1894 r2010 American Chemical Society pubs.acs.

org/EF
Energy Fuels 2010, 24, 18941898
:
DOI:10.1021/ef9013967
Published on Web 02/19/2010
Preparation and Melting/Freezing Characteristics of Cu/Paraffin Nanofluid
as Phase-Change Material (PCM)
Shuying Wu,

Dongsheng Zhu,*
,
Xiurong Zhang,

and Jin Huang

Key Lab of Enhanced Heat Transfer and Energy Conservation, the Ministry of Education, School of Chemistry and Chemical
Engineering, South China University of Technology, Guangzhou 510640, China, and

College of Material and Energy,
Guangdong University of Technology, Guangzhou 510006, China
Received November 17, 2009. Revised Manuscript Received February 1, 2010
A new sort of nanofluid phase-change material (PCM) is developed by suspending a small amount of
nanoparticles in melting paraffin. Cu, Al, and C/Cu nanoparticles were selected to add to the melting
paraffin to enhance the heat-transfer rate of paraffin. Cu nanoparticles have the best performance for heat
transfer. Five dispersants were chosen to make Cu nanoparticles stably suspended in melting paraffin. The
nanofluids with Cu nanoparticles show good stability in melting paraffin under the action of Hitenol BC-
10, even suspending for 12 h in a constant temperature trough. The Fourier transform infrared (FTIR)
spentrum shows that it is a physical interaction among Cu, paraffin, and Hitenol BC-10. The differential
scanning calorimetric (DSC) results reveal that the latent heats of Cu/paraffin shift to lower values
compared to those of pure paraffin; however, the melting and freezing temperatures are kept almost the
same as pure paraffin. The latent heats and phase-change temperatures change very little after 100 thermal
cycles. Furthermore, the heating and cooling rates of PCMs were significantly improved upon the addition
of Cu nanoparticles. For composites with 1 wt % Cu nanoparticle, the heating and cooling times can be
reduced by 30.3 and 28.2%, respectively.
1. Introduction
Since the outbreak of the energy crisis in 1973, thermal
energy storage technologies are receiving more and more
attention. There are various thermal energy storage methods,
but latent heat storage is the most attractive one because of the
advantages of its high storage density and isothermal charac-
teristics.
1
It has broad application prospects
2,3
in solar energy
use, electricity from peak to off peak, waste heat recovery, etc.
Paraffin is one of the most commonly used phase-change
materials (PCMs) in storing thermal energy. It is regarded as
the most promising PCM for large latent heat, low cost,
stability, nontoxicity, and no corrosion.
4
However, its inher-
ent low thermal conductivity limits its utility applications.
Many methods have been proposed to enhance the thermal
conducitvityof pure paraffin, suchas placing a metal structure
in PCM,
5
impregnating porous material,
6,7
and dispersing
high thermal conductivity particles in PCM.
8,9
Recently, with the development of nanotechnology, resear-
chers have started to study the thermal conductivity perfor-
mance of adding nanoparticles to various fluids, so-called
nanofluids,
10
which can result in the thermal conductivity
enhancement beingsignificantly higher thanthe predictions of
the classical solid-liquid models.
11-13
Ho et al.
14
enhanced
the thermal conductivity of paraffin (n-octadecane) by adding
Al
2
O
3
nanoparticles. Xie et al.
15
dispersed multi-walled car-
bon nanotubes (MWNTs) into paraffin (melting point, T
m
=
52-54 C) by the ball-milling method. For the composite with
a mass fraction of 2.0 wt %, the thermal conductivity enhan-
cement ratios reach 35.0 and 40.0% in solid and liquid states,
respectively. Zeng et al. studied the thermal conductivity
enhancement of Ag nanowires/1-tetradecanol
16
and carbon
nanotubes (CNTs)/palmitic acid
17
as PCMs for the formation
of the network in the PCMs. Elgafy et al.
18
prepared a
composite with carbon nanofibers filled in with paraffin,
and the results showed that the thermal conductivity of the
composite enhancedsignificantly, which increased the cooling
rate in the solidification process. Wu et al.
19
investigated the
Al
2
O
3
/H
2
O nanofluids as a PCM for cool storage, and the
*To whom correspondence should be addressed. E-mail: cedshzhu@
scut.edu.cn.
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Anal. Calorim. 2010, doi: 10.1007/s10973-009-0472-y.
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Acta 2009, 483, 73.
1895
Energy Fuels 2010, 24, 18941898
:
DOI:10.1021/ef9013967 Wu et al.
results stated that the total freezing time of Al
2
O
3
/H
2
O
nanofluids reduced by 20.5% with the addition of 0.2 wt %
nanoparticles. Liu et al.
20
evaluated the cool storage capacity
of the BaCl
2
aqueous solution by suspending TiO
2
nanopar-
ticles, and the cool storage/supply rate and the cool storage/
supply capacity both increased higher than those of BaCl
2
aqueous solution without nanoparticles. Khodadadi et al.
21
numerically simulated the solidification of Cu/water nano-
fluid in a vertical square enclosure. A higher heat extraction
rate of the freezing process was found as a result of the
addition of Cu nanoparticles. In other words, the addition
of nanoparticles could improve the thermal conductivity and
the heating-cooling rate. However, there are only a few
experimental studies focused on the phase-change properties
of nanofluids as a latent heat storage material. It is too limited
compared to the massive study on the viscosity, thermal con-
ductivities, mechanisms, and models of nanofluids.
22-24
In this paper, a new kind of nanofluid PCM was prepared
by adding nanoparticles to paraffin. Different nanoparticles
were chosen and added to melting paraffin to obtain the best
heat-transfer enhancement. Furthermore, different disper-
sants were added to melting Cu/paraffin toensure the stability
of PCMs. At last, the thermal reliability, latent heats, phase-
change temperatures, and heating-cooling rate of Cu/paraf-
fin were investigated experimentally.
2. Experimental Section
2.1. Materials. Paraffin (T
m
=58-60 C) was used as PCMin
the preparation of the composite PCMs. It was purchased from
the Shanghai Specimen and Model Factory (China). Cu, Al, and
C/Cu nanopowders (Shenzhen Junye Nano Material Ltd.,
China) with all contents >99.9% were used. The average
particle size of those particles was 25 nm. Five kinds of dis-
persants were used here. Their structures are shown in Figure 1.
GA, Span-80, cetyl trimethyl ammoniumbromide (CTAB), and
sodium dodecylbenzenesulfonate (SDBS) were supplied by the
Guangzhou Chemical Reagent Factory (China). Hitenol BC-10
was purchased from Montello, Inc., Japan. All chemicals used
were without any further purification.
2.2. Preparation of PCMs. Atwo-step method was selected to
prepare the PCMs. First, to confirm which nanoparticle should
be used, different nanoparticles were dispersed into melting
paraffin. To observe the stability of the composite, the PCMs
consisting of paraffin, Cu nanoparticles, and different disper-
sants were prepared. All of the preparation processes were
performed using an ultrasonic vibrator for 2 h. A longer time
of high-energy sonication would introduce defects.
25
The ultra-
sonic temperature was above 58 C to ensure that the samples
were kept sufficiently above the melting point of the paraffin.
2.3. Heating-Cooling Rate Test. A thermal performance test
was conducted to verify the improvement of heat-transfer rate in
the presence of Cu particles. The experimental setup is shown in
Figure 2. The water in the constant temperature trough was
maintained at 70 C for the heating process and 30 C for the
cooling process. For the cooling process, the melting PCMs were
transferred to the test tubes. Then, the tubes were placed into the
constant temperature trough for freezing. After this process, the
PCMs were immediately subjected to the heating process in the
same way at a constant temperature of 70 C. The transient
temperature response at the center of the tubes was recorded by
the temperature datalogger at a time interval of 10 s.
2.4. Analysis Methods. ATAdifferential scanning calorimeter
(DSC) was used to determine the latent heats and phase-change
temperatures of melting and freezing. It was performed at a
heating rate of 5 C/min in a purified argon atmosphere. Liquid
nitrogen was used as the cooling medium during the freezing
process. The melting and freezing temperatures were estimated
by the tangent at the point of greatest slope on the face portion
of the peak of the DSC curve. The latent heats of phase change
were determined by numerical integration of the area under the
peaks.
Infrared spectra of solid PCMs were obtained using a Fourier
transform infrared spectrometer (FTIR, Bruker TENSON 27)
with KBr pellets in the range of 4000-400 cm
-1
.
2.5. Thermal Cycling Test. The thermal cycling test was used
todetermine thermal reliability of PCMinterms of the change in
phase-change temperatures and latent heats with respect to the
thermal cycling number. A thermal cycling test consisted of a
Figure 1. Chemical structure of dispersants.
Figure 2. Experimental setup for the heating-cooling rate test.
(20) Liu, Y. D.; Zhou, Y. G.; Tong, M. W.; Zhou, X. S. Microfluid.
Nanofluid. 2009, 7, 579.
(21) Khodadadi, J. M.; Hosseinizadeh, S. F. Int. Commun. Heat Mass
Transfer 2007, 34, 534.
(22) Krishnamurthy, S.; Bhattacharya, P.; PhelanR, P. E.; Prasher, S.
Nano Lett. 2006, 6, 419.
(23) Lee, D. Langmuir 2007, 23, 6011.
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Chem. C 2007, 111, 1646.
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Strano, M. S.; Haroz, E. H.; Rialon, K. L.; Boul, P. J.; Noon, W. H.;
Kittrell, C.; Ma, J.; Hauge, R. H.; Weisman, R. B.; Smalley, R. E.
Science 2002, 297, 593.
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Energy Fuels 2010, 24, 18941898
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DOI:10.1021/ef9013967 Wu et al.
melting and freezing process of PCM. DSC analysis was per-
formed to determine the thermal stability of the composite PCM
after thermal cycles.
3. Results and Discussion
3.1. Selection of Nanoparticles. To select an effective
nanoparticle, a heating-cooling rate test was conducted
using the experimental setup shown in Figure 2. Cu, Al,
and C/Cu nanoparticles were chosen. The mass fractions
of Cu/paraffin, Al/paraffin, and (C/Cu)/paraffin all remain
0.1%. The heating and cooling curves of the PCMs are
shown in Figures 3 and 4. The results show that different
nanoparticles have different effects on the heat-transfer rate.
It took 1278, 1311, 1356, and 1416 s for Cu/paraffin, Al/
paraffin, (C/Cu)/paraffin, and pure paraffin to reach 67 C,
respectively. It took 1419, 1518, 1587, and 1512 s for Cu/
paraffin, Al/paraffin, (C/Cu)/paraffin, and pure paraffin to
drop to 30 C. The heating time was reduced by 9.7, 7.4, and
4.2% for Cu/paraffin, Al/paraffin, and (C/Cu)/paraffin,
respectively. The cooling time was reduced by 6.7, -0.4,
and -5% for them, respectively. Thus, the Cu particle has
the best performance for heat transfer. However, without the
dispersant, the melting Cu/paraffin will not be stable.
26
In
the next study, the work was focused on the thermal proper-
ties of Cu/paraffin in the presence of dispersants.
3.2. Preparation of Cu/Paraffin. Preparation of PCMs is
the first key step in applying nanophase particles to enhance
the heat-transfer performance of PCM. To improve the
dispersion behavior of nanoparticles in liquid fluids, the
methods, such as using ultrasonic vibration and adding dis-
persants, were widely usedin preparing nano-suspensions. In
this study, ultrasonication and different dispersants were
used at the same time. The mass ratio for Cu nanoparticles
and dispersants was controlled at 1:3. Figure 5 shows the
sediment photographs after 12 h. It clearly indicates that the
suspension with the surfactant of Hitenol BC-10 is the most
stable compared to others. The mechanism of Hitesol BC-10
on the copper suspension should be steric hindrance.
27
In the
structure of Hitesol BC-10, there is a long carbon chain and a
benzene ring, which make the steric hindrance very large.
The Cu nanoparticles in the suspension are hard to be close
to each other and could disperse stably.
3.3. Characterization of PCMs. FTIR is an effective
method to investigate a specific interaction in the composite
PCMs. Figure 6 shows the FTIR absorption spectrum of the
PCMs. No significant new peaks were observed. The FTIR
spectrum proved that there are only physical interactions
between the components of the composite PCM and no new
chemical-bond generation.
28
3.4. Thermal Properties of PCMs. DSC analysis was con-
ducted to investigate the influence of Cu addition on the ther-
mal properties of composite PCMs. The phase-change latent
heat and temperature of pure paraffin and Cu/paraffin com-
posites are shown in Figures 7 and 8. As can be seen from the
data, the changes in the melting and freezing temperatures are
very little for different contents of Cu nanoparticles. The maxi-
mum change is -0.6% for melting temperatures and 2% for
freezing temperatures, which could be negligible.
As can been seen in Figure 8, the maximum reduction is
11.1% for melting latent heats and 11.7% for freezing latent
heats, respectively. According to the theory of mixtures, the
latent heat of Cu/paraffin composite is equal to the values
calculated by multiplying the latent heat value of pure
paraffin with its mass fraction in the composite PCM. The
calculated values are shown in Figure 8. It shows that the
latent heat of each composite is lower than the calculated
latent heat. With the increase of the mass fractions of Cu, the
deviation becomes larger. Similar results were also found by
Sar and Karaipekli,
29-31
Ho and Gao,
14
and Xie et al.
15
However, only a vague reason was given for the discrepancy
Figure 3. Heating curves of the PCMs with different nanoparticles.
Figure 4. Cooling curves of the PCMs with different nanoparticles.
Figure 5. Sediment photographs with different dispersants deposit-
ing for 12 h.
(26) Li, X. F.; Zhu, D. S.; Wang, X. J. J. Colloid Interface Sci. 2007,
310, 456.
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Ahnb, Y. C.; Kim, S. H. Powder Technol. 2008, 186, 145.
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2009, 86, 170.
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1897
Energy Fuels 2010, 24, 18941898
:
DOI:10.1021/ef9013967 Wu et al.
between the experimental data and the predicted values. We
think that the heat-transfer performance of nanofluid is
different from the conventional solid-liquid mixture.
32
Sur-
face and size effects of the nanoparticle have effects on the
thermal characteristics.
33
Therefore, the equation for the
simple solid-liquid mixture does not suit the calculation of
the latent heat of nanofluid. A new model is needed for
nanofluid. Kenisarin et al.
34
reported that fatty acid compo-
sitions with latent heat capacity of about 120 kJ/kg can be
used for solar energy storage. The latent heats of all of the
PCM composites in our experiments are about 180 kJ/kg,
which indicates that these PCM composites are suitable for
latent heat thermal energy storage applications.
3.5. Heating-Cooling Rate Evaluation. The improvement
of the heat-transfer rate was verified by comparing the
heating-cooling rate process of pure paraffin and Cu/para-
ffin composite. The typical temperature curves of the PCMs
are shown in Figures 9 and 10, respectively. It shows that
both heating and cooling processes are influenced by the
addition of Cu particles.
The figures show a comparison of the heat-transfer rate
between pure paraffin and composite PCMs. When the
material with a high thermal conductivity is added, the ther-
mal response will become more sensitive. In Figure 9, the
temperatures of pure paraffin and the composite PCMs
are 30 C, the same at the beginning of the heating perfor-
mance test. The temperatures of the paraffin and the com-
posite PCM increased with time elapsing, and the phase
change (BC) from solid (AB) to liquid (CD) occurred. The
temperature-increasing curves of the composite were steeper
than the curve of pure paraffin. The heating times of Cu/
paraffin were typically shortened. For example, it took 1450 s
for pure paraffin to increase the temperature from 30 to
68 C, whereas it took only 1010 s for Cu/paraffin (1 wt %),
which was reduced 30.3% compared to that for pure paraf-
fin. It was obvious that the heating rate of the composite
PCM was higher than that of pure paraffin. It can also be
seen fromFigure 10 that the cooling rate of composite PCMs
was also higher than that of pure paraffin. It took 1810 s for
pure paraffin to drop its temperature from 68 to 30 C and
only 1300 s for Cu/paraffin (1 wt %), indicating that the
cooling time for Cu/paraffin (1 wt %) was reduced 28.2%
compared to that for pure paraffin. It was concluded from
these results that the heat-transfer rate in the composite PCMs
was obviously higher than that in pure paraffin because of
the addition of Cu particles.
There are two possible reasons to explain the behavior of
the higher heat-transfer rate. One is the higher thermal con-
ductivity for Cu/paraffin, because the crystal growth mainly
depends upon heat transfer. At the process of melting and
freezing, a large amount of heat will be discharged. If the heat
cannot be released timely, the heating and cooling process
will be hindered. The thermal conductivity of pure paraffin is
enhanced with the addition of nanoparticles. Therefore, the
heating and cooling speeds of PCMs are able to be accele-
rated. Thermal conductivities of samples were measured by
Figure 6. FTIR spectra of paraffin and Cu/paraffin.
Figure 7. Phase-change temperature of Cu/paraffin with different
mass fractions.
Figure 8. Latent heat of Cu/paraffin with different mass fractions.
Figure 9. Heating curves of paraffin and Cu/paraffin.
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94, No. 025901.
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Rev. 2007, 11, 1913.
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Energy Fuels 2010, 24, 18941898
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DOI:10.1021/ef9013967 Wu et al.
the transient hot-wire method. The values of 0 and 1 wt %
Cu/paraffin are 0.1687 and 0.1878 W m
-1
K
-1
in liquid and
0.2699 and 0.2908 W m
-1
K
-1
in solid, respectively. There is a
different extent on the increase of thermal conductivity, which
has been verified by many other groups.
35,36
Therefore, the
thermal conductivity improvement of paraffin confirms the
reduction of heating and cooling times of Cu/paraffin com-
pared to those of paraffin. The other reason may be the Cu
nanoparticles acting as a nucleating agent, and this is also
helpful for reducing the heating and cooling times.
20
As can be seen from Figures 9 and 10, the melting and
freezing temperatures of the Cu/paraffincomposite PCMare
almost equal to those of pure paraffin. However, the melting
and freezing temperatures for all PCMs are lower or higher
than those from DSC. The reason is that the measurement
principle and the sample weight are different between the
heating-cooling rate test and DSC method. The DSC mea-
surement is an express method and differs from the classical
thermophysical methods. A similar phenomena were also
found by Li et al.
37
3.6. Thermal Reliability of PCMs. In this experiment, the
composite PCM including 0.5 wt % Cu nanoparticles was
used to test its stability on the thermal performance after 0,
20, 50, 70, and 100 times thermal cycling. Figures 11 and 12
show the phase-change temperature and latent heat after
thermal cycling, respectively. The maximum change is
-1.6% for melting temperature and -1.9% for freezing
temperature. It shows little change for the phase-change
temperature, which is not significant for applications. It
can also be seen that Cu/paraffin has a good thermal
reliability in terms of the latent heat values. The greatest
change in the melting latent heat is -3.2%, and the greatest
change in the freezing latent heat is 2%. These changes are
negligible for latent heat thermal energy storage applica-
tions.
4. Conclusions
In conclusion, the addition of nanoparticles enhanced the
heat-transfer rate of PCM significantly. The Cu nanoparticle
has better effects than Al and C/Cu nanopowders. Because of
large steric hindrance, the Cu/paraffin composite PCM with
Hitenol BC-10 shows good dispersed property after 12 h. The
FTIRspectroscopy results indicate that there is just a physical
interactionamong Cu, Hitenol BC-10, andparaffin. WhenCu
particles are added to paraffin, the changes in the melting and
freezing temperatures are in negligible magnitudes. However,
the latent heats for melting and freezing are reduced. The
maximum reduction is 11.1% for melting latent heats and
11.7%for freezing latent heats, respectively. After 100 heating
and cooling cycles, Cu/paraffin still has a good thermal
reliability because of the little changes in latent heat and
phase-change temperature. The heat-transfer rate of the com-
posite PCM was obviously higher than that of pure paraffin.
The heating andcooling rate tests showedthat the heating and
cooling times were reduced by 30.3 and 28.2%for 1 wt %Cu/
paraffin, respectively. The experimental results reveal that the
addition of nanoparticles to paraffin is a good method to
enhance the heat-transfer performance of paraffin, because of
its good thermal properties, thermal and chemical reliability,
and heat-transfer rate.
Acknowledgment. The authors acknowledge the financial
support from the Plan Projects for Science and Technology of
Guangzhou (Grant 2008Z1-1061) and the Program for New
Century Excellent Talents in University (Grant NCET-04-0826).
Figure 10. Cooling curves of paraffin and Cu/paraffin.
Figure 11. Effect of thermal cycles on the phase-change tempera-
ture.
Figure 12. Effect of thermal cycles on the latent heat.
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