Accepted Manuscript: Applied Thermal Engineering
Accepted Manuscript: Applied Thermal Engineering
Accepted Manuscript: Applied Thermal Engineering
PII: S1359-4311(18)31500-X
DOI: https://doi.org/10.1016/j.applthermaleng.2018.05.114
Reference: ATE 12253
Please cite this article as: S. Chakraborty, I. Sarkar, A. Ashok, I. Sengupta, S.K. Pal, S. Chakraborty, Thermo-
physical properties of Cu-Zn-Al LDH nanofluid and its application in spray cooling, Applied Thermal
Engineering (2018), doi: https://doi.org/10.1016/j.applthermaleng.2018.05.114
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Thermo-physical properties of Cu-Zn-Al LDH nanofluid and its application in
spray cooling
Samarshi Chakraborty a, Ishita Sarkar a, Avinash Ashok a, Iman Senguptaa, Surjya K. Pal
b
, Sudipto Chakraborty a*
a
Department of Chemical Engineering, Indian Institute of Technology Kharagpur, India.
b
Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, India.
Abstract:
The current experimental investigation deals with the thermo-physical attributes of Cu-Zn-Al
LDH nanofluid its use in high temperature steel cooling. Here, authors used three metals
(Copper, Aluminium, and Zinc) having high thermal conductivity to synthesize a brand new
nanofluid for heat transfer application. Authors have achieved moderate increment (13.9%) in
thermal conductivity value compared to water. A section of this work also aims to maximize the
cooling rate which aids in improving mechanical properties of quenched steel plate. The
maximum cooling rate of 158.4oC/sec was attained at 160 ppm of nanofluid concentration which
is 18.5% higher than that attained by water. In addition to enhanced thermal conductivity,
nanoparticle deposition on the cooling surface also contributes to the heat transfer enhancement
nanofluid concentration both thermal conductivity and cooling rate values decline. Such trend is
owed to several factors namely poor suspension stability, high agglomeration tendency and
formation of nanoparticle layer on steel surface which prevents contact between coolant and
surface.
Keywords: Cu-Zn-Al LDH, nanofluid, spray cooling, thermal conductivity, cooling rate,
1
* Author to whom all the correspondence should be addressed
Sudipto Chakraborty,
Chemical Engineering Department, IIT Kharagpur,
Kharagpur-721302, West Bengal, India
1. Introduction:
In the past few decades with continuous growth in nanotechnology, synthesis of nanoparticle has
become a reality. In early 1990, an American scientist named Stephan U.S. Choi [1]first used
nanoparticle suspension as a coolant. The concept of particle suspension in base fluid is around
for an even longer time. However, in spite of giving higher thermal conductivity value than the
base fluid, the highly unstable nature of millimeter and micron sized particle suspension made it
undesired for heat transfer application. Poor stability of micron sized suspension gives rise to
higher sedimentation, higher erosion in heat transfer equipment, high pressure drop, increased
pipeline clogging, higher viscosity value and higher pumping cost etc. Therefore, there was a
need for a stable particle suspension which would also have a higher thermal conductivity value.
In order to achieve stable particle suspension, scientists have used nanoparticle and suspended it
beneficial attributes of nanofluids over micron sized particle suspension has been discussed by
Das et al. and Li et al. [2, 3] in details. Due to several advantageous attributes, nanofluid has
been used for wide range of applications starting from the heat exchanger, electronic chips,
microchannel, automobile engine, refrigerators, chillers, and nuclear reactor etc. Among all the
attributes of nanofluids, high thermal conductivity value makes it research worthy and
2
The present study partially focuses on the high temperature steel plate cooling using nanofluid
aided pressurized spray cooling scheme. In steel manufacturing process, run out table plays a
decisive part in creating desired microstructure which is responsible for improved mechanical
properties (tensile strength). Manufacturing of high strength steel is also possible via a metal
alloying technique which is much expensive as compared to the cheaper alternative named ultra-
fast cooling[4]. Attainment of ultrafast cooling in the run out table (ROT) (Temperature range
martensite, bainite and pearlite phase, etc.)[5]. When the product between cooling rate and steel
plate thickness goes above 800, and then ultrafast cooling is achieved. According to Zhang et
al.[6] by using conventional laminar jet cooling and conventional coolant (such as water)
attaining such a high cooling rate is difficult. The cooling rate achieved during jet or spray
cooling process (under ROT condition) is not only dependent on experimental flow parameters
and fluid properties but also on plate thickness and plate composition. To nullify the effect of
plate thickness, authors have used 6 mm thick steel plate for all the spray cooling experiments. In
order to attain desired cooling rate, both high mass flux spray cooling and advanced coolant are
needed. Nanofluid provides a suitable and more efficient alternative to any conventional coolant
due to its enhanced thermal properties. In this study, authors are focused on the high temperature
applications of nanofluid especially thermal treatment in the steel industry. Nanofluid based
Chakraborty et al. [7] explored the potential of TiO2-water nanofluid as a coolant to cool down
high temperature steel plate by using jet impingement technique and found improvement in
cooling rate. Mitra et al.[8] also conducted laminar jet impingement cooling of hot steel plate by
using water-TiO2 and water-MWCNT nanofluids and found substantial augmentation in heat
3
transfer rates. Water based cooper[9]and alumina[10] nanofluids were also used by researchers
along with an air-atomized spray to cool down high temperature steel plate(>900oC).
Implementation of nanofluid for high temperature metal quenching are motivated by several
factors such as, 1) increase thermal conductivity of coolant, 2) better suspension stability with
limited increase in pumping cost and 3) suspended nanoparticle deposits on the heat transfer
surface and aids in surface roughness increase, it provides additional nucleation site and also
restricts vapor film formation which can hamper the heat transfer. The possible roadblock for
large scale industrial application of nanofluid is its possible environmental impact on aquatic life,
human body as well as other environmental impact. In one of the recent works, authors have
invented a new breed of nanofluid for heat transfer application which is layered double
material (anionic clay) which has positively charged metal hydroxide sheets compensated by
anionic counter ions in the gallery space. LDH is represented by the following chemical formula:
and M3+ ,respectively[12].Its dynamic chemical formula enables researchers to add multiple
metal ions in a single compound. LDH is naturally occurring clay minerals, made out of mostly
biocompatible materials[13]. LDH has found application in several field human life including
medical application, water treatment process and biological application (ATP, DNA, enzyme
intercalation with LDH to avoid degradation). Mg-Al LDH has found application as an antacid
and anti-pepsin agent[14]. Mg-Al LDH, Zn-Al LDH, Li-Al LDH and Fe-Al LDH has also been
used as a drug delivery agent[15].Above studies confirm the bio-compatibility nature of LDH
nanoparticle. Water-Cu-Al LDH[16] and water-Zn-Al LDH[17] nanofluids have already been
4
used as a coolant for jet quenching hot steel plate which gave significant augmentation heat
In the current study, authors have combined three highly thermally conducting metal ions (Cu2+,
Zn2+, and Al3+) to form a novel nanofluid which is Cu-Zn-Al LDH nanofluid. No work reported
in the open literature has combined thermal attributes of three metal ions into a single nanofluid.
Present work centers on the consequence of Cu-Zn-Al LDH nanofluid loading on thermo-
physical properties as well as its heat transfer application. Implementation of this brand new
nanofluid for high temperature metal quenching application makes the present study worthy of
investigation.
In the present study, Cu-Zn-Al LDH nanofluid was synthesized by co-precipitation methods
which uses three metal nitrate salts namely copper (Cu(NO3)2.3H2O), zinc (Zn (NO3)2·6H2O )
and aluminium nitrate(Al (NO3)3·9H2O) and sodium nitrate (NaNO3) in the molar ratio of 4
(Cu2+):1 (Zn+):1 (Al3+):2 (Na+). NaNO3 is used to increase NO3 - ion concentration in the solution
and to prevent CO2 intercalation. The aforementioned nitrate salts were dissolved in water and 2
M NaOH was added to the solution until the pH of the solution reaches 10.7. NaOH works as a
precipitating agent. The synthesis scheme used in this study was adopted from our earlier work
on Cu-Al LDH nanofluid[11]. Post titration, the solution is stirred for 16 hrs and the solution is
filtered to bring down the filtrate pH level up to 7. The precipitate is then used to prepare the
final nanofluid solution by further stirring it for 12 hrs and followed by 30 minutes of sonication.
Nanofluid concentrations were varied between 40 ppm to 240 ppm, to verify its impact on the
5
heat transfer properties. Nanofluid synthesis scheme used for this current study has been depicted
in Fig. 1.
(TEM) analyses. XRD analysis of Cu-Zn-Al LDH nanoparticle was executed by Philips made X-
1.5406 Å. XRD analysis was conducted over a diffraction angle(2θ) range of 8o-70ohaving scan
speed of 0.5 sec-1and step increment of 0.05o. FESEM analysis (JEOL JSM 7610F, USA) was
performed for both particle morphology and nanoparticle deposition study. Energy dispersive
spectroscopy analysis was conducted for the elemental study. For particle size analysis, an FEI
6
made analytical TEM (TECNAI G2 20S Twin, USA) was used. The thermo-physical properties
of nanofluid include three main properties which are thermal conductivity, surface tension, and
viscosity. The thermal conductivity of all the samples was evaluated by using KD2 thermal
conductivity meter manufactured by Decagon Device (USA) which works on the principle of
transient needle probe method. The surface tension of nanofluids was measured by Jencon
(India) made du Noüy ring surface tensiometer. Static contact angle was measured by using a
goniometer (Rame-Hart 190-F2, USA). For viscosity measurement, authors have used a cone
and plate rheometer (Physica MCR 301, Austria). Viscosities of all the nanofluid samples were
measured at a fixed shear rate of 100 sec -1. All the thermo-physical properties were measured at
30oC.In order to sustain the temperature during thermal conductivity and surface tension
measurement, a temperature controlled water bath was used. However, in case of viscosity
measurement, liquid sample was kept for at least 5 minutes on a temperature controlled
rheometer plate (plate temperature: 30oC) prior to all the experiments. Stability of nanofluid is
one of the most crucial factors to be considered for industrial application. The stability of the
nanofluid was evaluated by taking sedimentation photograph (Nikon D7100 camera, Japan) and
zeta potential measurement of nanofluid samples at different time interval. Surface roughness
was measured for both prior and post nanoparticle deposition by using Mitutoyo surface
XRD patterns of nanoparticle provide its unique characteristics feature, the degree of
crystallinity, basal spacing, and crystal size. XRD analyses of Cu-Zn-Al LDH nanoparticles were
matched with JCPDS file (37-0629). JCPDS file contains characteristics peaks corresponding to
known Cu-Zn-Al LDH samples. The XRD patterns of Cu-Zn-Al LDH nanoparticle consists of
7
several distinctive peaks in the 2θ angle range of 8-70o (Fig. 2). From JCPDS file details, it was
found that nanoparticle is rhombohedral in character and its lattice is rhombo-centred. LDH is a
layered crystalline material which is made of metal hydroxide layers and anionic counter ions.
Nanoparticle sample was analyzed to determine basal spacing (Braggs Law) and crystal size
(Scherrer Law) of the nanoparticle[11, 18]. The basal spacing and crystal size data corresponding
Fig. 2. XRD pattern of Cu-Zn-Al LDH nanoparticle with varying diffraction angle
8
Table 1.Basal spacing and crystal size chart of Cu-Zn-Al LDH nanoparticleat different
diffracion angles.
(1 0 1) 33.81 0.26 24
(0 1 2) 34.71 0.26 43
(1 0 7) 44.83 0.20 95
(1 1 3) 61.57 0.15 11
FESEM analysis was carried out on Cu-Zn-Al LDH nanoparticle which is layered crystalline
material. High magnification image of Cu-Zn-Al LDH nanoparticle clearly shows its layered
morphology. It also shows that metal hydroxide sheets (flakes) are stacked upon each other and
its thickness is well below 100 nm. It confirms that at least one of the particle dimensions is in
the nanometer range (See Fig. 3 (a)). This observation can be further varied in TEM analysis.
The layered morphology of layered double hydroxide has also been observed by other scientists
[19-21]. Nanoparticles were also tested for elemental analysis by using Energy dispersive
9
spectroscopy (EDS). EDS analysis established the existence Cu, Zn, Al, O, and N in the
nanoparticle.
TEM analysis was carried out to check the average particle size as well as the aspect ratio of Cu-
Zn-Al LDH nanoparticle. Fig. 4 shows that the particles possess a layered geometry (flake type
structure) which has a high aspect ratio (See Fig. 4(b)).Cu-Zn-Al LDH nanoparticles are stacked
upon each other which clearly match with its characteristic feature. According to several
scientists [22-24], higher the aspect ratio of nanoparticles greater will be its thermal conductivity
in a suspension. The average particle length was observed to be 49 nm whereas average width
was 7 nm (average of 12 data points). Therefore, the aspect ratio was 7 which are significantly
higher than that of any sphere shaped nanoparticles and making it more effective for heat
extraction. Particles with high aspect ratio provide longer heat conduction path and create a mesh
for faster transport of heat. The current findings are in line with our earlier finding with Cu-Al
10
LDH[11] and Zn-Al LDH[17] nanoparticle as well as with the work of other scientists worked
on different LDH[25].
(a) (b)
Fig. 4. Size analysis of Cu-Zn-Al LDH nanoparticle, a) TEM image and b) histogram plot
are critical while considering it for thermal application. Thermal conductivity is the most crucial
factor for any nanofluid because higher the thermal conductivity of the coolant better will be its
thermal performance. The surface tension of any coolant and contact angle it creates with the
surface determines its spreadability over the same. A lower value of surface tension and contact
angle is desired for greater contact area with the hot surface. Nanofluid viscosity is also a factor
to be considered for its industrial application as higher viscosity will increase pressure drop
(increase in pumping cost) and also influence its spreadability over the surface.
11
3.4.1. Thermal Conductivity
The main driving force for creating nanofluid was to produce a coolant which will have superior
thermal conductivity compared to any conventional coolant such as water, alcohol, transformer
oil etc. In the present study, the focus is to find the effect of concentration variation on thermal
conductivity of Cu-Zn-Al LDH nanofluid. Figure 5 shows that with growing particle
starts to decline. The maximum enhancement in thermal conductivity value was observed at160
ppm concentration of Cu-Zn-Al LDH nanoparticle which is 13.9% greater than that of water.
The responsible mechanism behind both increase and decrease in thermal conductivity can be
owed to combination of several critical factors such as particle concentration[2, 11], Brownian
motion of suspended particle[26, 27], degree of agglomeration and clustering [23, 28, 29],
dispersion stability[30-32], liquid layering effect[33], particle size[34, 35] and aspect ratio/shape
[22, 36, 37]etc. It is to be noted that for spherical nanoparticles, the mechanism of Brownian
motion can estimate the thermal conductivity more precision than in case of particles with high
aspect ratio where both translational and rotational diffusion reduces the effect of Brownian
motion. The complex behaviour of asymmetric nanoparticle in the base fluid makes thermal
conductivity prediction harder using basic micro-convection model as it does not include shape
factor and ordered layer thickness [38-40].However, the positive impact of high aspect ratio of
nanoparticles on the thermal conductivity of nanofluid has been reaffirmed by several researcher
[37, 41]. At high particle concentration, clustering tendency has a detrimental effect on thermal
conductivity. According to Ozerinc et al.[42], there exists an optimal clustering level above
which thermal conductivity value declines. Increase in thermal conductivity value with
increasing particle loading is a common phenomenon with nanofluids. In this study also authors
12
have observed similar trend up to a concentration of 160 ppm. The improved thermal properties
can be linked to Brownian motion, optimum clustering tendency, proper heat conduction path,
high aspect ratio and small size (length 49 nm and width 7 nm) of the nanoparticle etc.
However, it is also to be noted that at higher particle concentration due to increased Van der
Waal attractive force (agglomeration tendency), poor stability and undesired shape modification,
thermal conductivity value declines. A table has been added in this section to show the
and the newly developed Cu-Zn-Al LDH nanofluid (See Table 2).
13
Table 2.Comparative summary of thermal conductivity improvement achieved by different
nanofluids
The surface tension of a coolant plays a vital role important in determining spreadability. Low
surface tension value of any coolant indicates better spreadability, low contact angle, and higher
contact area. Positive attributes of reduced surface tension on the heat transfer application have
been accepted by numerous researchers [9, 49-51]. Addition of nanoparticle can also play a role
in altering the surface tension value of nanofluid by changing the surface energy in the liquid-air
boundary. The increase and decrease in surface tension value of nanofluid samples depend on
14
three basic factors such as variation in the nanoparticle, base fluid, and concentration. It is also
concentration surface tension value tends to increase [52]. As the nanoparticle concentration
rises in the base fluid, large amount nanoparticles accumulates around the liquid surface. Due to
nanoparticle aggregation on the liquid-air interface, the cohesive force between each
nanoparticles increases which is responsible for increased surface tension value at higher
nanofluid depends on electrostatic repulsion force and Van der Waal (VDW) attractive force
between suspended particles. At low nanoparticle concentration (40 ppm), slight reduction in
surface tension value is observed as repulsive force can dominate over the VDW attractive force
due to the charges present on the nanoparticle surface. However, with further increase
concentration, surface tension value rises up again due to over dominating VDW force. In the
current study, authors have observed both of these trends with varying nanoparticle
concentration (See Fig. 6). The current trend is in synchronous with the observation made by
Tanvir and Qiao[54] for MWCNT/DI water nanofluid. However, it is to be noted that alteration
in surface tension value for Cu-Zn-Al LDH nanofluid with varying concentration is insignificant
nanofluids[54, 55].
15
Fig. 6. Effect of concentration on surface tension variation of Cu-Zn-Al LDH nanofluid
The importance of surface tension analysis is partly insignificant for this study because spreading
of impinging drops not only depends on liquid surface tension but also on the surface roughness
of steel. The surface roughness plays a crucial role in determining contact angle as well as the
spreadability of drop on the surface. With increase in surface roughness contact angle of reduces
for a fixed coolant. In order to validate our claim, contact angle was measured for different
nanofluid concentration at two different surfaces which includes steel plate prior to deposition
and steel plate post nanoparticle deposition. The result clearly shows that post particle deposition
as the surface roughness increases; it leads to lower contact angle value for all the nanofluid
concentration (See Fig. 7). The effect of nanoparticle deposition on reducing static contact angle
and improved surface wettability has also been observed by Kim et al.[56]. However, for a fixed
surface roughness increase in nanofluid concentration gives identical trend which is comparable
16
Fig. 7. Variation in static contact angle by varying nanofluid concentration and surface
3.4.3. Viscosity
Viscosity is one of the crucial parameters which impacts both flow properties as well as heat
transfer efficiency of the nanofluid. Viscosity can influence the heat transfer performance of any
system like thermal conductivity value. Here, in this study thermal conductivity of nanofluid
changes with the addition of nanoparticle concentration. Addition of nanoparticle increases the
viscosity of nanofluid which in turn increases the pressure drop and pumping cost. The
limit the viscosity rise significantly. High viscosity can also hinder the spreadability of coolant
over the hot surface. Several scientists have observed that with the increase in nanoparticle
concentration viscosity value also increases irrespective of nanoparticle nature such as metal
[57], metal oxide [58-61]and carbon based nanoparticle. The finding obtained in this current
study for Cu-Zn-Al LDH nanofluid also indicates towards the same conclusion. Figure 8 shows
17
increasing viscosity value with increasing particle concentration. When compared with the
viscosity of water increase in viscosity at 240 ppm concentration is 68.7%. It is also to be noted
that moderately high viscosity can be considered beneficial in some aspects as it increases the
residence time of the impinging drop on a solid surface. Hence, it can increase the contact time
between hot surface and coolant which indirectly influences the heat transfer rates [7].
3.5. Stability
Stability is one of the main parameters to be considered for nanofluid in order to use it
industrially. Stability analyses were conducted via sedimentation photography and zeta potential
value (See Fig. 9 and Table 3). Zeta potential values for different nanofluid concentrations were
reported at two different time interval (2 and 12 hours) to check the effect of time on nanofluid
stability. Table 3 clearly shows that nanofluid stability decreases slightly with increasing time
18
which true for all the samples reported here. It is also to be noted that even after 12 hours from
preparation the value remains above the desired zeta potential value of ± 30 mV.
Using sedimentation photography technique, it can be said that up to initial 12 hours, there is no
sign of sedimentation in all the samples. However, as the time progresses 120, 240 ppm solutions
start to show sedimentation after 12 hours. On the other hand, 40 ppm solution remained stable
up during the entire duration of the experiment. To give a clear idea on sedimentation,
photographs were taken after 24 hours from the bottom side which clearly shows no
sedimentation has taken place for 40 ppm solution whereas both 120 and 240 ppm solutions
show traces of sedimentation below the container. However, it is to be noted that Cu-Zn-Al LDH
nanofluid shows best stability within 2 hours from its preparation and it is preferred to be used
time duration
19
Table 3. Zeta potential value of Cu-Zn-Al LDH nanofluid at different particle loading and time
interval
Nanofluid Concentration Zeta potential value (mV) Zeta potential value (mV)
40 36.9 34.6
Detailed schematic diagram of spray cooling experimental setup is shown in Fig. 10. The
experimental setup contains several key components such as Lechler full cone spray nozzle,
pressure gauge, rotameter, centrifugal pump, coolant reservoir, solenoid valve, gate valve, muffle
furnace, insulating resting pad, data acquisition system and computer. The key objective of the
experiments is to check the effect nanofluid concentration on surface cooling rate. AISI 304
grade stainless steel plates were used for all experiments. The steel plate dimensions were 100
(Voltage 440V, Load 8/12 kW) which has a maximum heating range up to 1400oC was used to
heat up the steel plate. The test plates were heated up to 1050oC for spray cooling experiments. A
Lechler (Nozzle No: 460-843-17-CG) manufactured full cone water spray nozzle was used for
the cooling experiments. An insulating resting pad (made with fire brick) was fabricated to
ensure adiabatic boundary condition where the hot steel plate was kept during the experiment.
20
The transient temperature data during the experiments were collected by using 3 K-type
thermocouples which were connected to a National Instrument (USA) made data acquisition
system (NIcDAQ-9174 and NI 9211 card). The data acquisition system was then connected to a
computer for data storage. All the three thermocouples were placed at three specific locations to
capture the temperature variation across the steel. TC 1(x=20 mm, y= 3 mm; Distance from
spray/plate centerline = 30 mm) was placed farthest from spray/plate centre, TC 2 (x=50 mm, y=
3 mm; Distance from spray centerline = 0 mm) was placed right below the spray/place centre and
TC 3 (x= 70 mm, y= 3 mm; Distance from spray centerline = 20 mm) was placed on the opposite
side of TC1 and closer to the spray/plate centerline. Figure 10 also shows the position of the
three thermocouples and their coordinates. The thermocouples holes are drilled up to 50 mm in
the Z direction and the holes were sealed with a conducting paste to eliminate any air gap
between thermocouples and plate. In order to ensure that water does not fall on hot steel plate
until the spray is stabilized, a wooden board was used to prevent the spray impingement. The
board was only removed after the spray is stabilized and desired flow rate was attained. All other
Using the three subsurface thermocouple data, authors have calculated surface temperature
65]. For surface temperature distribution, calculations were done by transforming the entire
geometry in to two dimensions (x= 100 mm, y= 6 mm). The entire geometry is divided into 7781
nodes and 7500 elements (Δx= 0.0004 m, Δy= 0.0002 m). The transient thermocouple data is
taken as the input data. Only the top surface is considered of heat transfer as all other surface is
covered by insulating fire bricks. The boundary conditions for aforesaid 2 D computational
21
T
For x = 0 mm and y = 0 to 6 mm, 0
x
T
For x = 100 mm, and y= 0 to 6 mm, 0
x
T
For y = 0 mm, and x= 0 to 100 mm, 0
y
T
For y = 6 mm, and x= 0 to 100 mm, unknown
y
The principal equation for the computation of surface heat flux is given below:
T T T
k k C p
x x y y t
2T 2T T
k 2 k 2 C p
x y t
2T 2T C p T
2 2
x y k t
Where, k (Unit: W/m.K), ρ (Unit: Kg/m3), and Cp (Unit: J/Kg.K) denotes the thermal
To calculate surface heat flux and surface temperature from internal thermocouple data, the
software takes a guess value of surface heat flux and computes temperature data for all the nodes
as typical heat conduction problem. Nonlinear optimization technique is used to re-modify the
guess value of heat flux for the purpose of error minimization (difference between measured
temperature value and INTEMP calculated temperature at the same node). The INTEMP
calculation proceeds and iteration takes place until the error value goes below the predefined
tolerance limit. Several researchers have used INTEMP for surface heat flux and temperature
calculation [66, 67]. For the current study, three thermocouples were used for temperature
22
recording. Based on the position of three thermocouples in steel plate, authors have divided the
top surface into three heat flux zones, a) Flux zone 1 (x= 0 to 36 mm, y =6 mm), b) Flux zone 2
(x= 36 to 64 mm, y =6 mm), and c) Flux zone 3 (x=64 to 100 mm, y=6 mm) having different
heat flux value. It is assumed that heat flux value within each zone is uniform.
Fig. 10. Experimental setup for spray impingement cooling using Cu-Zn-Al LDH nanofluid
23
Table 4. Experimental design for Cu-Zn-Al LDH nanofluid based spray cooling experiments
Nanofluid Concentration 40, 80, 120, 160, 200 & 240 ppm
Implementation of Cu-Zn-Al LDH nanofluid for heat transfer enhancement during steel
quenching process is the core of the current study. In this section, authors have focused on the
effect of varying nanofluid concentration on cooling rate and effect of nanoparticle deposition
The transient surface temperature corresponding to three thermocouple locations was calculated
using INTEMP. Figure11(a-b) shows the variation of surface temperature with time during spray
cooling within a temperature range of 10500C to 2000C for pure water and 160 ppm Cu-Zn-Al
LDH nanofluid concentration. From the figure, it can be seen that both the curves follow an
24
identical trend with thermocouple TC2 showing the highest cooling rate.TC2 is located just
beneath the nozzle and hence the temperature declines faster as compared to other two
thermocouples. Based on its distance from the spray impingement zone, fastest temperature drop
was observed in TC2 which is followed by TC3 and TC1.Another distinctive feature observed in
all the graphs is the presence of two characteristic stages of temperature drop. Both the stages are
owed to different modes of heat transfer such as natural convection (first stage), forced
convection (second stage), and radiation (first stage). Temperature drop in the first stage is much
slower than the second stage as it only involves heat loss due to radiation and natural convection.
In Fig. 11, t= 0 sec is measured when the plate is removed from the furnace. The duration of the
first stage extends from the time when the plate is detached from the furnace and placed on the
fire brick till the time spray starts to fall on the hot steel plate. For the purpose of ensuring stable
and uniform spray impingement on a steel plate, a wooden board was used to prevent any spray
impingement until desired water flow rate; water pressure and uniform spray distribution are
attained. Once the wooden board is removed and spray impinges on the steel surface the
temperature profile starts to show rapid decline which is the onset point of the second stage.
From the slope of the transient temperature profile, both the stages can be easily identified.
25
(a) Water (b) 160 ppm
Fig. 11 (a-b). Transient surface temperature profile for all three thermocouple
locations,(a) water, and (b) 160 ppm concentration of Cu-Zn-Al LDH nanofluid
Temperature drop in TC2 thermocouple is the fastest among all three thermocouples. Therefore,
from here onwards only data corresponding to TC2 thermocouple has been reported in the
manuscript. For the current study, cooling rate value attained (between the temperature zone of
900-600oC) for all the nanofluid concentration has been displayed in Fig. 12. It was observed
that on increasing LDH concentration up to 160 ppm, cooling rate increases and thereafter it
decreases. At 160 ppm, the maximum cooling rate of 158oC/s was achieved which lies in the
ultra-fast cooling region indicating that UFC can be achieved with Cu-Zn-Al LDH nanofluid
assisted spray cooling. An increase of 18.5% in cooling rate was found out for a concentration of
160 ppm as compared to water. Authors have achieved 15.6% reduction in coolant consumption
at 160 ppm concentration when compared with pure water (Supplementary Table 1). During the
spray cooling of nanofluid, nanoparticles get deposited on the steel surface which creates
additional nucleation sites and helps to rupture the insulating vapour layer formed on the steel
surface. As observed in contact angle analysis, nanoparticle deposition also helps in improving
26
surface wettability and effective heat transfer rate. However, too high nanofluid concentration
can also adversely affect the cooling rates because the entire steel surface gets covered with LDH
nanoparticle layer which acts as a hindrance for heat transfer between the coolant and the steel
surface. The current trend in cooling rate plot is owed to both surface roughness of steel (owed to
change. The influence of particle deposition on heat transfer enhancement and the subsequent
decline has been clearly explained in section 5.4. To compare the cooling performance of the
current nanofluid with earlier reported nanofluids (at similar experimental condition), a
27
Fig. 12.Cooling rate alteration at different concentration of Cu-Zn-Al LDH nanofluid
Surface heat flux variation with surface temperature (900 0–2000C) during cooling at various Cu-
Zn-Al LDH nanofluid concentrations has been shown in Fig. 13. A nonlinear variation of surface
heat flux with surface temperature was observed irrespective of the LDH concentration. Initially,
an insulating vapour layer forms due to the high temperature difference between coolant and
steel surface resulting in a low heat flux. The formation of vapour cushion due large temperature
gradient is called as the Leidenfrost effect [69]. As the temperature decreases during cooling, the
heat flux increases and attains a peak value termed as critical heat flux (CHF) due to the rupture
of insulating vapour layer and this region is termed as transition boiling regime.On further
cooling, nucleate boiling dominates where the surface heat flux value decreases after CHF due to
the reduction in thermal energy. The highest enhancement in critical heat flux was achieved for a
28
It was also observed that the average heat flux (taking the average of heat flux values between
900-600oC) value increases with LDH concentration up to 160 ppm, thereafter it decreases as
shown in Table 6. Reduction in thermal conductivity of nanofluid and formation of a thick layer
of particles on steel surface is responsible for the lowering of heat transfer at high nanofluid
concentrations.
Fig. 13.Variation in surface heat flux with surface temperature at different concentration of Cu-
Heat transfer coefficient, h (W/m2.K) of a coolant is found out by using the following equation.
Q
h (1)
Ts Tc
29
Where, Q is the surface heat flux in W/m2, Ts is the surface temperature in K and T c is the
coolant temperature in K. Heat transfer coefficients for different nanofluid concentrations were
calculated and plotted against the surface temperature (9000-2000C) as shown in Fig. 14. It was
found out that irrespective of nanofluid concentration heat transfer coefficient values were
almost same at initial stages of cooling where the surface temperature was higher. However, heat
transfer coefficient value increases as cooling proceeds in all cases. This occurs due to the
rupture of insulting vapour layer during cooling. As cooling proceeds, nanoparticle deposition
increases leading to newer nucleation sites and thus enhances heat transfer. Heat transfer
coefficient value rises with nanofluid concentration up to 160 ppm, thereafter it decreases. Table
6 also shows that the highest average heat transfer coefficient (AHTC) value of 2.34 kW/m2K
was obtained for a nanofluid concentration of 160 ppm and in the surface temperature of the
range of 900-6000C. A maximum of 4.47% enhancement was observed at 160 ppm concentration
Fig. 14. Alteration in heat transfer coefficient value with surface temperature at varying
30
Table 6. Summary of average heat flux and heat transfer coefficient values obtained at different
nanofluid concentration
0 1.52
2.24
40 1.55
2.25
80 1.57
2.26
120 1.58
2.28
160 1.65
2.34
200 1.61
2.33
240 1.60
2.32
Presence of nanoparticle in the base fluid leads to increment in heat transfer rate by two ways
one is by elevating the thermal conductivity value of the coolant and secondly by increasing the
thermal conductivity value has already been discussed in thermal conductivity analysis section.
Therefore, in this section authors have mainly focused on the other aspect of heat transfer
enhancement which is nanoparticle deposition. During the steel quenching process, nanoparticle
suspended in water gets deposited on the steel surface which increases the surface roughness.
Enhanced surface roughness acts as an advantage in terms of the heat transfer aspects [16, 70].
The deposited particles act as additional nucleation sites. Increase in nucleation site by particle
31
deposition is considered to be one of the reasons behind improved cooling rate. The effect of
nanoparticle concentration on surface roughness has been displayed in Fig. 15. The figure shows
that with increasing particle concentration, surface roughness gradually increases up to 160 ppm
concentration, and then it starts to decline as the entire surface gets covered with the nanoparticle
layer. In order to explain the phenomenon, a schematic diagram (See Fig. 16) of nanoparticle
deposition with varying nanoparticle concentration has been added along with the actual FESEM
image to further validate the claim. FESEM image clearly shows that at concentration beyond
160 ppm, the steel surface gets covered by a layer of deposited nanoparticles which is
responsible for the reduced heat transfer rate. Nanoparticle layers hinder the contact between
impinging drops and the hot steel surface which in turn, reduces the cooling rates. Such
observation has also been made by few other researchers who have found similar attributes of
Chang et al.[74] also reported that at higher nanoparticle (Al2O3) loading, excess nanoparticle
deposition causes reduction in nucleation site and decline in convective heat transfer rate.
However, at lower concentration optimum particle deposition helps to improve both nucleation
site and heat transfer rate during spray cooling. The aforesaid observation is in sync with results
32
Fig. 15.Influence of nanofluid concentration on deposition induced surface roughness
33
6. Measurement uncertainty:
The error analysis or uncertainty measurement is one of the key studies for any experimental
important to go for uncertainty analysis. In this study, authors have used ASME recommended
test code for error analysis [75]. For ensuring measurement accuracy, all experimental data
reported in this study has been repeated multiple times to guarantee accuracy. All the parameters
from which uncertainties may arise have been reported in Table 7 along with their contribution.
34
7. Conclusion:
A new breed of nanofluid namely Cu-Zn-Al LDH has been synthesized by one step co-
precipitation technique. The current work focuses on the thermo-physical aspects of the
aforementioned nanofluid and its use in the spray cooling of hot steel plate (above 900oC).
Implementation of nanofluids aids in heat transfer enhancement during steel quenching via two
routes, firstly by enhancing the thermal conductivity of coolant and secondly by increasing the
number of nucleation site with nanoparticle deposition. The nanofluid concentration is varied in
the range of 40-240 ppm to check its impact on the thermo-physical property as well as its
thermal performance. The following summarized points are the key outcomes of the present
research,
1) Cu-Zn-Al LDH nanoparticles were rod shaped. The average Cu-Zn-Al LDH nanoparticle
2) The thermal conductivity of Cu-Zn-Al LDH nanofluid at 160 ppm was 13.9% higher than
that of water. Thermal conductivity increases with increasing particle loading upto 160
ppm concentration then it starts to decline again. Surface tension remains almost
3) The highest enhancement in surface cooling rate was reached at 160 ppm nanofluid
concentration which is 18.5% greater than what attained by pure water. The maximum
cooling rate of 158.43oC/sec was obtained at 160 ppm which is well above ultra-fast
35
4) Other than the thermal conductivity value, nanoparticle deposition on steel plate also
plays a crucial role in heat transfer enhancement. With increasing particle concentration,
nucleation site. However, as the particle concentration is further increased steel surface
becomes entirely covered with particles and it prevents incoming drop contact with the
hot surface. As a result, the overall heat transfer performance declines beyond 160 ppm
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List of Figures:
Fig. 2 XRD pattern of Cu-Zn-Al LDH nanoparticle with varying diffraction angle
Fig. 4 Size analysis of Cu-Zn-Al LDH nanoparticle, a) TEM image and b) histogram
plot
nanofluid
Fig. 7 Variation in static contact angle by varying nanofluid concentration and surface
Fig. 10 Experimental setup for spray impingement cooling using Cu-Zn-Al LDH
nanofluid
Fig. 11 (a-b) Transient surface temperature profile for all three thermocouple locations,(a)
Fig. 13 Variation in surface heat flux with surface temperature at different concentration
Fig. 14 Alteration in heat transfer coefficient value with surface temperature at varying
46
Cu-Zn-Al LDH nanofluid concentration
List of Tables:
Table 1 Basal spacing and crystal size chart of Cu-Zn-Al LDH nanoparticle at different
diffracion angles
Table 2 Comparative summary of thermal conductivity improvement achieved by different
nanofluids
Table 3 Zeta potential value of Cu-Zn-Al LDH nanofluid at different particle loading and
time interval
Table 4 Experimental design for Cu-Zn-Al LDH nanofluid based spray cooling experiments
Table 5 Comparison between cooling rate enhancement obtained by different nanofluid at
similar experimental condition
Table 6 Summary of average heat flux and heat transfer coefficient values obtained at
different nanofluid concentration
Table 7 Measurement uncertainty for different parameters
Supplementary Table:
Nomenclature:
d Basal spacing
47
h Heat transfer coefficient
L Crystal size
Q Heat flux
Ts Surface Temperature
Tc Coolant Temperature
Greek Letter:
λ X-Ray wavelength
Abbreviation:
48
TC Thermocouple
49
Graphical abstract
50
Highlights
Cu-Zn-Al LDH nanofluid was prepared and used for metal quenching.
Nanofluid was used for spray cooling of hot steel plate (above 900oC).
Maximum cooling rate of 158.4oC/sec was also achieved at 160 ppm concentration.
51