Accepted Manuscript

Artocarpus gomezianus aided green synthesis of ZnO nanoparticles: Lumines-

cence, Photocatalytic and Antioxidant Properties

D. Suresh, R.M. Shobharani, P.C. Nethravathi, M.A. Pavan Kumar, H.

Nagabhushana, S.C. Sharma

PII: S1386-1425(15)00069-4
DOI: http://dx.doi.org/10.1016/j.saa.2015.01.048
Reference: SAA 13216

To appear in: Spectrochimica Acta Part A: Molecular and Biomo-

lecular Spectroscopy

Received Date: 1 November 2014

Revised Date: 31 December 2014
Accepted Date: 14 January 2015

Please cite this article as: D. Suresh, R.M. Shobharani, P.C. Nethravathi, M.A. Pavan Kumar, H. Nagabhushana,
S.C. Sharma, Artocarpus gomezianus aided green synthesis of ZnO nanoparticles: Luminescence, Photocatalytic
and Antioxidant Properties, Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy (2015), doi:
http://dx.doi.org/10.1016/j.saa.2015.01.048

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Artocarpus gomezianus aided green synthesis of ZnO nanoparticles:
Luminescence, Photocatalytic and Antioxidant Properties

D. Suresh1*, R.M.Shobharani1, P.C. Nethravathi1, M.A. Pavan Kumar2, H. Nagabhushana3, S.C.Sharma4, 5

1
Department of Studies and Research in Chemistry, Tumkur University, Tumkur 572 103, Karnataka, India,
2
Department of Studies and Research in Biochemistry, Tumkur University, Tumkur 572 103, Karnataka, India,
3
Prof. C. N. R. Rao Centre for Advanced Materials, Tumkur University, Tumkur 572 103, Karnataka, India,
4
Vice Chancellor, Chattisgarh Swami Vivekanand Technical University, Bhilai, Chattisgarh, India.
5
Academic Mentor and Honorary Professor of Eminence, Department of Mechanical Engineering, Siddaganga Institute of
Technology, Tumkur, 572 103, Karnataka, India

Abstract

We report green synthesis of multifunctional ZnO nanoparticles (NPs) using Artocarpus

gomezianus (AG) extract as fuel by solution combustion synthesis. The formation of NPs was

confirmed by Powder XRD, SEM, TEM and UV Visible studies. The NPs were subjected for

photoluminescence, photodegradative and antioxidant studies. XRD data reveals that the ZnO

NPs possess wurtzite structure. UV - Visible spectrum shows absorbance maximum at 370 nm

which corresponds to the energy band gap of 3.3 eV. Morphology studies indicate the highly

porous nature of the NPs. PL spectra of NPs found to display very interesting blue, green and red

emissions upon excitation at 325 nm. The NPs exhibit potential photocatalytic activity towards

the degradation of Methylene blue (MB) dye upon exposure to Sun light and UV light. ZnO NPs

found to have considerable antioxidant activity against DPPH (2, 2-diphenyl-1-picrylhydrazyl)

free radicals. The study successfully demonstrates a simple and eco-friendly method for the

synthesis of efficient multifunctional ZnO nanoparticles using green synthetic approach.

Key-words: X-ray techniques, Luminescence, ZnO, Nano particles, Artocarpus gomezianus,

Green synthesis.
____________________________________________________________________________
*Corresponding Author: E-mail: pbdsuresh@gmail.com; Phone No: +91 9886465964

1
1. Introduction

Nanoparticles are endowed with a variety of properties due to the presence of large surface area.

ZnO nanoparticles are one of the widely studied classes of nanoparticles for various applications.

ZnO is one of the best likely materials for performing photocatalytic task, as an alternative to the

extensively used, comparatively expensive titanium oxide (TiO2). Although researchers

recognized comparable photocatalytic mechanisms with both TiO2 and ZnO, they showed that

ZnO was a better photocatalyst in degrading the herbicide triclopyr, pesticide carbetamide, pulp

mill bleaching wastewater, phenol, 2-phenylphenol, blue 19, and acid red 14 [1]. This advantage

of ZnO photocatalytic activity is because it contains large number of active sites, highly effective

in generating hydrogen peroxide and higher reaction rates [1, 2].

Owing to its straight, wide band gap of 3.37 eV, ZnO has a wide variety of applications in

optoelectronic devices such as photodetectors, light-emitting diodes and p-n homojunctions [3].

The large exciton binding energy of 60 meV [3] compared to that of Gallium Nitride (GaN)

epilayers (approximately 25 meV) [4], improves the luminescence effectiveness of the emitted

light even at room temperature in case of ZnO. The visible photoluminescence (PL) emission at

around 2.5 eV (around 495 nm), initiated from intrinsic defects [5], creates ZnO fit for

applications in vacuum fluorescent displays and field emission detectors.

Several routes were used for fabrication of ZnO nanoparticles namely, pulsed laser deposition

[6], chemical vapor deposition [7], molecular beam epitaxy [8], hydrothermal synthesis [9],

sputtering [10] and oxidation of metallic zinc powder [11-12] for numerous applications. Nano

particulate form improves the photocatalytic activity due to its vast surface area and the

occurrence of vacancies and un-coordinated particles at the edges and corners. The

photocatalytic activity can also be improved by band gap engineering due to quantum

2
confinement effect [13-15]. A well controlled synthesis is desired for the economical usage of

ZnO in catalytic applications such as aquatic treatment and other environmental claims. Herein,

we are reporting, for the first time, a direct and simple method for the green synthesis of

nanocrystalline ZnO via combustible method using fruit extract of Artocarpus gomezianus (AG)

as fuel which belongs to the family of Artocarpus. It is well known traditionally for treatment

against inflammation, malaria, diarrhoea, diabetes and tapeworm infection. It is widely

distributed in southern India in the Western Ghats-South, Central and Maharashtra, Sahyadris

and Sri Lanka [16].

Artocarpus species are found to be rich in phenolic compounds including flavonoids, stibenoids,

aryl benzofurons and jacalin, a lectin [17]. These phytochemical constituents with highly

reducing properties may act as good fuel during solution combustion synthesis that reduce metal

nitrates to form useful metal oxide nanoparticles. Moreover, there are no reports till date

exemplifying the use of Artocarpus gomezeanus towards the synthesis of nanoparticles.

Therefore, an effort has been made for the first time to exploit naturally occurring fruit extract of

AG as a combustible fuel by green synthetic approach for the synthesis of multifunctional ZnO

NPs. This process involves a self sustained reaction in homogeneous solution of Zinc nitrate as

an oxidizer and fruit extract of AG as fuel.

2. Materials and Methods

1, 1 - Diphenyl-2-picrylhydrazyl was procured from Sigma-Aldrich India Company. Ascrobic

acid, Gallic acid, Vanillin, Phloroglucinol, Methylene blue, Zn(NO3)3.6H2O and Methanol were

from S. D. Fine Chemicals Company. All other solvents were of AR grade and distilled before

3
use. Distilled water was employed for all the experiments. The plant material was shade dried

and powdered into 100 mesh size and stored at room temperature in an airtight container.

2.1 Preparation of the extract

About 1:10 proportion of AG fruits powder to solvent was taken in a round bottomed flask.

Extraction was carried out at boiling temperature of water with a reflux arrangement for about 3

hours with constant stirring. The extract was filtered and centrifuged to remove any suspended

particles and then dried using roto evaporator. The prepared extract was stored in air tight

bottles.

2.2 Polyphenols Assay

Folin Ciocalteu reagent (FC reagent) (0.1 N) was prepared by diluting commercially available

FC reagent (1:20) with distilled water to get the required concentration. Sodium carbonate

(7.5%) was prepared by dissolving 7.5 gm of sodium carbonate in 100 ml of de-ionized water.

Gallic acid (standard) stock I (conc. 0.1 mg/ml) was prepared by dissolving 1 mg of Gallic acid

in 10 ml with 50% Methanol. For making standard graph of Gallic acid, concentration range of

2 - 20 g/ml was used. The assay was carried out by using Singleton and Rossi method [18]. In a

typical process, 1000 l of FC reagent was added to 200 l of 50% methanol/standard/test

sample with various concentrations, mixed and incubated at RT for 5 min. followed by addition

of 800 l of 7.5% sodium carbonate solution. The resulting solution was mixed and incubated at

37oC for 30 min. The absorbance was recorded at 750 nm against blank using spectrophotometer.

Color correction was given with the same concentration of the test sample in 50% methanol

without FC reagent.

4
2.3 Flavonoids Assay

Vanillin, an aromatic aldehyde condenses with the flavon-3-ols and oligomers to form soluble

pigments in acidic medium with an absorbance maximum at 500 nm, which can be detected by

UV-Visible spectrophotometer. Vanillin Reagent (1%) was prepared by dissolving 1 g of

crystallized vanillin in 100 ml of 70% Conc. H2SO4.Conc. H2SO4 (70%) was prepared by

diluting 70 ml on Conc. H2SO4 in 100 ml de-ionized water. 10 mg of Phloroglucinol was

dissolved and made up to a volume of 10 ml with 50% Methanol followed by centrifugation at

12,000 rpm for 10 min and labeled as Stock I. Stock II was prepared by diluting stock I to a

conc. of 0.1mg/ml with 50 % methanol. For making standard graph of Phloroglucinol, 1 10 g

ml-1 concentration range was used. The flavonoid assay was carried out using Swain and Hillis

method [19]. In a typical experiment, to a 400 l of distilled water / positive control / test sample

with various concentrations, 800 l of 1% vanillin reagent was added, mixed and incubated at

RT for 15 min. The absorbance was recorded at 500 nm against blank using spectrophotometer.

Color correction was given with the same concentration of the test sample in distilled water

without vanillin reagent. The flavonoid content in the plant extract was measured with reference

to the standard Gallic acid values.

2.4 Synthesis

ZnO nanoparticles were prepared by solution combustion synthesis of AG fruit extract as fuel.

Stoichiometric amount of Zn(NO3)3.6H2O was dissolved in 10 ml of plant extract, and kept in a

preheated muffle furnace at 400oC [20]. A milky white powder was obtained with a vigorous

reaction in about 4 minutes. The experiment was carried with 15, 20, 25, 30 ml of plant extract.

5
2.5 Characterization

The phase purity and the crystallanity of the powders were examined by Shimadzu-7000 powder

X-ray diffractometer using Cu K (1.541 ) radiation with a nickel filter. The optical properties

such as UV-Visible, Photoluminescence studies were carried out by employing Thermo

Scientific Spectrophotometer and Horiba Spectroflourimeter respectively. Surface morphology

of the product was studied by employing Hitachi table top (7000) Scanning Electron Microscope

and TEM studies were performed using TECNAIF-30.

2.6 Photocatalytic degradation of dye

Photocatalytic experiments were carried out in a 150 X 75 mm batch reactor. A catalytic load of

50 mg in 100 ml of 5 ppm MB dye was prepared. The slurry containing dye solution & catalyst

was placed in the reactor and stirred magnetically for agitation with instantaneous exposure to

Sun light or UV light. Known volume or the slurry was withdrawn at various intervals of time

such as 0, 30, 60, 90, 120 minutes. Then they were centrifuged to get rid off any interference due

to the presence of catalyst and absorbance was measured using spectrophotometer at 663 nm to

assess the rate of degradation. The % degradation was calculated using the relation

 
%   
 =  100


Where Ci & Cf are the initial and final concentrations of the dye.

The same procedure was repeated for different catalytic load of samples (100, 150 and 200 mg)

and at different concentration of dye (10, 15 and 20 ppm) keeping the concentration of catalyst

constant and also at different pH (viz., 2, 4, 6, 8, 10, 12) and the % degradation was determined

[20].

6
2.7 Antioxidant activity

Antioxidant activity was carried out by DPPH assay using modified method of Brand-Williams

[21]. DPPH (oxidized form) is a stable free radical with purple color. In the presence of an

antioxidant which can donate an electron to DPPH radical decays, and the change in absorbance

at 520 nm is followed which can be measured spectrophotometrically. Exactly 39.4 mg of DPPH

was dissolved in 100 ml of methanol to get 0.14 mM concentration of DPPH in the assay.

Ascorbic acid standard stock I (conc. 200 g/ml) was prepared by dissolving 2 mg of Ascorbic

acid and made up to a volume of 10 ml with de-ionised water. For making standard graph of

ascorbic acid 2, 4, 6, 8, 10 g/ml concentration range was used. In brief, to an 860 l of 50%

methanol/ascorbic acid/test sample with various concentrations, 140 l of 1 mM DPPH was

added, mixed and incubated at 37 oC for 30 min. The absorbance was measured at 520 nm

against 50 % methanol blank using spectrophotometer. A control sample was maintained

without addition of the test sample. The antioxidant activity was measured with reference to the

standard ascorbic acid absorbance values. The actual absorbance was taken as the absorbance

difference of the control and the test sample and IC50 value was determined.

3. Results and Discussion

Plants are usually found to contain significant amounts of bioactive secondary metabolites such

as polyphenols. These classes of compounds act as good reducing agents during the solution

combustion synthesis of nanoparticles, consequently, they act as fuels. The water extract of

Artocarpus gomezianus was subjected for the determination of polyphenol content. It was

found that the extract contains 17.16 % of polyphenols. Also, the flavonoids, which form

another important class of secondary metabolites, may also act as good source of reducing

7
agents. Our results indicate that the extract was found to possess 22% of flavonoids. These

results suggest that the extract is a very good source of bioactive secondary metabolites which

could efficiently perform the role of reducing agents during the synthesis of nanoparticles.

30ml

25ml
Intensity (au)

20ml

15ml

10ml
(002)
(101)
(100)

(110)
(102)

(103)

(112)
(200)

20 30 40 50 60 70 80

Fig. 1. PXRD Pattern of ZnO NPs prepared with different concentrations of AG extract

8
 cos

1.2 1.4 1.6 1.8

4sin

Fig. 2. W-H plots of ZnO NPs prepared with different concentrations of AG extract

Particle sizes Lattice

Dislocation Micro strain
By Strain density spacing
Sample (x10-4)
Sherrers By W-H (x10-4) (x1014) X 10-10
formula plots (nm)
d
(nm)
10 ml 20 29 93 25 2.17183 40
15 ml 10 24 76 100 2.17684 20
20 ml 9 47 140 123 2.170854 84
25 ml 5 6 65 400 1.1631 51
30 ml 4 5 42 625 1.162615 64

Table 1. Particle sizes, strain, dislocation density, lattice pacing and micro strain of ZnO NPs
prepared with different concentrations of AG extract

9
Figure 1 shows XRD patterns of ZnO nanoparticles synthesized. The experiments were carried

out employing Shimadzu-7000 Powder X-Ray diffractometer with Cu-K (= 1.54 ) radiation.

The characteristic patterns are corresponding to the diffraction patterns of hexagonal wurtzite

phase of ZnO. No other peaks appeared in the patterns. The cell constants were observed to be

a = 3.25 A and c = 5.21 A and all the peaks were well matched with the JCPDS card No. 36-

1451. The sharp diffraction peaks reveal the crystallinity of the as prepared material. The area

under the diffraction peaks increase with increase in the ratio of fuel and Zinc nitrate. This

increase in area under the peak results in crystallite sizes decrease below 20 nm. The particle

size was calculated using the Debye Sherrer formula and strain produced in the as synthesized

material is calculated by plotting W-H plots.

.
= -------------------------- (1)


Where D is the crystallite size, is the wavelength of X-rays, is the full width half maximum,

is the Braggs diffraction angle, the average crystallite sizes were calculated are around 11.53

nm.

A graph is plotted (Fig. 2) fuel concentration v/s particle sizes by Debye Sherrer formula and

W-H plots. It is clear from the graphs that particle size decreases and then increases followed by

steep decrease with increase in fuel concentration. Dislocation is a crystallographic defect or

irregularity, within a crystal structure. The presence of dislocations strongly influences many of

the properties of materials. Where Dislocation densities are calculated using the formula

= 1/D2 ..(2).

10
Where D is the crystallite size is the dislocation density, and the number of unit cells was

calculated using the formula (table 1).

n=(4/3)x(D/2)3x(1/V) (3)

Figure 3 shows the room temperature UV- Visible spectra of the ZnO nanoparticles prepared

with various concentrations of the plant extract. The maximum absorbance was observed at 370

nm, corresponding to a band gap of 3.3 eV. Quantum size effects on electronic energy bands of

semiconductors become more prominent when the size of the nano crystallites is less than the

bulk excitation Bohr radius. Columbic interactions between holes and electrons play a crucial

role in nano sized solids. The quantum confinement of charge carriers modifies valence and

conduction bands of semiconductors.

370 nm
10 mL
15 mL
20 mL
25 mL
Absorbance (a.u)

30 mL

400 500 600

Wavelength (nm)

Fig. 3. UV - Visible Spectrum of ZnO NPs prepared with different concentrations of AG Extract

11
Fig. 4. SEM image of ZnO NPs synthesized using water extract of Artocarpus gomezianus fruit

Figure 4 shows the SEM micro graphs of as prepared ZnO Nano particles it is observed that

almost spherical in nature further, the particles are agglomerated to form foam like bunch of

particles. The agglomeration could be induced by densification resulting in the narrow space

between particles. When gas is escaping with high pressure, pores are formed with the

Fig. 5. TEM image of ZnO NPs synthesized using water extract of Artocarpus gomezianus fruit

12
simultaneous formation of small particles. The morphology of the powders reflects the inherent

nature of the combustion process. The observations of the SEM studies crystallite size

determination calculations were supported by TEM analysis (Fig. 5).

4
2.0x10
(546nm) (a) 10ml
4
1.8x10 (b) 15ml
(481nm)
4
(c) 20ml
1.6x10
(d) 25ml
1.4x10
4 (e) 30ml
PL Intensity (au)

4
1.2x10

4
1.0x10

3
8.0x10
(650nm)
3
6.0x10

3
(378nm)
4.0x10

3
2.0x10

400 500 600 700

Wavelength (nm)

3
6.0x10 10ml
15ml
20ml
25ml
30ml
PL Intensity (au)

3
4.0x10

3
2.0x10

620 640 660 680

Wavelength (nm)

Fig. 6. PL spectra for ZnO NPs prepared with different concentrations of AG Extract

Fig. 6 shows room temperature Photoluminescence (PL) spectra of as prepared ZnO NPs. The

spectra have four emission peaks centered at 378, 481, 546 and 650 nm when the material was

excited of 325 nm. The spectra shows characteristic blue band edge emission at 378 nm and the

peaks was found to be less intense and broad. The deep-level emission was observed due to

oxygen deficiencies and zinc interstices and structural defects in the ZnO Nps. The major edge

was at 546 nm corresponds to the green emission and second major edge was at 481 nm which

13
corresponds to the blue emission which is due to the quantum confinement effect. The third

major emission edge was observed at 650 nm which is pure red emission. Thus, the emission

resulted from the recombination of a photo-generated hole with a singly ionized charge state of

the specific defects (oxygen vacancies and zinc interstices).

Various concentrations of methylene blue such as 5, 10, 15, 20 ppm/100 ml of reaction mixture

were tested against fixed catalytic load of 50 mg. Then reaction mixture was exposed to UV and

Sun light. In both the cases of exposure, the photocatalytic activity remains almost same. It was

observed that 5 ppm/100 ml solution was degraded very effectively by ZnO nanoparticles having

a catalytic load of 50 mg/100 ml. With the increase in the concentration of dye (say 10, 15, 20

ppm) then the degradative activity decreases gradually. However it is not very appreciable.

Therefore 5 ppm/100 ml of dye would be optimum for further studies.

a) 120 b)
20

90
% degradation
% degradation

10 5 ppm
10 ppm 60
15 ppm 5 ppm
20 ppm 10 ppm
15 ppm
30 20 ppm

0
0 30 60 90 120 0 30 60 90 120
Time (min) Time (min)

Fig. 7. Percentage degradation of methylene blue with different concentration of dye under

a) UV light b) Sun light

The amount of catalyst used is directly related to number of active sites in the reaction mixture.

The catalytic load also affects the penetration of light in to the reaction mixture. By keeping the

14
concentration of dye constant (5 ppm) & varying the catalytic load with increasing order such as

50, 100, 150 and 200 mg/100 ml were tested against 5 ppm /100 ml concentration of dye.

From the Fig. 7 and 8, it can be concluded that with the increase in catalytic load, the

degradation increases. But this increase in degradation was not very significant with increase in

catalytic load. Therefore the lowest catalytic load of 50 mg/100 ml of reaction mixture was

considered for further studies.

30
a) b)

90
% degradation

% degradation

60
15

50 mg 30 50 mg
100 mg 100 mg
150 mg 150 mg
200 mg 200 mg
0 0
0 30 60 90 120 0 30 60 90 120
Time (min) Time (min)

Fig. 8. Percentage degradation of methylene blue with different concentration of catalytic load

under a) UV light b) Sun light

The effect of pH on the degradation of dye was assessed by keeping the catalytic load (50 mg)

and dye concentration (5 ppm/ 100 ml) constant and varying pH in the range of 2 12 (Fig. 9). It

was observed that the degradation was quite low at lower pH. However the degradation was

found to be very high in alkaline pH. This degradation may also be attributed to instability of the

dye in alkaline pH range [22].

15
 a) b)
60
90

2 pH
% degradation

4 pH

% degradation
2 pH 60 6 pH
4 pH 8 pH
30 6 pH 10 pH
8 pH 12 pH
10 pH
12 pH 30

0
0

0 30 60 90 120 0 30 60 90 120
Time (min) Time (min)

Fig. 9. Percentage degradation of methylene blue at different pH under a) UV light b) Sun light

DPPH, a stable free radical with a characteristic absorption at 517 520 nm, was used to

study the radical scavenging effects. The decrease in absorption is taken as a measure of the

extent of radical scavenging.

50
% Inhibition

IC50of ZnO = 10.8 mg/mL

0

0.0 2.5 5.0 7.5 10.0 12.5

Concentration (mg)

Fig. 10. DPPH Free radical Scavenging activity of ZnO Nanoparticles.

The radical-scavenging activity (RSA) values were expressed as the ratio percentage of sample

absorbance decrease and the absorbance of DPPH solution in the absence of extract at 520 nm

16
(Fig. 10). The ZnO nanoparticles were proved to be inhibiting the DPPH free radical scavenging

activity with IC50 value of 10.8 mg/ml.

Conclusion

We have developed greener approach for Zinc oxide Nanoparticles synthesis. The synthesis

method is faster, economical & greener since this avoids multiple reaction steps conventional

energy sources & harmful chemicals. This preparation of Zinc oxide nanoparticles using

Artocarpus gomezianus is eco-friendly & can be an effective substitute for the large scale

synthesis of ZnO nanoparticles. XRD studies shows that the ZnO nanoparticles synthesized has a

wurtzite structure. Electron microscope studies indicate highly porous nature of the

nanoparticles. UV- Visible studies show that the absorbance value is 370 nm which corresponds

to the energy band gap of 3.3 eV. PL spectra show the emission of prepared ZnO nanoparticles

has good photocatalytic activity towards the photodegradation of methylene blue. ZnO

Nanoparticles found to exhibit antioxidant property. The study successfully demonstrates facile,

economical and ecofriendly method of synthesis of multifunctional ZnO nanoparticles.

17
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20
Research Highlights

ZnO NPs synthesized using extract of Artocarpus gomezianus fruits

PXRD, SEM and UV Visible studies confirm the formation of Nps

PL spectra display blue, green and red emissions upon excitation at 325 nm

Nps exhibit excellent photocatalytic activity

NPs show good antioxidant activity against DPPH radicals

21
 GRAPHICAL ABSTRACT

ZnO-Ag-2(1)

3
6.0 x1 0 10m l
15m l
20m l
25m l
30m l

PL Intensity (au)
3
4.0 x1 0

http://www.biotik .org/india/species/a/artogoze/artogoze_12.jpg
2.0 x1 0 3

62 0 64 0 660 680
W a ve le ngth (nm )

a)
20
% degradation

10 5 ppm
10 ppm
15 ppm
20 ppm

0 30 60 90 120
Time (min)

22