 S. Reis et al. / Materials and Design 92 (2016) 906–910
Fig. 1. Right, ME measurement system with coils generating the HDC and HAC magnetic fields. Left, schematic representation of the ME laminated sample (below) and its corresponding
image (above).
Thus, this works focus on the determination of such characteristics
on an optimized polymer-based ME laminate composed of
Fe64Co17Si7B12 (Metglas) and poly(vinylidene fluoride), PVDF.
Such selection is related with the highest sensitivity and lowest
noise of Metglas among all magnetostrictive phases [21,30], as well as
its high magnetic permeability and piezomagnetic coefficient [31].
PVDF is selected as piezoelectric component due to its highest piezo-
electric coefficient among polymers, stability, flexibility, large electrical
resistivity, low dielectric losses and for the possibility of being processed
in different shapes at low processing temperatures [15]. Additionally,
PVDF/Metglas composites exhibit the highest ME response among
polymer-based ME materials, being in this way the best composite for
the present study [6].
2. Methods
Polymer-based ME laminates were produced by gluing two equal
amorphous magnetostrictive ribbons of Metglas with a Devcon 5 min
epoxy (0.7 GPa Young Modulus) to both sides of a commercial poled
β-PVDF film (Measurement Specialties, USA) in a magnetostrictive–pi-
ezoelectric–magnetostrictive(MPM) configuration, following the
optimized conditions presented in previous studies [32–34]. The
magnetostrictive ribbons (30 mm × 2 mm × 25 μm) were magnetized
along the longitudinal direction (magnetostrictive coefficient λ =
25 ppm) and the piezoelectric layer (30 mm × 3 mm × 52 μm) was
poled along the thickness direction (piezoelectric coefficient
d33 = −33 pC·N−1).
The voltage induced in the PVDF layer was measured with a lock-in-
amplifier (Stanford Research SR844).
Fig. 2. Magnetoelectric voltage response (V) as a function of: (a) frequency and (b) DC magnetic field.
907
Samples were measured in a system composed by two Helmholtz
coils (Fig. 1), one generating the DC magnetic field (HDC) in the range
0 to 20 Oe, and another generating the AC magnetic field (HAC) in the
range 0 to 0.2 Oe.
ME measurements were performed by applying simultaneously a
HDC magnetic field ranging from 0 to 20 Oe and a superimposed HAC
field up to 0.2 Oe. The ME voltage response of the laminate was mea-
sured with a SR830 DSP lock-in amplifier.
In order to determine the resonance frequency of the composite, HDC
and HAC values were maintained constant (4.75 Oe and 0.1 Oe, respec-
tively) and the frequency was changed from 20 kHz to 100 kHz.
The DC magnetic field sensor characterization was performed by
keeping constant HAC and frequency at 0.1 Oe and 48 kHz, respectively.
On the other hand, the AC magnetic field sensor characterization was
carried out by keeping constant HDC and frequency at 4.75 Oe and
48 kHz, respectively.
The linearity of the sensor was determined through the correlation
coefficient r2 and by the maximum deviation from the linear fit. The
sensitivity was determined through the ratio between the minimum
voltage variation divided by the DC magnetic field at the minimum volt-
age variation. The resolution of the sensor was obtained by the smallest
variation of the output signal and the accuracy by calculating the largest
deviation of three measurements with increasing magnetic field. Final-
ly, the hysteresis was measured by calculating the largest deviation of
cyclic measurements with increasing and decreasing magnetic fields.
The accuracy was studied by increasing the DC magnetic field from
0.2 Oe–0.7 Oe three times and hysteresis by making three increasing
and decreasing cycles between 0.2 Oe and 0.7 Oe.
Linearity, hysteresis and accuracy of a sensor are typically expressed
as a percentage of the Full-Scale Output (FSO), i.e., the ratio of the
908 S. Reis et al. / Materials and Design 92 (2016) 906–910

Fig. 3. DC magnetic field sensor characterization: (a) linearity, (b) resolution and sensitivity (c) accuracy and (d) hysteresis.

maximum output deviation (Δ) divided by the full-scale output, speci- 3. Results and discussion
fied as a percentage (Eq. (1)) [35–37].
Fig. 2 shows the ME voltage response of the Metglas/PVDF/Metglas
composite.
Δ
%FSO ¼  100% ð1Þ Fig. 2 shows that the highest ME voltage response is obtained at a
FSO
resonance frequency of 48 kHz (Fig. 2(a)). When the laminated
composite operates in the resonance mode, the ME coupling is largely
The full-scale output is 86.7 mV and 200 mV for the DC and AC char- enhanced, generating a ME voltage output nearly two orders of magni-
acterizations at resonance (48 kHz) and 2 mV for the AC characteriza- tude higher than for non-resonant conditions [38]. Further, the ME volt-
tion at non-resonance (95 kHz) frequencies. age increases with increasing applied HDC magnetic field until 4.75 Oe

Fig. 4. AC magnetic field sensor characterization at the resonance frequency (48 kHz): (a) linearity, sensitivity and resolution; (b) accuracy/hysteresis. AC magnetic field sensor charac-
terization at non-resonance frequencies (95 kHz): (c) linearity, sensitivity and resolution; (d) accuracy/hysteresis.
 S. Reis et al. / Materials and Design 92 (2016) 906–910
Table 1
Metglas/poly(vinylidene fluoride)/Metglas magnetic field sensor parameters.
Parameter DC magnetic field sensor
This work Literature
Sensitivitya (mV·Oe−1) 30 ≈10 ref. [26]
Linearity (r2/FSO%) 0.995/ – 0.9998/
95.9
Accuracy (% FSO) 99.4 – 99.2
Resolution (μ Oe) 8 70 ref. [28]
Hysteresis (FSO%) 1.22 – –
a
(minimum voltage variation)/(DC magnetic field at the minimum voltage variation)
when a maximum ME voltage of 100 mV is reached (Fig. 2(b)). A max-
imum ME coefficient (α33 — determined from Eq. (2)) of
190 V·cm−1·Oe−1 is obtained for such DC magnetic field;
ΔV
α 33 ¼ ð2Þ
t  H AC
where ΔV, t and HAC are the induced ME voltage, the thickness of the pi-
ezoelectric PVDF layer and the AC magnetic field, respectively. This be-
havior is related with the increase of the piezomagnetic coefficient until
the optimum DC magnetic field is reached. With further increase of the
DC magnetic field, a decrease of the induced voltage is observed,
resulting from the saturation of the magnetostrictive response [39–41].
Linearity, sensitivity, resolution and accuracy tests were performed
by increasing HDC in order to validate the use of the Metglas/PVDF/
Metglas as a DC magnetic field sensor (Fig. 3). Tests were performed
under a 0.1 Oe AC magnetic field.
The linearity of the response was obtained in the 0–3 Oe DC magnet-
ic field range (Fig. 3(a)). After a magnetic field of 3 Oe, the ME response
starts to reach saturation, which results in a loss of linearity. Resolution
and sensitivity (Fig. 3(b)), accuracy (Fig. 3(c)) and hysteresis (Fig. 3(d))
were determined at low DC magnetic fields (0.2 Oe–0.7 Oe) since for
such small DC magnetic fields, the electromagnetic noise will have
more influence on the data, thus ensuring that the sensor will be tested
in the worst possible conditions for low field signal detection.
From Fig. 3a a correlation coefficient r2 of 0.995 and a linearity value
of 95.9% FSO are obtained.
The accuracy, hysteresis, sensitivity and resolution are 99.4% FSO,
1.2% FSO, 30 mV·Oe−1 and 8 μOe, respectively. The observed ME hyster-
esis (Fig. 3(d)) is related with the magnetic hysteresis of the Metglas
alloy, that is more pronounced in the vicinity of the maximum perme-
ability ≈0.55 Oe [42].
Further, the behavior of the ME composite as AC magnetic field sen-
sor was evaluated and characterized at resonance (Fig. 4(a) and (b))
and non-resonance frequencies (Fig. 4(c) and (d)) with an applied DC
field of 4.7 Oe.
From the linear fit of the data presented in Fig. 4(a) a correlation co-
efficient r2 of 0.9998 and a linearity of 99.4% FSO is obtained for the AC
magnetic field sensor working at the resonance frequency of 48 kHz.
Additionally, the accuracy (Fig. 4(b)), sensitivity and resolution of the
sensor are 97.9% FSO, 992 mV·Oe−1 and 300 NOE, respectively. At the
non-resonance frequency of 95 kHz, r2, linearity, accuracy, sensitivity
and resolution are 0.998, 98.6%, 2.3%, 40 mV·Oe−1, 1 μ Oe, respectively.
Further, both for resonance and non-resonance conditions no hysteresis
is detected (Fig. 4(b) and (d), respectively).
The DC and AC ME sensor parameters are summarized in Table 1.
The sensitivity and resolution values are compared with the high-
sensitivity polymer-based ME materials reported in the literature.
Table 1 shows that the parameter values obtained for the AC/DC
magnetic field sensor reported in this study are favorably comparable
with the best ones reported in the literature in terms of DC sensitivity
and AC accuracy. Further, the full characterization of the sensor main
parameters is provided.
909
AC magnetic field sensor
This work Our work Literature
Resonance Non-resonance
992 40 10 ref. [27]
0.998/ –
99.43 98.6
97.7 –
0.3 1 10 ref. [27]
– –
In this way, the suitability of the developed laminated polymer-
based ME composite for magnetic field sensor applications is demon-
strated [6].
4. Conclusions
A Metglas/poly(vinylidene fluoride)/Metglas ME laminate compos-
ite has been developed in order to validate its use as AC/DC magnetic
field sensors.
Sensitivity and resolution values are 30 mV·Oe−1 and 8 μOe for the
DC magnetic field sensor and 992 mV·Oe−1 and 0.3 μOe for the AC mag-
netic field sensor. Such values are positively comparable with the ones
reported in the most recent and sensitive polymer-based ME sensors.
Additionally, the correlation coefficient, linearity and accuracy
values for the DC (0.995, 95.9% and 99.4%) and AC (0.9998, 99.4% and
99.2%) magnetic field, demonstrating the applicability of polymer-
based ME materials as innovative AC/DC magnetic field sensors, is
reported.
Acknowledgments and funding
The authors thank the FCT – Fundação para a Ciência e Tecnologia –
for the financial support under project PTDC/EEI-SII/5582/2014. P.M.,
V.C., S.R. and M.S. acknowledges support from FCT (SFRH/BPD/96227/
2013, SFRH/BPD/97739/2013, SFRH/BDE/406 51542/2011 and SFRH/
BD/70303/2010 grants respectively). This work was also supported by
Avel-electrónica Lda, Trofa, Portugal.
A. Lasheras wants to thank the Basque Government for FPI grant. The
authors thank the financial support from the Basque Government
Industry Department under Project Actimat, (ELKARTEK Program).
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