Thermochimica Acta 587 (2014) 5258

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Thermochimica Acta
journal homepage: www.elsevier.com/locate/tca

Preparation, characterization and thermal properties of binary nitrate

salts/expanded graphite as composite phase change material
Junbing Xiao a , Jin Huang a, , Panpan Zhu a , Changhong Wang a , Xinxi Li a,b
a

School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou, PR China
Center for Nanochemistry, Beijing National Laboratory for Molecular Sciences, State Key Laboratory for Structural Chemistry of Unstable and Stable
Species, College of Chemistry and Molecular Engineering, Peking University, Beijing, PR China
b

a r t i c l e

i n f o

Article history:
Received 1 March 2014
Received in revised form 18 April 2014
Accepted 22 April 2014
Available online 29 April 2014
Keywords:
Binary nitrate salt
Expanded graphite
Ultrasonic
Thermal energy storage
Latent heat

a b s t r a c t
The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were prepared
via adding different mass rate of EG to binary nitrate salts consisting of NaNO3 and KNO3 (6:4) by aqueous
solution method adopting ultrasonic. The morphology and chemical composition of EG and the composite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM),
energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser thermal conductivity instrument and differential scanning calorimeter (DSC) were employed to measure
thermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermal
conductivity coefcient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly
11.0%. The morphology and phase structure results indicated that EG were well dispersed into and physically combined with molten salts. In general, the prepared composite PCM could be a suitable phase
change material for thermal energy storage.
2014 Elsevier B.V. All rights reserved.

1. Introduction
Since serious shortage of energy resource and tremendous
requirement for renewable energy, phase change material (PCM)
with advantageous thermal properties has been applied to satisfy
the increasing demand [15]. Depending on the characteristics of
high latent heat, high specic heat and high thermal conductivity
and so on [6,7], PCM has played an important role in various elds
extensively [810].
In recent decades, several inorganic PCM and their mixtures
have been investigated for thermal energy storage [1113]. Due
to its better thermal properties, molten salts were usually used as
direct heat transfer medium in industrial applications [1416]. Various nitrate salts and their composite have attracted tremendous
researchers concern. The mixtures consisting of KNO3 , LiNO3 and
Ca(NO3 )2 with excellent thermal properties were proved to be a
promising PCM [17]. Iverson et al. [18] concluded that temperature
did not have a signicant effect on mechanical properties through

Corresponding author at: B58 100 West Waihuan Road, Guangzhou Higher Education Mega Center, 510006 Guangzhou, PR China. Tel.: +86 020 39322715;
fax: +86 020 39322715.
E-mail address: huangjiner@126.com (J. Huang).
http://dx.doi.org/10.1016/j.tca.2014.04.021
0040-6031/ 2014 Elsevier B.V. All rights reserved.

analyzing the thermal and mechanical properties of several nitrate

salts in common use.
Recently, researches have focused on improving the thermo
physical properties of heat transfer and energy storage medium.
The usage of different additives is a usual method to obtain better heat efciency of molten salts. A kind of inorganic compound
with the chlorides has given a rise to the thermal conductivities
of multi-component molten salts composed of potassium nitrate,
sodium nitrite and sodium nitrate [19].
According to the excellent thermal and mechanical properties, graphite and EG have been particularly chosen for improving
thermal conductivity of conventional PCM. Rao et al. [20] had
prepared parafn/graphite composite phase change materials and
demonstrated that the total latent heat value decreased as the
increasing mass rate of graphite. EG/parafn nanocomposites
were obtained by dispersing EG into parafn via intensive ultrasonic irradiation without dispersants. Owing to the distinctive
thermal properties of EG, the thermal conductivity of composite increased to 1.04 times higher than that of pure parafn
[21]. Kim et al. [22] had prepared the parafn/xGnP composite
PCM by stirring xGnP in liquid parafn. An almost linear relationship was concluded between thermal conductivity and mass
fraction of xGnP. Meanwhile, EG have gained spread application
in parafn [23,24] and other organics [25,26] for energy storage
systems.

J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

As EG has beneted the organic on thermal properties, great

efforts have been spent on the mixture of EG and inorganic. Martin
et al. [27] had prepared the binary salt consisting of 70 wt.% NaNO3
and 30 wt.% KNO3 and demonstrated that the melting temperature ranged from 223 C to 262 C and the enthalpy was about
118 2 kJ/kg. At room temperature, the apparent conductivities
of KNO3 /NaNO3 -graphite made by cold-compression were up to
20 W/(m K), which was 20 times higher than that of binary salts
[28,29]. Xiao et al. [30] had reported that the usage of EG to nitrates
had a improvement on thermal conductivity by about 3040% and
a reduction on latent heat per mass mixture by nearly 518%.
In present paper, we report a simple and convenient method to
prepare the nitrate salts/EG composite PCM by solution method
with ultrasonic, different from the conventional preparation
method. The binary nitrate salts were prepared by statically heating NaNO3 and KNO3 at mass ratio of 6:4 to completely melt. The
ultrasonic had played a role of breaking EG into nanoscale slices
and dispersing them into nitrates. The physical combined composite PCM was proved to have excellent latent heat and high thermal
conductivity.
2. Experimental
2.1. Materials
Potassium nitrate and sodium nitrate were obtained from samples with A.R. grade and no further purication. Deionized water
and graphite intercalation compounds [31] were self-restraint.

53

conductivity of binary nitrate salts and binary nitrate salts/EG composite PCM was measured by employing a laser heat conductive
instrument (Germany, NETZSCH, LFA 447) at room temperature.
The phase change temperature and latent heat of the nitrates and
nitrates/EG composite PCM were both measured by differential
scanning calorimetry (DSC; DSC-204, NETZSCH, Germany) under
a nitrogen atmosphere. The data were collected with a scan rate of
10 C min1 from room temperature to 260 C.
3. Results and discussion
3.1. Stripped graphite akes
The morphologies of EG and SGFs were observed by SEM as
shown in Fig. 1. As can be seen from Fig. 1a, EG has a 3D wormlike architecture within size of 150 m. The high-magnication
SEM photograph (Fig. 1b) of SGFs shows that EG altered to slices
in nanoscale after the ultrasonic.
The TEM photographs of SGFs from different angles were shown
in Fig. 2. As represented in Fig. 2a, SGFs were at and semitransparent slices with some wrinkles and folds. It could be observed
that its dimension was between 8 and 25 nm which corresponded
to observation of SEM photograph in Fig. 1b. As observed in Fig. 2b,
the folds with lamellar structure were slices as given in Fig. 1b.
The phase structure of EG and SGFs were characterized by XRD
as shown in Fig. 3. The sharp and intensive diffraction peaks at 26.3 ,
56.0 correspond to EG and SGFs, respectively. A third diffraction
peak of SGFs at 45.0 appeared particularly because ultrasonic made
structure of graphite ake into disorder.

2.2. Preparation
After being dried at 100 C, graphite intercalation compounds
were expanded through a rapid heating in microwave ovens as
reported in our previous work [31]. The expanded graphite was
prepared while the bright ame was out.
Potassium nitrate and sodium nitrate were put into an air oven
and dried at 120 C for 24 h respectively and then mixed at the mass
ratio of 6:4 uniformly. A mixture of binary nitrates salts was placed
into a crucible and then heated at 350 C for 30 min statically in
order to melt completely. Afterwards, the crucible was gradually
cooled down to room temperature. The molten salts were obtained.
Grinding the molten salts slowly and dissolved it in a breaker by
deionized water gradually. Then, EG was added into the previous
solution slowly under continuous stirring at different mass rate.
After the EG soaking into the solution, the solution was stirred by
the strong ultrasonic homogeneous instrument (SCIENTZ-IID) with
a power of 800 W for 1.0 h. Then, the breaker was put into a drying
oven and dried at 100 C for 24 h. By grinding the dried composite PCM, sample was obtained. Before drying of the solutions, one
was ltered and washed using deionized water until the stripped
graphite akes (SGFs) were enough visible. SGFs were obtained
after drying as mentioned.
2.3. Characterization and determination of thermal properties
X-ray diffraction (XRD; DMAX-Ultima IV, Rigaku Corporation,
Japan) was employed to identify the microstructure and chemical
composition of EG, SFGs and the composite PCM. The morphology and chemical composition of composite PCM were investigated
by scan electron microscope (SEM; S3400N, Hitachi, Japan) with
an energy dispersive X-ray spectroscopy detector, eld emission
scanning electron microscopy (FE-SEM; S-4800, Hitachi, Japan)
(EDS; EX-250, HORIBA, Japan) at room temperature. The morphology of SGFs was investigated with a high resolution transmission
electron microscope (HRTEM; JEM-2010HR, Jeol, Japan). Thermal

3.2. The composite PCM

The SEM images of binary molten salts and composite PCM samples were shown in Fig. 4. As shown in Fig. 4a, the NaNO3 KNO3
eutectic crystal was gray milky substance which looked like smooth
block. The images in Fig. 4be correspond to samples with EG
at mass rates of 0.5, 1.0, 1.5, 2.0%, respectively. Judging from the
images, we might draw the conclusion that SGFs were well dispersed in eutectic crystal with foliated and angular structure.
The phase structure of molten salts and composite PCM samples were characterized by XRD at room temperature as shown
in Fig. 5. The peaks at 26.3 , 56.0 correspond to SGFs. However,
the weak feature peak of SGFs centered at 45.0 completely disappears after the composite PCM composed. The peaks at 23.0 , 28.5 ,
38.0 correspond to potassium nitrate and the peaks at 31.5 , 46.0 ,
47.5 correspond to sodium nitrate, respectively. Obviously, potassium nitrate and sodium nitrate were the main crystal phases as
identied in Fig. 5(a). Further, the position of peaks was without
excursion which proved that the phase structure of nitrate crystal were no chemical reaction. Due to the little additive of EG, its
presentation was unobvious in the composite PCM.
The chemical composition of the prepared composite PCM was
further determined by EDX analysis attached to the SEM. The EDX
spectrum (Fig. 6b and c) sustains that the composite PCM (Fig. 6a)
consists of C, N, O, Na and K elements. The strong N, O, Na and
K signal originates from binary nitrates, while the C signal comes
from the EG. Whats more, the difference of percentage content of
C in the two samples (Fig. 6b and c) was caused by mutual interference of C and K element belonging to low atomic sequence and the
little quality of test samples, etc. According to the above analysis,
it is unambiguously demonstrated that EG had been successfully
combined into binary nitrate crystal.
The images of map scanning in Fig. 7bf correspond to C, N,
K, Na, and O elements attached to the SEM (Fig. 7a), respectively.
The dispersion of every element in samples could be easily judged.

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J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

Fig. 1. Scanning electron microphotographs of (a) EG and (b) SGFs by coating condition at room temperature.

Fig. 2. Transmission electron microscope of SGFs from different angles at room temperature.

The white spots presented homogeneous distribution of C element

in Fig. 7b and a white reunion was found in top-right corner. The
reunion was formed because mutual interference between the light
elements, the little quantity of measured samples and the inuence
of different area, etc.
The specic heat, thermal diffusivity and thermal conductivity
coefcient of composite PCM have had variations under the effect
of SGFs. These parameters of the PCM samples have been measured at room temperature as listed in Table 1. As the increasing

addition of EG, it could be seen that specic heat increased rst

sharply and then slowly, however, thermal diffusivity and thermal conductivity coefcient increased almost linearly. As shown in
Table 1, the specic heat of sample with 2.0 wt.% EG is 2.600 J/(g K),
thermal diffusivity is 0.930 mm2 /s, thermal conductivity coefcient
is 4.884 W/(m K), which correspond to 1.11 times, 1.95 times, 2.15
times than that of binary molten salts. The results proved that EG
had great contribution to thermal conductivity coefcient of binary
molten salts which was in accord with the report in Xiaos paper

Fig. 3. X-ray diffraction pattern obtained for EG and SGFs at room temperature.

J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

55

Fig. 4. The SEM images of binary molten salt and composite PCM samples at room temperature.

Table 1
The specic heat, thermal diffusivity and thermal conductivity coefcient of
samples.
No.

EG (wt.%)

Specic heat
J/(g K)

Thermal diffusivity
(mm2 /s)

Thermal conductivity
coefcient W/(m K)

1
2
3
4
5

0
0.5
1
1.5
2

2.351
2.485
2.586
2.593
2.6

0.477
0.573
0.639
0.791
0.93

2.27201
2.876
3.338
4.143
4.884

[30]. The enhancement of thermal conductivity coefcient could be

explained as following:
(1) According to the formula:  = c,  represents thermal
conductivity coefcient, represents thermal diffusivity,  represents density, c represents specic heat. Due to the close
density of graphite and binary molten salts and the little

addition of EG, the impact of density on thermal conductivity

coefcient could be ignored.
(2) During the preparation, SGFs were well dispersed into binary
molten salts after ultrasonic. As molten salts crystallizing, there
is certain crystallizing pressure which excludes SGFs to the
grain boundary surface. Then the very complex meshes are
formed by graphite slices which couple with molten salts. As
a result of its distinct thermal properties, the graphite is equivalent to small high conductive transport channels for heat
conduction and also overcome the interface thermal resistance
to a certain extent. Consequently, thermal conductivity coefcient of the composite PCM is improved signicantly.
As to the phase change characteristics, the phase transition temperature and latent heat were measured by DSC. The DSC curves of
binary molten salt and composite PCM samples at room temperature were presented in Fig. 8. The peak temperatures, latent heat
and other parameters were listed in Table 2. It should be noted

Fig. 5. X-ray diffraction pattern obtained for binary molten salt and composite PCM at room temperature.

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J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

Fig. 6. The X-ray energy spectrum curves of a composite PCM sample.

Fig. 7. Map scanning of a composite PCM sample.

Table 2
The parameters of phase change temperature and latent heat of samples.
No.

EG (wt.%)

Solidsolid phase change

1
2
3
4
5

0
0.5
1
1.5
2

Solidliquid phase change

Total latent heat (J/g)

Peak temperature ( C)

Latent heat (J/g)

Peak temperature ( C)

Latent heat (J/g)

130.6
130.1
130.4
130.0
130.2

17.26
19.95
18.69
18.71
17.51

223.2
225.6
224.8
224.7
225.3

142.2
128.7
128.4
128.1
124.4

159.46
148.65
147.09
146.81
141.91

J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

57

the increasing mass rate of EG, it could be seen that specic heat
increased rst sharply and then slowly, however, thermal diffusivity and thermal conductivity coefcient increased almost linearly.
It can be indicated that EG have given a great rise to thermal
conductivity coefcient which largely increased to 4.884 W/(m K)
and a nearly 11.0% reduction to latent heat. During the tests, we
can conclude that the melting curves contain two phase change:
solidsolid phase change and solidliquid phase change. The
uctuation of phase transition temperatures was very insignicant
and the total latent heat of composite PCM had a reduction about
6.7811.01%. In general, the nitrate salts/EG composite PCM
is suitable for heat transfer and thermal energy storage as EG
enhanced the thermal conductivity of binary nitrate salts.
Acknowledgements

Fig. 8. DSC curves of binary molten salt and composite PCM samples.

that every curve had two transformation peaks and the peaks were
matched nearly at same temperatures. These results nearly correspond to the DSC proles of the mixture of NaNO3 and KNO3 [32].
Concluding from the analysis of XRD and SEM, the peak at about
130.4 C was formed by solid-solid phase change and the peak at
about 224.8 C was formed by solidliquid phase change.
The uctuation of phase transition temperatures was very
insignicant and reduction on the total latent heat of composite
PCM (PTLH) was slight, as compared to binary molten salt correspondingly. The reduction on the total latent heat of composite
PCM (PTLH) was calculated by comparing to the total latent heat of
binary molten salt (BTLH). A non-dimensional parameter formulated as Eq. (1) was used for presenting the reduction percentage
on the total latent heat of composite PCM to binary molten salt.
=

(BTLH PTLH)
BTLH

(1)

It can be drawn from Table 2 that reduction percentage on

the total latent heat was about 6.7811.01%. According to Table 2,
it could also be known that the solidsolid phase change which
accounted for about 10% total latent heat had the relatively small
variations and the solidliquid phase change had a major contribution to total latent heat. The total latent heat of binary molten salt
sample has obvious difference with that of composite PCM samples, but results of composite PCM samples have similar latent heat.
This phenomenon could be explained that the addition of EG has
reduced the mass rate of binary molten salt without contribution
total latent heat and inuenced PTLH little by the same pattern.
The results of our samples had no difference to that in previous
researches [2730]. From what has been discussed above, it could
come to a conclusion that EG had little inuence on phase transition
and total latent heat of the composite PCM.
4. Conclusion
Based on the above results, the nitrate salts/EG composite PCM
shows an excellent thermo physical performance as a heat transfer
and energy storage material. The composite PCM was prepared via
adding different mass rate of EG to binary nitrate salts consisting
of NaNO3 and KNO3 (6:4) by aqueous solution method adopting
ultrasonic.
The investigated morphology and thermo physical properties
showed SGFs were well dispersed and homogeneous distributed
in eutectic crystal with no chemical reaction after ultrasonic. As

The authors would like to express their sincere thanks to the

nancial support from the National Natural Science Foundation of
China (Grant no. 51006024), the Special Funding of Combination
of Production, Teaching and Research of Guangdong Provincial and
National Ministry of Education (Grant no. 2011B090400446), the
Special Funding of discipline construction of Guangdong Province
(Grant no. 2012KJCX0041), and the Special Funding of applied basic
research of Guangzhou City (Grant no. 2013J4100010).
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