ASME District F - Early Career Technical Conference Proceedings

ASME District F - Early Career Technical Conference, ASME District F ECTC 2013
November 2 3, 2013 - Birmingham, Alabama USA

STRAIN SENSING PROPERTY OF GLASS MICROBALLOONS/CNF

NANOCOMPOSITE EMBEDDED IN SYNTACTIC FOAM
Ephraim F. Zegeye, Ali Kadkhoda Ghamsari
NextGen Composite CREST Center
Mechanical Engineering Department
Southern University and A & M College
Baton Rouge, LA , USA

ABSTRACT
The strain sensing property of a nanocomposite fabricated
from a free standing structure consisting of glass microballoons
(GMB) and carbon nanofibers (CNF) (GMB-CNF
nanocomposite) has been reported [1]. The strain measurement
was performed by attaching the nanocomposite on the surface
of a tensile specimen. In this study, the GMB-CNF
nanocomposite is embedded in compression test sample
fabricated from syntactic foams to measure internal strain. The
electrical resistance of the nanocomposite when subjected to a
compressive strain is investigated. It is found that the average
change in normalized electrical resistance decreases at lower
strain. After about 6.5 % of strain, a sharp increase in the
average change in normalized resistance is observed. The
possible reasons for these behaviors are explained. Results
provide significant information in the use of the nanocomposite
for determining the onset of microballoons fracture or
indicating the initiation of a crack in syntactic foam structures.
INTRODUCTION
The application of composite materials in aircraft,
spacecraft, marine vessels, and automobile structures has been
increasing in recent years. A structural health monitoring
(SHM) system with the ability to detect and monitor the
changes in the structure of composites used for these
applications is very important in order to improve the reliability
of using composite materials, and to reduce the risks associated
with their failure. SHM basically involves embedding a sensing
element (or a set of sensing elements) into a composite
structure for continuous remote monitoring of damage in the
structure. SHM systems are advantageous over traditional
inspection systems, as they can reduce down-time, eliminate
component tear-down inspections, and potentially prevent
failure during operation [2]. Due to their excellent
piezoresistive properties, carbon nanotubes (CNTs) and carbon
nanofibers (CNFs) may enable a new generation of sensors in
nano or micro scales and can be used to develop novel SHM
systems. Consequently, several studies have been carried out to
investigate the use of CNTs and CNFs for SHM applications [37].

ASME District F - ECTC 2013 Proceedings - Vol. 12

Eyassu Woldesenbet
Mechanical Engineering Department
Louisiana State University
Baton Rouge, LA , USA

In order to fabricate sensors for macro-strain

measurements, the CNTs/CNFs were either stacked to form a
thin film (buckypaper) or dispersed in polymeric materials [712]. In buckypaper and CNT/CNF polymer nanocomposite
sensors, the CNTs/CNFs may have direct physical contact or
may be separated with small gaps so that the electrons tunnel
(hop) across the gaps [13]. Application of load or deformation
on the nanocomposites can increase/decrease the gap between
the conductive fillers. This gap variation affects the electrical
properties of the nanocomposite system. Accordingly,
buckypapers and CNT/CNF polymer nanocomposites have
been investigated for macro-strain measurement and damage
sensing applications [12, 14]. One of the benefits of CNT/CNF
based strain sensors over metallic alloy foil based sensors is
their use as embedded sensors for multidirectional sensing at
multiple locations [15].
Embedded sensors could help in identifying internal
defects and determining the extent and propagation rate of
cracks in the hosting composite. They could also provide
information for maintenance and replacement of the structural
members before catastrophic failure. However, sensing
elements that are embedded and used for SHM systems need to
have closely similar properties with the hosting composite. This
is because embedded sensors may create possible structural
strength degradation of the host material and can be considered
as defects if they have mechanical properties that are different
than the host composite [16].
Recently, the strain sensing properties of a nanocomposite
fabricated from a paper like structure consisting of glass
microballoons (GMBs) and CNFs (GMB-CNF structure) was
investigated [1]. The strain measurement was performed by
attaching the nanocomposite on the surface of tensile
specimens. In order to fabricate the nanocomposite (GMB-CNF
nanocomposite), epoxy was infiltrated into the GMB-CNF
structure. Due to the presence of the glass microballoons in the
GMB-CNF nanocomposite, the nanocomposite has been
reported to have similar properties with syntactic foams, which
are also fabricated by dispersing microballoons in polymeric
matrices [17]. Hence it is anticipated that embedding the GMBCNF nanocomposite in a syntactic foam structure would not
affect the mechanical properties of the hosting structure.

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Therefore, in this paper, the potential use of the nanocomposite

as embedded sensor in syntactic foams was investigated.

order to maintain the wires on the sample surface and isolate

the electrical connections from the crosshead during the test.

EXPERIMENTAL
Fabrication of GMB-CNF nanocomposite sensors
Multilayered GMB-CNF nanocomposite sensors were
fabricated using a vacuum infiltration technique. Four GMBCNF structures were laid-up, one over the other, before the
infiltration process (Fig. 1a and b). A high purity bisphenol A
diglycidylether epoxy resin (D.E.R. 332) and an aliphatic
polyamine hardener (D.E.H. 24), both from DOW Chemical
Company, USA, were mixed at a volume ratio of 87:13.
Sufficient resin system was then poured around the region
represented by the green rectangle in Fig. 1a. After sealing the
vacuum bag, the resin system was infiltrated into the GMBCNF structures by applying a vacuum. The resin system was
sucked along the direction indicated in Fig. 1a. In order to
avoid warping of the nanocomposite, the structures were kept
between Teflon sheet covered plates. The bag was maintained
in vacuum for about 12 hours. The nanocomposites were then
removed from the bag and cured for 12 hours at room
temperature and post cured for 3 hours at 100 oC.
Fabrication of compression test samples
The multilayer sensor was embedded in samples prepared
for compression testing. The test samples fabricated were
syntactic foams containing 50 % by volume of S22 glass
microballoons. The matrix of the samples was composed of the
same epoxy resin system that was used to fabricate the GMBCNF nanocomposites. The dimension of the compression test
samples was 24.83 24.83 12.61 mm. In order to embed the
sensors, 5 mm wide strip of nanocomposite was first placed
across the length, in the middle of a mold prepared from Dow
corning 3120 RTV silicone rubber (Dow Corning Corporation,
USA) (Fig. 2a). A slurry prepared for compression test samples
was then poured into the molds and cured for 24 hours at room
temperature and post-cured for 3 hours at 100 C. The
fabricated sensor-embedded syntactic foam samples are shown
in Fig. 2b. Compression test samples that did not contain
sensors were also fabricated using the same materials and
curing procedure.
Installation of electrical connections to the sensors
The procedures used for making electrical connections to
the embedded sensors are shown in Fig. 3. The exposed edges
of the sensor were first painted with PELCO conductive Silver
187 paste. Single stranded tinned-copper wires (MicroMeasurements, USA) were affixed at conductive silver painted
ends of the sensor. In order to avoid wire pulling during the
test, M-bond 200 (Micro-Measurements, USA) was used to
attach the wires at the locations indicated by the arrows as
shown in Fig. 3a. Conductive sliver paste was then applied on
top of the wire to minimize contact resistance as shown in Fig.
3b. Finally, a plastic tape was wrapped around the sample in

ASME District F - ECTC 2013 Proceedings - Vol. 12

(a)

Sucking
direction

(b)

Figure 1. Vaccum infiltration process; (a) figure showing

how the process was performed, (b) a magnified image of
the rectangular region in part (a).
Testing
Compression tests were conducted on the samples using
QTEST 150 universal testing equipment. The tests were
performed at the crosshead speed of 0.5 mm/min. Mechanical
strain () developed along the thickness of the sample was
measured as the crosshead displacement normalized by the
gauge length (or platen separation) of the test specimen. The
samples that did not contain sensors were tested up to 60 % of
strain. Whereas, samples with the sensors were compressed up
to 15 % of strain while measuring the electrical resistance of
the sensors embedded in the samples. In order to record the
resistance, FLUKE 83 digital millimeter (Fluke Corporation,
USA) was used. Both the resistance and mechanical strain were
captured during the test and the change in resistance (R)
corresponding to the strain was obtained from the video. Fig. 4
shows the test setup and the orientation in which electrical
measurements were performed with respect to the applied strain
direction.

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(a)

electron beam. These white regions are resin dominated thin

layers on the surface that hinder the transport of electrons to the
conductive fillers in the nanocomposite. When these regions
were carefully removed with 600 grit paper, the nanocomposite
was shown to have consistent electrical property. The
resistances of the nanocomposite sensors were measured using
FLUKE 83 digital multimeter. The average no load resistance
of the nanocomposite sensors (Ro) was 10.87 2.29 K.

(b)

Figure 2. (a) Strip of sensors placed in a silicone rubber

mold, (b) sensor-embedded syntactic foam sample.
(a)
(b)

Figure 3. Steps for making electrical connections; (a)

painting silver paste and bonding the wire, (b) applying
silver paste on the wire and wrapping with a plastic tape.

Applied strain
direction

m
Figure 5. SEM micrograph of an edge of a GMB-CNF
nanocomposite.
25
20

Sensor

R/Ro (%)

15

Test
sample

10

Crosshead

5
0

Multimeter

Fixed support
Figure 4. Test setup showing strain direction and the
orientation of sensor in the compression test sample.
RESULTS AND DISCUSSION
Nanocomposite Characterization
A SEM micrograph of an edge of a fractured GMB-CNF
nanocomposite sensor is shown in Fig. 5. The average thickness
of the fabricate nanocomposite was 0.65 0.16 mm. In Fig. 5,
white thin regions (see the arrows in the figure) are observed on
the opposite surfaces of the nanocomposite. Such an artifact on
an SEM image is attributed to a charging effect that appears
when a non-conductive material is scanned by high voltage

ASME District F - ECTC 2013 Proceedings - Vol. 12

-5

10

15

20

Strain (%)

Figure 6. Normalized change in resistance versus strain

plot.
Electromechanical Property and Sensitivity
Fig. 6 presents the average normalized change in resistance
(R/Ro) plot of the embedded sensors with respect to the
applied strain. As it can be observed in figure, the normalized
change in resistance versus strain curve has two distinct
regions. For the strains less than 6.5 %, the average normalized
change in resistance is observed to reduce with strain. This can
be explained by the decrease in the tunnel junction gap width
between the CNFs upon the compressive strain. A decrease in
the tunnel junction gap width between the CNFs reduces the
contact resistance between adjacent CNFs. Consequently, the

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could have a strong potential to be used as embedded sensor for

investigating cracks in a syntactic foam structure. Being
seamlessly integrated with the hosting structural member, it
could provide information for maintenance or replacement of
the structural members before failure. Consequently, the GMBCNF nanocomposite sensors developed in this study could have
significant importance for in-situ health monitoring
applications in syntactic foam structures.

R/Ro (%)

(a)

Strain (%)
0

R/Ro = -0.48 - 0.66

R = 0.909

-1
-2
-3
-4
30

Strain (%)

20
R/Ro (%)

volume resistance of the sensors reduces. After about 7.0 %

strain, the resistance of the embedded sensors is observed to
increase with strain. In Fig. 7, the average normalized change in
resistances for the two regions are plotted separately. The data
can be fitted with straight lines having coefficient of
determination (R2) values greater than 0.90. For the strains less
than 6.5 %, the sensors have a gauge factor of about -0.48. The
gauge factor is negative since the resistance decreases with
applied strain in this region. Negative gauge factor is not
unique to GMB-CNF nanocomposite sensors. Previous works
have also reported negative gauge factors for CNT based
sensors [18]. Commercial semiconductor strain sensors with ntype doping material have also a negative gauge factor [19].
The gauge factor of the sensors embedded in samples for
strains 7.0 15 % is 2.6.
The behavior seen at strain about 6.5 % is credited to the
evolution of damage in the sensor as a result of microballoons
crushing in the sensor. The effect of such damage caused loss of
contact and widening of the adjacent CNFs and significantly
increased the contact resistance after this strain. It is important
to note that both the nanocomposites and the syntactic foam
samples were fabricated using the same type of microballoons.
Hence, application of 6.5 % strain could also fracture
microballoons in the syntactic foam samples. However, from
Fig. 8, yielding of the syntactic foam samples when subjected
to a compressive stress appears at about 12 % of strain. This
yielding is also attributed to the crushing of microballoons in
the syntactic foam sample. It can be noted that strain at which
change in slope of the normalized resistance versus strain plots
of the sensor (6.5 %) is much less than the yield strain of the
hosting syntactic foam sample (12 %). This is because the
electrical resistance changes are more sensitive to
microballoons crushing than the yield stress. In the
nanocomposite sensors, increase in the electrical resistance can
be instigated by the fracture of only few microballoons and
keep increasing as more microballoons are crushed. On the
other hand, in the syntactic foam samples, although
microballoons start crushing at lower strain, yielding may not
be seen until a certain number of microballoons are fractured.
The fact that the electrical resistance of the sensor is sensitive
to the fracture of a few microballoons would be advantageous,
as the embedded sensor could be used to identify structural
defects or cracks prior to failure.
In order to identify cracks or defects prior to failure, series
studies at different external conditions could be done to
investigate the electrical resistance response of the embedded
sensor due to the applied strain. From the study, a relationship
between the applied strain and the generated electrical
resistance could be obtained for structural member with known
microstructural property. Once this is determined, any peculiar
electrical resistance generated in the sensor could be attributed
to cracks or defects in the structural member. The extent and
propagation rate of cracks in the structure could also be
determined based on the measured electrical resistance. Since
the electrical resistance of the GMB-CNF nanocomposite
sensor is sensitive for the fracture of few microballoons, it

(b)

R/Ro = 2.6 - 22.91

R = 0.941

10
0

12

15

18

-10
Figure 7. Normalized change in resistance versus strain
plots with best fitting curves, (a) for 0 6.5 % strain, (b)
for 7.0 15.0 % strain.
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Stress (Mpa)

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