Applied Nanoscience

SYNTHESIS AND CHARACTERIZATION OF POLYANILINE/ZINC OXIDE

NANOCOMPOSITES FOR HYDROPHILIC APPLICATIONS
--Manuscript Draft-Manuscript Number:
Full Title:

SYNTHESIS AND CHARACTERIZATION OF POLYANILINE/ZINC OXIDE

NANOCOMPOSITES FOR HYDROPHILIC APPLICATIONS

Article Type:

Original Article

Keywords:

polyaniline; Zinc Oxide; Yeast; TEM; FT-IR; Contact Angle Goniometer; Anti-Fog;
ultrasonication

Corresponding Author:

siddhartha narasimhareddy morramreddy, M.Tech

jntu hyderabad
hyderabad, telangana INDIA

Corresponding Author Secondary

Information:
Corresponding Author's Institution:

jntu hyderabad

Corresponding Author's Secondary

Institution:
First Author:

siddhartha narasimhareddy morramreddy, M.Tech

First Author Secondary Information:

Order of Authors:

siddhartha narasimhareddy morramreddy, M.Tech

Order of Authors Secondary Information:

Funding Information:
Abstract:

A one step Polyaniline/ Zinc Oxide nanocomposite was prepared by self-assembly

method via ultrasonication with different weight ratios. Polyaniline is a conducting
polymer of the semi-flexible rod polymer family. Zinc Oxide was prepared by thermal
decomposition method with the help of microbial method using yeast as reducing
agent. Polyaniline was prepared by using oxidative polymerization technique in
emeraldine salt which is conducting in nature. The structure and morphological
characterization have been investigated by scanning electron microscopy (SEM),
transmission electron microscopy (TEM), X-Ray Diffraction (XRD), Fourier Transforms
infrared spectroscopy (FT-IR) and thermogrametric analysis (TGA). From
Thermograms it is evident that there is an increase of melting point of composites
when certain amounts of zinc oxide was to polymer. Furthermore with contact angle
goniometer (CAG) for PANI and different concentrations of PANI/ZnO nanocomposites
coatings were found to be hydrophilic in nature. Anti-fog property has also been
verified for the hydrophilic coatings made which were semi-permanent.

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SYNTHESIS AND CHARACTERIZATION OF POLYANILINE/ZINC

OXIDE NANOCOMPOSITES FOR HYDROPHILIC APPLICATIONS
Morramreddy Siddhartha Narasimha Reddy
Centre for Nano Science and Technology, I.S.T, Jawaharlal Nehru Technological University Hyderabad-500
085, Telanagana, India

Abstract:
A one step Polyaniline/ Zinc Oxide nanocomposite was prepared by self-assembly method via
ultrasonication with different weight ratios. Polyaniline is a conducting polymer of the semiflexible rod polymer family. Zinc Oxide was prepared by thermal decomposition method with
the help of microbial method using yeast as reducing agent. Polyaniline was prepared by using
oxidative polymerization technique in emeraldine salt which is conducting in nature. The
structure and morphological characterization have been investigated by scanning electron
microscopy (SEM), transmission electron microscopy (TEM), X-Ray Diffraction (XRD),
Fourier Transforms infrared spectroscopy (FT-IR) and thermogrametric analysis (TGA). From
Thermograms it is evident that there is an increase of melting point of composites when certain
amounts of zinc oxide was to polymer. Furthermore with contact angle goniometer (CAG) for
PANI and different concentrations of PANI/ZnO nanocomposites coatings were found to be
hydrophilic in nature. Anti-fog property has also been verified for the hydrophilic coatings
made which were semi-permanent.
Keywords: polyaniline, Zinc Oxide, Yeast, TEM, FT-IR, CAG, Anti-Fog.
forming droplets. Anti-fog applications are also

1. Introduction

found in our daily life such as when a food item is

In recent years, the necessity of anti-fog surfaces has
been reported for applications of PEM fuel cells [1].
Hydrophilic nature has been developed by different
phylogenetic independent group of plants and
organs

caused

by

different

nanostructures.

Hydrophilicity plant surfaces can be divided into

packed in refrigerator cabinet, the relative humidity

inside the package increases due to decrease of
temperature which tends the water molecules to
condense on the inner surface. Therefore, the
surfaces can retain its visual clarity even when
relative humidity is high.

those that are permanently wet, absorb water over

their surfaces and let water over the surface. These

Min

Nie

et

al

[2]

has

prepared

types of hydrophilic nature can be seen in plants

superhydrophilic Anti-Fog polyester film by oxygen

such as Ruellia devosiana, Alocasia odora, Anubias

plasma treatment. Yueken Lai et al

barteri and so on. The hydrophilicity induced by

transparent Superhydrophobic/ Superhydrophilic

polar functional groups such as OH and COOH

TiO2 based material for Anti-Fog coatings with high

bonds which leads in spreading of water on the

chemical stability and self-cleaning ability. Faheem

surface to form a thin layer of water instead of

ahmed et al

[4]

[3]

has prepared

has successfully synthesised

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polyaniline/ zinc oxide films by using solution

with 25ml of 1M H2SO4 at room temperature.

casting method. In this Paper, we demonstrate

Ammonium peroxy sulphate solution was prepared

polyaniline/ zinc oxide based hydrophilic coatings

by adding 2.3grams of Ammonium peroxy sulphate

for anti-fog application

powder in 5ml of 1M H2SO4 solution. As prepared,

(NH4)2S2O8 solution was added drop wise to the

2. Experimental
2.1.

Aniline solution with continuous magnetic stirring.

Materials Required

The stirring was continued for 2 hours and then,

Aniline monomer (Finar chemicals, India Pvt. Ltd),

Sulphuric Acid, Ammonium Peroxy sulphate (Finar
chemicals, India Pvt. Ltd), Yeast (eagle foods), Zinc
acetate (Finar chemicals, India Pvt. Ltd),M-Cresol (
merk chemicals), Tetrahydrofuran( finar chemicals),
poly vinyl pyrolidone(K-30), Acetone, Ethanol, and
Distilled Water were used in the synthesis process in
their pure form without any further modification.

2.2.

Synthesis

of

Zinc

Oxide

obtained dark green solution was vacuum filtered

and the precipitated wet cake was obtained. The
resulting emeraldine salt was filtered by vacuum
filtration, and washed copiously with ethanol,
acetone and deionized water in order to reduce its
pH to 7. Care must be taken that product is
completely washed so that any unreacted oil will be
removed. Finally, the solution was vacuum filtered
and the product was dried in vacuum oven for 24
hours. The final product was crushed to obtain

nanoparticles (ZnO)

polyaniline in emeraldine salt form which is

Zinc oxide nanoparticles were synthesized by

conductive in nature.

thermal reduction method using zinc acetate and

2.4.
Synthesis of Polyaniline zinc
oxide nanocomposite

yeast as precursors. 1.1 M of zinc acetate was

dissolved in distilled water and magnetically stirred
to attain homogenous mixture at 116F. 5 grams of
yeast was dissolved in distilled water. Then the
solution was heated 116 F temperature for activating

The zinc oxide and polyaniline obtained in the

previous steps were taken in the following weight
ratios as shown in table (1).

the yeast content in it and the solution is

magnetically stirred for 1 hour. The solution will

Name

Polyaniline

Zinc oxide

PZ1

0.1 grams

0.03 grams

PZ2

0.1 grams

0.07 grams

PZ3

0.1 grams

0.1 grams

slowly dissolve as the temperature increases which

indicates the activation of yeast. Then the activated
yeast solution was mixed in zinc acetate solution
drop by drop and magnetically stirred for 4 hours by
maintaining the temperature between 110F to 116F.
Then the homogenized mixture of yeast & zinc
precursor was kept on hotplate and heated at 2500C
for 3 hours. A brown precipitate was obtained and
0

further this was calcined at 450 C for 4 hours to

Table 1: different weight ratios taken for

composites preparation

remove the traces of impurities.

PZ1, PZ2, PZ3 sample were mixed with 20 ml of

2.3.

Tetrahydrofuran and sonicated in the ultrasonicator

Synthesis of Polyaniline (PANI)

Polyaniline (PANI) was prepared using chemical

polymerization route, briefly 2ml Aniline was mixed

for 3 hours. Then the solution is subjected to heat for

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solvent evaporation. Tetrahydrofuran is used to

pendent drop analysis method. The films showed

remove the unreacted oligomers.

hydrophilic nature due to the presence of OH

2.5.

Preparation of Pani/ZnO thin film

In brief, the preparation of Pani/ZnO thin film

A- 13.8

B- 12.6

D- 15.8

C- 13.4

includes the following procedure. At first 0.05

grams of PZ1, PZ2, PZ3, PANI were suspended in
20 ml of m-cresol in different beakers. These
solutions were ultrasonicated for 1 hour for
dissolving the samples in m-cresol. Then the
ultrasonicated sample is gravity filtered with the
help of whatmore filter paper with a pore size of 44
to remove the undissolved crystals. All the filtered

Fig 1. Contact angles of PANI(A), PZ1(B), PZ2(C), and

PZ3(D)

solutions were kept aside for further making of thin

films.

bondings. Due to porous nature of zinc oxide when

10 ml of the solutions were magnetically stirred at

the water molecule is dropped on the surface, the

900 rpm, 400C and further, 1.1grams of polyvinyl

water molecule spreads freely on the surface

pyrrolidone (k-30) was added slowly for obtaining

forming hydrophilic angles. Basically OH bondings,

gel for thin films coatings.

COO- bondings, Aln(OH)m bondings are more
The gels obtained so far were coated on to a plain
microscopic glass substrate of size 2cm*2cm at

wettable.

More

wettability

indicates

more

6000 RPM for 60 sec, the thin films obtained were

hydrophilicity which finds its major applications in

thermally dried at 1500C for 2 hours.

antifogging and antifouling applications.

3. Results and discussions

The below histogram shows the contact angle for as

3.1.

Contact

Angle

Measurement

prepared different concentrations of thin films.

Analysis
To know the hydrophilicity of the samples, we used
contact

angle

goniometer

for

contact

angle

measurement in random areas/spots. Fig1 (A.B.C.D)

shows the contact angle images of as prepared and
annealed Polyaniline/ZnO thin films. The readings
were taken at different areas of the substrates.
The as such films showed the contact angle of 13.80
for pure Polyaniline thin film which varied from
12.60 to 15.80 on addition of Zinc oxide to pure
polyaniline i.e. for samples named PZ1, PZ2, PZ3
and the contact angle was measured using the

Figure 2: contact angles of PANI, PANI/Zinc composites

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3.2. Energy Dispersive Analysis of XRay (EDAX)

From figure 3. (A, B) we can clearly infer that the

EDAX studies are generally carried out to test the

structures which indicates the presence of zinc oxide

composite has cubic structures and spherical

purity of the sample by giving the details of all the

elements present in given sample. The EDAX

and

polyaniline.

Fig

3(A)

shows

uniform

analysis of polyaniline contains 43.93%, 56.07% of

distribution of ZnO nanoparticles in the polyaniline

carbon and nitrogen respectively confirms the

matrix. Pristine ZnO lm is composed of well

authenticity of polyaniline. Zinc oxide sample

contains 19.36 %, 2.05 %, 78.59 % of oxygen,

crystalline, cubic shaped ZnO nanoparticles of size

potassium & zinc respectively. It confirms the

27 nm (from XRD) and 26.7 nm (from TEM), shown

presence of potassium impurity in zinc oxide

in Fig.3(A). The incorporation of ZnO nanoparticles

sample. Composite of polyaniline/zinc oxide PZ 2

has 30.29%, 27.38%, 17.71% & 24.62% of carbon,

into the PANI matrix in PANI/ZnO nanocomposites

nitrogen, oxygen and zinc elements % respectively

thin lm could be seen from Fig.3C and also there

and with the presence of zinc element in composite

exists a sandwiched layer which confirms that the

we can confirm that the composite has been formed.

composite has been formed .The average particle

3.3.

Transmission Electron
size calculated from figure.3 (D) is 30.8 nm. The

Microscope
particle size distribution is represented graphically
By

using

transmission

electron

microscope

in figure (4) where x axis represents particle size

micrographs we can find lattice structures and

interplanar spacing. Composite PZ2 was examined

and y-axis represents number of particles

for TEM micrographs.

A

Figure (4) particle size distribution of PANI/ZnO

nanocomposite

3.4.

Scanning Electron Microscope

Scanning Electron Microscope (SEM) was used to

image the morphology and structure data. Fig 5
Fig (3) - (A), (B), (C), (D) TEM micrographs of PANI/ZnO
composite

shows the micrographs of polyaniline, zinc oxide &

polyaniline/zinc oxide nanocomposite at different
magnifications. The particles were agglomerated to
form clusters of micro particles. Fig (5.B) states

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spherical shaped morphology for polyaniline SEM

peaks are given in Table (2). The characteristic

micrographs. In the figure (5.D) from the SEM

absorption bands of PANI are 511 cm-1 (C NC

micrograph we can infer that the zinc oxide is porous

bonding mode of aromatic ring), 621 cm-1 and

in nature and will increase liquid-solid interfacial

area, provides a path for movement for ions and
ensures a high reaction rate

[10]

.we can also observe

the connected like network in the form of Nanofibers

in fig. 5(f) which may have been due to the effect of
ultrasonication.
Fig 5. SEM micrographs of PANI, ZnO, PANI/Zinc

Fig 6 FT-IR spectra of (a) ZnO, (b) Pz1, (c) Pz2, (d) Pz3, (e) Pani

700cm-1 (CC, CH bonding mode of aromatic

ring), 875 cm_1 (CH out of plane bonding in
benzenoid ring), 1070 cm-1 and 1118 cm-1 (S=O
bonding for sulphuric acid), 1303 cm-1 and 1500 cm1

(CN stretching of benzenoid ring) and 1560 cm-1

(C=N stretching of quinoid ring).

Wavenum
ber (cm-1)
472
In fig 5(E) there exists a combination of dark and
white coloured particles where the white coloured

510-621

zinc oxide particles are decorated around the dark

651-700

coloured polyaniline. From The above information

775-900

we could possibly confirm the formation of

composite.

3.5. Fourier Transform

Spectroscopy (FTIR)

Infrared

To further know the functional moieties in the

composites,

FT-IR

was

recorded

and

Stretching of C-O bonding

C-N-C bonding mode of
aromatic ring
C-C, C-H bonding mode of
aromatic ring
C-H out of plane bonding in
benzenoid ring

1070-1118

S=O bonding for sulphuric acid

1230-1310

C-N stretching of benzenoid ring

C-C stretch in benzene ring
C=N stretching of quinoid ring
Interaction between ZnO and
PANI by formation of hydrogen
bonding between H-N and
oxygen of ZnO

1500-1400
1600-1585
3284

the
3500-4000

corresponding figure 6.

Functionality

Vibration band of -OH

Table 2: characteristic absorption peaks obtained from FT-IR

PANI

and

PANIZnO

nanocomposites

were

characterized by using the FTIR technique. Fig (6)

spectrum

shows the FTIR pattern of ZnO, PANI and PANI

The PANIZnO nanocomposites show some of the

ZnO nanocomposites and characteristic absorption

same characteristic peaks as for polyaniline and zinc

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oxide. However, there is an evidence of peak

polymer (PANI) chain. The PANI peak diffracted at

displacement when ZnO nanoparticles are added to

an angle of 2(theta) =19.97 and 2 (theta) =24.60. In

-1

the PANI. These shifts include 15601600 cm ,

the XRD pattern which shows low crystallinity of

15001529 cm-1, 11181141 cm-1, 10701047 cm,

the conductive polymers due to the repetition of

-1

-1

875775 cm , and 621651 cm . furthermore, in

PANIZnO nanocomposites, a broad peak appeared
in 3437 cm-1 which can be associated to the
interaction between ZnO and PANI by formation of
hydrogen bonding between HN and oxygen of
ZnO, so the peak displacement which was observed
in FTIR spectra may be ascribed to the formation of
hydrogen bonding between ZnO and the NH group
of PANI on the surface of the ZnO nanoparticles
7]

[6,

which inuences the electron densities of the

PANI chain. For instance, CN, CN and C=C

bonds are shifted to the higher wavenumbers which
are stronger in nanocomposites while NH is shifted
to the lower one which is weakened.

3.6.

XRD Analysis

XRD analysis was used to examine the structure of

the PANI and PANIZnO nanocomposites and
investigate the effect of the various amounts of ZnO

benzenoid and quinoid rings in PANI chains [8].

Fig. 7 shows that intensity of the peaks was
increased by increasing amount of ZnO nanorods
which means that there is an interaction of ZnO
nanorods and PANI by formation of hydrogen
bonding between HN and oxygen of ZnO

[5]

Presence of zinc peaks at 2 theta = 31.8 , 34.43 ,

36.230 in the composites PZ1, PZ2, PZ3 clearly
depicts the presence of zinc nanoparticles in the
nanocomposites. Moreover the crystal planes at 100,
002, and 101 of composites tends to reduce the
intensity as the amount of zinc oxide particles
reduces. There also appears a broad peak at 2 theta
= 70 where their intensity has been increasing with
decreasing amounts of ZnO nanoparticles probably
due to the interactions of impurities in zinc and
polyaniline.

3.7.

TG Analysis

nanoparticles on the PANI structure .Fig (7) shows

the typical XRD patterns of PANI and PANIZnO
nanocomposites.

The thermo gravimetric (TGA) analysis of PANI,

PANI/ZnO composites (PZ1, PZ2, PZ3) under
heating rate of 100C/min.

Fig 7 XRD patterns of PANI, PZ1, PZ2, and PZ3

Fig 8 Thermograms of PZ1, PZ2, PZ3 and PANI

As is evident in PANI and its nanocomposites, broad

As in Fig 8 the results reveal that the trend of PANI

diffraction peaks occur between 101 and 301 due to

ZnO nanocomposite degradation is similar to PANI.

the parallel and perpendicular periodicity of the

It can be seen that the thermal degradation of PANI

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occurs at 2600C and the initial mass loss at lower

uniform flow of steam as shown in figure 9(a). After

temperature is mainly due to release of either water

exposing the slides the water tends to spread flatly

(up to 150 C) or dopant anions. Also, the weight loss

to form a thin layer which can be verified with the

occurring right after 3000C corresponds to the

results of contact angle goniometer. On the uncoated

decomposition of the polymer.

side of the slide the water droplets started to form

In composites PZ1, PZ2 and PZ3 an initial weight

loss at 1400C, 2130C, 2160C occurred mainly due to
evaporation of water or due to dopant anions and

small droplets of water molecules but on the coated

side, the slide was clean without condensation of
water droplets as shown in fig 9(a).

weight loss occurring at 3600C, 3750C and 3800C

corresponds to the decomposition of polymer
material. In PANIZnO composites, decomposition
A

is reduced when compared to polyaniline because of

a strong interaction at the interface of ZnO and PANI
[8, 9]

, which supports our claim that the presence of

Fig 9 films after exposing to vapour (a) good film, (b) partially
damaged film

ZnO nanoparticles can improve properties of the

One disadvantage is after exposing the slide to high

polymer.

and

steam temperature for long time as shown in fig 9(b),

degradation of materials, total residues of 17.53

the film tends to break permanently but the film

(wt.%) for PANI and 4.15, 35.17 and 35.378 (wt.%)

continuous to exhibit anti-fog property with very

for nanocomposites namely PZ1, PZ2 and PZ3

less or no reduction.

Finally,

after

decomposition

respectively.

3.8.

Application Of Hydrophilicity

4. Conclusions
Polymer nanocomposites based coatings with
different ratios has been successfully coated using

Super-hydrophobic surface cannot stop fogging of

spin coater. Contact angle goniometer reveals that

the windshield unless the water drops is removed

the coatings (PANI, PZ1, PZ2, and PZ3) were

with wind power or vibration.

hydrophilic with an angles of 13.80, 12.60, 13.40 and

The steam fogs a mirror and a glass easily, because

moisture in the air is cooled down and numerous
water drops form on the surface of the usual
materials.

15.80 respectively. The increase in melting point

from 3000 to 3800 of PANI and composites was
observed using thermo gravimetric analysis. SEM &
TEM micrographs shows that there is a uniform
distribution of ZnO nanoparticles in PANI/ZnO

By utilizing the super-hydrophilic coating, water

nanocomposites. The peaks at 3284 cm-1 shows the

cannot exist in the shape of a drop, but spreads flatly

interaction between ZnO and polyaniline by

on the hydrophilic surface without fogging semi

formation of hydrogen bonding between H-N and

permanently.

oxygen of ZnO. From EDAX, the composition of

3.8.1.

Experimental part

nanocomposites has been verified with the presence

of appropriate percent of composition in composite

The slides were coated using drop casting technique

(PZ2). Also traces of potassium has been detected in

for the verification of anti-fogging property. The

Zinc oxide possibly a by-product of yeast. The

slides were exposed to a powerful vaporizer for a

polymer based composite coatings (PZ1, PZ2 and

PZ3) has exhibited anti-fog property with which its

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hydrophilic property can be cross checked.

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nanocomposites

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Table
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Table
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