International Journal of Heat and Mass Transfer 156 (2020) 119789

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International Journal of Heat and Mass Transfer

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

Investigation of heat capacity and viscosity enhancements of binary

carbonate salt mixture with SiO2 nanoparticles
Baha El Far, Syed Muhammad Mujtaba Rizvi, Yousof Nayfeh, Donghyun Shin∗
School of Engineering & Technology, Central Michigan University, Mt Pleasant MI 48859, United States

a r t i c l e i n f o a b s t r a c t

Article history: A binary carbonate salt mixture (Li2 CO3 -K2 CO3 at 62:38 molar ratio) was doped with SiO2 spherical
Received 24 January 2020 nanoparticles at 1% concentration by weight. A differential calorimeter and a rheometer were used to
Revised 25 March 2020
study the thermal and rheological characteristics of the binary carbonate salt mixture & its nanofluids
Accepted 9 April 2020
mixed with SiO2 nanoparticles. The results showed that the viscosity was enhanced by 34.0–94.4% and
the heat capacity was enhanced by 19%. Furthermore, the nanofluids showed significant non-Newtonian
Keywords: behavior (shear-thinning). Nanofluids are known to show non-Newtonian behavior when nanoparticles
Molten salt have a high aspect ratio (e.g., rod-like structure, nanotube, etc.) at high concentrations. Literature study
Nanofluid showed salt mixture can be micro-segregated near a nanoparticle. The segregated salts can crystallize
Heat capacity
on the nanoparticle surface and grow further to form dendritic nanostructures. To verify the nanostruc-
Viscosity
tural change, we added a minute concentration of hydroxide (0.03 wt.%) into a nanofluid to disrupt the
Shear-thinning
nanostructural change and measured their properties as reported in the literature. The result showed
that the heat capacity enhancement decreased from 19% to 9%. Also, the viscosity decreased from 34.0%
to 8.4% (at the highest shear rate) and 94.4% to 62.8% (at the lowest shear rate), respectively. Moreover,
the theoretical viscosity model predicted well at the highest shear rate (250/s), where the effect of the
nanostructural change is minimal, while it failed to predict the viscosity enhancement at a low shear
rate, where the nanostructural change is expected to dominate the flow. Our experimental results sup-
port that the dendritic salt nanostructures are primarily responsible for increasing both heat capacity and
the shear-thinning behavior of molten salt nanofluids.
© 2020 Elsevier Ltd. All rights reserved.

1. Introduction
Nanofluids are liquids doped with nanometer-sized particles.
Nanofluids are known for their enhanced thermal properties at
minute concentrations [1]. Since Choi [2] reported the first demon-
stration of thermal conductivity enhancement of a nanofluid, sev-
eral experimental results were published for enhanced thermal
conductivity values of nanoparticle dispersions in water, oil, ethy-
lene glycol, & their mixtures [1]. On the other hand, the heat ca-
pacity of nanofluids has shown controversial results. Most con-
ventional nanofluids, such as water, oil, or ethylene glycol-based
nanofluids showed a decrease of heat capacity with nanoparticles
[3]. Molten salt-based nanofluids showed an increase in heat ca-
pacity with nanoparticles [4–8]. Several models were proposed to
explain the enhanced heat capacity of molten salt-based nanoflu-
ids. They are (1) Increased heat capacity by nanoparticles than
their bulk, (2) interfacial thermal resistance as secondary heat stor-
age, & (3) dense layering of molten salt molecules around nanopar-
ticles [9]. However, these models could not explain why the en-
hancement in heat capacity is only observed in molten salt-based
nanofluids but other conventional nanofluids.
Recent studies have focused on a dendritic formation of sepa-
rated salt compounds due to nanoparticles [10,11]. Molten salts are
generally binary/ternary salt mixtures. When a nanoparticle is in-
troduced into such salt mixtures, salt compounds can be micro-
segregated (due to a difference in electrostatic interactions be-
tween each salt and nanoparticles). These micro-segregated salts
can grow on the surface of nanoparticles like dendritic forma-
tions. Hence, it was proposed that the effective specific heat model
should be modified to consider of the effect of such nano-dendritic
structure formed by salts as follows (Eq. (2) [10]):
mnp c p,np + m f c p,b f
c p,n f = (1)
mnp + mb f

 
∗ mnp c p,np + mns c p,ns + mb f − mns c p,b f
Corresponding author. c p,n f = (2)
E-mail address: shin1d@cmich.edu (D. Shin). mnp + mb f

https://doi.org/10.1016/j.ijheatmasstransfer.2020.119789
0017-9310/© 2020 Elsevier Ltd. All rights reserved.
2 B.E. Far, S.M.M. Rizvi and Y. Nayfeh et al. / International Journal of Heat and Mass Transfer 156 (2020) 119789

where m & cp are mass and heat capacity. Subscripts nf, bf, np, & ns hydroxide (0.03% by weight) into a nanofluid to disrupt the for-
denote nanofluid, base fluid, nanoparticle, & nanostructure, respec- mation of the dendritic nanostructures. We characterized the heat
tively. However, there are not enough experimental results avail- capacity and the viscosity of the nanofluids before and after NaOH
able to support the claim. The working temperature of such molten is added to confirm the effect of the nanostructures on the effec-
salt-based nanofluids is too high to visualize the formation of the tive heat capacity and the viscosity. This verification process was
salt dendritic nanostructures. Hence, it is necessary to find another necessary because there is no experimental tool that can visually
way to study the underlying mechanism behind the enhancement observe the formation of such dendritic nanostructure directly at
in the specific heat of molten salt-based nanofluids. the working temperature, which is beyond the melting point of the
In this study, we investigate the effective specific heat and the pure salt (490°C [12]). All sample preparations and experiments by
rheology of salt dendritic nanostructures. We apply a reported TGA, DSC, and rheometer took place inside a cleanroom environ-
technique to molten salt-based nanofluids to interrupt the forma- ment to prevent possible contamination by airborne particles.
tion of the salt dendritic nanostructures. We characterize the spe-
cific heat and the rheology of several molten salt-based nanofluids 3. Results and discussion
before and after the salt dendritic nanostructures are interrupted.
If the salt dendritic nanostructures are primarily responsible for To show the size distribution of SiO2 nanoparticles, a photon
the enhanced specific heat, the specific heat should be enhanced correlation spectroscopy (N4 PLUS Particle Size Analyzer, Beckman
first and then decreased after the structures are disturbed. More- Coulter) was conducted. The average size is 15.2 nm with a stan-
over, the presence of the salt dendritic nanostructures should af- dard deviation of 7.5 nm. To confirm the measurement reliability,
fect the rheologic behavior of the molten salt-based nanofluids. A we prepared 3 samples of Li2 CO3 - K2 CO3 on different days and
molten binary carbonate salt and its mixture with SiO2 nanoparti- tested in the DSC for their heat capacity (Fig. 1 and Table 1). The
cles were characterized in a differential scanning calorimeter (DSC average heat capacity value of the 3 samples was 1.51 kJ/kg °C
25, TA Instruments) and a rheometer (DHR-2, TA Instruments) to at 540°C. The literature value is 1.6 kJ/kg °C [12] and the error
characterize the specific heat and the rheology. A simple technique was only 5.6%. To confirm the reported enhancement of the heat
following the literature was employed to disturb the formation of capacity of Li2 CO3 -K2 CO3 doped with SiO2 nanoparticles (1 wt.%)
the salt dendritic nanostructures. The specific heat and the rheol- [5], we prepared 3 samples on different days and tested in the
ogy of the molten salt and its nanofluid were characterized before DSC. The average heat capacity was measured to be 1.79 kJ/kg
and after the technique was applied to evaluate the effect of the °C at 540°C with a standard deviation of 0.086 kJ/kg °C. The en-
salt dendritic nanostructures. hancement of the heat capacity over the pure Li2 CO3 -K2 CO3 was
18.5% and the calculated standard error of the mean was less than
2. Methods 5%. Then, we followed the reported technique [11] to verify the
effect of dendritic nanostructures on the effective heat capacity.
Li2 CO3 & K2 CO3 were procured by Fisher Chemical & SiO2 We added a small amount of NaOH (0.03 wt%) to disrupt the
nanoparticles were procured by Meliorum Technologies. The nom-
inal size of the nanoparticles from the manufacturer is 10
nanometers. To synthesize a binary carbonate salt mixture, Li2 CO3
(921.1 mg) & K2 CO3 (1058.8 mg) were dried and precisely weighted
by a microbalance (SECURA 225D, Sartorius) and mixed. Then, the
mixture was dissolved in 100 ml of distilled water with 20.0 mg of
SiO2 nanoparticles. The solution was ultra-sonicated for two hours
in a sonication bath (Branson 5200 ultrasonic cleaner, Branson Ul-
trasonics) to ensure homogeneous dispersion of nanoparticles. The
solution was poured into a petri dish (100 mm × 20 mm) on a
hot plate, which was maintained at 200°C for about 5 h to dry
the sample completely. The sample was characterized by thermo-
gravimetric analysis (TGA 55, TA Instruments) to ensure no mois-
ture was present. Heat capacity was characterized by a differential
scanning calorimeter (DSC 25, TA Instruments) using modulated
differential scanning calorimetry (MDSC) technique at a ramping
heating rate of 2 C°/minute. When preparing a sample for the heat
capacity measurement, the mass of each sample was kept in a
range of ~8–12 mg to minimize any effect of weight variations.
Humidity was maintained below 20%. Three samples were synthe-
sized and tested on different days to ensure the repeatability and Fig. 1. The DSC experiments show that the heat capacity was enhanced by 18.5%
with SiO2 nanoparticles (1 wt%) and the enhancement diminished with the addition
reliability of the measurement. The DSC signal was monitored for
of NaOH (0.03 wt%) at 540°C. The error bars show the minimum and maximum
each sample to ensure there was no endothermic or exothermic values.
reaction. A hybrid rheometer incorporated with an environmental
test chamber (Discovery DHR-2, TA Instruments) was employed to Table 1
study the rheological behavior of each sample. Parallel plates ge- Specific heat measurement results at 540°C.
ometry (25 mm in diameter) was installed to house each sample Pure salt Li2 CO3 -K2 CO3 + Li2 CO3 -K2 CO3 +
with a gap of 0.5 mm. All the measurements took place at a con- (Li2 CO3 - K2 CO3 ) SiO2 (1%) SiO2 (1%)+NaOH(0.03%)
stant temperature of 540°C. Three samples of the pure salt and Sample 1 1.48 1.88 1.62
its nanofluid were synthesized and characterized in the rheome- Sample 2 1.51 1.77 1.65
ter on different days to ensure the repeatability and reliability of Sample 3 1.53 1.71 1.66
the measurement. To study the effect of the salt dendritic nanos- Average 1.51 1.79 1.64
Enhancement – 19% 9%
tructure formed reported in the literature [10,11], we followed the Standard error 2% 5% 1%
reported technique [11] to add a minute concentration of sodium
 B.E. Far, S.M.M. Rizvi and Y. Nayfeh et al. / International Journal of Heat and Mass Transfer 156 (2020) 119789 3

investigation. Future work should be to study the properties of the

Fig. 2. Average viscosity values of Li2 CO3 -K2 CO3 , Li2 CO3 -K2 CO3 +SiO2 (1wt%), and
Li2 CO3 K2 CO3 +SiO2 (1%)+NaOH(0.03%) with shear rates.
formation of the reported dendritic nanostructures and, as a re-
sult, hinder the enhanced heat capacity shown in the nanofluids.
The amount of NaOH was expected to small enough not to affect
the heat capacity and the DSC signal was monitored to check any
unknown chemical reaction. No endothermic or exothermic peak
was observed. Three samples of Li2 CO3 -K2 CO3 -SiO2 (1 wt%)-NaOH
(0.03 wt%) were tested in the DSC. The result shows the average
heat capacity decreased from 1.79 kJ/kg °C to 1.64 kJ/kg °C. It im-
plies that the addition of NaOH might change the local chemistry
between nanoparticles and surrounding salt molecules and disrupt
the formation of most dendritic nanostructures which are known
for the reason behind the reported heat capacity enhancement
[10,11]. The prediction by Eq. (1) is 1.50 kJ/kg °C, which is slightly
lower than the heat capacity of the pure salt because the nanopar-
ticle heat capacity is lower than the heat capacity of the pure salt.
Moreover, the concentration of the nanoparticles is small (1% by
weight) and, therefore, the decrease of the heat capacity is small.
On the other hand, Eq. (2) accounts for the effect of the formation
of salt dendritic nanostructures; therefore, it is expected to bet-
ter predict the heat capacity of the nanofluids. However, the exact
heat capacity of such dendritic nanostructures is unknown and the
amount of the dendritic formation in the nanofluids is still under
dendritic nanostructures that will help develop an accurate model
to predict the heat capacity.
The heat capacity measurements with/without the addition of
NaOH support that the reported enhanced heat capacity might
be due to the effect of the salt dendritic nanostructures. How-
ever, there was no direct tool to visually characterize the forma-
tion of the dendritic nanostructures since Li2 CO3 -K2 CO3 is crys-
tallized at 490°C [12]. Hence, we employed a rheometer to con-
firm the effect of the salt dendritic nanostructures on the rheol-
ogy of Li2 CO3 -K2 CO3 . Three samples of pure Li2 CO3 -K2 CO3 , three
samples of Li2 CO3 -K2 CO3 doped with SiO2 nanoparticles at 1 wt.%
concentration, and three samples of Li2 CO3 -K2 CO3 doped with SiO2
nanoparticles at 1 wt.% & NaOH at 0.03 wt.% concentrations in the
same manner as reported in the literature [11]. Each sample was
repeated three times in the rheometer (DHR-2, TA Instruments) to
confirm the repeatability of the measurement. The rheological be-
havior of the samples is shown in Fig. 2 as a function of shear
rate and tabled in Table 2 for a range of shear rates from 28/s
to 250/s. The average viscosity of the three samples of Li2 CO3 -
K2 CO3 was 20.5 cP with a standard deviation of 0.43 cP. The mea-
sured viscosity was very consistent with samples and was inde-
pendent of the shear rate (i.e., Newtonian behavior). The literature
value was 14 cP [13] and the discrepancy between our measure-
ment and the literature could be due to the high measurement
temperature (over 500°C). While the pure Li2 CO3 -K2 CO3 showed
Newtonian behavior, the Li2 CO3 -K2 CO3 +SiO2 (1 wt.%) showed a
significant non-Newtonian behavior (i.e., shear-thinning). The av-
erage viscosity of the nanofluids at a low shear rate (28 /s) was
41.8 /s, which is 94.4% increased viscosity than the pure Li2 CO3 -
K2 CO3 . On the other hand, at a high shear rate (250 /s), the av-
erage viscosity of the nanofluids was 28.8 /s, which is 34.0% in-
creased viscosity than the pure Li2 CO3 -K2 CO3 . Then, we followed
the reported technique [11] to verify the effect of dendritic nanos-
tructures on the effective viscosity, we added a small amount of
NaOH (0.03 wt%) to disrupt the formation of the dendritic nanos-
tructures and therefore it was expected to diminish the increased
viscosity of the nanofluids. The result shows the average viscos-
ity at a low shear rate (28/s) was 35.0/s, which is 62.8% increased
viscosity. The average viscosity at a high shear rate (250/s) was
23.3/s, which is 8.4% increased viscosity. The increase of the vis-
cosity went down from 94.4% to 62.8% at low shear rate (28/s) and
from 34.0% to 8.4% at high shear rate (250/s). We have performed

Table 2
The average viscosity values of Li2 CO3 -K2 CO3 , Li2 CO3 -K2 CO3 +SiO2 (1wt%), and Li2 CO3 K2 CO3 +SiO2 (1%)+NaOH(0.03%) at a range of shear rates from 28/s to 250/s and the
predictions by Eq. (3) to (6).

Shear rate [/s] Li2 CO3 -K2 CO3 Li2 CO3 -K2 CO3 +SiO2 (1 wt%) Li2 CO3 -K2 CO3 +SiO2 (1%)+NaOH(0.03%)

Average STDEV Average STDEV Average STDEV

28 21.5 1.31 41.8 5.01 35.0 3.41

56 20.9 1.01 35.6 2.70 28.2 1.56
83 20.5 1.08 32.9 1.92 26.1 1.19
111 20.3 1.04 31.7 1.71 25.0 1.10
139 20.3 1.04 30.8 1.45 24.6 1.03
167 20.3 0.98 30.0 1.40 24.0 0.94
194 20.3 1.03 29.4 1.36 23.7 0.83
222 20.3 1.03 29.0 1.33 23.4 0.72
250 20.3 1.03 28.8 1.29 23.3 0.68

Experimental values (μnf /μbf ) Predictions by theoretical models (μnf /μbf )

Shear rate Li2 CO3 K2 CO3 + Li2 CO3 K2 CO3 + Eq. (3) Eq. (4) Eq. (5) Eq. (6)
SiO2 (1wt%) SiO2 (1wt%)+
NaOH(0.03wt%)

28 1.94 1.63 1.03 1.02 1.02 1.12∗

250 1.34 1.08∗
∗
Chen’s model made a good agreement with the increased relative viscosity of the nanofluid+hydroxide at the high shear rate.
4 B.E. Far, S.M.M. Rizvi and Y. Nayfeh et al. / International Journal of Heat and Mass Transfer 156 (2020) 119789
additional experiments to measure the density values of pure and
nanofluids. It made a good agreement with the literature [12]. The
density value of pure salt and nanofluids were around 1.95 gm/cm3
and 1.97 gm/cm3 , respectively.
The increase of the effective viscosity values of Li2 CO3 -
K2 CO3 , Li2 CO3 -K2 CO3 +SiO2 (1wt%), and Li2 CO3 K2 CO3 +
SiO2 (1wt%)+NaOH(0.03wt%) were compared with several the-
oretical models in the literature. They are Hatchek [14], Thomas
and Muthukumar [15], and Kitano [16] as follows:
μn f
μr = = 1 + 4.5φ
μb f
μnf
μr = = 1 + 2.5φ + 4.83φ 2 + 6.4φ 3
μbf
μ NaOH (0.03 wt%) was 9% which is between the nanofluids and the
1
μr = n f =   φ 2
μb f 1 − ϕm
where μr , μnf , μbf , φ , and ϕ m are relative viscosity, the viscos-
ity of nanofluids, viscosity of base fluids, volume concentration of
nanoparticles, and maximum volume concentration, respectively.
The comparison between the experimental values and the predic-
tion by these models is shown in Table 2. All of them significantly
underestimated the relative viscosity values. On the other hand,
Chen et al. [17] proposed a new model by accounting for particle
aggregation as follows:
μn f  ϕa −[μ]ϕm
μr = = 1− where ϕa = φ (aa /a )3−D
μb f ϕm
The other parameters were adopted from the same study [17].
The result shows that Chen’s model well predicted the increase of
the viscosity of the nanofluids doped with NaOH (0.03 wt%) well
at a high shear rate (250/s). At high shear rates, the unique shear
thinning behavior of the molten salt nanofluids diminishes. More-
over, the addition of NaOH (0.03 wt%) could further disrupt the for-
mation of the salt dendritic nanostructures. Hence, the nanofluid
became a simple mixture of molten salts and nanoparticle ag-
gregates. The Chen’s model (Eq. (6)) accounted for the aggregate
structures of nanoparticles and successfully estimated the increase
of the viscosity at high shear rates. Nonetheless, Chen’s model can-
not predict the highly increased viscosity without the addition of
NaOH (0.03wt%). It could be due to the formation of the salt den-
dritic nanostructures made of salt compounds [10,11]. The model
can only account for the aggregation of nanoparticles but the den-
drite formation by the base fluid (i.e., salt).
The shear-thinning behavior may depend on multiple factors
but mainly particle concentration and shape. The literature study
shows nanofluids show non-Newtonian behavior in the following
two cases [18]: (1) when the nanoparticles in a nanofluid are non-
spherical nanoparticles. In other words, when nanoparticles have
a high aspect ratio (e.g., nanotube, rod-like structure), & (2) when
the concentration of the floating particles in a nanofluid is high.
On the other hand, when nanofluids are doped with spherical
nanoparticles at low concentrations (~1wt%), the same as in the
present study, the viscosity of the nanofluids should show Newto-
nian behavior, whose viscosity is independent of shear strain; on
the other hand, shear-thinning behavior was reported for nanoflu-
ids doped with nanoparticles with high aspect ratio such as nan-
otubes or rod-like structures [18]. In the present experiment, we
dispersed spherical SiO2 nanoparticles in the molten salt mixture
(Li2 CO3 -K2 CO3 ) and, therefore, the viscosity should be indepen-
dent of shear rate similar to the reported studies. However, as
shown in Table 2 and Fig. 2, the nanofluids showed significant non-
Newtonian behavior (shear thinning). It means there were rod-
like (or tube-like) nanostructures at high concentrations as re-
ported in the literature [18]. Since the nanoparticles actually dis-
persed in the molten salt mixture were spherical nanoparticles at
a very low concentration (1 wt%), a possible explanation is that
the abnormality should result from the presence of the salt den-
dritic nanostructures. On the other hand, the addition of NaOH at
0.03 wt% did decrease the viscosity value as it was expected to
disrupt the formation of the salt dendritic structure; however, the
viscosity was not as low as the pure Li2 CO3 -K2 CO3 but stayed in
the middle between the nanofluids and the pure Li2 CO3 -K2 CO3 .
It is possible that the amount of NaOH was not enough to com-
pletely disrupt the formation of the salt dendritic nanostructures
and therefore the measured viscosity was between the viscosity of
(3)
the nanofluid and the viscosity of the pure Li2 CO3 -K2 CO3 . It also
agrees with the heat capacity measurements that the nanofluids
(Li2 CO3 -K2 CO3 -SiO2 (1 wt%)) showed 19% increased heat capacity
(4)
while the enhancement of the heat capacity of those treated with
(5) pure Li2 CO3 -K2 CO3 .
The results support the proposed hypotheses [10,11] claimed
salt dendritic nanostructures primarily responsible for the ob-
served heat capacity enhancement of various molten salt-based
nanofluids. Future work should be to explore the formation mech-
anism of the salt dendritic nanostructures and their effect on other
key properties in thermal storage and transport processes. Further-
more, the rheological behavior of molten salt nanofluids at differ-
ent concentrations and temperatures can be investigated. More-
over, theoretical model should be developed to estimate the en-
hanced viscosity of molten salt nanofluids taking into considera-
(6) tion the dendritic nanostructure formation.
4. Conclusion
Several molten salt nanofluids (SiO2 nanoparticles (1 wt.%) in
a carbonate salt mixture of Li2 CO3 - K2 CO3 ) were tested in a DSC
and a rheometer to characterize the heat capacity and the viscos-
ity. The result showed that the heat capacity was enhanced by 19%
and the viscosity was increased by 94% at 28 /s and 34% at 250
/s. Moreover, the result showed a significant shear thinning behav-
ior. The increase of the viscosity decreased from 94% to 34% from
a range of shear rates (28/s to 250/s). According to the literature
[18], shear thinning behavior is shown when nanoparticles have a
high aspect ratio (e.g., rod-like structure) at high concentrations.
Literature study shows molten salts are likely to form dendritic
nanostructures near nanoparticles that can enhance the effective
heat capacity of the mixture [10,11]. Hence, we followed the same
technique [11] to disrupt the formation of the salt dendritic nanos-
tructures by dispersing a small concentration of NaOH (0.03 wt%).
After dispersing the small amount of NaOH into the nanofluids,
the heat capacity decreased from 19% to 9% and the viscosity de-
creased from 34–94% to 8–63%.
Acknowledgments
This work was supported by CMU Faculty Startup Fund. The
authors acknowledge Dr. Jason Rama, Meliorum Technologies
(Rochester, NY) for conducting photon correlation spectroscopy
analysis.
Supplementary materials
Supplementary material associated with this article can be
found, in the online version, at doi:10.1016/j.ijheatmasstransfer.
2020.119789.
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