Solar Energy Materials & Solar Cells 94 (2010) 2158–2165

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Solar Energy Materials & Solar Cells

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

Paraffin wax mixtures as phase change materials

T. Kousksou a,n, A. Jamil b, T. El Rhafiki a, Y. Zeraouli a
a
Laboratoire de Thermique Energétique et Procédés, Université de Pau et des Pays de l’Adour (UPPA), Campus Universitaire, 64000 Pau, France
b
École Supérieure de Technologie de Fe s, Université Sidi Mohamed Ibn Abdelah Route d’Imouzzer, BP 2427, France

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

Article history: Melting of the binary mixture system of tetradecane and hexadecane in Differential Scanning
Received 11 May 2010 Calorimetry (DSC) cell has been investigated experimentally and numerically. Different concentrations
Accepted 12 July 2010 of tetradecane–hexadecane paraffin mixture were studied. It is found that the phase change process of
Available online 29 July 2010
the binary mixture takes place over a temperature range and the temperature range depends on both
Keywords: the heating rate and the mixture composition. The proposed study shows also that for the same
PCM concentration of tetradecane and using various heating rates, we will be able to predict the solidus and
Binary mixture liquidus temperature of the binary mixture from DSC curves.
Modeling & 2010 Elsevier B.V. All rights reserved.
Liquid–solid phase diagram
DSC

1. Introduction widely used as the PCM thermal storage because of such

The storage of energy in suitable forms, which can conven-
tionally be converted into the required form, is a present day
challenge to the technologists. Energy storage not only reduces
the mismatch between supply and demand, but also improves the
performance and reliability of energy systems and plays an
important role in conserving the energy [1–3]. It also leads to
saving of premium fuels and makes the system more cost
effective by reducing the wastage of energy and capital cost.
There are various thermal energy storage methods, but latent heat
storage is the most attractive one, due to high storage density and
small temperature variation from storage to retrieval. In a latent
heat storage system, energy is stored by phase change, solid–
solid, liquid–solid or gas–liquid of the storage medium [4]. In
terms of capacity, it also presents the advantage to cumulate the
sensible heat corresponding to the temperature difference
between charge and discharge steps. Different phase transition
for the charge/discharge process can be considered. In practice,
solid–liquid phase change is preferred because of simultaneous
weak volume variation and important enthalpy. Solid–liquid
phase change materials (PCMs) are often used for latent heat
storage applications [5–6]. Not all phase change materials (PCMs)
can be used in building or drying. The choice of the most
appropriate PCM is based on a number of factors including low
cost, high latent and sensible heat, high thermal conductivity in
both liquid and solid phases, high specific heat capacity, suitable
phase change temperature and no supercooling [4]. Water is
n
Corresponding author.
E-mail address: Tarik.kousksou@univ-pau.fr (T. Kousksou).
advantages as high latent heat of melting, stability, low cost and
easy acquisition, no environmental pollution concern and com-
patibility with the material of air-conditioning equipment.
However, there are a few disadvantages with the use of water
as PCM. One of the most serious problems is the supercooling
phenomenon that occurs in the process of solidifying water
during charging of the cold storage.
PCMs that are used as storage media in latent storage systems
can be classified into two major categories: inorganic and organic
compounds. Inorganic PCMs include salt hydrates, salts, metals
and alloys, whereas organic PCMs are comprised of paraffin, fatty
acids/esters. Paraffin wax is taken as the most promising PCM,
because it has large latent heat and proper thermal characteristics
such as little or no supercooling, varied phase change tempera-
ture, low vapor pressure in the melt, good thermal and chemical
stability and self nucleating behavior [7–11]. For these properties
of the paraffins, system-using paraffins usually have very long
freeze–melt cycle. Paraffin wax consists of a mixture of mostly
straight chain n-alkanes CH3–(CH2)–CH3. Both the melting point
and latent heat of fusion increase with chain length. Paraffin
qualifies as heat of fusion storage materials, due to their
availability in a large temperature range.
If PCMs are to be used for comfort cooling, they should have a
melting temperature of approximately 5–10 1C [12]. Paraffin
waxes with a phase-transition temperature near this range are
hexadecane, pentadecane and tetradecane [4]. Because pentade-
cane costs twice as much as hexadecane or tetradecane, it was
not considered as candidate. Table 1 lists thermal properties of
these paraffins. The melting point of alkane increases with the
increasing number of carbon atoms. Apart some favorable
characteristics of paraffin, such as congruent melting and good

0927-0248/$ - see front matter & 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.solmat.2010.07.005
 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165
Nomenclature
c specific heat capacity, J kg  1 K  1
DA area, (m2)
f liquid fraction
h1,2 heat transfer coefficient, (W m  2 K  1)
LF latent heat of fusion, (J kg  1)
M sample mass, (kg)
t time, (s)
T temperature, (K)
To initial temperature, (K)
R cell radius, (m)
Z cell height, (m)
x concentration
xo initial concentration
nucleating properties, they also show some undesirable
properties such as: (i) low thermal conductivity, (ii) non-
compatibility with the plastic container and (iii) moderate
flammability. All these undesirable effects can be partly
eliminated by slightly modifying the wax and the storage unit.
However, paraffin waxes exhibit low conductivity, which
decreases the overall power of the thermal storage device [13].
Great efforts have been attempted to improve the thermal
conductivity of the paraffin wax [14–16]. Metal foams,
additives, fins and carbon materials were used by researchers to
enhance the thermal conductivities [8].
The properties and characteristic of normal alkanes, and the
isobaric T–x phase diagrams of various alkane mixtures have been
discussed by Mazee [17], Mnyukh [18] and Turner [19]. They
describe different system possibilities. The simplest binary system
exhibits a single liquid phase and two completely immiscible
components in the solid state. These three phases (i.e. the liquid,
pure solid I and pure solid II) will be in equilibrium at the eutectic
point. The next simplest binary mixture is the isomorphous (solid
solution) type, in which the two components are completely
miscible in both the liquid and the solid phases. Other binary
systems are those which present a minimum and/or maximum
(i.e. an azeotrope), a fact pointing to a less ideal behavior of the
components. Many researches have been conducted to study the
thermal performance of Paraffin as PCM in storage systems and
numerous publications have been found [20–23]. In these studies,
most of the PCMs are binary or ternary mixtures of paraffin
waxes, and they have been considered to have a constant phase
change temperature during phase change process. For example,
Cho and Choi [24] have reported the thermal characteristics of
paraffin in a spherical capsule during the phase change process.
Experiments were performed with a mixture of tetradecane (40%)
and hexadecane (60%), and the melting temperature was
Table 1
Thermal properties of tetradecane and hexadecane [4].
Melting point (1C) Heat of fusion (kJ/kg)
Tetradecane
5.8 227
Hexadecane
18.1 236
2159
Greek symbols
b heating rate, (K min  1)
l thermal conductivity, W m  1 K  1
r density, kg m3
F specific heat flow rate, (W kg  1)
Subscripts
l liquid phase
o initial
s solid phase
supposed to be at 6.8 1C, with corresponding heat of fusion of
121 kJ/kg. The determination of the heat of fusion and the melting
point of some paraffin wax mixtures was described by Choi et al.
[25]. In that paper, the authors used the Differential Scanning
Calorimetry (DSC) method only to obtain the melting points and
the latent of fusion of the mixtures. The Choi et al. [25] paper
stresses the use of DSC results in calculating the melting
temperature depression constant of the mixture’s main compo-
nent rather than in practical applications. However, they did not
discuss DSC extensively and give the heating rate in DSC
measurement, which is a very important parameter for the result
of DSC. He et al. [26], n-paraffin waxes with a phase-transition
temperature suitable for comfort cooling have been defined as
hexadecane, tetradecane and their mixtures. Their experimental
results indicated that these mixtures are excellent PCM candi-
dates for cool storage. The phase diagram of these mixtures was
studied theoretically as well as experimentally by the same
authors [27]. This diagram was then used to investigate
the interrelationship involved in the phase change process [27].
In He et al. [27] paper, DSC was run at different ramp and results
indicate that these mixtures melt and freeze over a temperature
range and the temperature range depends on the DSC ramp, and
in a short mixture concentration interval appears a low tempera-
ture solid–solid peak.
The purpose of this paper is to report results of an
experimental and numerical study on melting of a binary mixture.
A concentrated solution of hexadecane and tetradecane is used as
binary mixture. Differential Scanning Calorimetry (DSC) has been
used to study experimentally the phase transformation of the
binary system. Two-dimensional model has been proposed and
model predictions are compared with measured experimental
data. Some conclusions are drawn based on the observed
experimental and numerical results.
Specific heat State at room Temperature
Range (1C) Cp (kJ/kg 1C)
 20 to 0 1.68 Solid
+ 25 2.18 Liquid
42–65 2.22 Liquid
+ 20–0 1.75 Solid
+ 28 2.22 Liquid
48–75 2.13 Liquid
2160 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165
2. Liquid–solid phase diagram for binary mixture system of
C14H30 and C16H34
Fig. 1 is the temperature–composition phase diagram for the
binary system of tetradecane–hexadecane. The upper curve is the
liquidus or freezing points curve as obtained by [27]. The lower
curve is the solidus or melting points curve, obtained by the
calculation UNIFAC method. Any system represented by a point
above the liquidus is completely at the liquid state, and any point
below the solidus is completely at the solid state. A point within
the area enclosed by the liquidus and solidus curves indicates an
equilibrium mixture of liquid and solid solutions. These two
curves approach and touch at point M.
3. Experiments
Different ratios of hexadecane and tetradecane were prepared.
Each mixture was stirred well in a breaker with a magnetic stirrer
and was transformed in a test tube.
The thermal behavior of the mixtures was studied using PYRIS
DIAMOND DSC of Perkin-Elmer. The temperature scale of the
Fig. 1. The liquid–solid phase diagram of binary mixture system of C14H30 and
C16H34 [7].
Fig. 2. Experiment DSC cell and scheme for model.
instrument was carefully calibrated by the melting point of pure
ice (273.15 K or 0 1C) and mercury (234.32 K or 38.82 1C). The
principle of the power-compensation is widely detailed in Refs.
[28–29]. We have already presented the experimental cell in Ref.
[29], which consists of a cylindrical cell of height Zo ¼1.1 mm and
radius R¼2.215 mm (see Fig. 2).
The DSC experiments were conducted by placing approxi-
mately 6–1 mg of each binary mixture in a standard aluminum
DSC sample pan. The resolution of the balance is about
70.001 mg. A sample encapsulating press was used to seal
samples in these pans. An empty hermetic pan was used as a
reference in all measurements. The DSC was calibrated for
temperature and heat flow values using the melting point and
enthalpy of fusion of high purity indium according to the standard
procedures described in the user’s manual.
Different thermal treatment steps were employed for each
sample in the present study. At first, each sample was put in
equilibrium at 30 1C, and modulated 70.51 C every 60 s, keeping
it isothermal for 5 min. Then the sample was cooled at a rate
5 1C/min to  20 1C, after which it was kept isothermal for 5 min,
and then heated again to 30 1C at the same rate. The same
procedures were repeated at different rates.
4. Physical model
Motivated by experimental observations of the melting
process, a two-dimensional melting model has been proposed.
The model allows for diffusion as the only energy transport
mechanism in the system. Based on the fact that the Lewis
number (defined as the ratio of thermal diffusivity to mass
diffusivity) for typical binary mixtures is of order 100 [30], it was
concluded that diffusion of heat occurs much more rapidly than
diffusion of species. Consequently, the model proposed neglects
diffusion of species in both the solid and the liquid phases,
assuming that an average concentration remain uniform at the
initial concentration of xo tetradecane everywhere in the system.
Additionally, it is proposed that the melting is an equilibrium
process, and hence the local liquid fraction and local temperature
are coupled by the phase diagram.
4.1. Governing equations
Based on the above assumptions, the equation governing
energy transport in the cylindrical DSC cell (see Fig. 2) is
@T @f @T
rc ¼ r:ðl rTÞ þ rl LF l ð1Þ
@t @T @t
 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165 2161

where r, c and l are the density, specific heat capacity and the the fluxes across the faces of the control volume with the
heat conductivity of the sample, respectively. transient storage and latent heat source terms. The energy Eq. (1)
Constant but different thermophysical properties for each was solved quasi-implicitly, the whole field being determined
phase have been assumed. The last term on the right-hand side of simultaneously. The solution scheme is termed quasi-implicit
Eq. (1) accounts for the absorption of latent heat due to the because temperature information from previous time step is used
melting process. in calculating the latent heat term. This avoids the iterative
Due to the higher thermal conductivity of the cell metal, it is procedure that would normally be required. The solidus and
assumed that the envelope of the sample is at the plate liquidus lines were prescribed by fitting the data [27] to
temperature. polynomials.
At t ¼0, the temperature of the sample is known. A slip
boundary condition is imposed on the symmetry axis
 
@T 6. Results and discussion
¼0 ð2Þ
@r r ¼ 0
Thermal analyses were carried out using a PYRIS DIAMOND
To take into account the air between the sample and the cover
DSC of Perkin-Elmer. For the numerical calculation, we have
of the cell, we consider two different heat exchange coefficients:
h1 the heat transfer between the sample and the air at the top of
the cell and h2 the heat transfer between the sample and both
lateral and the bottom surface areas of the cell.
 
@T
l ¼ h1 ðTz ¼ Z Tplt Þ ð3Þ
@z z ¼ Z
 
@T
l ¼ h2 ðTr ¼ R Tplt Þ ð4Þ
@r r ¼ R
 
@T
l ¼ h2 ðTz ¼ 0 Tplt Þ ð5Þ
@z z ¼ 0
The coefficients of heat exchange (h1 and h2) have determined
by simulation from exploratory experiments.where Tplt, the
temperature of plates, is programmed to be a linear function
Tplt ¼ b t þ T0 ð6Þ
Assuming the high conductivity of the metallic cell, we
consider that the specific heat flow rate F, which attains the
plate, is the sum of the thermal fluxes through their walls.
1X
F¼ h ðT T Þ DAi ð7Þ
m i i i plt

Since the liquid fraction and temperature are assumed to be

dependent through the phase diagram of the mixture, the term Fig. 3. Numerical and experimental thermogram.
relating the change in liquid fraction with temperature may be
treated as follows. From the lever rule, the liquid fraction is given
by
x0 xs
fl ¼ ð8Þ
xl xs
where the liquid and solid concentrations, xl and xs, are both
functions of temperature. If the liquidus and solidus lines are
represented by polynomials as
X
N X
M
xl ¼ ai T i1 ; xs ¼ bi T i1 ð9Þ
i¼1 i¼1

Then the liquid fraction change with temperature @fl =@T may
be easily determined from a differentiation of the lever rule,
Eq. (8), with the substitution of the appropriate polynomial
representation of xl and xs, Eq. (9).

5. Numerical method

It is unlikely that the governing partial differential equation of

energy transport, Eq. (1), with associated boundary conditions
and material-dependent solidus and liquidus curves specifications
is amenable to an exact solution. Recourse was therefore taken to
numerical methods. The energy equation was integrated over a
small DSC cell. A set of algebraic equations result from balancing Fig. 4. Binary mixture temperature versus cell radius.
2162 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165

applied the procedure described in the previous section. The

values of physical characteristics required in the different
equations have been taken in the literature [4].
A comparison between the experimental thermogram and the
calculated one is shown in Fig. 3. The fit between both
thermograms is good: the rounded form of the top of the peak
is reproduced and its width is the same. The observed one-peak
thermogram is a clear indication of the progressive melting of the
binary mixture solution.
Fig. 4 presents the temperatures at different points in the
sample versus the plate temperature Tplt. Temperature differences
can be observed as a function of the sample radius. These
differences can reach 2 1C at certain points. We note that the
temperature differences inside the sample are due to the heat
conduction within the binary mixture.
Fig. 5 presents the numerical thermogram and the calculated
liquid fraction inside the DSC cell versus the plate temperature.
Tpeak represents the value of the plate temperature when the
energy exchange between the DSC plate and the sample is
maximum. We show that the maximum of the peak at Tpeak does
not correspond to the end of the phase change process inside the
DSC cell. Fig. 6. Effect of heating rate on the thermogram shape.

6.1. Effects of heating rate on the shape of thermograms

Fig. 6 shows the thermal plots obtained by the physical model

versus the plate temperature for different heating rates b.
The peak temperatures range becomes broader and it shifts to
greater temperatures with increasing heating rate. Fig. 7 presents
the effect of the heating rate on the sample temperature at the
centre of the DSC cell. We note that the temperature gradient
inside the sample becomes important as the heating rate
increases. The temperature gradient is obviously due to the
overall thermal resistance (both between the sample and the DSC
plate forms and inside the sample) and is enlarged when the
heating rate b increases. Because of the lack of thermal
equilibrium within the sample, DSC measurements at a higher
scanning rate will fail to provide correct information. DSC gives
better results at very low scanning rate.

Fig. 7. Influence of the heating rate on the binary mixture temperature at the
centre of the sample.

6.2. Effects of the initial concentration, xo, of tetradecane on the

shape of thermograms

Hammami and Mehrotra [31] and Paunovic and Mehrota [32]

Fig. 5. Specific heat flow rate and liquid fraction inside the DSC cell versus Tplt.
reported that in a binary mixture system of alkanes, the DSC curve
of the binary mixture system of C14H30 and C16H34 is independent
of the mixture composition and appears at a constant tempera-
ture. However, the results obtained by He et al. [27] indicated
that the binary mixture melts and freezes over a temperature
range and the temperature range depends on both the
composition mixture and heating rate. He et al. [27] observed
that over the C14H30 mole fraction range 21.98–36.03%, DSC
 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165 2163

Fig. 8. Influence of the initial concentration of tetradecane xo on the DSC curve.

curves show the existence of two peaks. The lower temperature

peak is very weak and could possibly be due to the fact that
perfect miscibility does not occur. In order to prove that the
binary system of C14H30 and C16H34 is a solid-solution system and
not a eutectic system, four binary mixtures (5%, 10%, 20% and 30%)
have been tested (see Fig. 8). All components exhibited one peak
corresponding to liquid–solid phase transition. We note that an
increase in the mole fraction brings about a decrease in the peak
height and the movement of the peak to lower temperature
direction. The results confirmed that phase change process of
the binary mixture takes place over a temperature range and the
temperature range depends on the composition mixture (see
Fig. 9).

6.3. Liquid–solid equilibrium temperature of tetradecane and

hexadecane binary mixtures

Before melting kinetics of the binary system of C14H30 and

C16H34 is studied, it is interesting to find the relation between the
DSC curve and the liquid–solid phase diagram of the binary Fig. 9. Influence of the initial concentration, xo, on the temperature at the centre
mixture. Knowing the initial concentration, xo, in the binary of the sample.
2164 T. Kousksou et al. / Solar Energy Materials & Solar Cells 94 (2010) 2158–2165
Fig. 10. Determination of the solidus and liquidus temperatures for various
concentrations xo.
system before the phase change process, makes it possible to
determine, by means of the DSC thermograms, their solidus and
liquidus temperatures.
From Fig. 10, it is found that for different heating rates, the
instant of the beginning point of the progressive melting within
the sample coincides with the real solidus temperature, Ts, of the
mixture. This result is evident because the beginning points of
the melting process correspond to the solidus temperature of the
binary mixture. We also note that all points whose abscissa is
Tpeak form a straight line, which cuts the axis of abscissas to the
liquidus temperature of the binary mixture. These results are
natural because the more the heating rate decreases and becomes
near to zero, the more the gradients of temperature within the
sample become negligible [28]. In the case of the smaller heating
rates, the end point of the phase transformation corresponds
practically to the maximum peak. So the peak temperature given
on the axis of abscissa indicates the limit of the thermograms
when b ¼0 and it coincides with the liquidus temperature Tl of the
binary mixture. These results reveal that for the same
concentration, xo, and using various heating rates, we will be
able to predict the solidus and liquidus temperature of the binary
mixture from DSC curves.
7. Conclusion
In this study, we have presented a two-dimensional model
simulating a non-isothermal melting of the binary mixture
solution (tetradecane–hexadecane). The good agreement between
experimental and calculated thermograms has permitted a
validation of the model and deduces some inaccessible values,
such as the distribution of the temperature and the evolution of
the liquid fraction versus the plate temperature. The proposed
study reveals that for the same concentration, xo, and using
various heating rates, we will be able to predict the solidus and
liquidus temperatures of the binary mixture from DSC curves
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