Composites Science and Technology 68 (2008) 3178–3183

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Composites Science and Technology

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

The use of the transient hot-wire technique for measurement of the thermal
conductivity of an epoxy-resin reinforced with glass fibres and/or carbon
multi-walled nanotubes
M.J. Assael a, K.D. Antoniadis a, D. Tzetzis b,*
a
Thermophysical Properties Laboratory, Chemical Engineering Department, Aristotle University, Thessaloniki 54124, Greece
b
Queen Mary College, University of London, Materials Department, London E1 4NS, UK

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

Article history: Carbon nanotubes are considered to be ideal candidates for matrix reinforcement in fibre-reinforced
Received 5 February 2008 composite materials. In order these new multifunctional materials to be used at their optimum potential,
Received in revised form 21 July 2008 precise measurements are completely essential. This article is focused in the accurate measurement of
Accepted 29 July 2008
the enhancement of the thermal conductivity of an epoxy-resin, reinforced initially with plies of plain
Available online 13 August 2008
weave glass fabric then by carbon multi-walled nanotubes (C-MWNT), and finally with both these two
macroscopic and nanoscopic reinforcements at hand. The technique employed was the transient hot-wire
Keywords:
technique, as it was recently modified to be able to measure the thermal conductivity of solids in an abso-
Nano composites
B. Thermal properties
lute way, with an uncertainty of better than 1%. Following validation of the technique, the results
C. Finite element analysis (FEA) revealed that in the case of reinforcing the epoxy with glass fibres, with volume fraction of 28%, the ther-
Transient hot-wire mal conductivity increase was 27% compared to plain epoxy-resin. When reinforced with 2% by weight
C-MWNT the enhancement was 9% and when reinforced with both the C-MWNT and glass fibres the
enhancement was the highest value obtained, being 48%.
Ó 2008 Elsevier Ltd. All rights reserved.

1. Introduction
In recent years there have been an increasing number of
applications requiring more efficient and lightweight thermal
management such as communication satellites, high-density
electronics, and advanced aircraft. The fibre-reinforced compos-
ites are considered as ideal candidates for many of these appli-
cations and knowledge of the mechanical as well as physical
properties, pertinent to these materials, has become a very cru-
cial design input. Despite the fact that there is a plethora of
established standards and/or procedures for the measurement
of the various mechanical properties of composites, the same
does not apply to the measurement of a number of physical
properties, including the effective thermal conductivity. As a re-
sult, the lack of reliable thermo-physical data may hinder the
full utilization of composites. It should be mentioned, that the
thermal conductivities of a fibre-reinforced composites can be
calculated from various theoretical, empirical, as well as numer-
ical methods. However, each of these methods has certain
assumptions applicable for certain specific cases and ranges
[1–6]. Thus, the determination of reliable experimental data for
validation purposes is of paramount importance.
* Corresponding author.
E-mail address: t.dimitris@qmul.ac.uk (D. Tzetzis).
Nowadays the use of nanoparticles for the polymer matrix rein-
forcement becomes a highly desirable procedure in order to en-
hance both the physical and the mechanical properties of the
composite [7]. It should be noted that the numerical and the ana-
lytical methods and assumptions regarding the calculation of the
effective thermal conductivity made for conventional composites
have to be reanalysed in order to be applied for the nanocompos-
ites. Clearly, such analyses also necessitate very accurate and reli-
able experimental data for comparison.
Various techniques have been used in the past in order to
measure experimentally the thermal conductivity of conven-
tional fibre-reinforced materials [8–10]. Nevertheless, no single
technique exists for measuring the thermal conductivity of com-
posites that can provide the basis for establishment of a stan-
dard. The reliability of a specific method depends on various
factors, such as the speed of operation, the required accuracy
and execution under various environmental conditions, and the
size and shape of the available specimen. Therefore, the develop-
ment of new experimental methods to measure this property
accurately for composite materials under different environmental
conditions is highly attractive.
Over the last 5 years the transient hot-wire technique was fur-
ther advanced to allow absolute, very accurate measurements of
the thermal conductivity of solids [11–15]. In addition, the
enhancement of the thermal conductivity of fluids in the presence

0266-3538/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2008.07.019
 M.J. Assael et al. / Composites Science and Technology 68 (2008) 3178–3183
of small amounts of nanoparticles was also recently examined [16].
Thus, it is of interest to use this specific technique for the measure-
ment of the thermal conductivity of a solidified epoxy polymer
along with certain reinforcements. To this respect, in this article
the transient hot-wire technique is employed in the measurement
of the thermal conductivity of conventional glass fibre-reinforced
composites as well nanotube-reinforced composites. It should be
noted that very few reports can be found for the measurement of
the thermal conductivity of glass fibre composites and even fewer
with the transient hot-wire technique [17]. Most importantly the
enhancement of the thermal conductivity of glass fibre composite
laminates in the presence of carbon multi-walled nanotubes
(C-MWNT) has not been considered yet.
In the current study, plain epoxy-resin blocks were initially
measured in order to obtain the thermal conductivity of the matrix
and serve as the control measurements. Then specimens were
manufactured and measured using as reinforcements: (a) glass fi-
bres, (b) carbon multi-walled nanotubes (C-MWNT), and (c) glass
fibres and carbon multi-walled nanotubes (C-MWNT). It is noted
at this point, that the term ‘thermal conductivity’ is referred only
for homogeneous materials. Therefore, when it is used in connec-
tion with a reinforced polymer, the term ‘effective thermal conduc-
tivity’ should strictly be employed. In this article, for simplicity, the
term ‘thermal conductivity’ is used throughout the text.
2. Experimental procedures
2.1. Materials and sample preparation
2.1.1. Epoxy-resin polymer
In order to measure the thermal conductivity of the epoxy-resin
polymer different sets of epoxy-resin blocks were prepared. Each
set consisted of two blocks. The epoxy-resin used was the EPIKOTE
816 LV and the curing agent EpikureTM 207, available from Hexion
Specialty Chemicals, Inc. The mixing ratio was 100/47 by weight,
respectively. The two components of the epoxy-resin were mixed
and the mixture was stirred mechanically. The mixture was poured
into molds with dimensions 10 cm  5 cm and then left to cure at
room temperature for 24 h followed by post-curing for 2 h at 90° C.
After the post-curing process, both sides of the samples were pol-
ished in order to reduce the contact resistance during
measurements.
2.1.2. Glass fibre-reinforced epoxy-resin polymer
For the preparation of the reinforced epoxy-resin samples, an E-
glass plain weave fabric of 0.15 mm thickness available from HEX-
CEL was utilized in this work. The plain weave fabric was chosen
because it is characterized by the simplest repetitive geometry
among all woven fabrics that would not create great measurement
uncertainties. The unit cell of a balanced plain weave consists of
two yarns in both the fill and warp directions.
The laminate was fabricated by the wet lay up method. The
laminate thickness was about 3 mm, and the stacking sequence
was (0°/90°)20. The fibre volume fraction was kept low, approxi-
mately 28%, in order to measure the minimum effect that the fibres
may have on the enhancement of the thermal conductivity. The
laminate was left to cure at room temperature for about 48 h
and then it was post-cured in an oven for 2 h at 90° C. After the
post-curing process nine smaller samples (5 cm  10 cm) were
cut out of the laminate using a diamond tipped rotary saw. It
should be noted that five of the samples had the 0° direction of
fibres in parallel with the longer axis of the sample, while the rest
of them were cut so as to have an angle of 60° with that axis.
2.1.3. C-MWNT-reinforced epoxy-resin polymer
The C-MWNT employed in this work was produced by MER Cor-
poration, USA, by the catalytic decomposition method. The pristine
3179
Fig. 1. Typical scanning electron micrograh of the nanotubes used.
material was examined by Scanning Electron Microscopy (SEM,
JEOL Model JSM–6300, 20 keV). Fig. 1 shows a typical scanning
electron micrograph revealing large agglomeration and entangle-
ment of the nanotubes.
Two different sets of carbon multi-walled nanotubes (C-MWNT)
reinforced epoxy-resin samples were prepared. The first one con-
sisted of epoxy-resin with 2% by weight C-MWNT. The second
set was similar to the first one but containing also glass fabric with
volume fraction of 28%. The C-MWNTs were added in the epoxy/
hardener system and the mixture was stirred mechanically in or-
der to achieve better homogeneity of the samples and to minimize
agglomeration of the nanotubes.
A preliminary study has shown that the volume fraction of the
C-MWNT in the epoxy-resin formulation was limited by the dra-
matic increase in viscosity. It is known that the C-MWNT is typi-
cally held together as bundles with intrinsic van der Waals forces
in most solvents [7]. When mixed with the epoxy-resin the C-
MWNT exist as entangled aggregates, which lead to an increased
viscosity in the C-MWNT/epoxy system. Surfactant-assisted meth-
ods are reported to achieve a good dispersion, but surfactants are
difficult to remove from the composites [18]. Also, some studies
also reported that functionalization could improve the dispersion
[19] but in this study non-functionalized nanotubes were used.
This behaviour of the C-MWNT-reinforced epoxy, having high
viscosity, singled out the choice of the fabrication method to the
wet lay up technique in the second set of samples. Clearly, the
impregnation of the resin in advanced composite fabrication tech-
niques such as the resin transfer molding (RTM) and the vacuum
infusion (VI) processes is a complex process and is greatly influ-
enced by the resin viscosity. Also, in such processes the phenome-
non of filtering the nanotubes has been observed [20]. This is due
to the fabric structure that contains gaps of different scales that
are blocked and lead to a very slow or even insufficient resin
impregnation.
2.2. The transient hot-wire technique
In the transient hot-wire technique the temporal rise of a thin
wire placed in the test material, initially at equilibrium, is observed
following the application of a step voltage across the wire. The wire
acts both as a heat source producing a time-dependent field within
the material, and as a thermometer, registering the temporal resis-
tance change and thus its temperature rise. To eliminate end
effects, two wires differing only in length are employed. In the spe-
cific case of measurements of the thermal conductivity of solid
3180 M.J. Assael et al. / Composites Science and Technology 68 (2008) 3178–3183
samples, in order to minimize contact resistance between the wire
sensor and the solid, the wire sensor is placed inside a flat layer of
soft silicone paste which in turn is squeezed between two blocks of
the solid. Heat is transferred from the wire via the silicone paste to
the solid.
In Fig. 2, the new sensor, composed of two 25-lm-diameter
Ta wires, is shown. The solid material is considered in this case
as the plain epoxy-resin blocks or the composite laminates and
nanocomposites. As details of the sensor and the technique are
given elsewhere [11,15], only a brief description is included here.
The two wires, of 2 cm and 5 cm lengths, are spot-welded on
1 mm Ta support wires which are flattened to 0.5 mm at their
ends. Two 1-mm-thick SS strips on the top and bottom of the
sensor ensure that the samples are kept exactly 1 mm apart,
and hence the paste thickness is also equal to 1 mm. In a spe-
cially made base, two 25-lm-thick polyimide films (Kapton, Du-
Pont) (10 cm  5 cm) are held while a silicon paste (HIGH TEMP
Red silicone, Type 650, VersaChem) is laid over them. The sensor
with the wires is placed on top of one of them, while the other
is placed over it. Then the specially made base is squeezed tight
to 1 mm. After about 1 week, the silicone paste becomes harder
but still retains some elastic properties. This produces an elastic
layer of exactly 1 mm thickness, with Kapton on the outside, and
the silicone paste with the two wires on the inside. Furthermore,
this assembly ensures that the Ta wires are in the middle of the
silicone layer. To measure the thermal conductivity, the sensor is
squeezed between the two pieces of the sample.
The whole arrangement is placed in the center of an accurate,
vertical three-zone tubular furnace (Carbolite, Model TVS 12).
The temperature is determined using two platinum resistance
thermometers embedded on the top and bottom of the half cylin-
der. The thermometers are calibrated versus a Class I certified,
Tinsley platinum resistance thermometer to a maximum uncer-
tainty of less than ±80 mK (all temperatures refer to ITS-90). Preli-
minary measurements with platinum resistance thermometers
placed in the position of the wires, showed a 0.4 K maximum dif-
ference between the top and the bottom of the sensor cylinder
Fig. 2. The new sensor of the transient hot-wire technique.
and a 0.05 K maximum difference radially. These differences have
no significant effect in the final quoted uncertainty of the thermal
conductivity measurement.
During a single run, 1000 temperature versus time points are
registered usually from 20 ls up to 10 s, with a very accurate
bridge that has been described elsewhere [11]. In this technique
in general, there are five unknown parameters:
– the thickness of the paste (which, in the new sensor, is exactly
equal to 1 mm);
– the paste’s thermal conductivity and the (density  specific
heat capacity) product;
– the sample’s thermal conductivity and the (density  specific
heat capacity) product.
The parameters concerning the paste properties are obtained
from measurements at short times (20–0.3 s). Having acquired
those, the parameters related to the sample can be obtained from
measurements at longer times (0.3–10 s).
In order to fully describe the complete geometry of the sensor,
the COMSOL Multiphysics V.3.2b finite element package is em-
ployed. This allows precise modeling of the sensor, i.e. the wire,
the silicone paste, the Kapton film (negligible effect), and the solid,
resulting in perfect agreement between the experimental points
and the calculated temperature versus time curve from 20 ls to
the last time measurement. Hence, full advantage of the whole
temperature versus time curve is obtained.
3. Results and discussion
3.1. Validation of the technique
Validation of the proposed configuration was performed using
the liquid toluene that has been proposed by the Subcommittee
on Transport Properties of the International Union of Pure and
Applied Chemistry as a standard thermal conductivity liquid with
 M.J. Assael et al. / Composites Science and Technology 68 (2008) 3178–3183 3181

Fig. 3. Typical temperature rise as a function of time for toluene at 302 K.

an uncertainty of ±0.6% [21]. Evidently, an advantage of the pro- Taking into account the aforementioned discussion as well as
posed thermal conductivity measurement configuration is that it the uncertainty in the temperature of the furnace discussed previ-
can also be employed to measure the thermal conductivity of flu- ously, the estimated absolute uncertainty of the technique is better
ids. The wires with their support were placed in toluene at 302 K than ±1%. This estimate concurs very well with the measured value
and 1000 points of temperature versus time were obtained. To cal- for the thermal conductivity of toluene (and of Pyroceram 9606
culate the thermal conductivity of toluene, the COMSOL package [15]). Also, the uncertainty in the measurement of the product
was employed, but instead of the properties of the silicone layer, (density  specific heat capacity) is about ±5%.
the Kapton film, and the solid, the properties of liquid toluene were
used. In Fig. 3 the temperature rise versus the logarithm of the time 3.2. Thermal conductivity of plain epoxy-resin blocks
is shown. The thermal conductivity value obtained from the super-
imposition of the COMSOL calculated values and the experimental Following the validation procedure, the wires were placed in
ones, deviates by 0.4% from the proposed value by the Subcommit- the silicone paste, and the sensor, prepared as described in the pre-
tee on Transport Properties of the International Union of Pure and vious section, was placed between two blocks of the epoxy-resin
Applied Chemistry, whereas the product (density  specific heat polymer. Seven different sets of epoxy-resin blocks were prepared
capacity) was found to deviate by ±0.3% from literature values by weighing as described above. The values of the thermal conduc-
[22,23]. tivity of these samples are shown in Fig. 4. These values indicate
It was mentioned in the previous sections that the technique that although the technique is accurate to ±1%, the actual values
employed is an absolute technique. The total uncertainty is associ- measured differ by ±2% because of inhomogeneities in the samples
ated with the uncertainties in the following variables [15]: probably attributed to factors like imperfect mixing or non-identi-
cal composition.
(a) Uncertainty in the voltage supplied to the wires. A digital Fig. 5 shows a typical run at 298.15 K (1000 measurements
voltmeter (HP 34401A) was employed with an uncertainty between 0.01 s and 10 s). The first part of the curve is related to
of ±1 lV. This resulted in an uncertainty in the final thermal the properties of the silicone paste and the second part to the
conductivity value of the order of 106%.
(b) Uncertainty in the temperature coefficient of resistance of
the tantalum wires. This was obtained by measuring accu-
rately the resistance of the wires at known temperatures.
The resistance of the wires was measured with a ±0.01%
uncertainty, while the temperature was recorded by a Class
I (±1 mK) certified Tinsley platinum resistance thermometer.
Hence, the temperature rise was obtained with an uncer-
tainty of better than ±20 mK, which results to an uncertainty
of the final value of the thermal conductivity of less than
±0.05%.
(c) Uncertainty in the real time measurement. Time was
recorded in a 16 bit mode, i.e. with an uncertainty of
±1 ls. However, in the thermal conductivity calculation,
the logarithm of the real time is involved. This results in
an uncertainty in the final thermal conductivity value of
±0.001%. Fig. 4. The thermal conductivity of different sets of epoxy-resin polymer at 307.5 K.
3182 M.J. Assael et al. / Composites Science and Technology 68 (2008) 3178–3183

Fig. 5. Typical temperature rise as a function of time for epoxy-resin polymer at 298.15 K.

properties of the epoxy-resin polymer. The results for the thermal shown in Table 1 and plotted in Fig. 6. In the same figure the pre-
conductivity of the epoxy-resin polymer as a function of tempera- vious measurements of the thermal conductivity of the epoxy-
ture are shown in Table 1 and plotted in Fig. 5. The thermal con- resin are shown for comparison purposes. It can be seen that rein-
ductivity, k (W m1 K1), values shown in Table 1, were fitted as forcing the polymer with the glass fabric resulted approximately in
a function of the absolute temperature T (K) to an equation, a 27% increase in the thermal conductivity. That increase may be a
   result of the relatively good conducting nature of the glass fibres
T
k ¼ kð298:15 KÞ 0:1118 þ 0:880 ; ð1Þ compared to the epoxy-resin matrix. Since the fibre interaction be-
298:15
comes more important as the fibre volume fraction increases, the
where the value of the thermal conductivity, k(298.15 K) thermal conductivity would be expected to increase as the conduc-
(W m1 K1) is given in Table 1. The maximum deviation of the tive effect would become more significant. Regarding the behav-
experimental points presented in Table 1 from the above equation iour of the composite with the temperature, the observed
is 1.07%, and the standard deviation at the 95% confidence level increase in thermal conductivity follows a linear relationship that
is 0.69%. has resulted from the stronger dependence of the epoxy matrix
with the temperature, i.e. a parallel (linear) relationship was ob-
3.3. Thermal conductivity of glass fibre-reinforced epoxy tained between the thermal conductivity and the temperature in
the measurements of the plain epoxy blocks (Fig. 6).
The measurements of the thermal conductivity of the glass The values in Table 1 were obtained by placing the samples
fibre-reinforced epoxy-resin as a function of the temperature are with the glass fibres parallel to the sample axis, thus parallel to
the wires of the sensor. Measurements on samples with the 60°
angle show that the orientation of the fibres had no real effect on
Table 1
the thermal conductivity. It seems that the isotropic nature result-
Measured properties of the composites as a function of temperature ing from the amorphous character of the glass fibres probably nul-
lifies the effect of orientation of the fibres in the composite.
Material T (K) k (W m1 K1) Dka (%)
The thermal conductivity, k (W m1 K1), values shown in Table
Epoxy-resin polymer 298.15 0.252 0.83 1, were fitted as a function of the absolute temperature T (K) to an
307.46 0.255 0.72
equation,
320.32 0.267 0.22
335.84 0.275 1.07
  
T
348.78 0.290 0.84 k ¼ kð298:15 KÞ 0:3784 þ 0:6254 ; ð2Þ
298:15
Epoxy-resin polymer + 298.15 0.320 0.38
glass fabric (0°/90°)20 312.20 0.330 0.20 where the value of the thermal conductivity, k(298.15 K)
320.12 0.338 0.61 (W m1 K1) is given in Table 1. The maximum deviation of the
333.81 0.347 0.54
experimental points presented in Table 1 from the above equation
348.50 0.353 0.57
is 0.61%, and the standard deviation at the 95% confidence level is
Epoxy-resin polymer + C-MWNT + 298.15 0.324
0.29%.
glass fabric (0°/90°)20 (laminate cut 306.93 0.332
at 60° angle from principal axis) 320.27 0.345
3.4. Thermal conductivity of carbon nanotube-reinforced epoxy
Epoxy-resin polymer + C-MWNT 298.15 0.275
Epoxy-resin polymer + C-MWNT + 298.15 0.373
The thermal conductivity of the two sets of samples was mea-
glass fabric (0°/90°)20
sured at room temperature and the results are shown in Table 1
a
Dk = 100  [(k  kfit)/kfit], with kfit from Eqs. (1) and (2). and plotted in Fig. 6, along with all previous measurements for
 M.J. Assael et al. / Composites Science and Technology 68 (2008) 3178–3183
Fig. 6. Thermal conductivity measurements as a function of temperature. (e)
Epoxy-resin polymer, (h) epoxy-resin polymer + glass fibres, (4) epoxy-resin
polymer + glass fibres (samples cut at 60° angle from principal axis), (j) epoxy-
resin polymer + C-MWNT, (N) epoxy-resin polymer + C-MWNT + glass fibres.
comparison purposes. Reinforcing the polymer only with C-MWNT
resulted approximately in a 9% increase in the thermal conductiv-
ity. Similar thermal conductivity values are reported elsewhere
[24], however both the great uncertainties presented and the per-
centage increase reported for each set of measurements make the
results rather questionable. It should be noted though, that the
quality of the nanotubes, the preparation method, and the measur-
ing technique can all affect the measured effective thermal
conductivity.
Reinforcing the epoxy-resin with both C-MWNTs and glass
fibres produced an enhancement of 48%, which is higher from
the simple addition of the 9% of thermal conductivity increase
merely with nanotube reinforcement and the 27% increase in the
case the reinforcement was glass fibres. A study that has investi-
gated nanotube-reinforced glass fibre composites reported that
the C-MWNTs are repelled by the glass fibres [25]. It is possible
that the nanotubes may have created a better conductive pathway
between the plies of the glass fabric thus the observed increase in
thermal conductivity. The conductive pathway has been seen also
to be the prime cause for the thermal conductivity enhancement in
nanofluids [16]. In that case the important parameter was the
length to diameter ratio. Certainly, more work is required in the fu-
ture to identify if such parameter among others is responsible for
the prominent results presented regarding the nanotube-rein-
forced fibre composites.
4. Conclusions
The current work focused in the accurate measurement of the
thermal conductivity of composites and nanocomposites using
the transient hot-wire technique that is capable of measuring ther-
mal conductivity of solid materials in an absolute way, with an
uncertainty of better than 1%. Validation of the technique was
achieved using liquid toluene. Then, in the case of composites
and in particular glass fibre-reinforced laminates, the enhance-
ment in the thermal conductivity was measured as 27% in relation
to the thermal conductivity of the epoxy-resin polymer, which is
satisfactory taking into account the low volume fraction (28%) of
the glass fibres used in the composite. When 2% by weight
C-MWNT were mixed with the epoxy-resin, the enhancement
was 9% while using both glass fibres and C-MWNT the enhance-
3183
ment was 48%. In order to fully exploit the potential of the tran-
sient hot-wire technique and the associated accuracy in the
measurements, experimental quantification of the thermal con-
ductivity of new advanced materials is under schedule considering
the tremendous advances in the topic of nanocomposites.
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