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Title: Efficient UV photocatalytic dye decomposition activity with cost


effective solid state reaction grown Zinc Orthotitanate (Zn2TiO4)
nanoparticles

Article Type: Full Length Article

Keywords: Photocatalysis, Dye decomposition, Nanoparticle, Zinc


Orthotitanate, Solid state reaction.

Corresponding Author: Dr. SUSANTA KUMAR DAS, Ph.D

Corresponding Author's Institution: KIIT University

First Author: Lizina Khatua, M. Tech

Order of Authors: Lizina Khatua, M. Tech; Rudrashish Panda, M. Phil;


Arpana Nayak, M.Sc; , Avanendra Singh; Pratap Kumar Sahoo, Ph. D.;
Debabrata Pradhan, Ph. D.; Udai Pratap Singh, Ph.D; SUSANTA KUMAR DAS,
Ph.D

Abstract: In this work, detail investigation on UV photocatalytic dye


decomposition activity is done with Zinc Orthotitanate (Zn2TiO4)
nanoparticles grown by solid state reaction method and shown that these
nanoparticles can show 6 times higher activity than standard commercial
TiO2 nanoparticles Degussa P25. This activity is the highest among all
the nanoparticles that have been compared with P25 so far. The potential
cause for higher activity is explored through absorption spectroscopy.
The Zn2TiO4 nanoparticles are prepared from laboratory grade ZnO and TiO2
powder of extremely low cost Excellent recycling ability of Zn2TiO4
nanoparticles is shown through their multiple usages.
Cover Letter

SCHOOL OF APPLIED SCIENCE


KALINGA INSTITUTE OF INDUSTRIAL TECHNOLOGY
DEEMED TO BE UNIVERSITY, BHUBANESWAR , INDIA, 751024
Date: 2nd March 2018

To
The Editor-in-Chief
Journal of Alloys and Compounds

Respected Sir,

Uploaded please find a manuscript for your kind consideration for publication in your esteemed journal.
The brief details of the manuscript are given below:

 Title: Efficient UV photocatalytic dye decomposition activity with cost effective solid state
reaction grown Zinc Orthotitanate (Zn2TiO4) nanoparticles.
 Type: Full Length Article
 Authors:
Lizina Khatua, Rudrashish Panda, Arpan Kumar Nayak, Avadendra Singh, Pratap Kumar Sahoo,
Debabrata Pradhan, Udai Pratap Singh, Susanta Kumar Das.

 Significance of the work


Industries like textile, leather, plastic, pharmaceutical, paper etc. release various dyes as the waste
products. These dyes are non-biodegradable in nature and generally cannot be removed by the
conventional water treatment processes. These dyes even at parts per million (ppm) level can
cause serious water pollution. At this moment heterogeneous ultraviolet (UV) photocatalytic dye
decomposition with semiconductor nanostructures is one of the best methods for removal of these
dyes. In this work we did detail investigation on the UV photocatalytic activity of solid state
reaction grown compound semiconductor Zinc Orthotitanate (Zn2TiO4) nanoparticles and
demonstrated that they can show 6 times higher reaction constant than that of standard
commercial TiO2 nanoparticles Degussa P25. This is the world’s highest reported value on UV
photocatalytic reaction constant in comparison to P25. The cause for this superior photocatalytic
activity is explored through absorption spectroscopy. The reported nanoparticles were prepared
from the laboratory grade ZnO and TiO2 powder of extremely low cost ($10 for 500 g) in
comparison to P25 ($200 for 100g). So the overall cost of these nanoparticles is much less than
that of P25. Excellent recycling ability of the nanoparticles is shown through their multiple uses.
Low cost, significantly high reaction constant and extremely good recycling ability can make
these nanoparticles a better choice for applications of UV photocatalytic dye decomposition.

Thanking you.
Yours sincerely,

Dr. Susanta Kumar Das


Associate Professor, Coordinator
Dept. of Physics, School of Applied Sciences
Kalinga Institute of Industrial Technology Deemed to be University
Bhubaneswar, Odisha, India, 751024
skdasfpy@kiit.ac.in, +919658039777
*Prime Novelty Statement

Efficient UV photocatalytic dye decomposition activity with cost


effective solid state reaction grown Zinc Orthotitanate (Zn2TiO4)
nanoparticles

Prime Novelty Statement

In this work, we did detail investigation on the UV photocatalytic activity of solid state reaction

grown compound semiconductor Zinc Orthotitanate (Zn2TiO4) nanoparticles and demonstrated that

they can show 6 times higher reaction constant than that of standard commercial TiO2 nanoparticles

Degussa P25. This is the world’s highest reported value on UV photocatalytic reaction constant in

comparison to P25. The cause for this superior photocatalytic activity is explored through absorption

spectroscopy. The reported nanoparticles were prepared from the laboratory grade ZnO and TiO2

powder of extremely low cost ($10 for 500 g) in comparison to P25 ($200 for 100g). So the overall

cost of these nanoparticles is much less than that of P25. Excellent recycling ability of the

nanoparticles is shown through their multiple uses. Low cost, significantly high reaction constant and

extremely good recycling ability can make these nanoparticles a better choice for applications of UV

photocatalytic dye decomposition.


*Manuscript
Click here to view linked References

Efficient UV photocatalytic dye decomposition activity with cost


effective solid state reaction grown Zinc Orthotitanate (Zn2TiO4)
nanoparticles

Lizina Khatua a, Rudrashish Pandab, Arpana Nayak c, Avanendra Singhd, Pratap Kumar
Sahoo d, Debabrata Pradhan c, Udai Pratap Singha, Susanta Kumar Das b,*

a
School of Electronics Engineering, Kalinga Institute of Industrial Technology, Deemed to be
University, Bhubaneswar, Odisha, 751024, India
b
Dept. of Physics, School of Applied Sciences, Kalinga Institute of Industrial Technology,
Deemed to be University, Bhubaneswar, Odisha, 751024, India
c
Materials Science Center, Indian Institute of Technology, Kharagpur, West Bengal 721302,
India
d
School of Physical Sciences, NISER, Bhubaneswar, Odisha, 752050, India

*
Corresponding author: skdasfpy@kiit.ac.in

ABSTRACT
In this work, detail investigation on UV photocatalytic dye decomposition activity is done
with Zinc Orthotitanate (Zn2TiO4) nanoparticles grown by solid state reaction method and
shown that these nanoparticles can show 6 times higher activity than standard commercial
TiO2 nanoparticles Degussa P25. This activity is the highest among all the nanoparticles
that have been compared with P25 so far. The potential cause for higher activity is explored
through absorption spectroscopy. The Zn2TiO4 nanoparticles are prepared from laboratory
grade ZnO and TiO2 powder of extremely low cost Excellent recycling ability of Zn2TiO4
nanoparticles is shown through their multiple usages.

Keywords: Photocatalysis, Dye decomposition, Nanoparticle, Zinc Orthotitanate,


Solid state reaction.

1
1. Introduction

Industries like textile, leather, plastic, pharmaceutical, paper etc. release various dyes as

the waste products. These dyes are non-biodegradable in nature and generally cannot be

removed by the conventional water treatment processes. These dyes even at parts per million

(ppm) level can cause serious water pollution. At this moment, heterogeneous ultraviolet

(UV) photocatalytic dye decomposition with semiconductor nanostructures is one of the best

methods for removal of these dyes. The absorption of UV radiation by these semiconductor

nanostructures produces electron and hole pairs, which facilitate the breaking of dye

molecules into smaller harmless molecules through the redox reaction. The semiconductor

nanostructures like Zinc oxide (ZnO) and Titania (TiO2) have been found to be very efficient

for this purpose [1–8]. Therefore, worldwide very active research is going on the growth of

various types of nanostructures of these materials and their application for UV photocatalytic

dye decomposition. Efforts have also been made to get nanostructures of their compound

nanostructured materials for efficient photocatalytic dye decomposition , H2 generation for

green fuel etc. [9–21]. However in all reported works of UV photocatalytic dye

decomposition the nanostructures were grown by solution method[9,12, 14]. Solid state

reaction is one of the simplest methods for growth of new materials. Hence, in this work we

did the detail investigation on UV photocatalytic dye decomposition activity with the

nanoparticles of the compound material of Zinc Orthotitanate (Zn2TiO4 ) grown by this

method. In particular studies like estimation of reaction kinetics and rate constant,

comparison of the performance with that of standard commercial TiO2 nanoparticles


2
(Degussa P25) etc. were done and shown that these nanoparticles can show 6 times higher

UV photocatalytic activity than P25. The potential cause for this is explored through the

absorption spectroscopy. The obtained result is compared with the previously reported results

on efficient UV photocatalytic materials. The recycling ability of photocatalyst is an

important factor for practical applications of the catalyst. So this aspect of Zn2TiO4

nanoparticles has also been studied in present work.

Experimental Details

2.1 Material preparation and characterization

The nanoparticles were grown by solid state reaction method by taking the powder

precursors of TiO2 (Product No. 28375, Fisher Scientific, purity: 98.99%) and ZnO (Product

No.28975, Fisher Scientific, purity: 98.99%). These precursors were taken in the molar ratio

of 2:1 and ground for 3 hours by taking acetone as the medium. The grinded powder mixture

was calcined at 950oC for 2 hours. The X-ray diffraction (XRD), field emission scanning

electron microscopy (FESEM) and Brunauer–Emmett–Teller (BET) studies were carried out

to characterize the nanoparticles.

The XRD pattern of the sample (Fig. 1(a)) shows the strong peaks at angle 2θ =

31.97, 34.62, 36.46, 53.98 and 56.81 degrees. These peaks were identified as (201), (211),

(202), (204) and (105) planes of Zn2TiO4 respectively. The obtained results are found to be in

good agreement with the result published by Nikam et al. and Santhaveesuk et al. [22,23]

indicating that the dominant phase of the grown material is Zn2TiO4. Some minor peaks were

also found at angle 2θ = 38, 48 and 55 degrees originating from residual ZnO and TiO2. From

the statistical analysis of this FESEM image (Fig. 1(b)) the size of the nanoparticles were
3
found to be in the range 40-180 nm with maximum number at 58 nm. From the BET study

the estimated specific surface area of the nanoparticles was found to be 8.78 m2/g.

Fig. 1 XRD patterns (a), FESEM image (b) of the Zn2TiO4 nanoparticles.

2.2 Photocatalytic studies

Three sets of UV photocatalytic dye decomposition studies were done. In the first set

of experiment, photocatalytic dye decomposition studies with Zn2TiO4 nanoparticles and its

constituents were done for the fixed time of UV light exposure. A reactor consisting of a 6
4
Watt UV light source (wavelength = 365 nm) and a magnetic stirrer is used for this purpose.

Firstly, 40 ml of aqueous solution of methylene blue (MB) dye (2.5x10-5 M) and 0.02 g of

nanoparticles were taken in a beaker of 50 ml capacity. The solution container (placed over

magnetic stirrer) was kept at a distance of 10 cm from the light source. Prior to light

irradiation, the solution was kept for 30 minutes in dark condition for complete adsorption-

desorption of dyes on the catalyst surface. Finally, the sample was irradiated with UV light

for fixed amount of time (8 minutes). The whole photoreaction (dark as well light exposure

condition) was carried out under continuous slow stirring. The dye decomposition was

measured through the absorption spectroscopy of the solution after filtering out the

nanoparticles. For comparison, the photocatalysis with the same condition was carried out

with the constituents of Zn2TiO4 i.e. with ZnO and TiO2 after grinding them for the same

time as mentioned above for Zn2TiO4 nanoparticles growth.

In the second set of experiment, further studies like photocatalytic reaction kinetics,

estimation of reaction rate constant and comparison of the reaction rate constant with P25

were done for the Zn2TiO4 nanoparticles. For this, the procedure given in the above section

was followed. However, the UV exposure time was not fixed for this case. Here, the

photocatalysis was carried out at different intervals of time until the dye gets almost

decomposed. After the photocatalytic activity for a certain interval of time, 3 ml of sample

was taken to do the absorption spectroscopy to find the concentration of the dye.

The third set of experiment is similar to the second set except the fact that in this case

methyl orange (MO) was taken as the test dye and recycling ability study was conducted by

repeating the experiment five times with the same nanoparticles.


5
3. Results

3.1 Comparative UV photocatalytic activity of Zn2TiO4 and its constituents

Fig. 2 shows the UV photocatalytic dye decomposition activity of Zn2TiO4

nanoparticles and its constituents ZnO and TiO2 nanoparticles (all grinded for the same

amount of time 2 hours). From this, it is found that after 8 minutes of UV light exposure,

Zn2TiO4, ZnO and TiO2 nanoparticles can decompose 90%, 63% and 32 % of the methylene

blue (MB) dye respectively.

Fig. 2. Dye decomposition behavior of Zn2TiO4 nanoparticles and its constituents (ZnO and TiO2)
after 8 minutes of UV photocatalytic activity.

This figure clearly indicates that solid state grown Zn2TiO4 nanoparticles can show much

superior UV photocatalytic activity than its individual components. Better charge separation

ability and enhanced life time of the photoexcited carriers in Zn2TiO4 nanoparticles [9] may

be attributed to this superior photocatalytic activity.

6
3.2 Photocatalytic reaction kinetics, estimation of reaction rate constant and comparative
performance of Zn2TiO4 with the standard commercial nanoparticles

Fig. 3 shows the UV-visible absorption spectra of MB dye solution around its highest

absorption peak (664 nm) after 0, 4, 8 and 12 minutes of UV photocatalytic activity with

Zn2TiO4 nanoparticles.

Fig. 3. Absorption spectra of MB dye solution after 0, 4, 8 and 12 minutes of UV photocatalytic


activity with Zn2TiO4 nanoparticles

Fig.4(a) shows the photocatalytic degradation of MB dye (plot of C/C0 vs. time) in the

presence of UV-light with Zn2TiO4 nanoparticles and P25 (Sigma-Aldrich, BET surface area

50±15 m2/g, average size 21 nm). Here, C0 is the initial concentration of aqueous solution of

MB dye (2.5x10-5 M) and C is its concentration after a certain time of photocatalytic reaction.

In the absence of nanoparticles, no degradation of MB dye occurred under UV-light

irradiation even after 30 minutes. The degradation efficiency [(C0 − C)/C0 × 100] of Zn2TiO4

nanoparticles was found to be 99% after 12 minutes of UV-light irradiation, which is much

higher than that of standard P25 nanoparticles (37.48%) for the same duration. The P25

nanoparticles took 80 minutes for complete degradation of MB dye under UV-light

7
irradiation. This suggests the superior UV photocatalytic activity of Zn2TiO4 nanoparticles

for the degradation of MB dye. The plot of ln(C0/C) vs. irradiation time (Fig. 4(b), scatter

points) shows a linear behavior indicating pseudo first order dye degradation kinetics. The

rate constant of MB dye degradation was estimated from the slope of the linear fit line (solid

line) of this plot. The rate constants of Zn2TiO4 nanoparticles and P25 as estimated by this

method are 0.179 min-1 and 0.030 min-1 respectively. So, the dye decomposition activity of

Zn2TiO4 nanoparticles is found to be 6 times higher than that of the standard P25 TiO2

nanoparticles.

Fig. 4. Photocatalytic decomposition of MB dye in the presence of UV-light with different catalysts
(a), ln(C0/C) Vs. time graph (scatter points experimental data, solid line linear fit) (b).

3.3 Recycling ability behavior of Zn2TiO4 nanoparticles

Fig. 5 shows the experimental results of the UV photocatalytic decomposition study

of MO dye with solid state reaction grown Zn2TiO4 nanoparticles. Fig. 5(a) represents the

UV-visible absorption spectra of MO dye around its highest absorption peak (463 nm)

8
indicating the decomposition in the presence of UV-light irradiation for different durations.

Here the inset image displays the change in the color of MO dye solution after 0, 4 and 8

minutes of UV photocatalytic activity. As can be seen from this figure, the MO dye was

completely decomposed within 8 minutes.

Fig. 5. Absorption spectra of MO dye solution after 0, 2, 4, 6 and 8 minutes of photocatalytic activity
with Zn2TiO4 nanoparticles(a) (Inset : Image of MO dye solution after 0, 4 and 8 minutes of UV
photocatalytic activity), C/C0 Vs. time graph for five cycles of photocatalytic dye decomposition (b).

The C/C0 vs. Time graph for this is shown in Fig. 5(b) (curve: 1st, C0 =5x10-5 M),

which indicates that the MO dye got decomposed by 98% within 8 minutes of UV exposure.

In order to explore the recycling ability of the solid state grown Zn2TiO4 nanoparticles, we

repeated this study for four more times with the same nanoparticles and the results are also

shown in Fig. 5(b) (curve: 2nd-5th). As can be observed from this, the dye decomposition

efficiency is found to be almost same for all the five cycles. This suggests that the as-

9
synthesized Zn2TiO4 nanoparticles can be used multiple times for the UV photocatalytic dye

decomposition.

4. Discussion

The comparative study with a standard commercial nanoparticle like Degussa P25 is one

of the best methods to quantitatively evaluate the activity of the efficient UV photocatalytic

nanoparticles [24–28]. This study has been done for the first time with Zn2TiO4 nanoparticles

in this work and shown that it can show 6 times higher activity than P25. This is the highest

activity than all the previously reported efficient UV photocatalytic nanomaterials that have

been compared with P25 for standarization (Table 1).

Table 1 : Comparative table of reaction rate constant (k) w.r.t P25

Nanomaterials “k” w. r. t P25 Reference


ZnO-TiO2 1.26 [24]
ZnO-TiO2 1.03 [25]
Pt-TiO2 2.00 [26]
CNT -TiO2 2.67 [27]
ZnO 2.70 [28]
Zn2TiO4 6 Current work
(Our material)

In order to find the cause of superior photocatalytic behavior of Zn2TiO4 nanoparticles

than P25, we did the UV absorbance study of these materials by diffuse reflectance method

using an integrating sphere attached spectrophotometer. The result of this study is shown in

Fig. 6.

10
Fig. 6. UV absorbance behavior of Zn2TiO4 nanoparticles and P25 (Dotted line corresponds
to the working wavelength).

From this, we found that the UV absorbance of Zn2TiO4 nanoparticles is higher than that of

P25. This higher absorbance may be attributed to the superior UV photocatalytic activity of

Zn2TiO4 nanoparticles.

Lastly, it is to be noted that, the presently reported Zn2TiO4 nanoparticles were

prepared from the laboratory grade ZnO and TiO2 powders of extremely low cost ($10 for

500 g) which is much less than that of standard commercial material P25 ($200 for 100g).

This low cost together with significantly higher reaction constant and extremely good

recycling ability can make the solid state reaction grown Zn2TiO4 nanoparticles a better

choice for UV photocatalytic dye decomposition application.

5. Conclusions

In summary, Zn2TiO4 nanoparticles of BET surface area of 8.78 m2/g was grown by

solid state reaction method and used for UV photocatalytic dye decomposition. In the
11
comparative study, it was found that these Zn2TiO4 nanoparticles could completely

decompose the MB dye within 12 minutes whereas the standard commercial TiO2

nanoparticles P25 (BET surface area 50±15 m2/g) took 80 minutes for doing this in the same

experimental condition. The reaction rate constant of Zn2TiO4 (k= 0.179 min-1) nanoparticles

was found to be 6 times higher than that of P25 (k=0.030 min-1). The cost of the prepared

nanoparticles is much less than the standard commercial nanoparticles P25 and has extremely

good recycling ability. Therefore, these nanoparticles can be found to be very useful for

industrial application of UV photocatalytic dye decomposition.

Acknowledgement: SKD thanks, Science & Engineering Research Board (SERB), Govt. of

India (Project File Number: EMR/2015/001175) for the financial support.

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17
Graphical Abstract (for review)
*Highlights (for review)

Efficient UV photocatalytic dye decomposition activity with cost


effective solid state reaction grown Zinc Orthotitanate (Zn2TiO4)
nanoparticles

Highlights

 UV photocatalytic dye decomposition activity is studied with Zn2TiO4 nanoparticles

 Reaction rate of these nanoparticles is demonstrated to be 6 times higher than P25

 This is the world’s highest reported value in comparison to P25

 Cause for superior activity is explored through absorption spectroscopy

 Excellent recycling ability of nanoparticles is demonstrated by the multiple uses


Figure
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