Solar Energy Materials & Solar Cells 132 (2015) 425430

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Solar Energy Materials & Solar Cells

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

Graphenenickel/n-carboxylic acids composites as form-stable phase

change materials for thermal energy storage
Weidong Liang, Guodong Zhang, Hanxue Sun, Pinsong Chen, Zhaoqi Zhu, An Li n
College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou, PR China

art ic l e i nf o a b s t r a c t

Article history: Superoleophilic graphenenickel foam (PDMSGNF), which was prepared by coating graphene nanosheets
Received 30 May 2014 onto nickel foam followed by surface modication with polydimethylsiloxane (PDMS), was used as porous
Received in revised form supporting material to prepare form-stable phase change materials (PCMs) composites. Owing to the strong
22 September 2014
hydrophobic and superhydrophilic wettability of PDMSGNF, PCMs can be absorbed spontaneously into
Accepted 26 September 2014
PDMSGNF and can stay stable without leakage even over their melting points. The incorporation of PCMs
into PDMSGNF does not change the crystal structure but lowers the crystallinity size of PCMs in the com-
Keywords: posites, which is conrmed by X-ray powder diffraction (XRD) analysis. The latent heat of PDMSGNF/PCM
Graphene composites was measured in the range of 42.3123.41 kJ kg
1. Taking advantages of the simple process and
Nickel foam
good stability the PDMSGNF should be ideal candidates as an alternative to traditional PCMs, which may
PCMs
have great potentials for renewable energy saving applications.
Superoleophilicity
Latent heat & 2014 Elsevier B.V. All rights reserved.

1. Introduction capacity and appropriate thermal properties [68]. However they

The increasingly serious energy crisis and continuous increase
in greenhouse gas emissions drive people to more effectively
utilize various sources of energy. However, most of renewable
resources are intermittent providers of energy due to environ-
mental constraints, e.g. solar energy. Therefore, efcient energy
storage devices and systems are of critical importance to improve
the energy efciency and reduce the gap between energy demand
and energy generation. Phase change materials (PCMs) can store
and release latent heat when its phase change occurs [13]. Taking
advantages of high heat storage density, thermal heat storage and
release at small temperature change and easy control, PCMs
possess great potentials for various applications such as solar
energy saving, industrial waste heat recovery, building energy
saving, electronic temperature control equipment, etc.
Generally speaking, phase change materials are mainly com-
posed of organic and inorganic materials. Compared with inor-
ganic PCMs, organic PCMs have the characteristic of low corrosion;
they melt and freeze repeatedly without phase segregation that
leads to consequent degradation of their latent heat of fusion [4,5].
The organic phase change materials includes parafn waxes (or n-
alkanes), polyethylene glycols (PEGs), and fatty acids. Fatty acids
have been widely studied due to their high latent heat storage
n
Corresponding author. Tel./fax: 86 931 2973305.
E-mail address: lian2010@lut.cn (A. Li).
have low thermal conductivity, and need encapsulation in order to
prevent leakage of the melted PCM during the phase change
process. This problem is expected to be solved by storing the
PCMs into supporting materials to form form-stable PCM compo-
sites. In recent years a plenty of form-stable PCM composites have
been reported in previous literatures by incorporating PCM
immerses into porous materials, including gypsum [9], diatomite
[10], graphene aerogel [11], SiO2 [12], conjugated microporous
polymers [13] and ceramic composites [14] by means of natural
immersion approach. Therefore, preparing porous materials with a
better thermal conductivity as form-stable PCM composites should
be a signicant topic.
Graphene has recently been reported to possess unique elec-
trical, optical and thermal transport properties [1520]. The
desired thermal conductivity [18] and electrical conductivity make
graphene signicant in providing enhanced thermal and specic
surface area properties in thermal management systems [21].
Moreover porous graphene acts as superwetting coatings on a
grid, due to its hydrophobic property, good mechanical exibility
and van der Waals interactions between the graphene nanosheets
and with other substrates [22]. In this study, we coated graphene
nanosheets onto nickel foam followed by surface modication to
prepare superoleophilic graphenenickel foam as porous support-
ing material. By a simple impregnation method, various n-car-
boxylic acids can be easily absorbed into the supporting material
to form-stable composites. The prepared composites show not

http://dx.doi.org/10.1016/j.solmat.2014.09.032
0927-0248/& 2014 Elsevier B.V. All rights reserved.
426 W. Liang et al. / Solar Energy Materials & Solar Cells 132 (2015) 425430

only good thermal stability but also high latent heat, which make
them promising candidates as heat storage materials for real
application.
2. Experimental
2.1. Sample preparation
2.1.1. Preparation of superoleophilic graphenenickel foam (GNF)
We prepared graphene with chemical reduction of graphene
oxide in DMF as reported [23,24]. The resulting graphene/DMF
suspension, which was centrifuged to remove the bigger particles
and diluted with DMF, was used in the following experiments. The
commercial nickel foam substrate which was washed with acetone
and dried before using was dipped into the graphene/DMF suspen-
sion and dried at 100 1C. This process was repeated to coat the
graphene nanosheets on the substrate. Subsequently, some amount
of graphenenickel foam and a piece of polydimethylsiloxane
(PDMS) lm were placed in a sealed glass container and heated at
234 1C for 1 h. The resulting product was named as PDMSGNF.
2.1.2. Preparation of PCMs
The PDMSGNF sample which was placed on a glass container
was immersed into the molten PCM (such as PA). Due to the
superoleophilicity of PDMSGNF and capillarity, the molten PCM
was absorbed naturally into PDMSGNF. Then, the PDMSGNF/
PCM composite was dried to constant weight (90 1C, 0.07 MPa).
The results of PDMSGNF as form-stable phase change materials
composites with different n-carboxylic acids are shown in Table 1.
2.2. Analytical instrumentation
Scanning electron microscopy (SEM) images were obtained
with a eld emission gun scanning electron microscope (JSM-
6701F, JEOL, Ltd.) after coating samples with Au lm. Water
contact angle measurements for samples were performed on a
contact angle meter (DSA100, Kruss). X-ray photoelectron spectro-
scopy (XPS) analysis was performed on an ESCALAB250xi spectro-
meter (Thermon Scientic). XRD measurements were performed
on a Rigaku with a Cu tube source and scans were taken at 2 from
21 to 501. The thermal properties of microcapsule was measured
by differential scanning calorimetry (DSC, 851e, METTLER-
TOLEDO) at a heating or cooling rate of 5 1C/min in the range of
10100 1C under a argon atmosphere. The thermal conductivities
of the samples were investigated by using a thermal conductivity
testing instrument (LFA 447 Nanoash, NETZSCH).
3. Results and discussion
SEM was performed to evaluate the morphology of materials. As
seen in Fig. 1a, the treated nickel foam exhibited nano- or micro-
size along with rough surface composed of stacked layers of
graphene sheets (Fig. 1a inset). The higher-magnication image
reveals more clearly the graphene nanosheets with wrinkled sur-
face topology and folding edges on the skeleton of nickel foam
(Fig. 1b), whose intrinsic hydrophobicity is favorable to the absorp-
tion of PCM [2529]. To further improve its hydrophobic property,
modication with a low-surface-energy material such as PDMS is
necessary. The water contact angles (CA) of GNF were measured to
be 144.91 after modication with PDMS. Such strong surface
hydrophobicity makes water droplets sperial on the surface of
PDMSGNF (Fig. 1e). The diesel oil CA for the PDMSGNF samples
was found to be nearly 01, implying a strong afnity to oils. Based
on the strong surface superoleophilicity of the PDMSGNF sample,
the n-carboxylic acids such as PA, MA and SA can be easily inc-
orporated into the PDMSGNF samples to form-stable PCM com-
posites. As shown in Fig. 1c and d the pores of PDMSGNF are
homogeneously lled by PA, which illustrates that n-carboxylic
acids have been impregnated into PDMSGNF due to the effect
of superoleophilicity and the surface absorption of graphene. As
shown in Fig. 1f the melt PA (dyed with Red oil O) distributed on the
surface of a hot water bath (85 1C) is quickly and spontaneously
absorbed into the PDMSGNF, owing to both the capillary action of
its surface pores and its superoleophilicity [30,31].
In addition to superoleophilicity, these prepared graphene-
coated nickel foam samples also show excellent thermal stability.
As shown in Fig. 2, the thermal decomposition temperature for
both G-NF and PDMSGNF samples is higher than 500 1C with
weight loss 1.7% and 0.4%, respectively. The thermal stability of
PDMSGNF was better than that of the G-NF, due to the PDMS
lm as a protective layer which prevented the decomposition of
graphene. Moreover the PDMSGNF sample is totally insoluble in
any organic solvent, indicating excellent chemical stability [32,33].
These unique physicochemical properties as well as their super-
oleophilicity make the PDMSGNF samples promising candidates
as porous medium for preparation of PDMSGNF/PCMs compo-
sites, which are used for practical energy storage.
To further investigate the effect of surface chemical compositions
on the surface wettability of PDMS-treated GNF, XPS was per-
formed. As seen in Fig. 3, the pure nickel foam peaks at 854.6 eV and
531.6 eV are attributed to Ni2p, and O1s, respectively. In contrast, the
peaks of the G-NF at 856.7 eV, 532.5 eV and 285.06 eV are attributed
to Ni2p, O1s, and C1s, respectively. Furthermore, the content was
calculated to be 3.53 at% of nickel. It illustrates that the surface of
nickel foam is almost covered by graphene lm. For PDMS-treated

Table 1
The thermal properties of the n-carboxylic acids and composite PCMs.

Samples names PCM percentage Melting Freezing

(%)
Onset temperature Peak temperature Latent heat Onset temperature Peak temperature Latent heat
(1C) (1C) (kJ kg
1) (1C) (1C) (kJ kg
1)

Pure paran 100.0 50.6 58.2 130.54 54.6 52.1 135.7

PDMSGNF/paran 31.17 51.3 58.5 41.52 57.2 50.9 42.3
Pure MA 100.0 52.0 55.8 207.69 50.6 51.8 207.0
PDMSGNF/MA 49.90 54.2 59.8 102.54 53.1 47.7 103.3
Pure PA 100.0 62.4 65.2 188.00 60.8 59.1 209.1
NF/PA 17.30 62.4 65.5 34.87 60.3 58.6 36.18
G-NF/PA 43.68 62.7 68.4 86.24 60.2 55.8 91.34
PDMSGNF/PA 59.02 62.4 68.4 126.34 60.0 54.9 123.41
PDMSGNF/PA 200 54.60 62.8 69.3 113.81 60.2 54.7 114.18
cycles
Pure SA 100.0 54.1 56.7 173.07 53.2 52.0 197.8
PDMSGNF/SA 53.29 51.4 59.6 89.49 53.1 50.5 105.4
 W. Liang et al. / Solar Energy Materials & Solar Cells 132 (2015) 425430 427

Fig. 1. SEM images of G-NF (a), the graphene lms on the surface of G-NF (b), PA-PDMSGNF (c) and the structure of pores of PA-PDMSGNF (d). Scale bar: (a, c) 100 mm;
(b) 1 mm; (b inset): 100 nm and (a inset, d): 10 mm. (e) Water droplets on the surface of the PDMSGNF. (f) Camera image showing that the melt PA (dyed with Red oil O)
distributed on the surface of a hot water bath (85 1C) can be quickly and spontaneously absorbed into the PDMSGNF at 85 1C.

Fig. 2. TGA curves of G-NF and PDMSGNF. Fig. 3. XPS spectra of samples.
428 W. Liang et al. / Solar Energy Materials & Solar Cells 132 (2015) 425430
G-NF a peak at 102.5 eV is observed obviously, which is attributed to
Si2p and in good accordance with previous literatures [34], corre-
sponding to 12.6 at% silicon. That is, after PDMS treatment, the
silicon-containing moieties originating from PDMS have been suc-
cessfully deposited on the surface of as-prepared G-NF. As demon-
strated by Wanget al. [35] the SiO bond would be pyrolysed and
generated short PDMS chains some extent during the CVD process,
which would form a conformal layer and subsequently to crosslink,
resulting in the formation of a silicon coating on the surface of the as-
prepared G-NF. Thus, according to the previous study on the key
factors to obtain surface hydrophobicity and surperophilicity [36,37],
the superwetting surface of PDMS-treated G-NF should be attributed
to the low-surface-energy of the formed silicon-containing coating.
To the best of our knowledge, using hydrophobic and superoleophilic
PDMSGNF with strong afnity to PCM materials for fabrication of
PCM composites has rarely been reported.
Fig. 4 shows the XRD patterns of PA, the pure nickel foam and the
PDMSGNF/PA composite. As seen in Fig. 4b, a broad and high
intensity peak at around 44.21 was observed for nickel. Obvious and
sharp peaks at 21.721 and 24.31 are observed for PA, which is in good
agreement with previous literatures [12,38]. In the case of PDMS
GNF/PA composite both the characteristic peaks of nickel and
PA exist in the product, indicating that the PA has been incorporated
successfully into PDMSGNF/PA. The result was conrmed by SEM
(Fig. 1c and d). Furthermore, the peak position of PA does not change
in the composite. However, the intensity became lower compared
with that of pure PA. That is, the incorporation of PDMSGNF dec-
reases the crystal size of PA in the composite [12], which is similar to
the PA/SiO2 composites system [35]. The mass fraction of crystallized
n-carboxylic acids in the composites can be calculated by the
following equation in previous studies [36,38]:
HPCMs composites
wt%
Hpure PCM
where the H (PCMs composite) and H (pure PCM) are the
latent heat of the composite PCMs and pure n-carboxylic acids,
respectively. As shown in Table 1, the mass fraction of PA in the NF,
G-NF and PDMSGNF is calculated to be 17.3 wt%, 43.68 wt% and
59.02 wt%. Higher value suggests larger preservation of the
crystalline phase in the composites [15]. It can be seen from
Table 1 that PDMSGNF/PCM with better hydrophobic and sur-
peroleophilic properties can adsorb more PCMs in the composite
during the melting, which results in the bigger value for the
PDMSGNF/PCM composites.
DSC was performed to evaluate the phase change latent heat and
temperature, as shown in Fig. 5. The phase change latent heat of the
Fig. 4. XRD patterns of PA (a), the pure nickel foam (b) and the PDMSGNF/PA (c).
shape-stabilized PCMs is calculated by the area under the exothermic
peak in DSC curves and presented in Table 1. It can be seen from
Table 1 that the melting and freezing latent heat was calculated to be
respectively, 207.69 and 207 kJ kg
1 for PA, 34.87 and 36.18 kJ kg
1
for NF/PA, 86.24 and 91.34 kJ kg
1 for G-NF/PA, 126.34 and
123.41 kJ kg
1 for PDMSGNF/PA. Obviously, the latent heats of
GNF/PA are 148% and 152% higher than those of NF/PA, and the
PDMSGNF/PA possesses thermal storage 46% and 35% higher. It is
an intriguing phenomenon that the composite phase change materi-
als can greatly improve the performance of thermal storage through
simple superhydrophobic and superoleophilicity surface modica-
tion process steps. The phase latent heats increased when molten
PA was incorporated into superoleophilicity medium with higher
value for PA. The same trend was observed in PDMSGNF/PA
composite, which should be attributed to the attractive interaction
between PDMSGNF and n-carboxylic acids [38]. Furthermore, an
obvious decrease in the latent heats of PDMSGNF composites with
various n-carboxylic acids was observed with the decreasing of
value for PCMs. In PCMs composites, only the crystallized PCMs
would contribute to latent heat during the melting and freezing
processes, thus higher value means larger content of crystallized
PCMs, resulting in higher latent heat [39]. With this value, PDMSG
NF/SA could compete with that of SA based PCM composites such as
graphite oxideSA [39], SiO2SA [40], porous graphene/ceramic
composites [14] and other systems [41,42].
Moreover, from the DSC curves that the melting and freezing
temperatures of product composites were found. In addition to
FM/PA and PA with similar melting temperature the others decrease
2.94.0 1C compared with those of pure n-carboxylic acids, PA and
SA. However, PDMSGNF/parafn and parafn were closed to the
melting point. As demonstrated by Radhakrishnan et al., during the
PCMs melting process, a strong attractive interaction between uids
1 and pores surface would elevate PCMs temperature. Here, due to
the little effect of pure nickel foam on PA, the melting point of
PDMSGNF/PA remained nearly unchanged. Meanwhile parafn is
composed of different n-alkanes (18n30) without any hydrophi-
lic groups such as COOH, which shows high afnity to graphene
nanosheets, due to its intrinsic hydrophobicity. Such strong afnity
of parafn to graphene as well as better thermal conductivity of
graphene nanosheets may be responsible for the to the similar
melting temperature of PDMSGNF/parafn and parafn. Besides,
a stronger attractive interaction between uid and pores surface
resulted in decrease of freezing temperature. For example the
freezing temperature was measured to be 59.1 1C for PA, 58.6 1C
for FM/PA and 54.9 1C for PDMSGNF/PA, which decreases by
0.5 1C and 4.2 1C compared with that of pure MA (Table 1). Similar
results were observed in PA/active aluminum oxide PCM compo-
sites [43].
We also implemented leakage test by taking numerous melting/
freezing cycles of composite PCMs. For example, we have carried out
200 melting/freezing cycles of the PDMSGNF/PA between 25 1C and
80 1C. Afterwards, the thermal properties are investigated by DSC
analysis and the corresponding data is listed in Table 1. The PDMS
GNF/PA was able to retain a high melting latent heat (113.81 kJ kg
1)
after numerous melting/cooling cycles, though achieving a decre-
ase of 10% compared to that of initial PDMSGNF/PA sample
(126.34 kJ kg
1). The result suggested that no appreciable loss of
latent heat occurred during cycles. As a result, the composite PCMs
exhibited good thermal durability and stability.
To investigate the effect of the PDMSGNF supporting materials
on the thermal conductivity of the n-carboxylic acids, the thermal
conductivities of the samples were measured by using the thermal
conductivity testing instrument. The thermal conductivities of the
PCMs (MA, PA and SA) [44] and PDMSGNF/PCM composites are
listed in Table 2. The PDMSGNF/PCM composites have higher
thermal conductivities than those of the PCMs. For instance, since
 W. Liang et al. / Solar Energy Materials & Solar Cells 132 (2015) 425430 429

Fig. 5. DSC curves for heating and cooling of different n-carboxylic acids and composites. (a) Parafn and PDMSGNF/parafn. (b) MA and PDMSGNF/MA. (c) PA, NF/PA,
G-NF/PA and PDMSGNF/PA. (d) SA and PDMSGNF/SA.

Table 2 materials and PDMSGNF as porous supporting medium. Due to

The thermal conductivities of the n-carboxylic acids and composite PCMs. the porosity and excellent thermal stability as well as the unique
wettability of PDMSGNF, PCMs could be absorbed sponta-
Samples Thermal Specic heat Density Thermal
neously into PDMSGNF without leakage of PCMs loaded in the
diffusivity (J g
1 K
1) (g cm
3) conductivity
(mm2 s
1) (W m
1 K
1)
CMP samples even on heating the PDMSGNF/PCMs composite
over their melting points. Results obtained from XRD show that
Pure SA 0.092 2.200 0.848 0.172 the incorporation of PDMSGNF does not change the crystal
Pure PA 0.068 2.800 0.850 0.162 structure but lowers the crystal size of PCM in the composites. The
Pure MA 0.073 2.400 0.861 0.150
latent heat of PDMSGNF/PCM composites was measured to be in
PDMSG 1.118 1.166 1.224 1.596
NF/SA the range of 42.3123.41 kJ kg
1, which has great potentials for
PDMSG 1.626 1.205 1.154 2.262 renewable energy saving application.
NF/PA
PDMSG 1.118 1.380 1.106 1.707
NF/MA
Acknowledgment
the pores in the PDMSGNF supporting materials were lled by
the PA, the thermal conductivity of the composite This work was supported by the National Natural Science
(2.262 W m
1 K
1) at a PA loading fraction of 59.02 wt% increased Foundation of China (Grant no. 51263012, 51262019) and Gansu
about 14 times as compared with that of the PA (0.162 W m
1 K
1). Provincial Science Fund for Distinguished Young Scholars, China
This suggested that the PDMSGNF could enhance the thermal (Grant no. 1308RJDA012).
conductivities of the n-carboxylic acids. It is of great importance for
its practical industrial applications.
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4. Conclusions
Form-stable PDMSGNF/PCMs were prepared by a simple
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