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Copyright 2013 American Scientic Publishers
All rights reserved
Printed in the United States of America
Journal of
Colloid Science and Biotechnology
Vol. 2, 18, 2013
Investigation of Phase Change Material
Encapsulation by Complex Coacervation
Lucas Fagundes Veiga Ribeiro
1
, Vanessa Martins Silva
2
, and
Ana Silvia Prata Soares
1
1
School of Applied Sciences, University of Campinas, UNICAMP, Limeira, So Paulo, Brazil
2
Faculty of Food Engineering, University of Campinas, UNICAMP, Campinas, So Paulo, Brazil
Two potential phase change materials (PCMs) were microencapsulated by complex coacerva-
tion with gelatin-gum arabic and the characteristics of these microparticles were investigated.
Methyl-palmitate and parafn wax were used as core material, since they provide two different melt-
ing points (around to 30

C and 50

C, respectively). The protective barrier provided by microencap-
sulation prevents the material from sticking on and spreading out the surrounding material during
the phase change. These systems can be applied in solar systems or building materials and tex-
tiles, for heat storage and release. Some operational variables were investigated to select suitable
production conditions for parafn wax: temperature, surfactant addition, time of addition and amount
of core material. The encapsulation ratio (ER%) of these systems was indirectly determined by dif-
ferential scanning calorimetry (DSC). As results, an increased core to coating ratio from 50 to 75%
and the ER raised from 25% to 50%. The parafn inuenced the complexation of the polymers and
with the largest amount of this hydrocarbon, about 39% of the polymer was not complexed. The
use of methyl palmitate did not have this inuence on the coacervation process. Energy storage
capacities of 58.49 J g
1
and 107 J g
1
were observed, respectively, for parafn wax and methyl
palmitate systems, indicating the potentiality of both for use as energy storage systems. The melt-
ing point of microcapsules produced with parafn was 46

C, and with methyl palmitate was 28

C,
both near of the melting point of the pure compounds. The average particle size of the parafn and
methyl palmitate microcapsules obtained was 69.43 m and 111.55 m, respectively.
Keywords: Microencapsulation, Complex Coacervation, Parafn Wax, Phase Change Material,
Methyl Palmitate.
1. INTRODUCTION
Phase change materials (PCMs) are materials that have a
high latent heat of fusion, i.e., they absorb or release large
quantities of energy per mass when they undergo a change
in physical state. Moreover, this change takes place at a
clearly dened temperature of fusion.
1, 2
These materials
are frequently exploited in a variety of industrial appli-
cations, including the control of thermal comfort in con-
struction, electronic components and textile industries, as
well as for the storage of heat energy for later use, such
as is necessary in solar heating systems.
3
One of the prob-
lems with their use is the expansion undergone during the
phase transition process. Moreover, liquids do not maintain
their shape, but spread out and stick to the surrounding
material. Even after subsequent solidication, their future
performance will no longer be as efcient.

Author to whom correspondence should be addressed.

One way of dealing with this problem is the conne-
ment of these materials via microencapsulation. This pro-
cess, either chemical or physical, involves the coating or
embedding of solid or liquid particles in a matrix or wall
material, thus producing small capsules with characteristic
properties of protection and release of the core material.
These capsules not only conne the core material during
expansion and contraction, but also provide a controlled
increase in the surface area of the PCM.
Various studies have been conducted using tradi-
tional techniques to encapsulate PCMs, especially in situ
polymerization and interfacial polycondensation;
49
some
work has been done with spray-drying
10
and complex
coacervation.
1113
Complex coacervation consists of the formation of an
emulsion between a fatty core material with a polymer,
which temporarily stabilizes it in droplets; another poly-
mer is then added to complex with the initial polymer,
enclosing the core material in insoluble capsules. This
J. Colloid Sci. Biotechnol. 2013, Vol. 2, No. 2 2164-9634/2013/2/001/008 doi:10.1166/jcsb.2013.1047 1
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Investigation of Phase Change Material Encapsulation by Complex Coacervation Ribeiro et al.
process is especially efcient in the production of capsules
with a high load of PCM.
Most PCMs are organic materials, thus avoiding some
of the problems inherent in inorganic materials, such as
supercooling and segregation.
14
They are non-corrosive
and chemically stable, with high latent heat per unit of
weight and low vapor pressure. Parafn waxes, derived
from a petroleum source, and fatty acids esters from
renewable vegetable oils or animal fats have similar prop-
erties for PCM applications. Both have suitable melting
temperature range for various heat storage applications,
and they can absorb and release a large amount of heat
repeatedly during phase conversions between solid and liq-
uid phases.
15
Target melting points will depend upon the applica-
tion. The most commonly studied is parafns, which have
phase transition values ranging from 2836

C, the tem-
perature of a comfortable environment. However, different
fusion temperatures could lead to the development of other
applications.
The present study thus investigated the microencapsula-
tion of two PCMs by complex coacervation: a commercial
parafn wax with melting point of 50

C and a fatty acid
ester, with melting point of 30

C.
2. EXPERIMENTAL DETAILS
2.1. Materials
The wall materials used were gelatin from porcine skin
(type B, gel strength bloom 244, lot LFP5136) purchased
from NP Comrcio de Produtos Alimentcios Ltda (Granja
Viana, Brazil) and gum Arabic supplied by Colloids
Naturels International (IRX49345, So Paulo, Brazil). The
core materials used were Parafn wax (Solven wax 120
from Solven Solventes e qumicos Ltda, Hortolndia,
Brazil) and methyl palmitate (MapricProdutos Farma-
cuticos e Cosmticos, So Paulo, Brazil) were used and
their characteristics are described in Table I. Polysorbate
80 was used as a surfactant (Mapric, Brazil). The solvents
and other reagents were analytical grade, and deionized
water was used in all experiments.
2.2. Preparation of Microparticles
Microparticles were produced using gum Arabic and
gelatin, according to the methodology of Lamprecht,
Table I. Properties of commercial PCMs investigated (manufacturers
specication).
Molecular AH fusion Melting
PCM weight (g/mol) (J g
1
) point (

C)
Methyl palmitate 270.46 196 28
Parafn wax 324 210 4548
Schafer and Lehr.
16
The procedure includes the following
steps:
(a) Emulsication of 2.5 g of core material in 100 mL of
gelatin solution (2.5%, wt./wt.) at a relevant temperature
using a homogenizer (Turrax, T-18 basic, IKA, Staufen,
Germany) at 14,000 rpm for 1 min.
(b) Incorporation into 100 mL of gum Arabic solution
(2.5%, wt./wt.) at the same temperature as the gelatin solu-
tion, with 400 mL of deionized water added.
(c) Reduction of pH to coacervation pH (pH 4.0) using
HCl 0.5 or 5N).
(d) Cooling to 10

C. No chemical crosslinking was
promoted.
The coacervated phase was separated after 12 hours in the
refrigerator at 4

C. The moisture content of the micropar-
ticles was determined gravimetrically, in triplicate. The
particles were then dried in a vacuum at a temperature
below the melting point until a constant weight.
The yield was calculated as the ratio between the solid
content of the coacervated phase and the total solid mate-
rial used, as follows:
%PY =
(M
m
%TS)
(M

+M
oc
)
(1)
where M
m
is the moist mass of coacervated phase (g),
%TS, the total solid content of this phase, M
P
, the total
dry mass of polymer used in the process (g) and M
oc
, the
mass of the active compound (g).
The uncoacervated mass (M
puc
), which indicates the ef-
ciency of complexation of polymers, is the mass of free
polymer in solution. This parameter can be calculated as
follows:
M
puc
=M

M
ac
M

+M
ac

%EEM
c

M
c
(2)
where M
puc
is the mass of uncoacervate polymer (g), %EE
the percent of encapsulation efciency and M
c
, the total
dry mass of the coacervate formed (g).
The morphology of the moist microparticles was eval-
uated with an optical microscope (NIKON, Eclipse E800,
Tokyo, Japan) equipped with image analysis software
(Image Pro Plus 4.0), with magnication of 12 and 25.
Size distribution of the microparticles was determined
by light scattering using a MasterSizer 2000 Instrument
(Malvern Instruments Ltd., Malvern, UK), based on the
average of ve tests. Particle size was expressed as the
mean diameter over the volume distribution D(4.3) (De
Brouckere mean diameter). The measure of the range of
the volume distribution relative to the median diameter was
measured using their span. The span is the width of the
distribution based on the 10%, 50% and 90% quantile:
Span =|D(v, 0.9) D(v, 0.1)],D(v, 0.5) (3)
where D(v, 0.9), D(v, 0.1), and D(v, 0.5) are volume
median diameters where 90%, 10%, and 50% of the vol-
ume distribution is below this values, respectively.
2 J. Colloid Sci. Biotechnol. 2, 18, 2013
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Ribeiro et al. Investigation of Phase Change Material Encapsulation by Complex Coacervation
2.3. Determination of Thermal Properties
Phase change temperatures and energy storage capaci-
ties of methyl palmitate and parafn wax were measured
using differential scanning calorimetry (DSC). A 2920
Modulated DSC calorimeter was employed equipped with
TA Instrument analyzer (New Castle, DE, USA) and a
mechanical refrigeration system. The melting point and
heat of fusion were determined for the pure substances as
well as for their microcapsules.
Pure methyl palmitate and parafn wax, as well as
about 5 mg of their capsules, were placed in aluminum
pans (20 jL). These samples were hermetically sealed,
weighed, and taken for DSC analysis. The samples were
heated at a rate of 10

C/min, from 0 to 100

C, with an
empty pan used as a reference. DSC analyses were per-
formed in triplicate in order to ensure the reliability of the
measurement. Indium (T
m
=156.6

C) was used as the cal-
ibration standard, and the data were analyzed using Uni-
versal Analysis 3.9 software (TA Instruments). Dry helium
(25 ml/min) was used as the purge gas. The melting tem-
perature of the PCM (T
m
) was determined by extending
the line of greatest slope of the leading edge of the DSC
peak to where it crosses the extrapolation of the base
line.
The percentage of PCM in the microcapsules was
calculated as the ratio between the latent heat of the
microcapsules (DHmc) and that of the corresponding pure
compound (DHpure) multiplied by 100 (Eq. (4)).
ER(wt.%) =DHmc,DHpure 100 (4)
3. RESULTS AND DISCUSSION
3.1. Evaluation of Operational Variables
The polymer pair of gelatin and gum Arabic was used
to produce PCM microparticles with different melting
points. The optimal conditions for the formation of the
wall reported by Prata
17
were used. However, depending
on the core material, these conditions may require modi-
cation. For methyl-palmitate, an ester of fatty acid which
presents naturally low surface tension, the standard method
led to highly efcient encapsulation at 50

C, without
the addition of a surfactant, and no modications were
necessary.
For parafn wax, however, the probability of complex
coacervation was greatly reduced, with only one out of
three attempts being successful in the encapsulation of the
wax. The others resulted in empty capsules and a paraf-
nic mass oating on the surface of the water. These
results suggest the process conditions require adjustment.
The inuence of various parameters of the process (tem-
perature, surfactant addition, time of addition and amount
of core material) were thus investigated in order to obtain
encapsulated parafn wax.
3.2. Conditions for Encapsulation of Parafn Wax
Coacervation can be undertaken with either a liquid or a
solid material. The parafn wax chosen melts at 60

C.
Softened wax (at 50

C) and liquid wax (at 70

C) were
both subjected to homogenization and, subsequently, poly-
mer complexation. Polymer complexation occurred in both
cases, but at the lower temperature with a solid core, no
encapsulation occurred. At 70

C, encapsulation did occur,
but part of the core material remained in the supernatant.
Parafn is a long hydrocarbon molecule, and that used
in this paper has 20 carbons, which makes it extremely
non-polar. This combination of size and lack of polarity
complicates the encapsulating process, making it difcult
for enclosure in small capsules.
In an attempt to enhance the efciency of the encap-
sulation, the addition of a surfactant was tried. Such sub-
stances, which reduce the surface tension of the aqueous
phase, are often used to improve the encapsulation process.
The use of a surfactant with a high hydrophilic-lipophilic
balance (HLB) can thus improve the emulsication of the
wax and Polysorbate 80 (Tween 80) which present HLB
of 15 was choose.
Various levels of surfactant in the core material were
tested (2%, 4% and 6% wt./wt. of wax). The droplets
formed were evaluated by optical microscopy (Fig. 1); the
images indicate that the droplets obtained by the addition
of 6% wt./wt. Tween 80 were the smallest, which would
theoretically be most easily encapsulated, yet much of the
core material was still located in the supernatant.
The concentration of 6% wt./wt. Tween 80 was then
tested in the emulsifying gelatin solution. In this case,
however, the surfactant failed to improve efciency of
encapsulation. The result was a cloudy system, with more
empty particles and all the wax outside them (Fig. 2,
center).
The stabilization of complexes depends on lowering the
pH, and the speed of this reduction, which was tested
next, proved be crucial to the process. The slower com-
plexation resulting from the use of a more diluted acid
allowed the parafn wax to escape from the capsule in for-
mation, making effective encapsulation almost impossible.
The use of 0.5 N HCl thus reduced the chances of success
to 25%, i.e., only one out four attempts was successful.
With a more concentrated acid (5 N), however, only a few
drops were necessary. The rapid drop in pH led to the
rapid formation of the capsules around the still intact wax
droplets (Fig. 2, right). The speed of lm formation, which
is able to prevent the escape of the hydrophobic parafn
from the emulsion, was crucial to increase the efciency
of encapsulation.
Once the encapsulation conditions for the two core
materials were established, an attempt was made to maxi-
mize the amount of core material encapsulated. Two ratios
of core material to wall material were tested: 50% and
75%. Four conditions of capsule formation were thus
J. Colloid Sci. Biotechnol. 2, 18, 2013 3
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Investigation of Phase Change Material Encapsulation by Complex Coacervation Ribeiro et al.
Fig. 1. Light microscopic images of parafn droplets (70

C), with 2% of surfactant (left), 4% (center), 6% (right). Scale bars represent 80 jm.
Fig. 2. Light microscopic images of parafn wax microparticles produced with addition of surfactant to core material (left), to the gelatin phase
(center), as well as with rapid pH reduction and no surfactant (right). Scale bars represent 50 jm.
employed: those containing 50% and 75% of methyl-
palmitate (MP50 and MP75) and those with 50% and 75%
of parafn wax (P50 and P75).
3.3. Characterization of Manufactured
Microcapsules Containing PCMs
The ideal encapsulated microparticle will maintain a high
capacity for energy storage and enclose a high concentra-
tion of the active PCM core material in a shell which is
strong enough to ensure stability.
The graphs in Figures 3 and 4 summarize the effect of
the temperature on heat ow. These thermograms show
the melting and crystallization temperatures and the latent
heat of fusion and crystallization for both the pure core
compounds and the microparticles encapsulating them.
Figure 3 shows the behavior of methyl palmitate and its
microcapsules. The peak corresponding to the solidliquid
transition temperature was the same for both (approx-
imately 28

C), but the average latent heat of fusion
decreased signicantly from the 192.2 J g
1
for the pure
methyl palmitate to 107 J g
1
, for the microcapsules with
75% of core material to 44.26 J g
1
for microparticles
with 50% of core material. The crystallization point for
methyl palmitate was displaced approximately 5

C from
the melting peak in 24

C, which was maintained for their
particles (Fig. 4). The solidliquid phase transitions were
reversible, i.e., the heat absorbed as latent heat of fusion
was released as heat of solidication.
Figure 4 shows the typical DSC thermograms of the
pure parafn wax and its microcapsules. This material
has two phase change peaks, a larger one for the solid
liquid change (at about 46

C) and a smaller one for a
solidsolid transition, when its molecular structure is mod-
ied (at about 26

C). Despite thus secondary transition
point, the energy involved is much less, and only the main
peak is typically considered in application for storage of
heat.
18
In the literature, some microparticles also produced by
coacervation and containing different types of parafn pre-
sented similar energy capacities, indicating that the par-
ticles produced in this research are appropriate for use
in heat storage. Hawlader et al.
19
prepared microparticles
using complex coacervation of gelatin-gum Arabic and
found heat storage ranging from 20 J g
1
to 90 J g
1
.
Bays-Garca et al.
12
also using complex coacervation,
produced particles with an enthalpy of fusion of 79 J g
1
.
Uddin et al.
20
produced particles by simple coacervation
with 56 J g
1
of heat storage.
The thermal properties of parafn wax microcapsules
were evaluated and the same two peaks were observed
at approximately the same temperatures. The latent heat
of fusion for parafn also decreased when encapsulated,
with the percent of loss being equivalent to that observed
for methyl palmitate, with 50% or 75% of core mate-
rial. Moreover, the latent heat of storage of the pure
methyl palmitate is almost 60% higher than that of parafn
wax, and this difference was maintained for their capsules
(Table II). The average values obtained for these micropar-
ticles were 58.49 J g
1
for the microcapsules with 75% of
core material and 29.31 J g
1
for microparticles with 50%
of parafn wax.
But the PCM adopted has an inuence on the enthalpy
of the particles produced, not only due to the differ-
ence in latent heat of the non encapsulated material.
Onder et al.
11
studied the encapsulation of n-hexadecane
(185 J g
1
), n-octadecane (234 J g
1
) and n-nonadecane
(194.3 J g
1
) through complex coacervation of a gum
Arabic and gelatin mixture and observed encapsulation
ratios of 78.22% for the coacervates with n-hexadecane,
4 J. Colloid Sci. Biotechnol. 2, 18, 2013
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Ribeiro et al. Investigation of Phase Change Material Encapsulation by Complex Coacervation
(A)
(B)
Fig. 3. DSC thermograms at 10

C/min for pure methyl palmitate (A) and its microparticles with 75% of core material (B).
70.85% for those containing n-octadecane and 29.59% for
n-nonadecane microcapsules.
The parafn, however, showed a clear point of crystal-
lization (at 44.59

C), close to the melting point, showing
the total reversibility of the solidliquid phase transitions.
Also, as the temperature of crystallization is above room
temperature, parafn wax is in a solid state when it is
not in service, contrary to what happens with methyl
palmitate.
The microscopic images of the moist microparti-
cles show the particulate nature of the wax at room
temperature (Fig. 5).
The more core compound encapsulated, the more ef-
cient is the product. The encapsulation ratio, i.e., con-
centration of the active core material, is calculated with
the equation based on enthalpy values obtained from DSC
measurements (Eq. (4)). This information is included in
Table II, which summarizes the effect of all parameters
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Investigation of Phase Change Material Encapsulation by Complex Coacervation Ribeiro et al.
(A)
(B)
Fig. 4. DSC thermograms at 10

C/min for pure parafn wax (A) and its microparticles with 25% (P2.5) and 50% (P5) of core material (B).
of successful microencapsulation realized during this
research.
The encapsulation ratio was found to be directly related
to the amount of core material added for the production of
the particles, with inclusion of more core material leading
to greater efciency of encapsulation. An encapsulation
ratio of about 23% was observed for microcapsules pro-
duced with 50% of core material, and of about 50% when
microparticles were produced with 75% of core material.
Figure 3 shows that the capsules formed are similar in size,
independent of the amount of core material enclosed.
This results is contrary to what was observed by
Hawlader et al.
19
who encapsulated a commercial parafn
wax by complex coacervation with gelatin and gum Ara-
bic and found that a higher coating to parafn ratio led to
a higher parafn encapsulation ratio.
Although in this research the type of PCM had no inu-
ence on the encapsulation efciency, the presence of paraf-
n wax hindered the occurrence of complexation during
coacervation, with from 1039% of the polymeric material
failing to precipitate.
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Ribeiro et al. Investigation of Phase Change Material Encapsulation by Complex Coacervation
Fig. 5. Light microscopic images of methyl-palmitate and parafn wax
and their microparticles shown capsules lled with core material for the
four conditions studied MP50(A), MP75(B), P50(C) and P75(D).
Table II. Effect of different parameters on microparticles produced.
Mpuc Mpuc
Processor TS%
1
Mc (g) YP%
2
(g) (%) ER%
Parafn wax microparticles
P50 5.00.5 4.940.9 66.76 0.4815 9.6 24.671.3
P75 5.00.7 4.02.2 38.38 1.967 39.34 47.611.0
Methyl palmitate microparticles
MP50 7.20.9 5.421.1 73.24 0 0 22.700.3
MP75 8.50.5 6.771.7 68.38 0.046 0.92 55.451.5
Notes:
1
TS%, the total solid content of coacervate phase (%),
2
%YP: yield of the
process (Eq. (1)).
Fig. 6. Particle size distribution of microparticles produced with
methyl-palmitate (black) and parafn wax (red).
Various sizes of microcapsules were produced, ranging
from less than 1 jm up to 400 jm (see Fig. 6). Greater
variation was found for methyl-palmitate microparticles
(span 2.14) than for those for parafn wax (span 1.44).
Moreover, the number of smaller particles was greater
for methyl palmitate. This large percentage of small
capsules (50% smaller than 57.76 jm) would make
methyl-palmitate especially appropriate for textile appli-
cation as seen in the work of Voncina et al.
21
who pro-
duced microcapsules of 2072 jm for application onto
cotton textiles of rosemary oil and Cheng et al.
22
who used
microencapsulated Vitamin C ranging in size from 5.0 to
44.1 jm in the development of cosmetic textiles.
The average microcapsules, independent of core mate-
rial, were larger for parafn (111.55 jm) than for
methyl-palmitate (69.45 jm). Complex coacervation
between gum Arabic and gelatin has produced particles
with sizes ranging from 50100 jm with parafn wax
19
or natural coco fatty acid mixture.
23
4. CONCLUSION
We have shown that complex coacervation was success-
ful in producing microcapsules with different PCMs. The
coacervates, manufactured with two percentages of core
material (50% and 75%) presented high heat storage
capacities ranging from 30 to 108 J g
1
. Microcapsules
performed their function effectively under both heating
and cooling conditions within the intervals coinciding with
those of the PCMs.
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Investigation of Phase Change Material Encapsulation by Complex Coacervation Ribeiro et al.
Microparticles produced with methyl palmitate were
easier to make, and did not inuence the complexation
of polymers; they also presented higher energy capacities
than microparticles produced with parafn.
For parafn wax, some difculties emerged during the
microencapsulation process, and a fast rate of pH reduc-
tion was necessary to increase the encapsulation ratio. The
encapsulation ratio (ER%) of these systems was indirectly
determined by differential scanning calorimetry (DSC). As
results, the core to coatings ratio increased from 50 to
75%, the ER increased from 25% to 50%. The paraf-
n inuenced the complexation of the polymers; for the
largest amounts of this hydrocarbon, about 39% of the
polymer was not complexed. The use of methyl palmitate
did not have this inuence on the coacervation process.
Energy storage capacities of 58.49 J g
1
and 107 J g
1
were observed, respectively, for parafn wax and methyl
palmitate systems, indicating their potential for use as
energy storage systems. The melting point of microcap-
sules produced with parafn was 46.30

C, and with
methyl palmitate 27.6

C, both near the melting point
of the pure compounds. The average particle size of the
parafn and methyl palmitate microcapsules obtained was
69.43 jm and 111.55 jm, respectively.
Acknowledgments: This project was supported by the
CNPqPIBIC, in partnership with UNICAMP. Fund-
ing was also provided by FAPESP (process number:
2011/04230-5) and FAEPEX (PAPIDIC).
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Received: 30 December 2012. Accepted: 6 March 2013.
8 J. Colloid Sci. Biotechnol. 2, 18, 2013