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Title Page

Scalable Microwave-Assisted Continuous Flow Synthesis of CuO

Nanoparticles and Their Thermal Conductivity Applications as Nanofluids

Arun V. Nikam*ab and Arun H. Dadwalb

a
Chemical Engineering and Process Development Division, bPhysical and Material Chemistry
Division.
CSIR-National Chemical Laboratory, Homi Bhabha Road, Pashan, Pune, 411008, INDIA.
a
Corresponding Author Email address: av.nikam@ncl.res.in, arun11nikam@gmail.com
Telephone no. - +9102025902175,
b
Author Email address: a.dadwal@ncl.res.in, arunchd29@gmail.com
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Abstract:

We have demonstrated the novel and scalable synthesis of CuO nanoparticles by an integration
of microwave and flow synthesis. The shape and size of CuO nanoparticles were tuned by
changing the concentration of copper precursor. The production rate of CuO nanoparticles was
found to be 5g/h with 70% conversion of copper acetate into the CuO nanoparticles. The thermal
conductivity of CuO nanofluid prepared in ethylene glycol showed linear enhancement with
increase in the volume content of CuO nanoparticles produced in batch and flow reactors.

1. Introduction:

Metal oxide nanoparticles have received an immense attention owing to their specific properties in
reference to their bulk and atomic/molecular counterparts. Among the metal oxide nanomaterials,
CuO is widely investigated owing to its narrow band gap (1.2eV) [1], high solar absorbance [2,3]
and high value of thermal conductivity (33 W/m K) [4]. Due to these properties,CuO
nanoparticles find their use in various sectors ranging from sensors [5], energy storage [6],
catalysis [7] and heat transfer application [8]. The smaller size of the nanoparticles results in high
surface to volume ratio, distinctive physical and chemical properties. These properties are highly
sensitive to shape and size of the nanomaterials [9,10]. The shape and size of the nanoparticles
are governed by reaction parameters and the type of synthetic procedure used. A small change in
reaction parameters drastically alters the size and shape of nanoparticles. Thereby, paramount
attention has been paid to get the desired shape and size of the nanoparticles by tuning the
reaction parameters.

There are many reports available in the literature on the batch synthesis of CuO
nanoparticles using wet chemical approaches such as solvothermal, thermal decomposition,
microwave-assisted synthesis and co-precipitation [11-14] etc. Liu et al. reported the synthesis of
monodispersed hollow CuO nanospheres by using the hydrothermal method at 160 °C for 6h
[15]. Ahmad et al. prepared uniformly grown CuO nanoparticles in the size range of 5-8 nm by
employing precipitation method [16]. Fan et al. reported precipitation-pyrolysis method to
prepare monodispersed nanocrystal of copper oxide [17]. The batch synthesis of CuO
nanoparticles has various drawbacks such as the use of multiple reagents, time consuming
procedure, less control over shape and size of the nanoparticles, low yield, and requirement of
high temperature and pressure conditions. All these drawbacks make batch synthesis unsuitable
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from the industrial point of view. There is a need to develop a simple scalable and cost effective
synthesis of CuO nanoparticles from an industrial perspective. Recently, a continuous flow
synthesis of the nanomaterials has gained tremendous traction owing to high yield as well as
good control over shape and size of the nanoparticles as compared to batch synthesis [18, 19].
Thereby, flow synthesis offers us a better alternative over the classical batch synthesis. There are
very few reports in the literature on the continuous flow synthesis of CuO nanoparticles. Reilly et
al. synthesized CuO nanorods using droplet flow reactor [20]. Zhou et al. produced CuO
nanoparticles in a tubular reactor using supercritical water hydrothermal synthesis (SWHS)
approach which required high temperature and pressure conditions [21].

In this work, we have demonstrated microwave-assisted continuous flow synthesis of size

controlled CuO nanoparticles. The effects of reaction parameters have been systematically
studied to obtain small sized spherical CuO nanoparticles. Also, their use in the heat transfer
applications is investigated.

2. Experimental Section:

2.1 Materials and Chemicals:

Cu(ac)2.H2O (98%) is received from S D Fine-Chem Limited and used without purification.
Benzyl alcohol (99.99%) and Sodium hydroxide (99%) have been purchased from Merck Life
Science Private Limited. Ethylene Glycol (99% purity) purchased from Loba Chemie and used as
received.

2.2 Synthesis of CuO nanoparticles in batch:

0.20 M of Cu(ac)2.H2O solution was prepared in benzyl alcohol. 30 μL of the 0.1M aqueous
solution of NaOH was added to the 15 mL of Cu(ac)2.H2O solution and the mixture was sonicated
for a minute. The resulting solution was transferred to round bottom flask and kept in the
microwave oven (2.45 GHz, 700W Ragatech Pvt. Ltd. India). After a minute of microwave
irradiation, a color change of the reaction solution occurred from blue to dark black. This black
colored product was allowed to cool down to room temperature and washed three times with
water and ethanol. The resulting product was separated using a centrifuge and kept for drying at
75 °C for 12 h.
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2.3 Microwave-assisted flow synthesis of CuO nanoparticles:

The experimental setup used for microwave-assisted flow synthesis is shown in schematics (see
Figure 3a). The continuous stirred tank reactor (CSTR) of 25 mL volume placed in the
microwave oven. The inlet and outlet of CSTR were connected to the peristaltic pump through
silicon tubing. The reaction parameters (concentration, residence time, and microwave power)
optimized in batch synthesis was kept same to conduct flow synthesis of CuO nanoparticles.5
mL solution of 0.1M NaOH was added drop wise to the 500 mL solution of 0.05M Cu(ac)2.H2O.
Upon continuous microwave irradiation, Cu(ac)2 solution was injected into the CSTR using a
peristaltic pump. A magnetic needle was placed into the CSTR for stirring the reaction mixture.
The flow rate of Cu(ac)2 solution was set at 25 mL/ min to maintain 1 min residence time. At
last, CuO nanoparticles were withdrawn at the outlet using a peristaltic pump. Washing and
drying of CuO nanoparticles were carried out using the procedure mentioned in the section 2.2.

2.4 Characterization:

The powder samples of CuO nanoparticles were characterized using powder X-ray diffraction on
a PANanalyticalX'Pert PRO X-ray diffractometer with Cu Kα radiation (Ni filter, λ = 0.15418
nm). The size and morphology analysis of the particles were performed by transmission electron
microscope (TEM) FEI model TECNAI G2 F30 operated at an accelerating voltage of 200 kV.
The samples for TEM analysis were prepared on the carbon coated copper grid by drop casting 8
μL dilute solution of CuO nanoparticles in ethanol and dried at room temperature.

3. Results and Discussion:

In this work, we have presented the scalable approach for the synthesis of small sized CuO
nanoparticles by using microwave-assisted flow synthesis. The suitable reaction parameters
required for the scalable approach were optimized with the help of microwave-assisted batch
synthesis and then optimized parameters were used for the flow synthesis. In particular, we have
optimized reaction parameters like concentration of metal precursor and reaction volume using
microwave-assisted batch synthesis. Initially, we started by varying the concentration of metal
precursor. The synthesis of CuO nanoparticles was carried out at two different concentration of
Cu(ac)2 viz. 0.20M and 0.05M. The TEM studies were carried out to check the morphology of
synthesized CuO nanoparticles. Interestingly, we observed a drastic difference in morphology, as
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shown in Figure 1. At 0.20M concentration of Cu(ac)2, the CuO nanobelts were observed (see
Figure 1a). The average length and width of CuO nanobelts were measured to be 14 nm and 120
nm, respectively. In contrast, at 0.05M concentration of Cu(ac)2, the spherical and small sized
CuO nanoparticles were obtained (see Figure 1b). The average particle size of CuO nanoparticles
calculated from TEM images was found to be 4.5 nm. The small size of CuO nanoparticles at
low concentration can be attributed to low availability of Cu-precursor in solution needed for
nanoparticles growth. Thereby, to obtain small size CuO nanoparticles, concentration of Cu-
precursor should be low. We have also investigated the role of copper precursor on synthesized
CuO nanoparticles by choosing Cu(ac)2 and Cu(acac)2 as copper precursor. The Cu(ac)2 and
Cu(acac)2 were dissolved in 15 mL of benzyl alcohol and 30 μL of 0.1M NaOH was added in
both the precursor solution, respectively. Both solutions were kept in microwave oven for 1 min
and 12 min, respectively. The product obtained was washed and dried under vacuum oven for 12
h. PXRD pattern of product obtained from precursor Cu(ac)2 clearly indicate that Cu(ac)2
produces monoclinic CuO, while product obtained from precursor Cu(acac)2 ends up with mixed
phase of monoclinic CuO and cubic Cu2O (see Figure 1C. Curve-I and Curve-II). To summarize
PXRD results, Cu(ac)2 is suitable copper precursor which produces phase pure monoclinic CuO
nanoparticles upon microwave irradiation.

Figure 1: TEM images of CuO nanoparticles synthesized by microwave-assisted synthesis at

Cu(ac)2 concentration a) 0.20M and b) 0.05M, c) XRD patterns of copper oxide nanoparticles
prepared from Cu(ac)2[ Curve-I ] and Cu(acac)2[ Curve-II ] (*Cu2O).

After optimizing the suitable precursor concentration, our next step was to optimize the reaction
volume, best suited for achieving scalable synthesis of CuO nanoparticles. Hence, the synthesis
of CuO nanoparticles was carried out at different reaction volumes i.e. at 25, 50 and 100 mL,
respectively by maintaining the 0.05M concentration of Cu(ac)2 in each case. The percentage
yield of CuO nanoparticles was estimated by the gravimetric estimation. It was observed that
higher is the reaction volume, lower is yield of the CuO nanoparticles. When the reaction volume
is 16 and 25 mL, the gravimetric yield of CuO nanoparticles obtained is 71 % and 70 %,
respectively. As the reaction volume is increased to 50 mL and even 100 mL, the obtained
gravimetric yields were 50% and 45%, respectively (see Figure 2a). The observed decrease in the
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yield of CuO nanoparticles with increase in the reaction volume is ascribed to the slow rise in
temperature with the microwave heating. To validate the given hypothesis, temperature
measurement experiment was performed with pure benzyl alcohol at different reaction volumes
using inbuilt thermocouple in a microwave oven and microwave was continuously operated for 1
min. Figure 2b depicts that the temperature rise under microwave radiation is very rapid in case of
16 and 25 mL in comparison to 50 and 100 mL reaction volumes. This is due to the limitation of
microwave irradiation heating to spot size or small area and the efficient microwave heating occurs
only at 16 and 25 mL reaction volumes. These results validate our hypothesis of slow
temperature increase with the reaction volume from 16 to 100 mL. Thereby, for 0.05M
concentration of Cu(ac)2, both 16 and 25 mL reaction volumes are suitable to conduct flow
synthesis for scalable production of CuO nanoparticles. Among the 16 mL and 25 mL reaction
volume, we selected the 25 mL variant which helps in producing CuO nanoparticle at high
production rate. From the thermal profile, we also conclude that reaction temperature below 204
˚C gives low % yield of CuO nanoparticles and there is no significant variation in the size as well
as shape of CuO nanoparticles. On other hand, further increase in temperature is impossible as
benzyl alcohol has a boiling point of 205 °C. The choice of solvent is very important in the
microwave-assisted synthesis of materials. The heating characteristics of a solvent under
microwave irradiation are governed by its dielectric properties [22]. Usually, microwave active
(high tan𝛿, which determines efficiency of conversion of microwave energy into heat by
dipolar heating mechanism) and high boiling solvents are suitable for microwave-assisted
synthesis of nanoparticles at high temperatures. Among several other microwave active solvent,
we restricted our study for benzyl alcohol owing to its high boiling point and high tan𝛿 value of
0.667 [23].
After optimizing the reaction parameters in microwave-assisted batch synthesis, the
microwave-assisted flow synthesis experiment was performed using CSTR with 25 mL, which
was placed in microwave oven (see Figure 3a). The optimized batch reaction parameters were
considered for flow synthesis (batch volume, concentration, residence time). The Cu(ac)2
solution was injected into CSTR placed in a microwave oven at the flow rate of 25 mL/min upon
continuous microwave irradiation. The CuO nanoparticles were collected from the outlet using a
peristaltic pump followed by washing and drying of the nanoparticles. Figure 3b shows the
PXRD pattern of the CuO nanoparticles. The PXRD patterns of both batch and flow synthesized
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CuO nanoparticles exactly match with each other. Using Scherrer equation, D = 0.9λ/βcosθ,
where D is the average crystallite size, λ is the wavelength of X-rays, β is the full width at half
maximum corrected for the broadening due to the instrumental contribution and θ is the angle of
diffraction, the crystal size of CuO nanoparticle for batch and flow methods were obtained as 3.5
nm and 3.9 nm, respectively. The average crystallite sizes of CuO NPs obtained from batch and
flow methods are nearly same. The TEM images of CuO nanoparticles synthesized using
microwave-assisted flow synthesis show that particles are of spherical shape (see Figure 3 c and
d) and average particle size calculated from TEM analysis is found to be 4.2 nm. Our results
confirm that we have successfully translated batch process parameters to the continuous flow
process that can help us to synthesize CuO nanoparticles at a higher production rate of 5g/h with
maintaining good product quality.

Figure 2. a) Schematic of synthesis of CuO nanoparticles in different batch volume, b)

Temperature profile for the different batch volumes, c), d), e) and f) TEM images of CuO
nanoparticles synthesized at 16, 25, 50 and 100 mL batch volumes, respectively.

Figure 3. a) Schematic of the experimental setup for microwave-assisted flow synthesis of CuO
nanoparticles, b) PXRD patterns, c) and d) TEM images of CuO nanoparticles.

Thermal Conductivity of CuO nanofluids: Nanofluids are prepared by dispersing

nanoparticles of size ranging over 1-100 nm in the base fluid. Water, ethylene glycol and oil are
the most frequently used base fluids. Commonly, solids have higher thermal conductivity than
corresponding base fluids or liquids. So, the idea is to increase the thermal conductivity of base
fluids by dispersing solid nanoparticles in the base fluid. There are reports in the literature
showing the enhancement in the thermal conductivity of nanofluids [24-27]. As a result of this,
nanofluids have garnered a lot of interest owing to their better heat transfer characteristics. The
heat transfer performance of nanofluids is strongly affected by thermo physical properties such
as thermal conductivity, viscosity, specific heat, and density. These properties govern the overall
heat performance of a nanofluids. Among all these properties, thermal conductivity is of
paramount importance for nanofluids application as being heat transfer fluids. The thermal
conductivity of the nanofluids is affected by different factors such as particle size and shape,
base fluid properties, surfactant coating, temperature, agglomeration/clustering of the
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nanoparticles. Nanoparticles have tendency to aggregate due to van der Waals interactions
between the nanoparticles. Aggregation/clustering between the nanoparticles also affects the
overall thermal conductivity of the nanofluids [28-29]. As a solid phase, metal oxide
nanoparticles are a usual choice in nanofluids pertaining to the high thermal conductivity of
metal oxides nanoparticles. Such metal oxides TiO2, Al2O3, SiO2 and CuO nanoparticles were used in
the nanofluids preparation. Among these metal oxides, nanofluids containing copper oxide (CuO)
nanoparticles have been widely investigated for the heat transfer applications owing to their high
value of thermal conductivity i.e. 33 W/m.K [4]. There are a great number of reports in the
literature showing considerable enhancement in the thermal conductivity of CuO-ethylene glycol
based nanofluids at a very low volume % of CuO nanoparticles [4, 30-32]

In the present work, to compare the heat transfer capabilities of CuO nanoparticles synthesized
by batch and flow methods, we measured the thermal conductivity of nanofluids prepared by
dispersing CuO nanoparticles in ethylene glycol. The nanofluids prepared by dispersing CuO
nanoparticles synthesized from batch and flow methods were named as CuO-B and CuO-F,
respectively. The thermal conductivity of CuO nanofluids was measured using transient hot-wire
(THW) method reported earlier [33]. The error in the measurement of thermal conductivity is ±1
%. All the measurements were performed at room temperature and freshly prepared samples
were used for all the measurements. The variation of relative thermal conductivity of CuO
nanoparticles dispersed in ethylene glycol with the volume % of CuO nanoparticles is shown in
Figure 4. Both the CuO-B and CuO-F nanofluids showed the linear thermal conductivity
enhancement with the increase in volume % of CuO nanoparticles. We observed that thermal
conductivity enhancement in both the nanofluids is comparable at all the volume % of
nanoparticles. This could be due to the similarity in particle size and shape of the synthesized
CuO nanoparticles in both batch and flow methods as optimized batch parameters were only
used for synthesizing CuO nanoparticles in the flow method. Also, there was no surfactant
coating on the surface of CuO nanoparticles. However, due to large scale production of CuO
nanoparticles in flow synthesis as compared to batch synthesis, flow synthesis still offers us the
advantage of preparing cost-effective nanofluids at a large scale.

Figure 4. Comparison of the relative thermal conductivity (k/kf) of CuO nanofluids.

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4. Conclusion:

We have successfully demonstrated the synthesis of size controlled CuO nanoparticles at a

production rate of 5g/h using microwave-assisted continuous flow synthesis. The concentration
copper acetate as a precursor, significantly affects the size and shape of CuO nanoparticles. The
reaction temperature was found to be highly sensitive to reactor volume that determined the yield
of CuO nanoparticles i.e. 71 % at 16 mL and 70 % at 25 mL. The thermal conductivity of the
nanofluids shows linear enhancement with the increase in volume % of CuO nanoparticles.
Similar enhancement in the thermal conductivity of nanofluids prepared by dispersing flow and
batch synthesized CuO nanoparticles could be to the similarity in particle shape and size of the
nanoparticles. Our results indicate that integration of microwave and continuous flow approaches
could be used for the scalable and controlled synthesis of bimetallic, inorganic-inorganic, and
inorganic-organic hybrid nanomaterials.

5. Acknowledgment

AK and AD thanks to CSIR-New Delhi and UGC, India, for fellowship. Authors would like to
thank Dr. A. A. Kulkarni, Dr. B. L. V. Prasad and Dr. P. A. Joy for their support and
encouragement.

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