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

have low thermal conductivity, and need encapsulation in order to
The increasingly serious energy crisis and continuous increase prevent leakage of the melted PCM during the phase change
in greenhouse gas emissions drive people to more effectively process. This problem is expected to be solved by storing the
utilize various sources of energy. However, most of renewable PCMs into supporting materials to form form-stable PCM compo-
resources are intermittent providers of energy due to environ- sites. In recent years a plenty of form-stable PCM composites have
mental constraints, e.g. solar energy. Therefore, efcient energy been reported in previous literatures by incorporating PCM
storage devices and systems are of critical importance to improve immerses into porous materials, including gypsum [9], diatomite
the energy efciency and reduce the gap between energy demand [10], graphene aerogel [11], SiO2 [12], conjugated microporous
and energy generation. Phase change materials (PCMs) can store polymers [13] and ceramic composites [14] by means of natural
and release latent heat when its phase change occurs [13]. Taking immersion approach. Therefore, preparing porous materials with a
advantages of high heat storage density, thermal heat storage and
better thermal conductivity as form-stable PCM composites should
release at small temperature change and easy control, PCMs
be a signicant topic.
possess great potentials for various applications such as solar
Graphene has recently been reported to possess unique elec-
energy saving, industrial waste heat recovery, building energy
trical, optical and thermal transport properties [1520]. The
saving, electronic temperature control equipment, etc.
desired thermal conductivity [18] and electrical conductivity make
Generally speaking, phase change materials are mainly com-
graphene signicant in providing enhanced thermal and specic
posed of organic and inorganic materials. Compared with inor-
surface area properties in thermal management systems [21].
ganic PCMs, organic PCMs have the characteristic of low corrosion;
Moreover porous graphene acts as superwetting coatings on a
they melt and freeze repeatedly without phase segregation that
grid, due to its hydrophobic property, good mechanical exibility
leads to consequent degradation of their latent heat of fusion [4,5].
and van der Waals interactions between the graphene nanosheets
The organic phase change materials includes parafn waxes (or n-
and with other substrates [22]. In this study, we coated graphene
alkanes), polyethylene glycols (PEGs), and fatty acids. Fatty acids
nanosheets onto nickel foam followed by surface modication to
have been widely studied due to their high latent heat storage
prepare superoleophilic graphenenickel foam as porous support-
ing material. By a simple impregnation method, various n-car-
n
Corresponding author. Tel./fax: 86 931 2973305. boxylic acids can be easily absorbed into the supporting material
E-mail address: [email protected] (A. Li). 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 3. Results and discussion
them promising candidates as heat storage materials for real
application. 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
2. Experimental graphene sheets (Fig. 1a inset). The higher-magnication image
reveals more clearly the graphene nanosheets with wrinkled sur-
2.1. Sample preparation face topology and folding edges on the skeleton of nickel foam
(Fig. 1b), whose intrinsic hydrophobicity is favorable to the absorp-
2.1.1. Preparation of superoleophilic graphenenickel foam (GNF) tion of PCM [2529]. To further improve its hydrophobic property,
We prepared graphene with chemical reduction of graphene modication with a low-surface-energy material such as PDMS is
oxide in DMF as reported [23,24]. The resulting graphene/DMF necessary. The water contact angles (CA) of GNF were measured to
suspension, which was centrifuged to remove the bigger particles be 144.91 after modication with PDMS. Such strong surface
and diluted with DMF, was used in the following experiments. The hydrophobicity makes water droplets sperial on the surface of
commercial nickel foam substrate which was washed with acetone PDMSGNF (Fig. 1e). The diesel oil CA for the PDMSGNF samples
and dried before using was dipped into the graphene/DMF suspen- was found to be nearly 01, implying a strong afnity to oils. Based
sion and dried at 100 1C. This process was repeated to coat the on the strong surface superoleophilicity of the PDMSGNF sample,
graphene nanosheets on the substrate. Subsequently, some amount the n-carboxylic acids such as PA, MA and SA can be easily inc-
of graphenenickel foam and a piece of polydimethylsiloxane orporated into the PDMSGNF samples to form-stable PCM com-
(PDMS) lm were placed in a sealed glass container and heated at posites. As shown in Fig. 1c and d the pores of PDMSGNF are
234 1C for 1 h. The resulting product was named as PDMSGNF. 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
2.1.2. Preparation of PCMs
shown in Fig. 1f the melt PA (dyed with Red oil O) distributed on the
The PDMSGNF sample which was placed on a glass container
surface of a hot water bath (85 1C) is quickly and spontaneously
was immersed into the molten PCM (such as PA). Due to the
absorbed into the PDMSGNF, owing to both the capillary action of
superoleophilicity of PDMSGNF and capillarity, the molten PCM
its surface pores and its superoleophilicity [30,31].
was absorbed naturally into PDMSGNF. Then, the PDMSGNF/
In addition to superoleophilicity, these prepared graphene-
PCM composite was dried to constant weight (90 1C, 0.07 MPa).
coated nickel foam samples also show excellent thermal stability.
The results of PDMSGNF as form-stable phase change materials
As shown in Fig. 2, the thermal decomposition temperature for
composites with different n-carboxylic acids are shown in Table 1.
both G-NF and PDMSGNF samples is higher than 500 1C with
weight loss 1.7% and 0.4%, respectively. The thermal stability of
2.2. Analytical instrumentation PDMSGNF was better than that of the G-NF, due to the PDMS
lm as a protective layer which prevented the decomposition of
Scanning electron microscopy (SEM) images were obtained graphene. Moreover the PDMSGNF sample is totally insoluble in
with a eld emission gun scanning electron microscope (JSM- any organic solvent, indicating excellent chemical stability [32,33].
6701F, JEOL, Ltd.) after coating samples with Au lm. Water These unique physicochemical properties as well as their super-
contact angle measurements for samples were performed on a oleophilicity make the PDMSGNF samples promising candidates
contact angle meter (DSA100, Kruss). X-ray photoelectron spectro- as porous medium for preparation of PDMSGNF/PCMs compo-
scopy (XPS) analysis was performed on an ESCALAB250xi spectro- sites, which are used for practical energy storage.
meter (Thermon Scientic). XRD measurements were performed To further investigate the effect of surface chemical compositions
on a Rigaku with a Cu tube source and scans were taken at 2 from on the surface wettability of PDMS-treated GNF, XPS was per-
21 to 501. The thermal properties of microcapsule was measured formed. As seen in Fig. 3, the pure nickel foam peaks at 854.6 eV and
by differential scanning calorimetry (DSC, 851e, METTLER- 531.6 eV are attributed to Ni2p, and O1s, respectively. In contrast, the
TOLEDO) at a heating or cooling rate of 5 1C/min in the range of peaks of the G-NF at 856.7 eV, 532.5 eV and 285.06 eV are attributed
10100 1C under a argon atmosphere. The thermal conductivities to Ni2p, O1s, and C1s, respectively. Furthermore, the content was
of the samples were investigated by using a thermal conductivity calculated to be 3.53 at% of nickel. It illustrates that the surface of
testing instrument (LFA 447 Nanoash, NETZSCH). 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 shape-stabilized PCMs is calculated by the area under the exothermic
Si2p and in good accordance with previous literatures [34], corre- peak in DSC curves and presented in Table 1. It can be seen from
sponding to 12.6 at% silicon. That is, after PDMS treatment, the Table 1 that the melting and freezing latent heat was calculated to be
silicon-containing moieties originating from PDMS have been suc- respectively, 207.69 and 207 kJ kg
1 for PA, 34.87 and 36.18 kJ kg
1
cessfully deposited on the surface of as-prepared G-NF. As demon- for NF/PA, 86.24 and 91.34 kJ kg
1 for G-NF/PA, 126.34 and
strated by Wanget al. [35] the SiO bond would be pyrolysed and 123.41 kJ kg
1 for PDMSGNF/PA. Obviously, the latent heats of
generated short PDMS chains some extent during the CVD process, GNF/PA are 148% and 152% higher than those of NF/PA, and the
which would form a conformal layer and subsequently to crosslink, PDMSGNF/PA possesses thermal storage 46% and 35% higher. It is
resulting in the formation of a silicon coating on the surface of the as- an intriguing phenomenon that the composite phase change materi-
prepared G-NF. Thus, according to the previous study on the key als can greatly improve the performance of thermal storage through
factors to obtain surface hydrophobicity and surperophilicity [36,37], simple superhydrophobic and superoleophilicity surface modica-
the superwetting surface of PDMS-treated G-NF should be attributed tion process steps. The phase latent heats increased when molten
to the low-surface-energy of the formed silicon-containing coating. PA was incorporated into superoleophilicity medium with higher
To the best of our knowledge, using hydrophobic and superoleophilic value for PA. The same trend was observed in PDMSGNF/PA
PDMSGNF with strong afnity to PCM materials for fabrication of composite, which should be attributed to the attractive interaction
PCM composites has rarely been reported. between PDMSGNF and n-carboxylic acids [38]. Furthermore, an
Fig. 4 shows the XRD patterns of PA, the pure nickel foam and the obvious decrease in the latent heats of PDMSGNF composites with
PDMSGNF/PA composite. As seen in Fig. 4b, a broad and high various n-carboxylic acids was observed with the decreasing of
intensity peak at around 44.21 was observed for nickel. Obvious and value for PCMs. In PCMs composites, only the crystallized PCMs
sharp peaks at 21.721 and 24.31 are observed for PA, which is in good would contribute to latent heat during the melting and freezing
agreement with previous literatures [12,38]. In the case of PDMS processes, thus higher value means larger content of crystallized
GNF/PA composite both the characteristic peaks of nickel and PCMs, resulting in higher latent heat [39]. With this value, PDMSG
PA exist in the product, indicating that the PA has been incorporated NF/SA could compete with that of SA based PCM composites such as
successfully into PDMSGNF/PA. The result was conrmed by SEM graphite oxideSA [39], SiO2SA [40], porous graphene/ceramic
(Fig. 1c and d). Furthermore, the peak position of PA does not change composites [14] and other systems [41,42].
in the composite. However, the intensity became lower compared Moreover, from the DSC curves that the melting and freezing
with that of pure PA. That is, the incorporation of PDMSGNF dec- temperatures of product composites were found. In addition to
reases the crystal size of PA in the composite [12], which is similar to FM/PA and PA with similar melting temperature the others decrease
the PA/SiO2 composites system [35]. The mass fraction of crystallized 2.94.0 1C compared with those of pure n-carboxylic acids, PA and
n-carboxylic acids in the composites can be calculated by the SA. However, PDMSGNF/parafn and parafn were closed to the
following equation in previous studies [36,38]: melting point. As demonstrated by Radhakrishnan et al., during the
PCMs melting process, a strong attractive interaction between uids
HPCMs composites
wt% 1 and pores surface would elevate PCMs temperature. Here, due to
Hpure PCM the little effect of pure nickel foam on PA, the melting point of
where the H (PCMs composite) and H (pure PCM) are the PDMSGNF/PA remained nearly unchanged. Meanwhile parafn is
latent heat of the composite PCMs and pure n-carboxylic acids, composed of different n-alkanes (18n30) without any hydrophi-
respectively. As shown in Table 1, the mass fraction of PA in the NF, lic groups such as COOH, which shows high afnity to graphene
G-NF and PDMSGNF is calculated to be 17.3 wt%, 43.68 wt% and nanosheets, due to its intrinsic hydrophobicity. Such strong afnity
59.02 wt%. Higher value suggests larger preservation of the of parafn to graphene as well as better thermal conductivity of
crystalline phase in the composites [15]. It can be seen from graphene nanosheets may be responsible for the to the similar
Table 1 that PDMSGNF/PCM with better hydrophobic and sur- melting temperature of PDMSGNF/parafn and parafn. Besides,
peroleophilic properties can adsorb more PCMs in the composite a stronger attractive interaction between uid and pores surface
during the melting, which results in the bigger value for the resulted in decrease of freezing temperature. For example the
PDMSGNF/PCM composites. freezing temperature was measured to be 59.1 1C for PA, 58.6 1C
DSC was performed to evaluate the phase change latent heat and for FM/PA and 54.9 1C for PDMSGNF/PA, which decreases by
temperature, as shown in Fig. 5. The phase change latent heat of the 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
Fig. 4. XRD patterns of PA (a), the pure nickel foam (b) and the PDMSGNF/PA (c). 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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