J. Coat. Technol. Res.
https://doi.org/10.1007/s11998-021-00484-y
Functional properties of zinc-nanographite based nanocomposite
paints for 2–9 GHz microwave absorption
Anjali Prakash, Saranya Narayanan, Kesavamurthy Thangavelu, Avanish K. Srivastava, Mritunjay Kumar Pandey,
Ramamoorthy Nagarajan, Amitava Bhattacharyya
Received: 22 October 2020 / Revised: 1 February 2021 / Accepted: 11 February 2021
Ó American Coatings Association 2021
Abstract Nanographite-zinc particles in various ratios
were synthesized by high energy ball milling and
dispersed in epoxy based aero grade resins for studying
their microwaves absorption in the lower frequency
band of 2–9 GHz using a coaxial waveguide measure-
ment system. Morphological characterizations of the
synthesized particles showed that shuttle shaped zinc is
well embedded on the exfoliated nanographite parti-
cles without any agglomeration. The higher interfacial
polarization of both the graphite and zinc particles
contributes to the excellent electrical conductivity and
hence refers it as an ideal microwave absorber in
defense applications. The paint with 20% (w/v) loading
of nanographite-zinc (1:1 ratio) particles is proficient in
providing microwave absorption of 18.06 dB at 8.19
GHz with a coating thickness of 1.43 mm.
Keywords Nanographite, Zinc, Nanocomposite,
Radar absorbent paints, Microwaves absorbency
A. Prakash, R. Nagarajan, A. Bhattacharyya (&)
Functional, Innovative and Smart Textiles, PSG Institute of
Advanced Studies, Coimbatore 641004, India
e-mail: abh@psgias.ac.in
S. Narayanan, K. Thangavelu
PSG- Keysight Centre of Excellence in Advance Wireless
Technology, PSG College of Technology, Coimbatore
641004, India
A. K. Srivastava
Defence Laboratory, DRDO, Jodhpur, Rajasthan 342011,
India
M. K. Pandey
Directorate of Extra Mural Research and Intellectual
Property Right, DRDO HQ, New Delhi 110011, India
Introduction
Radar absorbing materials (RAMs), also known as
microwave absorbing materials (MAMs), are con-
signed into two categories; one is the magnetic loss
type microwave absorbers attributed to their high
magnetic permeability, and the other is the electric loss
type microwave absorbers where complex permittivity
contributes to the excellent microwave absorption.
Magnetic microwave absorbers include materials such
as ferrites, cobalt, and nickel. They exhibit high mag-
netic permeability owing to their excellent nature of
resonance loss and hysteresis loss. Carbon family
materials, including graphite, graphene, carbon nan-
otubes, and carbon nanowires, are well-known for
their high complex permittivity due to their unrivaled
electrical conductivity and relaxation loss.1 Compared
with such magnetic materials, conductive loss materials
have lower density, good complex permittivity,
and better corrosion resistance as well as weather
resistance.2 Recent years saw the emerging trend of
nanostructured metal oxides being used as microwave
radiation absorbing and shielding materials in the
broad frequency band. Among all the metal oxides
used as microwave absorbing materials, zinc oxide
(ZnO) based materials are preferred considering their
light weight and semiconductor properties.3,4 The
optical, piezoelectric and pyroelectric properties pos-
sessed by ZnO makes it a wide gap semiconductor well
equipped for next generation electronic and optoelec-
tronic applications. Also nanostructured ZnO pos-
sesses novel and unique physical properties such as size
effect, confinement effect, peculiar exciton polariza-
tion, electronic photon coupling, photoluminescence,
spectrum properties, strong-exciton photon coupling
effect, blue emission, volt effect, solar cell, and super
hydrophobic behavior.5 Recently, the microwave
absorption properties of ZnO have attained huge
interest among researchers. Chen et al. reported the
J. Coat. Technol. Res.
use of ZnO based materials for microwave absorption
in 2004. They synthesized ZnO nanowires by the direct
evaporation of metal zinc powders under air ambient
without any catalyst. It was reported that the micro-
waves absorption of the composites (thickness 1 mm)
with 6% and 7% ZnO nanowires were 8.37 and 12.28
dB, respectively, in the X band frequency range.6 Yan
et al. reported the use of three-layered graded ZnO
nano whiskers/ polyester composites for studying their
dielectric response and microwave absorption proper-
ties. The highest absorption obtained was 21.48 dB at
16.4 GHz frequency suggesting that the three layer
gradient distribution exhibits excellent absorption
performance and concluded that as the thickness of
the absorber increased, the absorption also reached a
maximal value.7 Cao et al. reported the use of cage like
ZnO/SiO2 nanocomposites for microwaves absorption.
The micro current network produced in the composite
due to the unique geometrical morphology of the cage
like ZnO nanostructures contributes well to the con-
duction losses and hence exhibits relatively strong
attenuation to the microwave in the X band.8 Fang
et al. reported that tetra needle like ZnO nanostruc-
tures showed a strong microwave absorption of 12 dB
at 11 GHz. The literature also stated that even though
the ZnO nanostructures show excellent absorption
properties both in the X band and Ku band region, the
mechanisms of microwave response and quantitative
energy attenuation have not yet been ascertained.9
Later, Feng et al. synthesized reduced graphene oxide
decorated with ZnO nanocrystals that exhibits extre-
mely high microwave absorption of 54.2 dB at 6.7
GHz and with an absorber thickness of 2.4 mm, and
they explained the mechanisms inside the composite in
detail.10 Huang et al., in their literature based on the
tunable electromagnetic properties and enhanced
microwave absorption ability of flaky graphite/cobalt
zinc ferrite composites, reported that the real part and
imaginary part of complex permittivity increased
dramatically with the increase of graphite weight ratio
in the composite owing to the well-known conductive
and dielectric loss of the carbon materials including
flaky graphite. The composite with 20 wt% graphite
showed a microwave absorbency of 33.85 dB at 11.7
GHz when the coating thickness was 2.5 mm.5 Yang
et al. reported the wide frequency absorption band of
the nanostructured zinc oxide/zinc/carbon fiber over
the ranges of 2.7–18.0 GHz and the reflection loss (RL)
values obtained were less than 5 dB and 7 dB,
respectively, for 1.0 mm and 4.5 mm thicknesses.11 In
2019, Yang et al.12 reported the synthesis of 3 dimen-
sional graphene/ shuttle shaped zinc oxide composites
which exhibited an outstanding microwave absorption
performance of 48.05 dB at 11.07 GHz at a given
thickness of 1.5 mm.
While comparing all the works mentioned above,
only a few studies reported the microwave absorption
properties of zinc metal or its oxide combined with
carbon allotropes for their microwaves absorption in
the lower frequency bands of 2–9 GHz. The microwave
absorption and attenuation properties of zinc metal
powder have not yet been explored. The conventional
microwave absorbent materials, such as carbonyl iron,
ferrites, and nickel, are quite heavy in nature due to
high density. These types of ferrite materials also lack
corrosion resistance and weather resistance when used
in various defense applications.
In this study, different ratios of nanographite-zinc
powders were prepared using high energy ball milling
and characterized. Further, they were dispersed in aero
grade epoxy resins and tested for their microwave
absorbency at a lower thickness of 1.4 mm to
understand their suitability for microwave absorption
in the range of 2–9 GHz.
Materials and methods
Graphite fine powder extra pure was procured from
Loba Chemie, India, which is insoluble in water with
99.9% carbon content and particle size of 60 mesh.
Zinc metal powder with a molecular weight of 65.39
and 99.995% trace metals basis with a particle size of
about 150 lm was purchased from Sigma Aldrich,
USA. Solvents like toluene were purchased from
Sigma Aldrich, USA. Epoxy based aero grade resins
(Zigmalac Epoxy HB ZP 2K Primer) were pur-
chased from Ishan Paint Industries, India. Unless
otherwise stated, all reagents were of analytical
grade and used as received without further purifica-
tion. Hybrid nanographite-zinc powder samples were
synthesized by wet ball milling, where both nano-
graphite powder and zinc metal powder were intro-
duced with toluene in ball milling equipment
(FRITSCH PULVERISETTE 5 Classic Line) (300
rpm, 10 h, Stainless steel ball: Sample powder; 10:1
w/v; vial capacity 35–50 g each, ball diameter 3 mm)
followed by 48 h solvent drying at room tempera-
ture. Nanographite powders were prepared from
graphite13 using our laboratory optimized protocol of
10 h wet ball milling in toluene using the same
machine conditions. Five sample powders with dif-
ferent ratios of nanographite and zinc were prepared
(yield 98%). The prepared powder samples (20% w/
v) were dispersed in epoxy based aero grade resins
(Zigmalac Epoxy HB ZP 2K Primer) in a bead
milling equipment (NETZSCH MINICER Labora-
tory Bead mill; 140 mL capacity; zirconia beads of
0.3 mm diameter). The process was continued for 1 h
at 15 rpm and 1200 rpm peristaltic pump speed and
chamber speed, respectively, and then further in-
creased to 4200 rpm. Finally, the product obtained
after dispersion was mixed with hardener (resin:
hardener; 3:1). All 5 paint samples thus obtained
were used for coating on aluminum sheets (4 cm 9
4 cm; 0.5 mm thickness). A primer coating was
applied prior to the sample coating. The final
thickness of the Al sheets after coating the paint
samples are coded as per Table 1.

Table 1: Thickness of the Al sheets after final sample coating
Sl. no. Sample code Nanographite:zinc weight ratio
1 NG 0.1Zn 0.9 1:9
2 NG 0.2Zn 0.8 2:8
3 NG 0.3Zn 0.7 3:7
4 NG 0.4Zn 0.6 4:6
5 NG 0.5Zn0.5 5:5
Characterization
Crystal phase characterizations of the samples were
done by X-ray power diffraction using CuKa (k = 1.54
A°) radiation (XRD, Empyrean Malvern Panalytical
multipurpose diffractometer). The samples were
scanned from 5° to 130° in 2h. The surface morphology
and microstructure of the sample powders were deter-
mined by scanning electron microscopy (SEM, ZEISS,
EVO18, Germany), followed by energy dispersive X-
ray spectroscopy. Rheological properties were mea-
sured using a modular compact rheometer (MCR 102,
Anton Paar, GTD 620). For that, an equal amount of
paint thinner was added to the paints for dilution. 20%
(w/v) powders were used to prepare the paints similar
to the process mentioned above. To study the electro-
magnetic waves absorption of the samples and to
understand the complex permittivity and permeability
of the materials along with its reflection loss, measure-
ments were done using a vector network analyzer
(Keysight Technologies, Agilent Keysight Field Fox
Microwave analyzer N9915A) where aluminum sheets
(4 cm 9 4 cm; 0.5 mm thickness) coated with paint
samples were probed on to the waveguide. Impedance
analysis of the samples was carried out in E4990A
impedance analyzer, Keysight Technologies, USA,
using dielectric test fixture. Impedance from 20 Hz to
20 MHz frequency range was reported.
Results and discussions
Morphological analysis and microstructure
of samples
The phase structures of all the samples were measured
by X-ray diffraction spectroscopy (Fig. 1). The main
diffraction peaks at 2h = 36.0, 38.7, 54.1, and 69.9
corresponding to the (002), (100), (102), and (103)
crystal planes, respectively, can be well indexed to the
shuttle shaped zinc metal particles in accordance with
JCPDS 04-0831.11 It can be observed from the spectra
that the intensity and peak broadening are decreased
with the reduction in zinc ratio in the samples. A small
amount of zinc oxide is also formed during the wet ball
milling process and the minor peak at 2h = 31.77 is
observed for hexagonal structured zinc oxide with the
J. Coat. Technol. Res.
Epoxy primer-4 layer + top coat 20% loading thickness (mm)
1.45±0.005
1.42±0.005
1.39±0.005
1.42±0.005
1.43±0.005
e NG 0.5 Zn 0.5
d NG 0.4 Zn 0.6
c NG 0.3 Zn 0.7
Intensity (a.u.)
b NG 0.2 Zn 0.8
a NG 0.1 Zn 0.9
20 40 60 80 100 120
2θ (degree)
Fig. 1: XRD plot of the nanographite-zinc powder samples
crystal plane (100) (JCPDS 36-1451).10 The diffraction
peaks at 2h = 26.5, 44.4, and 83.3 correspond to the
(002), (101), and (112) crystal planes of nanographite
referred to JCPDS 41-1487.4 The lower intensity
diffraction peaks correspond to nanographite are not
found in the samples suggesting that the Zn metal or
zinc oxide particles may have aggregated on the
graphite particles and a portion of graphite may
have converted to amorphous during high energy ball
milling. The diffraction peaks of the samples are coded
in Table 2.
The structural morphologies and microstructures of
the samples were further studied by SEM analysis.
Fig. 2 shows the SEM images of all 5 samples. The
SEM images of zinc under low magnification show that
the particles are agglomerated and complete separa-
tion does not occur in the initial stage. The zinc
nanoparticles observed at high magnification reveal
that the particles are held together due to weak
physical forces.14 SEM image (Fig. 2b) shows that the
sizes of the zinc nanoparticles are in the range of 400
J. Coat. Technol. Res.

Table 2: Major X-ray peaks observed in accordance with the Joint Committee on Powder Diffraction Standards
database
Sl. no. Peak (2h degree) Miller indices Contribution JCPDS no.

1 26.5 002 Nanographite 41-1487

2 31.77 100 Zinc Oxide 36-1451
3 36.0 002 Zinc 04-0831
4 38.7 100 Zinc 04-0831
5 44.4 101 Nanographite 41-1487
6 54.1 102 Zinc 04-0831
7 69.9 103 Zinc 04-0831
8 83.3 112 Nanographite 41-1487

Fig. 2: SEM and EDAX images of (a) nanographite particles, (b) NG 0.1 Zn 0.9, (c) NG 0.2 Zn 0.8, (d) NG 0.3 Zn 0.7, (e) NG 0.4
Zn 0.6, (f) NG 0.5 Zn 0.5, respectively

nm to 2 lm. As the size of the particle gets reduced, the
surface to volume ratio of the nanostructured materials
increases and hence can be correlated to the strong
absorption. It is also noticed that the sample with equal
ratios of nanographite and zinc exhibits better exfoli-
ation and intercalation which can also be attributed to
better microwaves absorption. This effect may be due
to the increase in interfacial polarization of the
crystallites. The results from EDAX spectroscopy give
a proof for the uniformity and dispersity of the
particles in the composite which could be beneficial
to increase the interface interaction between the
materials. Wet ball milling instead of dry ball milling
allows easy introduction of surface active media which
reduces the required energy for the inhibition of
aggregation of fine particles. Due to wide adsorption,
it is only possible to introduce such materials in
gaseous or vapor form into dry milling and thus the
only practicable method of introducing substance in
gaseous form is wet ball milling. Due to the formation
of oxides during this wet milling process, traces of such
can also be seen in the EDAX spectrum. The
percentage weights of each component in the samples
are shown as Table 3.
Rheological properties and behavior
The rheology of nanographite-zinc suspensions plays
an important role in the painting process. An addi-
 J. Coat. Technol. Res.

Table 3: Weight percentage of carbon, zinc, and oxygen in each powder sample as per EDAX data
Sl. no. Composition of particles Weight % of carbon (C) Weight % of zinc (Zn) Weight % of oxygen (O)

1 NG 0.1 Zn 0.9 27.84 69.71 2.45

2 NG 0.2 Zn 0.8 31.09 65.68 3.22
3 NG 0.3 Zn 0.7 53 43.62 3.38
4 NG 0.4 Zn 0.6 73.44 23.12 3.44
5 NG 0.5 Zn 0.5 67.01 26.47 6.52

tional loading of 20% (w/v) micro/nano particle on 400

a NG 0.1 Zn 0.9
paint would change the rheological properties of the b NG 0.2 Zn 0.8
paint which may make it unsuitable for painting or c NG 0.3 Zn 0.7
coating. The increase in viscosity due to addition of any 300 d NG 0.4 Zn 0.6

additive is dependent on the specific volume and
surface area of the additive. The lower the density,
the higher the specific volume is, which in turn
increases the viscosity of the paint. As the density of
graphite (2.266 g/cm3) is much less than zinc (7.133 g/
cm3), the specific volume and surface area of the
nanographite-zinc nanoparticles will also increase with
the increase in nanographite content (weight ratio).
Hence, the viscosity increase effect would be higher for
higher nanographite containing nanoparticles with
similar amount of additive loading (20% w/v). Loading
of zinc rich nanoparticles in the paint is easier than
nanographite rich nanoparticles due to their lower
volume and surface area. Our observations are also
similar to this. Due to the higher aspect ratio and
surface area of nanographite compared to zinc, NG 0.5
Zn 0.5 sample shows higher shear stress and higher
viscosity which make it challenging for a continuous
coating process (Fig. 3). On the other hand, it shows
much better shear thinning property with the power
law index decreasing. However, even at high shear
rate, it did not reach to the lower viscosity level of the
pure paint or low graphite content paints. It can be thus
stated that with an increase in the graphite content, the
paint viscosity significantly increases, though the shear
thinning tendency also enhances which may help in
uniform coating or painting processes. Figure 3 exhibits
the same trend along with the decrease in viscosity due
to low graphite content.
Electromagnetic characteristics and microwave
absorption properties
The reflection loss (RL) of the nanographite-zinc
samples were measured in the 2–9 GHz frequency
band. The measured RL values of all 5 nanographite-
zinc samples are shown in Fig. 4a. The maximum
absorption of 18.06 dB at 8.19 GHz is shown by the
painted sample with equal ratios of nanographite and
zinc particles; i.e. NG 0.5Zn 0.5. This may be due to
the increase in interfacial polarization at the sample
Viscosity (Pa·s)
e NG 0.5 Zn 0.5
f Control sample
200
(e)
100
(c, d)
(a, b, f)
0
5 10 15 20 25
Shear rate (1/s)
Fig. 3: Viscosity vs shear rate of nanographite-zinc based
paints
interfaces with increase in surface area percentage.
Also with a decrease in the particle size, the zinc
interstitial size increases which contributes to the
higher electrical conductivity due to the properties
exhibited by n-type semiconductors. In the samples
with equal amounts of zinc metal particles and
nanographite particles, intercalation becomes much
easier so that the electromagnetic wave impedance
matching could be more enhanced by reducing the
reflection of incident EM waves from the absorber
surface.10 Strong microwave absorbency properties can
be achieved further by increasing of mass fraction in
the composites.15 The maximum reflection loss values
of the measured nanographite-zinc samples improved
with increase in nanographite fractions, but the band
width becomes narrower. The maximum RL values
with an increase in graphite content are 3.94 dB at 8.00
GHz, 5.93 dB at 8.28 GHz, 11.28 dB at 8.59 GHz, 14.33
dB at 7.74 GHz, and 18.06 dB at 8.19 GHz, respec-
tively.
The impedance values of the nanographite-zinc
coating samples were measured and the values were
plotted against frequency from 20 Hz to 20 MHz
(Fig. 4b). Among all the sample coatings, NG 0.5 Zn
0.5 and NG 0.4 Zn 0.6 showed linear impedance or
frequency-independent electrical conductivity over the
frequency range, indicating the formation of a com-
J. Coat. Technol. Res.
(a)
0
a
—5
R.L (dB)
—10
—50
—20
2 4 6 8
Frequency (GHz)
Fig. 4: Nanographite-zinc based painted samples: (a) reflection loss curves (inset, laboratory wave guide measurement
setup), (b) impedance curves
plete conducting network. The formation of such a
continuous network was achieved because of the high
aspect ratio and more surface to volume ratio of
nanographite. The nanoparticles of graphite form a
continuous conductive network in the composite coat-
ing, attributed to the easy electron transfer throughout
the composite.16,17 It can also be observed from the
figure that the coatings with lower nanographite
content show the higher impedance along with fre-
quency dependence.
Conclusions
Nanographite-zinc particles in various ratios were
synthesized using the high energy ball milling instru-
ment. These powder samples of various ratios were
dispersed in aero grade epoxy paints for producing
hybrid radar-absorbent paints. The impedance proper-
ties and reflection loss of the prepared coatings were
measured using a waveguide microwave analyzer and
the sample with equal ratio of nanographite and zinc
gave the best absorption results with reflection loss of
18.06 dB at 8.19 GHz. As the weight percentage of
nanographite increases, the absorption of EM waves
also increases.
Acknowledgments Authors like to express their deep
gratitude to the Directorate of Extramural Research
and Intellectual Property Rights, Defence Research
and Development Organization (DRDO) (ERIP/ER/
1502251/M/01/1674), Govt. of India, for the financial
support and the management of PSG Institutions, for
their laboratory supports to carry out this work.
Conflict of interest The authors declare that they
have no conflict of interest.
105
(b) a NG 0.1 Zn 0.9
b NG 0.2 Zn 0.8
c NG 0.3 Zn 0.7
104 d NG 0.4 Zn 0.6
a e NG 0.5 Zn 0.5
b 103 b
|Z| (ohm)
c
d
102
c
d 101 e
e
100
0.0 5.0 × 106 1.0 × 107 1.5 × 107 2.0 × 107
Frequency (Hz)
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