HEAT TRANSFER ENGINEERING, 2018

VOL. 39, NO. 15, 1331–1343

https://doi.org/./..

A Multiscale Morphological Insight into Graphene Based Coatings for Pool Boiling
Applications
Anju Guptaa , Arvind Jaikumarb , Satish G. Kandlikarb,c , Aniket Rishic , and Andrew Laymand
a
Department of Chemical Engineering, Rochester Institute of Technology, Rochester, NY, USA; b Department of Microsystems Engineering,
Rochester Institute of Technology, Rochester, NY, USA; c Department of Mechanical Engineering, Rochester Institute of Technology, Rochester,
NY, USA; d School of Chemistry and Materials Science, Rochester Institute of Technology, Rochester, NY, USA

ABSTRACT
The application of graphene for pool boiling is an attractive option to facilitate compaction and pro-
mote efficient heat removal from high power density devices. In this context, chemical characteriza-
tion of the depositions achieved through commonly employed coating techniques are an important
topic of discussion. A detailed structure-property relationship between the morphologies obtained
on the mono and multilayered graphene coatings and their corresponding pool boiling performance
quantified by the experimental critical heat fluxes is presented. Three different types of graphene
(G) and graphene oxide (GO) substrates are characterized: (i) nanoscale: mono and multilayer sam-
ples developed through chemical vapor deposition, (ii) Rochester Institute of Technology (RIT)-G/GO
colloid generated through an oxygen embrittlement electrochemical process, and (iii) commercially
available chemical vapor deposited (CVD)-G/GO colloid. The morphological features were character-
ized with scanning electron microscope while X-Ray Diffractometer analysis and Raman spectroscopy
were used to examine the ordering and stacking of the sheets that result in the unique structural fea-
tures. Fourier transform infrared and energy dispersive X-ray spectroscopy were employed to identify
the overall compositional characteristics of the coated surfaces. The wettability changes and addi-
tional nucleation sites for nanoscale coatings, and multiscale roughness features and ridge microstruc-
tures for microscale coatings were identified as enhancement mechanisms.

Introduction
The versatility offered by graphene and its excellent ther-
mal and electrical properties make it a suitable choice for
a wide range of applications including optics, electronics,
thermal and solar. The manufacturing process since its
invention has revolved around producing pristine and
high quality single layer graphene. In recent years, the
focus has shifted towards producing novel and cost-
effective graphene coatings through a variety of mass
manufacturing techniques. Geim and Novoselov [1],
Geim [2] and Fuhrer et al. [3] presented comprehensive
reviews and roadmaps for the different manufacturing
techniques. They further identified potential applications
areas for graphene in various industries. Some of the
commonly employed manufacturing techniques include:
(i) mechanical exfoliation [4], (ii) chemical oxidation
[5], (iii) exfoliation using surfactants [6], (iv) chemical
vapor deposition [7], and (v) electrochemical oxidation
of graphite [8]. All these techniques rely on overcoming
the weak Van-der-Waals forces holding the graphitic
layers together. In addition to the challenges encountered
during the synthesis (such as fragmentation of the hexag-
onal plane during mechanical exfoliation and addition
of functional groups during wet chemical process) the
transfer of graphene on substrates remains a significant
hurdle for its industrial adoption. In this context, chem-
ical characterization of the prepared colloidal solutions
and transferred coatings provides a step towards its
application in industries.
Carbon-based coatings [9–13] is an attractive option
for phase-change heat transfer and it can be employed
to address the increasing demand for efficient heat
removal systems in microelectronics, refrigeration, air-
conditioning, process and nuclear industry. Since the
graphene based coatings are in the sub-10 micron range,
it enables high heat flux dissipation and facilitates com-
paction of devices at the micro and nanoscales [14–17].
Protich et al. [8] demonstrated the use of graphene
based coatings to improve the pool boiling heat transfer
performance and attributed the enhancement to the

CONTACT Professor Satish G. Kandlikar sgkeme@rit.edu Department of Mechanical Engineering, Rochester Institute of Technology,  Lomb Memorial
Dr, Rochester, NY, , USA.
Color versions of one or more of the figures in this paper can be found online at www.tandfonline.com/uhte.
©  Taylor & Francis Group, LLC
1332 A. GUPTA ET AL.
morphology of the coating. Thus, a detailed morpholog-
ical characterization of the coated surfaces is required
to elucidate the underlying heat transfer mechanisms to
exploit the structure-property relationship of graphene
for advanced thermal management based applications.
Therefore, the key objectives of this paper were to:
(a) provide a morphological insight into graphene
based coatings through optical and spectroscopic char-
acterization techniques to understand the structure-
activity relationships between the morphologies and their
enhanced bool boiling performance, (b) compare the pool
boiling performance of nano and micro scale surfaces
resulting from the two commonly applied coating tech-
niques: chemical vapor deposition (CVD) and dip coating
techniques, and (c) demonstrate the efficacy of a simple
dip-coating technique to generate unique morphological
structures that result in higher heat transfer coefficients
and critical heat fluxes.
Dip-coating is identified over the other sophisticated
coating methods (spin coating, powder coating, com-
paction techniques, etc.) to produce highly stable coatings
that either involve complicated processes or large invest-
ment on the equipment’s. Unique morphological features
such as flakes, ridges and granules were obtained and are
demonstrated in this paper. It is a simple technique that
transfers the produced solution on the substrate and the
subsequent air drying results in multiscale morphologies.
Extensive studies on the pool-boiling performance by
time-dependent dip-coated substrates, and the validating
mechanisms have been recently reported [18, 19]. This
paper highlights structure-activity relationship studies of
the nano and microscale coated surfaces to correlate their
enhanced pool boiling performances by using a variety
of analytical and microscopy characterization techniques
to fully understand the morphology and composition of
the generated surfaces. Field-emission scanning electron
microscope (SEM) was used to examine the details of the
surface morphology of the graphene coatings. Fourier
transform infrared (FTIR) and energy dispersive X-ray
spectroscopy techniques were employed to confirm the
presence of graphene (G) and graphene oxide (GO)
on the coatings through detection of the characteristic
chemical species and to inspect the overall composition
of the coatings. Ordering and stacking of the graphene
sheets that are imperative to the diverse morphologies
were investigated using X-Ray diffractometer and Raman
spectroscopy.
Experimental
Multiscale coatings and their characterization
A variety of copper substrates were prepared to possess
nano and micro scale coatings using commercial and
synthesized G/GO colloidal solutions. The nanoscale
coatings were developed through a CVD process to
exercise control over the number of deposited layers. The
microscale coatings were generated through a dip coating
technique with an electrochemical liquid exfoliation
process referred to as Rochester Institute of Technology
(RIT)-G/GO [20], and a commercially available CVD
solution (Graphene Supermarket, NY) referred to as
CVD G/GO.
Nanoscale coatings via chemical vapor deposition
An atmospheric pressure CVD technique was used to coat
the GO on to the copper substrates. The copper substrates
were mirror finished to obtain a smooth surface. The mea-
sured arithmetic mean roughness was less than 1µm prior
to the deposition process for all the surfaces. The details
of the CVD process is described in detail in Ref. [21]. A
consequence of using bulk copper substrates in the CVD
process is that it introduces roughness effects arising due
to thermal deformation of the bulk copper substrate. This
aspect of using CVD process is extremely beneficial as
it introduces a morphological change of the underlying
substrate over which a conformal coating of graphene
was achieved. Although previous depositions [22] of G
or GO using this technique highlight the importance of
decoupling the substrate from the layers by depositing
on thin foils, this work identifies the effect of bulk cop-
per deformations as a factor in improving the boiling per-
formance characteristics. At the nanoscale, the morpho-
logical change due to thermal deformation is expected to
change the liquid wettability due to roughness induced
effects. This wettability manifests in the form of hystere-
sis, where the receding contact angle is seen to be influ-
enced by the roughness. The monolayer sample exhibited
an unusually high contact angle hysteresis of 48° mea-
sured using a video contact angle optima goniometer. The
high contact angle hysteresis was also reported by Raj et
al. [23] in their work.
Microscale coatings via dip coating
Preparation of graphene solutions: Microscale coatings
were achieved by dip-coating two colloidal solutions –
RIT-G/GO and commercially available CVD-G/GO. The
RIT-G/GO colloidal solution was prepared using a sin-
gle step electrochemical process using an oxygen embrit-
tlement process that resulted in the cleavage of graphite
electrode to produce GO and its subsequent reduction
into graphene. The process was carried out in an electro-
chemical cell consisting of graphite as anode and copper
test chip as cathode in an electrolyte comprising of car-
bon tetrachloride and deionized water (10% v/v) [20]. The
merits of combining the production of GO and its sub-
sequent reduction in a single step eliminates the defects

(carbon vacancy, attachment of functional groups etc.)
that arise due to conventionally employed reduction tech-
niques (thermal and chemical). This was achieved by
using a constant current density which causes resistance
heating of the electrolyte held between the electrodes.
This heating technique results in the removal of oxygen
attached to the graphene hexagonal plane and thereby
improving the quality of G/GO sheets produced. Con-
sequently, the degree of reduction depends on the cur-
rent density supplied which regulated the temperature of
the bath. In the current arrangement, a density of 300
mA/cm2 was applied, which produced a combination of
G and GO particles dispersed in the solution.
Dip coating: The copper test section was thoroughly
cleaned in a 6M hydrochloric acid solution and washed
in distilled water before the dip coating process. The test
section was prepared to ensure that only the 1 cm2 boiling
surface was exposed to RIT-G/GO and CVD-G/GO col-
loidal solutions and the rest of the chip was covered with
a layer of Kapton tape. This tape prevents the excess area
from participating in heat transfer during the boiling pro-
cess. The exposed 1 cm2 area of the copper test section was
immersed in the G/GO colloidal solutions for four differ-
ent durations. Four chips were prepared by dip coating for
2, 5, 10 and 20 minutes.
Characterizations techniques: Coatings and colloidal
solutions
A deeper understanding of the chemical composition and
G/GO layers coated on copper chips were gained using
a variety of optical-analytical techniques: X-ray Diffrac-
tometer, Fourier transform infrared, and Raman Spec-
troscopy. The morphology and elemental make-up of the
coated surfaces were investigated using scanning electron
microscope. Dynamic light scattering and thermogravi-
metric analyzer were used to quantify the size of the G/GO
colloids and composition of each component respectively.
X-Ray Diffractometer: The crystalline phases of the
RIT-G/GO coated substrates were investigated using a
Rigaku DMAZ-IIB X-Ray Diffractometer (XRD) with
(Cu Kα radiation; wavelength 1.5418 Å). The spectra were
recorded for 2θ ranges between 5° and 75° at a rate of
3°/min rate. The step size was 0.02° with an X-ray power
of 40 kV and 35 mA. This range is expected to capture
peaks from carbon and the underlying copper substrate.
The location of characteristic peaks determines the pres-
ence of elements on the surface. The RIT-G/GO solution
was dip coated on the copper test section and allowed to
dry before the analysis.
Fourier transform infrared: Analytical spectra of
RIT-G/GO coated on the copper substrate were taken
using a Fourier transform infrared (FTIR) spectroscopy
HEAT TRANSFER ENGINEERING 1333
(Shimadzu, IR Prestige 21, Kyoto, Japan) in the frequency
range of 4000–600 cm−1 , a scan number of 40 times, and
a resolution of 4 cm−1 . A small quantity (∼2 µL) of the
sample was deposited with the use of a Pasteur pipette
between two well-polished KBr disks, creating a thin film.
Duplicate spectra were collected for the same sample.
Raman Spectroscopy: A multi-wavelength Jobin Yvon
Horriba LabRAM HR Raman Spectroscope using He-Ne
Laser (λ = 632.8 nm) was used to measure the thickness
and quality of graphene layers with 10 second acquisition
time. To produce repeatable and reliable data a total of 10
scans were taken by observing the characteristic D and G
peaks of G and GO.
Scanning electron microscopy: The morphology of the
substrates was studied by both a TESCAN Field Emission
Mira III LMU (Czech Republic) and JSM-6400 V scan-
ning electron microscope (SEM), JEOL, Ltd., Tokyo, Japan
at an accelerating voltage of 15 kV. The energy disper-
sive X-ray spectroscopy (EDS) measurements were done
on Bruker Quantax EDS with XFLASH 5010 detector
attached to a field emission scanning electron microscope
MIRA II LMH.
Dynamic Light Scattering: Dynamic light scattering
(DLS) and zeta potential (ζ ) of the RIT-G/GO solu-
tion were conducted on a Malvern Instruments Zeta-
sizer Nano ZS (Worcestershire, UK) equipped with a
backscattering detector angle of 173° and a 4 mW, 633
nm He–Ne laser at 25° C. Hydrodynamic diameters were
measured by placing 1mL of sample in quartz cuvettes
(10 × 10 × 45 mm) at 173° backscatter angle with 120s
equilibration time. The average hydrodynamic diameters
reported were based on 11 scans and three measurement
cycles. For zeta potential measurement, the sample was
placed in a disposable zeta-potential cell to the level the
electrodes. Zeta potential was determined by combined
Doppler electrophoretic velocimetry that acquires the
electrophoretic mobility (μEP ) of the suspended G/GO
particles in the solvent and phase analysis light scattering
that provides accuracy in measurements for low mobil-
ity suspended particles by performing a phase compari-
son of the scattered light with that of the reference fre-
quency, which was computed over 3 cycles (30 data points
per cycle) using the following equation
 
φ =< A > (4π n/λ) (sin θ/2) μEP E dt (1)
where φ is the phase shift of the scattered light, <A> rep-
resents the average scattered amplitude, n is the refrac-
tive index of the medium, λ is the wavelength of the light
used for the measurements, θ is the scattering angle, Ē
is the applied electric field over the duration (t) of the
measurements [24].
Thermogravimetric analysis: Composition of the
RIT-G/GO solution was studied using a TA Instruments
1334 A. GUPTA ET AL.
Q500 Thermogravimetric analyzer (TGA). Data was
analyzed using the Universal Analysis 2000 software (TA
Instruments). The sample was heated at 5°C/min from
25°C to 950°C under nitrogen atmosphere (40 mL/min)
in a graphite crucible.
Pool boiling test apparatus
Pool boiling is a simple technique in which the liquid flow
occurs by natural convection in the vicinity of nucleating
bubbles on the heater surface. Experimental investigation
of the pool boiling performance was carried out using a
setup consisting of three components: (a) test section, (b)
water reservoir, and (c) heater block. The details of the
apparatus can be found in Ref. [18]. Briefly, the copper test
chip is encapsulated in a ceramic chip holder exposing the
top boiling surface to the working fluid (distilled water).
The bottom part of the test section made contact with the
heater block to supply the required heat through 4 × 200
W cartridge heaters. A glass water bath is assembled over
the test chip to hold the boiling liquid secured by a rub-
ber gasket. This work focussed on determining the two
important performance parameters viz. critical heat flux
(CHF) and heat transfer coefficient. The boiling tests were
Figure . TESCAN Field Emission Mira III LMU scanning electron microscope and Bruker Quantax EDS images of CVD deposited graphene
(a) monolayer with (b) carbon mapping, and (c) multilayer with (d) carbon mapping.
conducted on the coated substrates with distilled water
at atmospheric pressure. The distilled water was degassed
to eliminate the influence of non-condensable gases. The
nucleate pool boiling data was obtained until CHF was
reached.
Results and discussion
Characterization of the coatings
Nanoscale coatings: The morphology of the graphene
coating achieved via CVD as mono and multilayer
on the copper substrate was conducted using a field
emission scanning electron microscope as illustrated in
Fig. 1. Electron microscopy studies were accompanied
by carbon mapping that was performed using energy
dispersive X-ray spectroscopy to confirm the presence of
carbon on the uniform coating of G/GO on the copper
substrate. Fig. 1a shows the presence of wrinkles on the
graphene sheet which is indicative of the presence of
monolayer graphene coatings. The wrinkles are surface
features introduced by the thermal deformation of the
underlying substrate during the CVD process. Fig 1b
is the corresponding image generated on EDS mapping
 HEAT TRANSFER ENGINEERING 1335

the presence of carbon on the sample. With subsequent

addition and stacking of graphene layers, the wrinkles
began to diminish from the surface (Fig. 1c) and the pres-
ence of additional graphene layers were verified by the
increased intensity of the mapped carbon as seen by the
brighter green regions on Fig. 1d. This was additionally
confirmed by the intensity ratios obtained in the Raman
spectroscopy results which is discussed in detail later.
The formation of nanoscale wrinkles is expected to
influence the wettability characteristics on the surface.
These wrinkles were attributed to the functional groups
attached on the basal plane of the graphene structure [24].
The functional groups induce local wettability changes
along the contact line which influences the heat transfer
at this location. Additionally, the CVD process creates a
mono to multilayer transition on the multilayer sample
due to the deposition parameters. This is further expected
to amplify the wettability effects on the surface.

X-ray diffraction
X-ray diffraction was used to probe the differences in
the characteristic peaks of G/GO observed for mono and
multiplayer substrates as seen in Fig. 2a. X-ray diffraction
measurements showed 2θ reflections peak between 6–10°
that corresponds to the presence of G and GO. Typically,
graphene and graphene oxide peaks occur in the range
of ∼5–12°. The peaks observed between 40–70° corre-
spond to the copper substrate. The diffraction graph for
mono and multilayer were seen to be influenced by the
variation of number of graphene layers on both the sub-
strates and the distance between the layers in the case of
multilayer samples. The presence of a small peak around
28° is attributed to the excessive oxidation of the sam-
ple from the exposure to the X-rays. The XRD pattern
of mono and multilayers were analyzed around the 002
peak, and the Laue diffraction fitting function was used
to determine the number of layers in the multilayer sub-
strate [25]. The current analysis showed 3 layers on the
multilayer samples. The distance between the layers in
the multilayer samples is an important parameter which
dictates the degree of wrinkle formations on the surface.
The receding contact angle is shown to be influenced
by the interlayer spacing, which was attributed to be the
cause for the unusually large contact angle hysteresis [23].
Figure . (a) X-Ray Diffractometer spectrum, (b) Fourier trans-
The carbon density and the additional contaminants form infrared spectroscopy, and (c) Raman spectroscopy of CVD
in the sample is shown in the X-ray diffraction plot. The deposited graphene mono (top) and multilayers (bottom).
oxide formation in the nanoscale coatings is expected to
the presence of chemical bonds on the substrates. Fig. 2b
mask the benefits of the graphene coatings. Additionally,
shows the light absorbance by the graphene molecules
the oxide formation hampers the heat transfer.
as a function of wavelength depicting the characteristic
peaks of GO: C=O stretching vibration of carboxyl group
Fourier transform infrared spectroscopy
at 1726 cm−1 , O-H deformation vibration resulting from
Fourier transform infrared spectroscopy was employed C–OH at 1390 cm−1 , and C–O stretching vibration at
to further confirm the presence of G/GO by detecting 1050 cm−1 . The peak at 1570 cm−1 corresponding to the
1336 A. GUPTA ET AL.

aromatic rings (C=C) was also seen. The FTIR pattern colloids. Similar to the nanoscale coatings, the composi-
for the two substrates were identical as expected due tional analysis of the two solutions were also obtained.
to similar molecular composition, however the high Characterization of RIT- G/GO solution- The stability
intensity peaks as seen with multilayer sample indicate and composition of RIT G/GO colloidal solution was
presence of larger number of molecules [18]. found by DLS which is a widely used technique to esti-
mate the average diameter of spherical shaped colloids.
Raman spectroscopy The average hydrodynamic diameter of the G/GO col-
loids were found to be 1000 nm (Fig. 3a). G/GO colloids
Raman spectroscopy was used to further quantify the
typically have large ratios of length to thickness in micro
number of layers for the CVD coated multilayer sub-
scale. The resultant size measurements of RIT-G/GO
strates. The laser excitation during Raman spectroscopy
yielded convoluted results which are attributed to the
measurements caused a shift of the Stokes phonon
energy, which resulted in three characteristic peaks for
graphene – G (1580 cm−1 ), a primary in-plane vibrational
mode, a 2D peak (2690 cm−1 ), and a different in-plane
vibration, D (1350 cm−1 ) as seen in Fig. 2c. The CVD
deposited graphene multilayer demonstrated a promi-
nent G and 2D peak with a negligible D band indicating a
relatively defect free and high quality of graphene coating.
As expected, due to the lesser number of graphene layers
on the substrate, the intensity of G peak for monolayer
was lower than the multiplayer peak. The broader 2D
peak was attributed to the wrinkled graphene sheets as
seen in Fig. 1a or 1c, which arises due to the coupling
effects with the underlying copper substrate [26, 27].
Typically, an increase in the number of layers results in
a decrease in the thermal conductivity along the z-plane.
Jaikumar et al. [18] have shown that the nanoscale coat-
ings are influenced by the wettability and not the thermal
conductivity. Raj et al. [23] have further shown that
very large interlamellar spacing results in elimination of
wettability effects with the underlying substrate. On the
other hand, Rafiee et al. [28] have shown the influence of
the underlying substrate exists for a threshold of 6 layers
for copper and water wetting systems. In this context,
this study highlights the importance of wettability with
an increase in the number of graphene layers which
manifests as a large change in the contact angle hysteresis.
This change is expected to influence the microconvection
and transient conduction heat transfer mechanisms.

Microscale coatings
The microscale coatings were achieved by dip-coating the
copper substrates with the electrochemically generated
(RIT-G/GO) and commercially available CVD-G/GO
solutions. The RIT-G/GO solution was characterized to
gain information on the size and zeta potential which is a
measure of the colloidal stability of the samples. In a stable
solution, the colloids remain dispersed for longer dura-
tions without forming aggregates or agglomerates that
may prevent the formation of even coating layers. Visual
inspection of RIT-G/GO solution vial showed no phase Figure . (a) Size analysis, (b) Thermogravimetric analysis, and (c)
separation or agglomeration of G/GO particles in the vial Fourier transform infrared spectroscopy of electrochemically pro-
for longer durations of time confirming the stability of the duced RIT-GO solution.

lateral measurements of the G/GO sheets. From a general
understanding of colloids, zeta potentials with absolute
values larger than 30 mV can result in stable dispersions
via mutual repulsion between the particles [6, 9, 15]. In
the present study, the absolute zeta-potential value for
the electrochemically synthesized G/GO oxide solution
was found to be 60 mV, reported as intensity-weighted
z-averages based on 15 scans.
The quantification of the composition of G/GO in the
colloidal solution was obtained by thermogravimetric
analysis by determining the loss of mass as a function
of increasing temperature. The resultant thermograph
shown in Fig. 3b reveals the presence of both G/GO. The
loss of mass observed at 100°C is usually associated with
removal of adsorbed water and gas molecules. The loss of
mass at 200°C corresponded to the decomposition of GO,
yielding CO and CO2 as the byproducts. GO being less
thermally stable, decomposes before pure graphene and
is also reported in Ref. [22, 29]. The loss of mass at higher
temperatures from 800° C corresponds to the remaining
unstable carbon from graphene [26]. It is reported that
complete decomposition of graphene occurs post 950°C
as seen in Fig. 3b. The thermogravimetric analysis con-
firms the chemical stability of G/GO coated on the copper
substrates. No discernable chemical change was observed
while heating between 100 – 130°C, which replicates the
temperature ranges generally observed with pool boiling
studies with graphene [18]. The percent composition by
weight of GO was 12.5%.
The FTIR spectroscopy spectrum of G/GO showed
peaks at 3290 cm−1 , 1624 cm−1 and 1411 cm−1 as seen
in Fig. 3c. The peak at 3290 cm−1 was attributed to O-H
stretching from water. The peak was strong and it over-
lapped with C-H stretching at 2930 cm−1 . The peak at
1624 cm−1 was attributed to the presence of aromatic
rings (C=C) and the peak at 1411 cm−1 was due to C–H
bending. The aromatic CH2 and C–O peaks overlap caus-
ing them to be absent in their expected locations. These
results further indicate the presence of a carboxyl group
in the G/GO coated on copper [18, 19]. The analysis
of commercially available CVD-G/GO colloidal solution
rendered similar size and compositional data.
Characterization of RIT-G/GO dip-coated chips: The
detailed characterization of time dependent dip-coated
substrates with RIT G/GO colloidal solution was per-
formed on SEM, XRD, FTIR spectroscopy, elemental
analysis, and Raman spectroscopy. Fig. 4 summarizes the
various morphologies of the G/GO oxide coatings on
the copper test section achieved for different dip-coating
durations.
The substrate with shortest coating duration of 2-min
exhibited mixed morphology which comprised of flakes
and granule-like structures extended on the copper sub-
strate as seen in Fig. 4a. Further observation at higher
HEAT TRANSFER ENGINEERING 1337
magnification and 70° stage tilt (Fig. 4e) showed the
presence of ridges that are approximately 11 µm tall. The
ridges are shown to act as liquid reservoir slabs through
which the microlayer evaporation is enhanced [18].
The microlayer increases the nucleation activity on the
surface and hence the heat flux dissipation. Additionally,
these type of structures create roughness and wettability
changes at the microscale. In the case of 5, 10 and 20-min
coated substrates (Fig. 4 b-d) the granule like structures
were seen predominantly and with increased coating
durations, a tighter packing of these granules were
observed. These tighter packing appear as a laminated
film which is expected to deteriorate the heat transfer
performance due to lack of morphological features. This
trend was confirmed by the low CHF values reported
for longer dip-coating durations by Jaikumar et al. [18]
in their study. Fig. 4f represents the image obtained for
20-min coated substrates generated by tilting the micro-
scope stage to 70° indicating that the shorter granular
structures (less than 1 µm in height) result in a smoother
surface profile. This was also corroborated by the surface
roughness measurements that were conducted using a
confocal laser scanning microscope. The average surface
roughness measured for the shorter coating duration
was ∼10 µm, while it was less than 1 µm for the longer
coating duration.
A number of reports have shown the importance of
morphology to the pool boiling performance. Typically
in the microscale coatings, the morphology appears as
roughness structures with a range of multiscale cavities.
A closer examination of the SEM results show that the
longer dip-coating duration resulted in tighter packing of
the G/GO coatings which creates a smooth laminated film
lacking roughness features which results in lower CHFs
as reported in Ref. [18]. The shorter coating duration
results in distinct ridge microstructures which are capa-
ble of trapping a thin liquid film that promotes bubble for-
mation. These ridge microstructures increase the growth
rates [18] which significantly improves the heat transfer
performance as shown in Fig. 7.
Fig. 5 summarizes these spectroscopic investigations
of the time-dependent RIT-G/GO coated substrates.
X-ray diffraction studies were performed to confirm the
presence of G and GO by observing the location and
intensity of the distinct peaks of G and GO, and any
variation in these peaks as a result of coating durations
as seen in Fig. 5a. Differences in intensities of the peaks
observed on XRD plot indicate the presence of different
amounts of G/GO on the coated substrates. A compo-
sitional change creates a local wettability change along
the contact line which affects the boiling characteristics.
The compositional change is attributed to the different
functional groups attached to the G basal plane. This is
supplemented with the FTIR results as discussed next.
1338 A. GUPTA ET AL.

Figure . JSM- V scanning electron microscope images of (a) -min,  X, (b) -min, (c) -min, (d) -min coated surface; top view
X, (e) -min, (f) -min at  X, ° stage tilt RIT-GO coated substrates.

The characteristic peaks of GO were shown by the diffrac-
tion peaks in the range of ∼5–12°. 2θ location indicates
the layering dynamics between the sheets in the GO film
[27]. The broad diffraction peak are an indication of poor
ordering of the coated graphene sheets that implies the
sample comprised of single to very few layers [30]. The
underlying weaker and broader peaks identified for the 2,
5 and 10-mins were due to the disordered carbon mate-
rials that were absent on the sample coated for 20-min
duration, verifying a pertinently coated copper substrate.
The disordered carbon material creates defects on the
surface which causes contact line pinning. This pinning
induces a large contact angle hysteresis as seen here. Raj et
al. [23] have that the pinning is prevalent in the receding
motion of the liquid which seems to be influenced by the
defects. The characteristic copper peaks at 42°, 50° and
74° demonstrated a decrease in intensity with increased
dip-coated durations establishing the larger amounts of
G and GO being coated on the copper substrates with
increased dip-coated duration. The peaks corresponding
to the copper metal displayed the lowest intensity for
20-min coating duration.
FTIR analysis of G/GO solution coated on copper sub-
strate at different durations (Fig. 5b) was correlated with
the observations made with scanning electron micro-
scope studies. The samples that were coated for 2-min
did not render enough G/GO on the substrate to present
IR spectra with distinct peaks and therefore, the 2-min
data was not included in the FTIR and EDS analysis on
Fig. 5b-d. The samples coated for 5, 10 and 20-min

Figure . (a) X-Ray Diffractometer spectrum, (b) Fourier transform infrared spectroscopy, (c) EDS elemental analysis, and (d) Raman spec-
troscopy of time-dependent RIT-GO dip coated substrates.
exhibited characteristic peaks of G/GO consistent with
the peaks seen with nanoscale coated samples. The back-
ground peaks correspond to the residual carbon tetra-
chloride seen at 1000 cm−1 is from the seal which is used
to protect the optics on the spectrometer and the peak at
3000 cm−1 is from the water vapor.
Fig. 5c illustrates the SEM-EDS analysis of carbon,
oxygen and copper elements that were present on the
substrates coated at various time durations. A decrease
in intensity is depictive of copper from ∼10,000 counts
to 8,500 counts for 10-min and 20-min coated sam-
ples respectively, whereas the intensity of carbon peak
for 5-min coated substrate was observed to be slightly
higher than 10 and 20-min coated. This difference in
intensities of copper and carbon peaks probably stem
from the presence of taller graphene ridges that could
have been more easily detected by the electron beam
than the flatter carbon structures (as observed in Fig. 4e).
This observation was consistent with the Raman spec-
troscopy data obtained for 5, 10 and 20-min coated
substrates. The Raman spectra verify the characteristic
peaks of G/GO (1580 cm−1 ) and a different in-plane
vibration, D (1350 cm−1 ). The 2D-bands are sensitive
to the stacking order of the graphene layers along the
z-axis, the disappearance of 2D peak in Fig. 5d, verifies
the disordering of graphene sheets also observed with
XRD analysis (Fig. 5a). Such disordering along the z-axis
is caused due to the alignment with respect to each
graphene sheet and due to the presence of oxygenated
functional groups from the existence of graphene oxide
HEAT TRANSFER ENGINEERING 1339
in the sample [31]. In addition to the wettability effects,
the disordering is beneficial as it creates crevices or gaps
on the surface which can act as potential nucleation
sites.
Characterization of CVD-G/GO dip-coated chips: The
characterization and performance of a commercially
available graphene solution prepared via CVD method
(CVD-G/GO) and suspended in a colloid were also
investigated to compare with the RIT-G/GO colloidal
solutions. The CVD-G/GO solution was dip-coated on
the copper substrate for both shorter (2 and 5-mins) and
longer durations (10 and 20-min). Fig. 6 outlines the
scanning electron microscope images of the substrates
coated with CVD-G/GO solutions for 5 and 20-min
durations. The 5-min coated sample produced ridge
like structures that were also reported in Ref. [9] with
similar effects to the ridges observed in the case of 2-min
dip-coating of RIT-G/GO solution in Fig. 4e [19, 32]. The
20-min coating yielded smoother surfaces probably due
to the filling up of the void surfaces between the ridges
due to excess graphene coating similar to RIT-G/GO 20-
min coated samples. This is similar to the laminated film
coating discussed previously. This was also verified by
the broad and splitting 2D peak seen with Raman spec-
troscopy in Fig. 6c for the CVD-G/GO coated substrates
at 20-min duration. The secondary D peak (referred to as
2D peak) was more pronounced showing high intensity
peaks in the case of CVD deposited nanoscale coatings
in Fig. 2c. The lower intensity 2D peaks as seen in Fig. 6c,
result from the splitting of phonon bands and in-plane
1340 A. GUPTA ET AL.

Effect of surface morphology on pool boiling

performance
The CHF obtained for nanoscale (mono and three lay-
ered substrates) and microscale coatings obtained via dip
coating of electrochemically generated and commercially
available G/GO solutions are summarized in Fig 7. In case
of monolayer and multilayer (3 layers) coating the resul-
tant CHF enhancements were found to be 149 W/cm2
and 157 W/cm2 respectively which was ∼20% more than
that of plain copper chip (128W/cm2 ). The microscale
coatings with shortest coating time of 2-min rendered
a CHF enhancement of 182W/cm2 which was ∼45%
as compared to a plain copper chip. The variation in
the CHF values for different graphene coated substrates
and enhancements in case of microscale coatings are
attributed to the surface features arising from rough-
ness modifications, enhanced microlayer evaporation,
and wettability effects. The enhancement observed with
nanoscale coatings was attributed to the liquid wetta-
bility and larger contact angle hysteresis that plays a
pivotal role in the case of coatings comprising of few
layer graphene sheets that lack microscale roughness
features. The microscale coatings contributed to a variety
of morphologies of varying thickness (or heights) as
illustrated in Fig. 4, and 6a,b. As discussed previously,
the 2-min dip-coating of electrochemically generated
RIT-G/GO substrate delivered taller ridge like structures
that extended on the copper surface creating a rough
surface profile as compared to longer duration coated
samples. The enhancement in CHF for 2-min coated
samples is attributed to the combined effects of contact
angle hysteresis, roughness and enhanced microlayer
evaporation as supported by the heat transfer analysis

Figure . JSM- V scanning electron microscope images of (a)

-min,  X, ° tilt, (b) -min  X, top view, and (c) Raman
spectroscopy of time-dependent CVD obtained graphene coated
substrate.

vibrations from parallel and perpendicular alignment

also seen with RIT-G/GO dip coated samples in Fig. 5d
[33, 34]. Thus, in spite of similar structures obtained
for RIT-G/GO and CVD-G/GO time-dependent coated
solutions as observed by scanning electron microscope,
the in-depth Raman analysis demonstrated superior
Figure . Pool boiling data for nanoscale and microscale graphene
ordering of the sheets with RIT-G/GO coatings. and graphene oxide coatings.
 HEAT TRANSFER ENGINEERING 1341

Table . Summary of characterization results and their relation to the pool boiling enhancement mechanisms.
Surface/ Enhancement
Characterization XRD TGA FTIR Raman SEM mechanisms

Monolayer — Chemically stable in Presence of carboxyl High intensity G peak Wrinkle sheets Large contact angle
the boiling and aromatic due to presence of through thermal hysteresis due to
temperature ranges compounds wrinkles deformation of the wrinkled sheets
influencing local underlying copper
wettability substrate
Multilayer Interlayer distance Chemically stable in Presence of chemical Three layers with Wrinkle sheets with Wettability affects
controls the degree the boiling compounds broad D peak disordered layers through large
of wrinkle temperature ranges (carboxyl, aromatic indicating stacking contact angle
formation rings, etc.) disorder hysteresis
influences local Additional
wettability nucleation sites
from stacking
disorder
Long duration Broad peaks Chemically stable Carboxyl and aromatic Parallel and Tightly packed Lacks morphological
dip-coating comprising of between - °C rings influence local perpendicular granules appearing features that
densely packed wettability alignment of as a Laminated film contribute to the
carbon carbon material enhancement
Short duration Broad peaks due to Chemically stable — Morphological Ridges Multiscale roughness
dip-coating disordered carbon between - °C features induced by microstructures features Ridges act
materials disordering of layers as water retaining
slabs for enhanced
microlayer
evaporation

investigation using optical and microscopy techniques in
addition to the correlating with models as demonstrated
earlier [18].
The chemical characterization results are linked to the
pool boiling enhancement mechanisms. A key finding
of this work is the difference in the morphologies and
the mechanisms that determine the varying pool-boiling
performances of multiscale substrates as summarized in
Table 1. This table illustrates the benefits of the monolayer,
multilayer, and dip-coated samples that can be exploited
for pool boiling enhancement. Based on the characteriza-
tion data provided in the present work, it is concluded that
the nanoscale coatings benefit from wettability changes
and additional nucleation sites, while the microscale coat-
ings were influenced by the multiscale roughness features
and ridge microstructures.
samples in the boiling temperature ranges. The Raman
spectroscopy is utilized to understand the stacking order
of the multilayer samples. A disordered stacking results in
the formation of cracks and crevices that serve as poten-
tial nucleation sites. Finally, the SEM sheds lights on the
morphological features which identify the scale effects
that introduce different boiling mechanisms (wettability,
roughness, etc.) at play.
The findings of this work can be incorporated in the
design of efficient pool boiling heat transfer surfaces by
varying the duration of the coatings. The stacking and
ordering dynamics presented here captures the effect of
simple coating techniques that introduce roughness fea-
tures for enhanced heat transfer. This method offers sim-
ple and cost-effective coating method that can easily be
adopted to render varying surface morphology features.

Conclusions Acknowledgments

This paper highlights the structure-property relationship This work was conducted in the Soft Nanomaterials Laboratory,
Department of Chemical Engineering and the Thermal Analy-
of graphene based multiscale coatings and their pool sis, Microfluidics and Fuel Cell Laboratory in the Mechanical
boiling performance quantified by the increase in the Engineering Department at Rochester Institute of Technology,
critical heat flux as compared to a plain uncoated copper Rochester, NY. The authors gratefully acknowledge the finan-
surfaces. A variety of optical and microscopy techniques cial support provided by the National Science Foundation under
is provided to shed light on the composition, ordering CBET Award No. 1335927.
and morphology of the graphene sheets to exemplify the
underlying mechanisms responsible for CHF enhance-
Nomenclature
ment. CVD and dip-coating methods were evaluated <A> Average scattered amplitude
to achieve coatings of varying thicknesses and unique CHF Critical heat flux
CVD Chemical vapor deposition
morphologies. In summary, the XRD results provide
DLS Dynamic Light Scattering
information on the interlayer spacing which determines Ē Applied electric field
the packing of wrinkles and carbon materials in the coat- EDS Energy dispersive –X-ray spectroscopy
ings. TGA and FTIR prove the chemical stability of the FTIR Fourier transform infrared spectroscopy
1342 A. GUPTA ET AL.
G Graphene
GO Graphene oxide
n Refractive index of the medium
RIT Rochester Institute of Technology
SEM Scanning Electron Microscopy
T time
TGA Thermogravimetric analysis
XRD X-ray diffraction
Greek symbols
μEP Electrophoretic mobility
φ Phase shift of the scattered light
λ Wavelength of the light
θ Scattering angle
Notes on contributors
Anju Gupta is an Assistant
Professor in the Chemical Engi-
neering program and Principal
Investigator of the Soft Nanoma-
terials Laboratory at Rochester
Institute of Technology. Her
research interests include for-
mation of microemulsions,
self-assemblies, nanostruc-
tured composites and their
characterization using thermal
analysis (DSC, TGA) and elec-
tron microscopy (cryogenic
SEM and TEM) techniques for biomedical and environmental
applications.
Arvind Jaikumar is a Ph.D.
candidate in the microsys-
tems engineering department
at Rochester Institute of Tech-
nology (RIT). He obtained his
Bachelor’s degree in mechanical
engineering from Visvesvaraya
Technological University, India.
He received his Master of Sci-
ence degree in mechanical
engineering from RIT with a
specialization in thermal and
fluids engineering. He is cur-
rently engaged in creating multiscale structures for enhanced
pool boiling heat transfer.
Satish G. Kandlikar has been
at Rochester Institute of Tech-
nology since 1980 and is cur-
rently the Gleason Professor
of Mechanical Engineering.
He received his Ph.D. degree
from the IIT Bombay in 1975.
He has worked extensively in
the area of flow boiling and
CHF phenomena at microscale,
single-phase flow in microchan-
nels, electronics cooling, and
water management in PEM fuel
cells. He has published over 400 journal and conference papers.
He is the recipient of the 2012 ASME Heat Transfer Memorial
Award. His recent work on pool and flow boiling has produced
exceptionally high heat fluxes along with very high heat transfer
coefficients.
Aniket Rishi is currently pursu-
ing his Master’s Degree in the
Thermal Analysis Microfluidics
and Fuel Cell Laboratory at
Rochester Institute of Technol-
ogy. He completed his Bachelor’s
degree in Mechanical Engineer-
ing from MITCOE, Pune, India.
He is currently working on
enhancing the heat transfer per-
formance using different electro-
chemical deposition methods.
Andrew Layman is currently fin-
ishing up his bachelors in Chem-
istry at Rochester Institute of
Technology (RIT). He will con-
tinue at RIT to pursue his Mas-
ter of Science in Materials Sci-
ence. He is currently engaged in
the creation/study of liposomes
and their interaction with pre-
scription drugs.
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