Sensor Review

Graphene film development on flexible substrate using a new technique: temperature dependency of gauge
factor for graphene-based strain sensors
SahourSayed, MohammedGamil, AhmedFath El-Bab, KoichiNakamura, ToshiyukiTsuchiya, OsamuTabata, AhmedAbd El-
Moneim,
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gauge factor for graphene-based strain sensors", Sensor Review, Vol. 36 Issue: 2, pp.140-147, https://doi.org/10.1108/
SR-07-2015-0114
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 Graphene film development on flexible
substrate using a new technique: temperature
dependency of gauge factor for
graphene-based strain sensors
Sahour Sayed and Mohammed Gamil
Department of Materials Science and Engineering, Egypt-Japan University of Science and Technology, Alexandria, Egypt
Ahmed Fath El-Bab
Department of Mechanical Engineering, Faculty of Engineering, Assiut University, Assiut, Egypt
Koichi Nakamura
Center for the Promotion of Interdisciplinary Education and Research, Kyoto University, Kyoto, Japan
Toshiyuki Tsuchiya
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Department of Micro Engineering, Kyoto University, Kyoto, Japan

Osamu Tabata
Graduate School of Engineering, Department of Micro Engineering, Kyoto University, Kyoto, Japan, and
Ahmed Abd El-Moneim
Department of Materials Science and Engineering, Egypt-Japan University of Science and Technology, Alexandria, Egypt
Abstract
Purpose – The purpose of this paper is to develop a new simple technique to synthesize graphene film on a flexible polyethylene terephthalate (PET)
substrate and applied as a strain sensor.
Design/methodology/approach – Graphene film was synthesized using laser treatment of graphene oxide (GO) film deposited on PET substrate.
A universal laser system was used to simultaneously reduce and pattern the GO film into laser reduced graphene oxide (LRGO) film.
Findings – The laser treatment synthesizes a multilayer graphene film with overlapped flakes, which shows structure integrity, mechanical flexibility
and electrical conductivity of 1,330 S/m. The developed LRGO/PET film was used to fabricate a high sensitivity strain sensor. The sensitivity and
temperature dependency of its gauge factor (GF) was examined at applied strains up to 0.25 per cent and operating temperatures up to 80°C. The
fabricated sensor shows stable GF of approximately 78 up to 60°C with standard error of the mean not exceeding approximately ⫾ 0.2.
Originality/value – The proposed method offers a new simple and productive technique of fabricating large-scale graphene-based flexible devices at a
low cost.
Keywords Gauge factor, Graphene synthesis, Laser treatment, Strain sensor
Paper type Research paper

1. Introduction sensitive strain gauges such as doped silicon and nano-carbon

materials, e.g. graphene and carbon nanotubes (CNTs), with
Strain detection plays an important role in engineering
their attractive piezoresistive properties (Geim, 2009).
applications. The use of strain gauges is the most common
Nowadays, graphene has attracted a great interest in a wide
way to detect dimensional changes in large structures and
range of applications because of its exceptional electrical and
delicate electronic applications. The sensitivity of strain gauge
mechanical properties as well as high thermal stability. Also its
is determined in terms of its gauge factor (GF), which could
planar structure is an important merit which makes it compatible
be simply defined as the ratio of relative change in electrical
with microfabrication techniques. The unique monocrystalline
resistance to the applied mechanical strain. Different novel
planar structure with covalent carbon/carbon ␴-bonds is
and smart materials with high GF have been used to produce
responsible for fast electron mobility, ultra-high modulus of
elasticity and negligible internal mechanical hysteresis (Bolotin
et al., 2008; Poot and van der Zant, 2008; Wang et al., 2008).
The current issue and full text archive of this journal is available on
Emerald Insight at: www.emeraldinsight.com/0260-2288.htm Many techniques are used to synthesize graphene such as
mechanical exfoliation, chemical vapor deposition (CVD), and

Sensor Review Received 14 July 2015

36/2 (2016) 140 –147 Revised 20 September 2015
© Emerald Group Publishing Limited [ISSN 0260-2288] 26 October 2015
[DOI 10.1108/SR-07-2015-0114] Accepted 27 October 2015

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reduction of chemically exfoliated graphene oxide (GO) using analyzed. Finally, the strain sensing mechanism was discussed
reducing agents like hydrazine, etc. (Chang et al., 2012; Hummers in terms of LRGO film microstructure.
and Offeman, 1958; Li et al., 2009; Stankovich et al., 2007; Yu et al.,
2008a, 2008b; Zhao et al., 2010). 2. Experiment
So far, many researchers have developed graphene-based
strain gauges and reported their GFs. Zheng et al. (2013) stated 2.1 Graphene oxide synthesis
that the GF of mechanically exfoliated graphene on Si/SiO2 Graphite oxide was prepared using the modified Hummer’s
substrate ranges from 10 to 15, depending on its number of method from graphite powder by oxidation with NaNO3, H2SO4
layers, but their production method was time-consuming and and KMnO4 in an ice bath (Hummers and Offeman, 1958; Zhao
produced graphene at low yields. Lee et al. (2010) reported that et al., 2010). A suspension of graphene oxide (GO) sheets was
obtained by sonication of the prepared graphite oxide powder in
the GF of graphene grown by chemical vapor deposition (CVD)
distilled water (5 mg/mL) for 2 h, followed by mild centrifugation
on a copper film deposited on Si/SiO2 substrate is 6.1. On the
at 5,000 rpm for 30 min to remove non-exfoliated materials,
other hand, Fu et al. (2011) measured a GF of 151 for monolayer
leading to a brownish color solution of exfoliated GO sheets with
graphene prepared by CVD and then transferred to
a final concentration of 3.7 mg/mL, as determined from the
polydimethylsiloxane (PDMS) substrate. In a similar research
residual weight of the dried aliquot.
(Gamil et al., 2014a, 2014b), a higher GF of 255 was measured
for monolayer graphene film grown by CVD on a copper foil and
then transferred to Si/SiO2 substrate. Furthermore, many 2.2 Device fabrication
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investigations have been conducted to increase the sensitivity of The graphene-based strain sensor fabrication process consists of
graphene-based strain sensors using various techniques which four main stages as shown in Figures 1(a-d). First (Figure 1(a)),
the GO precursor solution was drop casted at 20°C on the
depend on different structures and mechanisms such as structure
flexible PET square substrate with 10-cm edge length and 100
deformation (Jin et al., 2009; Yu et al., 2008a, 2008b),
overlapped graphene sheets (Hempel et al., 2012; Kim et al.,
2011) and tunneling effect between neighboring graphene Figure 1 Fabrication processes of the flexible LRGO/PET strain sensor
islands (Zhao et al., 2012).
Despite the fact that CVD technique provides monolayer
graphene film with high GF, but the subsequent complicated
transferring and pattering techniques of this film make the
batch fabrication of graphene-based devices not feasible.
Therefore, there is a need for simple fabrication technology
which avoids the use of harsh chemicals, high synthesis
temperature and well suites the batch fabrication of
graphene-based strain sensors.
On the other hand, merging the flexibility with devices has
recently become a great challenge for researchers trying to
develop flexible micro-devices. In this regard, the excellent
flexibility of graphene comes in handy when aiming to produce a (a)
whole new class of state-of-the-art devices for many industrial
Laser beam
applications. As a result, some attempts have been made to
achieve that goal. Strong et al. (2012) used laser source of DVD
drive to reduce graphene oxide deposited on a polyethylene
terephthalate (PET) substrate to fabricate flexible sensors. (b)
Although this process is quite simple, but the produced graphene
Connecting pads
has insufficient quality due to incomplete reduction, as a
consequence of the small laser power of the DVD drive. Also, Gamil
et al. (2014a, 2014b) have recently synthesized a reduced graphene
oxide film on PET substrate using high-power CO2 laser and used
it as a strain sensor. The fabricated sensor showed a GF of 61.5 at (c)
applied strains up to 0.05 per cent at room temperature. Copper wires
In the present study, a universal laser system was utilized to
pattern and reduce a drop-casted GO film on a flexible PET
substrate into laser reduced graphene oxide (LRGO) film. By
utilizing this technique, any special preparations or
adjustments for the samples were avoided, thus allowing the (d)
fabrication of a flexible and sensitive strain sensor with a
simple and low-cost technique. The sensitivity and stability of Notes: (a) Drop-casting of GO solution on
the developed LRGO/PET strain sensor were tested at applied PET substrate; (b) simultaneous reduction
strains up to 0.25 per cent and under operating temperatures and patterning for GO film by Laser beam;
up to 80°C. Furthermore, the effectiveness of laser reduction (c) deposition of silver connecting pads by
technique on the properties of the synthesized graphene was thermal evaporation; (d)wire bonding process

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␮m in thickness (Figure 1(a)). The spreaded GO solution was in a full Wheatstone bridge circuit. These strain gauges were
left to dry for 48 h in air at room temperature. Then in the second glued on the cantilever beam to measure the axial strain at
step (Figure 1(b)), the dried GO film was simultaneously different applied loads. Power screw with 1.25-mm pitch was
reduced and patterned into graphene rectangular strips (5 ⫻ 10 used to apply different loads on a cantilever beam with 1-mm
mm) using a CO2 laser beam, with wavelength of 10.6 ␮m and thickness. The trapezoidal beam was used to have a uniform
diameter of 70 ␮m, generated from a universal laser printing uniaxial stress distribution inside the beam (Chen et al.,
machine (model: Universal Laser Systems VLS2.30) with a focal 2011). Finally, the LRGO/PET sensor was fixed on the top
length of 50 mm. The desired shape was reduced and patterned surface of the cantilever beam at the same distance from the
with a resolution of 1,000 pulses per inch and speed of 25.4 fixed end and the commercial strain gauges to ensure receiving
mm/s. The used laser power for this process was 2 W with an the same axial strain as the strain gauges. The change in the
average reduction time of 30 s. The laser processing parameters electrical resistance because of the different applied strains
were optimized after several experimental trials to give the best was recorded to determine the GF.
results concerning graphene film quality and properties. For The effect of operating temperature on the stability of GF
instance, the higher power damages the GO film and the PET was studied up to 80°C. The test rig was placed inside a
substrate, while lower values only produce a partially reduced furnace, while the connecting wires (terminals) were kept
graphene film with undesired properties. In the third step (Figure outside it, as shown in Figure 2.
1(c)), silver connecting pads were deposited through a stencil
mask onto the LRGO strip ends by thermal evaporation 3. Results and discussion
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(Edwards Auto 306A Vacuum Coating system). Finally (Figure

1(d)), copper wires were bonded to the connecting pads for 3.1 Characterization of LRGO film
electrical resistance measurement. A 3D laser microscope image for the deposited LRGO film on
the PET substrate is presented in Figure 3. The image shows the
formation of a rough, cracks-free film with an average thickness of 3
2.3 Characterization of LRGO film
To assess the efficiency of the reduction process and the ␮m. This reflects that the fast laser treatment of GO film allows
maintaining the structural integrity of the parent GO film.
quality of LRGO film, the thickness, electrical conductivity,
structure and morphology of the deposited GO and LRGO Figures 4(a-c) show SEM images of the LRGO film at
films were characterized using 3D laser scanning microscope various magnifications. The image in Figure 4(a) presents a
(KEYENCE VK-X200), four-probe technique (Pro4, clear transformation of the prepared non-conductive GO film
LUCAS LABS), Fourier transform infrared spectroscopy with dark contrast (lower part) into patterned conductive LRGO
(FTIR) (BRUKER VERTEX 70), X-ray diffraction (XRD) film with bright contrast (upper part). Figures 4(b and c) clearly
(SHIMADZU XRD-6100), Raman spectroscopy (HORIBA illustrate the existence of overlapped flakes structure in the
Jobin Yvon LabRAM HR-800 SSM) and scanning electron LRGO film. The overlapped flakes connect together through
microscopy (SEM) (JEOL JSM-6010 LV). electrostatic forces (Van der Waals forces) to form a
continuous and conductive network (Koenig et al., 2011).
To estimate the efficiency of the laser reduction process,
2.4 Gauge factor measurement
XRD, SEM, FTIR, Raman spectroscopy and conductivity
2.4.1 Test rig preparation.
measurements were conducted. Figure 5 shows the XRD
To measure the GF of the fabricated LRGO/PET device, test
patterns of graphite powder (Curve a), GO (Curve b) and
rig consisting of rigid frame, trapezoidal steel cantilever beam,
LRGO (Curve c) films. Typical intense peak at 26.4° with an
fine pitch power screw and four commercial strain gauges, was
estimated interlayer distance of 3.38 Å is identified for
utilized, as shown in Figure 2. A 350-⍀ four commercial strain
graphite powder, as shown in Figure 5 (curve a). This
gauges with GF of 2.1 were used to represent the resistances
interlayer distance expands to 8.14 Å upon the oxidation of

Figure 2 Schematic representation of the used test rig to estimate

the GF of the LRGO/PET strain sensor Figure 3 Thickness of the LRGO film on PET substrate using 3D
scanning laser microscopy

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Figure 4 SEM images of LRGO film at various magnifications: (a) Figure 5 XRD patterns for graphite (Curve a), GO (Curve b) and
border line between LRGO and dark GO films; (b) overlapped LRGO LRGO (Curve c)
flakes structure; (c) integrated network of multilayer LRGO flakes
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Figure 6 FTIR spectra for graphite (Curve a), GO (Curve b) and

LRGO (Curve c)

FTIR spectrum of GO shows the existence of different

functional groups because of the chemical exfoliation process
of graphite using strong oxidizers by means of modified
Hummer’s method. The (O–H) group absorption causes
broad and intense peak at 3,400 cm⫺1, and the (C⫽O) group
gives another peak at 1,720 cm⫺1. Also stretching vibration
peaks because of various deformations are observed at 1,220
graphite to graphene oxide by the modified Hummer’s and 1,060 cm⫺1 because of (C–OH) and (C–O) groups;
method, as shown in Figure 5 (curve b). By applying the laser respectively. The formation of hydroxyl, carboxylic and alkoxy
beam on the GO film, a characteristic halo peak of amorphous groups can explain the recorded expansion in the typical
carbon is detected at 25.9° with interlayer distance of 3.43 Å, interlayer distance of the starting bulk graphite after oxidizing
as revealed in Figure 5 (curve c). This reduction in interlayer it to GO, as observed in Figure 5. On the other hand, the
distance reflects the successful removal of oxygen functional FTIR spectrum for LRGO indicates that the exposure to the
groups and water molecules from the interlayer spacing of the laser irradiation removes (C⫽O), (C–OH) and (C–O) groups,
GO film upon laser reduction process. while (O–H) stretching vibrations observed at 3,400 cm⫺1 is
Figure 6 shows the FTIR spectra of graphite (Curve a), GO significantly decreased because of deoxygenation and
(Curve b) and LRGO (Curve c). Graphite spectrum shows the carbon-carbon bonding is simultaneously restored. The
absorption band of (O–H) group at 3,400 cm⫺1, while the remnants of hydroxyl groups were reported to be related to
peak located at 1,600 cm⫺1 is attributed to unoxidized water molecules intercalated among graphene layers (Li et al.,
graphitic domains and skeletal vibration of C⫽C bonds. The 2007; Wojtoniszak et al., 2012).

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Figure 7 Raman spectra for GO (Curve a) and LRGO (Curve b) films Table I shows that the laser treatment of the GO film renders
higher values of I(2D)/I(G) and I(G)/I(D) ratios for LRGO
film than those for GO film. Besides, it confirms the
multilayer, disorder and defective nature of LRGO film. In
correlation with the previous facts, the GO film shows a very
low electrical conductivity (9 ⫻ 10⫺2 S/m), while the
application of suitable laser power makes the film electrically
active by increasing its conductivity in five orders of
magnitude to reach 1.33 ⫻ 103 S/m. This likely means that the
removal of oxygen-containing functional groups from the GO
film with the laser reduction process leads to an efficient
recovery of the sp2 network structure, which subsequently
enhances the conductivity among the graphitic domains. On
the other hand, Vallés et al. (2012) reported that the I(2D)/
I(G), I(G)/I(D) and the electrical conductivity values obtained
for hydrazine reduced GO film were 0.183, 1.4 and 1.75 ⫻
102 S/m, respectively. These values are much lower than those
measured for the LRGO film presented in this study, as
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illustrated in Table I. Therefore, the treatment with laser

Figure 7 shows Raman spectra for the synthesized GO (Curve power presents a highly efficient method to improve the
a) and LRGO (Curve b) films. The characterizing peaks of reduction of GO film than chemical treatment, wherein it
GO film are the D-band at 1,345 cm⫺1 and the G-band at leads to a significant removal of oxygen-containing functional
1,600 cm⫺1. For LRGO film, three predominant peaks could groups and efficiently recovers the sp2 network structure.
be noticed in Raman spectrum (Curve b), the 2D-band at Moreover, the laser treatment of GO film allows
2,700 cm⫺1, G-band at 1,580 cm⫺1 and the D-band at 1,350 maintaining the structural integrity and flexibility of the GO
cm⫺1. film, which enables the use of LRGO film as a strain sensor. In
The G-band and the 2D-band are characteristic of the other words, the proposed approach sets the base for an easy,
sp2-hybridized carbon-carbon bonds in graphene (Ferrari et al., fast, cost-effective and environment-friendly fabrication route
2006; Gupta et al., 2006; Mattevi et al., 2009; Ni et al., 2008; for flexible graphene films with great application potential in
Pimenta et al., 2007). The 2D-band is the second-order Raman various fields of technology.
feature of the D-band and originates from a double-resonance
process (Ferrari and Robertson, 2000). The presence of the 3.2 Gauge factor measurement results at different
D-band (at 1,350 cm⫺1) indicates the presence of structural operating temperatures
imperfections or disorder induced by the attachment of oxygen The feasibility of the fabricated LRGO/PET device in strain
functional groups on the carbon basal plane (Mattevi et al., sensing was tested by studying the effect of applied axial
2009). This band usually disappears in highly ordered graphene strains, up to 0.25 per cent, on its electrical resistance at
layers. On the other hand, both I(2D)/I(G) and I(G)/I(D) ratios different operating temperatures up to 80°C, as shown in
are widely used to provide structural information of the GO with Figure 8. Each sequence of measurements was repeated three
different degree of reduction. A higher I(2D)/I(G) ratio, as well as times for three different samples. Under strain-free condition,
increased intensity and decreased width of the 2D-band, is the average electrical resistance of the device slightly decreases
commonly used to indicate the restoration of sp2-hybridized with the increase in temperature, wherein the recorded
carbon-carbon bonds in graphitic structures and the presence of a
fewer number of graphene layers (Chieu et al., 1982). Meanwhile, a Figure 8 Electrical resistance change of the LRGO-based sensor
lower I(G)/I(D) ratio is related to the presence of more disordered with axial strain at temperatures of 20, 40, 60 and 80°C
carbon and/or functionalities attached to the graphene sheets.
Table I summarizes the values of the calculated I(2D)/I(G)
and I(G)/I(D) ratios for GO and LRGO films. To correlate
the effects of the structural changes and the restoration degree
of sp2 carbon network structure on the recovery of the
electrical properties of GO film (obtained upon the laser
reduction process), the electrical conductivities of the GO and
LRGO films were measured using four-probe technique, and
the obtained values are compiled in Table I.

Table I I(2D)/I(G), I(G)/I(D) ratios and electrical conductivity for GO

and LRGO films
Film type I(2D)/I(G) I(G)/I(D) Electrical conductivity (S/m)
GO 0.065 1.02 9 ⫻ 10⫺2
LRGO 0.74 1.54 1.33 ⫻ 103

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resistances were 124.8, 118.2, 112.9 and 108 ⍀ at 20, 40, 60 GF is decreased to 71.1 with standard error of the mean of
and 80°C, respectively. The plots of the resistance vs strain at approximately ⫾1.05 (Figure 9(d)). The reason for this
different operating temperatures up to 60°C show strong instability and inconsistency of the GF measurement at 80°C is
linear trends with very good fits which reflects the structural the softening and properties change of the PET substrate,
integrity and continuity of the graphene film network under wherein the average glass transition temperature of the PET is
the applied mechanical strain during the test. On the other about 70°C and that subsequently affects the adhesion between
hand, a clear deviation from linearity in strain-resistance curve the LRGO film and its PET substrate.
is observed at temperature of 80°C. The measured temperature dependency of the
The GF of the LRGO-based sensor can be calculated from the LRGO-based sensor GF is smaller than that of doped silicon
following equation equation (1), which relates it to the relation strain sensors, wherein doped silicon shows significant
between electrical resistance change and the applied strain: decrease in GF with temperature increase. Although the
temperature dependency of doped silicon GF can be
⌬R/R decreased by heavily doping with concentration of 1020 cm⫺3
GF ⫽ (1)
␧ but on the expense of the GF approximately 65, which is
comparable with that of LRGO-based strain sensor (Kulite
where R is the resistance of strain-free LRGO and ⌬R is the Semiconductor Products, 2004).
change in its electrical resistance owing to an applied strain å.
Based on GF calculations; the relation between the applied axial
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strain and GF at 20 (a), 40 (b), 60 (c) and 80°C (d) are shown 3.3 Strain sensing mechanism
in Figures 9(a-d). Figures 9(a-c) show that the LRGO-based Flexible LRGO-based strain sensor has shown in the present
sensor has a stable GF with an average values of 77.8, 77.74 and investigation a potential application as a highly sensitive strain
77.7 at 20, 40 and 60°C, respectively, with a standard error of the sensor. Therefore, the underlying mechanism should be
mean of approximately ⫾0.2. On contrary, the GF measurement clearly investigated to achieve better sensitivity and stability of
at 80°C shows a large error bars where the average value of the our novel LRGO-based strain sensor in the future.

Figure 9 Relation between GF of LRGO-based sensor and axial strain at 20 (a), 40 (b), 60 (c) and 80°C (d)

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Figure 10 Schematic illustration of resistance change mechanism due to change in contact area between the overlapped flakes

According to the presented SEM results, the developed References

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Pimenta, M., Dresselhaus, G., Dresselhaus, M.S., Corresponding author
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disorder in graphite-based systems by Raman ahmed.abdelmoneim@ejust.edu.eg

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