Professional Documents
Culture Documents
Sar 2014
Sar 2014
art ic l e i nf o a b s t r a c t
Article history: This study is focused on the preparation, characterization and determination of latent heat thermal
Received 3 January 2014 energy storage (LHTES) properties of polystyrene (PS)/n-heptadecane micro/nano-capsules as a novel
Received in revised form encapsulated phase change material (EPCM). The micro/nano-EPCM was synthesized via emulsion
31 January 2014
polymerization method and characterized chemically using Fourier transform infrared (FTIR) spectro-
Accepted 11 March 2014
scopy. The surface morphology and particle size of the micro/nano-capsules were investigated by
particle size distribution (PSD) analysis, polarized optical microscopy (POM) and scanning electron
Keywords: microscopy (SEM) techniques. From differential scanning calorimetry (DSC) analysis, the melting
Micro/nano-EPCM temperature and latent heat of the prepared EPCM were measured as 21.48 1C and 136.89 J/g,
n-heptadecane
respectively. The results of thermogravimetric (TG) analysis showed that the fabricated micro/nano-
Emulsion polymerization
EPCM had good thermal durability. Thermal reliability, chemical stability, thermal conductivity and
Polystyrene
Latent heat phase change reversibility of the micro/nano-EPCM were also studied. All of the results revealed that the
Thermal energy storage fabricated PS/n-heptadecane micro/nano-capsules had promising LHTES potential especially for passive
solar thermal regulation of textile, building, food storage container, medical and electronic materials.
& 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.solmat.2014.03.023
0927-0248/& 2014 Elsevier B.V. All rights reserved.
A. Sarı et al. / Solar Energy Materials & Solar Cells 126 (2014) 42–50 43
polymer shells such as melamine–formaldehyde resin [39,40], thermal conductivity and phase change reversibility properties of the
urea–formaldehyde resin [41,42], polyurea [43–45], and acrylic- prepared EPCM were studied.
based polymers [46–50]. Among these, especially melamine–
formaldehyde and urea–formaldehyde resins-based EPCMs may
contain irrepressible residue formaldehyde and isocyanides after 2. Experimental
shell forming reaction, which have negative effects on the envir-
onment and health. It is also hard to find useful ways to eradicate 2.1. Materials
the wastes that are dissociative and can be incessantly released
from the products. The chemicals used in the synthesis of micro/nano-capsules
Polystyrene (PS) is one of the aromatic polymers made from include monomer styrene (Sigma-Aldrich Company), n-heptadecane
monomer styrene in the chemical industry. It is very inexpen- (Merck Company), divinylbenzene (Merck Company), Triton X100
sive and therefore commonly used in several trading applica- (Merck Company), and ferrous sulfate heptahydrate and ammonium
tions [51,52]. Polystyrene foams are also suitable for the persulphate (Sigma-Aldrich Company). The monomer styrene was
insulation of building concrete materials and panel systems. It washed three times with an aqueous solution of 10 wt% NaOH prior to
has also reasonably good mechanical and protective properties use. The other chemicals were used without further purification.
against the exterior environment. All of these advantages have
facilitated it to be considered as shell material in the fabrication of 2.2. Preparation of the PS/n-heptadecane micro/nano-capsules
new EPCMs [53–56]. Therefore, the utilization scale of PS can be
extended by its usage in different passive solar LHTES systems. n- PS/n-heptadecane micro/nano-capsules were synthesized using
Heptadecane known as a hydrocarbon with linear chain has a the experimental set-ups shown in Fig. 1(a and b). For the prepara-
desirable melting temperature of about 21 1C and relatively high tion of PS/n-heptadecane(2:1) micro/nano-capsules, the initial
latent heat of fusion (about 216 J/g). By taking into account the weight ratio of styrene monomer/n-heptadecane was selected as
literature survey, it can be noted that there is no study about the about 67%/33% (w/w). According to this ratio, 6.7 g monomer and
preparation and thermal characterization of micro/nano-encapsu- 2 g divinylbenzene as cross linking agents were mixed with 40 mL
lated n-heptadecane using PS shell. With this purpose, the present deionized water in the three-necked glass reactor (Fig. 1a). 3.3 g
work was focused on the syhnthesis of PS/n-heptadecane micro/ n-heptadecane in melted state was added to the reactor. This
nano-capsules as novel EPCM using emulsion polymerization mixture was homogenized using a homogenizer at 12,000 rpm for
method and chemical characterization by FT-IR spectroscopy techni- 15 min. Then, 3 g Triton X-100 surfactant was added to the mixture
que. The morphology and particle size of the fabricated EPCM were and the solution was re-homogenized at 50 1C for 60 min at the
investigated using SEM, POM and PSD analyses. The LHTES proper- same homogenization rate. In the next step, 1 mL initiator (freshly
ties, thermal reliability and thermal durability were determined prepared by solving ferrous sulfate heptahydrate (0.15 g) and
using DSC and TG techniques. In addition, the chemical stability, ammonium persulphate (0.1 g) into 100 mL deionized water) was
Fig. 1. Photograph images of experimental apparatus used in the synthesis processes and the obtained final product.
44 A. Sarı et al. / Solar Energy Materials & Solar Cells 126 (2014) 42–50
added to the reaction medium. This resultant blend was stirred to (1:2)-capsules, they were also exposed to thermal cycling test
form an oil-in-water emulsion system at 70 1C for 6 h at 500 rpm using a thermal cycler (BIOER TC-25/H model). The thermal
using a mechanical stirrer (Fig. 1b). When the mixture was of the cycling test was continued until the number of consecutive
consistency of honey, the polymerization reaction was ended and it heating/cooling processes was reached 5000.
was filtered using a filter paper. The filtrate was washed several The temperature–time histories of fabricated PS/n-heptadecane
times and dried at 40 1C in an oven to evaporate the water. The micro/nano(1:2)-capsules were also determined by using same
same synthesis procedure was also repeated in the preparation of experimental set-up and method as given in literature [57]. The
the micro/nano-capsules with two different styrene/n-heptadecane temperature–time variations obtained during the heating and
combinations as 1:1 (corresponds to 50%/50% (w/w)) and 1:2 cooling process of the micro/nano-capsules were recorded using
(corresponds to about 33%/67% (w/w)). The dried product is also a data logger (Nova5000 model). In addition, the thermal con-
shown in Fig. 1c. ductivities of n-heptadecane, PS and PS/n-heptadecane micro/
nano(1:2)-capsules were measured at 25 1C using a thermal
property analyzer (KD2 model).
2.3. Characterization of PS/n-heptadecane micro/nano-capsules
Fig. 2. FT-IR spectra of (a) n-heptadecane, (b) PS, and (c) n-heptadecane/PS micro/nano-capsules(1:2).
A. Sarı et al. / Solar Energy Materials & Solar Cells 126 (2014) 42–50 45
were associated with the C–H stretching vibration bands. The with 30.00 magnification and POM images are presented in
peak seen at 1412 cm 1 is attributed to the C–H deformation Fig. 3a and b, respectively. As clearly seen from micrographs, the
vibration. The peaks detected at 1522 and 1462 cm 1 were assigned PS/n-heptadecane micro/nano(1:2)-capsules are not completely
as aliphatic and aromatic CQC stretching vibration bands of the sphere-shaped in appearance and some of them have partially
benzene ring, respectively. As also clearly seen from the spectrum of rough external surface or cluster-structure. On the other hand, the
synthesized EPCM (Fig. 2c), the C–H stretching peaks of PS are reason for not being able to observe such type of cluster-structures
overlapped with the same group peaks of n-heptadecane observed in in POM micrographs (Fig. 3a) is due to the fact that the particles
the range of 2920, 3030 and 3044 cm 1. The peak detected at were dispersed in aqueous medium prior to taking the micro-
1482 cm 1 was regarding CQC stretching vibration bands of the graphs. Moreover, based on the scales on the SEM and POM
benzene ring. Moreover, the stretching vibration band related with micrographs, it can be realized that the fabricated EPCM relatively
the aliphatic vinyl C–H group bonded the benzene ring (at consisted of nano-spheres. Thus, such a micro/nano type structure
1522 cm 1) disappeared due to the polymerization of styrene. All can present extended surface area, which acts to accelerate heat
these spectroscopic results confirm the presence of n-heptadecane as transfer rate in LHTES systems [29].
core material and the formation of PS as shell material around the The PSD analysis results (Fig. 4) show the prepared PS/n-
core material. heptadecane micro/nano-capsules have unimodal particle
size distributions with relatively narrow interval (0.01–60 mm,
3.2. Morphological and PSD analysis of micro/nano-capsules 0.01–30 mm and 0.01–40 mm for EPCM with the combination of
2:1, 1:1 and 1:2, respectively). The particle sizes are mainly in the
The morphology and particle size of the synthesized PS/n- range of 1–15 mm, 1–12 mm and 1–20 mm for the prepared EPCMs
heptadecane micro/nano(1:2)-capsules were investigated using SEM, with the combination of 2:1, 1:1 and 1:2, respectively. Moreover,
POM and PSD analysis methods. The obtained SEM microphotographs the mean sizes of the particles was found to be 6.3, 6.1 and 5.4 mm.
Fig. 3. (a) POM micrographs of n-heptadecane/PS micro/nano-capsules(1:2) and (b) SEM micrographs n-heptadecane/PS micro/nano-capsules(1:2).
Fig. 4. Particle size distribution of prepared micro/nano-capsules with different styrene/n-heptadecane ratios.
46 A. Sarı et al. / Solar Energy Materials & Solar Cells 126 (2014) 42–50
Fig. 5. DSC thermograms of n-heptadecane and prepared micro/nano-capsules with different styrene/n-heptadecane ratios.
These results showed that the increase in the combination ratio of in textile, building, food storage container, medical and electronic
the paraffin did not influence the particle sizes of the capsules. In applications.
addition, the particle sizes of the EPCMs determined by PSD The latent heat capacity of an EPCM is dependent on the mass
analysis are slightly higher than that observed from SEM and fraction of its PCM content. In this work, in order to achieve the
POM micrographs. This is due to the formation of cluster struc- maximum encapsulation ratio, the micro/nano-EPCMs were
tures thus being detected as a single sphere by the PSD instru- prepared by changing the weight combination ratio of styrene/
ment. However, even if the prepared PS/n-heptadecane micro/ n-heptadecane. As also clearly seen from Table 1, the latent heat
nano-capsules(1:2) have spheres with cluster state, they can be values of prepared micro/nano-EPCM were raised proportion-
used for LHTES purposes. ally with increasing the mass fraction of PCM content. Espe-
cially, the micro/nano-EPCM with combination ratio of 1:2 (w/
3.3. Thermal properties and thermal stability of micro/nano-capsules w) has a latent heat of melting of 136.89 J/g while n-heptade-
cane storages latent heat of fusion as 216.21 J/g. This result
Fig. 5 shows the DSC curves of n-heptadecane and the micro/ indicated that the fabricated PS/n-heptadecane micro/nano
nano-EPCM fabricated at different monomer/PCM ratios. The (1:2)-capsules had good LHTES potential for thermal regulation
LHTES properties obtained for n-heptadecane and the micro/ objectives in textile, building, food storage, medical and elec-
nano-EPCMs from the DSC curves were also presented in tronic applications.
Table 1. By considering these data, it can be clearly stated that On the other hand, the actual encapsulation percentage
all of the micro/nano-capsules exhibit very stable and reversible of n-heptadecane by PS can be calculated as below
phase change behaviors during both their heating and cooling
ΔH PS=heptadecane
periods. The n-heptadecane has solid–solid peaks at 10.87 1C (for Encapsulation of n heptadecane ð%Þ ¼ 100
ΔH heptadecane
heating period) and 9.86 1C (for cooling period) and also melting
peak at 21.36 1C, and freezing peak at 21.30 1C. In the similar trend, where, ΔH PS=heptadecane and ΔH heptadecane correspond to the measured
the prepared PS/n-heptadecane micro/nano(1:2)-capsules show latent heat values of synthesized EPCM and n-heptadecane,
solid–solid transitions at 10.93 1C (for heating period) and 8.83 1C respectively. By using this equation, the real encapsulation ratio
(for cooling period), and a melting phase change at 21.48 1C and of n-heptadecane by PS shell was found as 63.3%. This result
freezing phase change at 21.37 1C. The sub-cooling degree of the means that the actual PCM content is almost same as the
PS/n-heptadecane micro/nano(1:2)-capsules was found to be calculated percentage of PCM content (about 67%) based on the
0.11 1C. The little sub-cooling provides an important advantage initial combination ratio. On the other hand, in the previous study,
for reversible LHTES processes. Moreover, the melting temperature the latent heat capacity and encapsulation ratio for n-heptade-
of the prepared PS/n-heptadecane micro/nano(1:2)-capsules cane/poly(methyl methacrylate) micro-capsules were found as
makes it a promising LHTES material for thermal regulating aim 81.5 J/g and 38 wt%, respectively [20]. The encapsulation ratio
A. Sarı et al. / Solar Energy Materials & Solar Cells 126 (2014) 42–50 47
Table 1
Measured LHTES properties of n-heptadecane and the prepared EPCMs at different weight ratios of monomer/PCM using DSC analysis method.
Solid–solid phase Solid–liquid phase Latent heat of Solid–solid phase Liquid–solid phase Latent heat of
transition change (melting) melting (J/g) transition change (freezing) freezing (J/g)
temperature (1C) temperature (1C) temperature (1C) temperature (1C)
found in this study was also higher than that obtained for various
micro-EPCMs including PS shell and other core materials such as
n-octadecane [16,55], n-tetradecane and n-nonadecane [54].
Fig. 7. FT-IR spectra of n-heptadecane/PS micro/nano-capsules(1:2): (a) before thermal cycling and (b) after thermal cycling.
Fig. 9. Temperature–time curves obtained during the heating and cooling periods
Fig. 8. TG curves of n-heptadecane, PS and the prepared n-heptadecane/PS micro/ of the prepared PS/n-heptadecane micro/nano-capsules(1:2).
nano-capsules(1:2).
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