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Photocatalysts and Electrocatalysts
in Water Remediation
Photocatalysts and Electrocatalysts
in Water Remediation
Edited by
Dr Prasenjit Bhunia
Silda Chandra Sekhar College, India
Dr Kingshuk Dutta
Central Institute of Petrochemicals Engineering and Technology (CIPET), India
Dr S. Vadivel
Saveetha Institute of Medical and Technical Sciences, India
This edition first published 2023
© 2023 John Wiley & Sons Ltd.
All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or
transmitted, in any form or by any means, electronic, mechanical, photocopying, recording or otherwise,
except as permitted by law. Advice on how to obtain permission to reuse material from this title is
available at http://www.wiley.com/go/permissions.
The right of Prasenjit Bhunia, Kingshuk Dutta, Vadivel to be identified as the authors of this editorial
material in this work has been asserted in accordance with law.
Registered Office(s)
John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, USA
John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex, PO19 8SQ, UK
Editorial Office
The Atrium, Southern Gate, Chichester, West Sussex, PO19 8SQ, UK
Boschstr. 12, 69469 Weinheim, Germany
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visit us at www.wiley.com.
Wiley also publishes its books in a variety of electronic formats and by print-on-demand. Some content
that appears in standard print versions of this book may not be available in other formats.
A catalogue record for this book is available from the Library of Congress
Set in 9.5/12.5pt STIXTwoText by Integra Software Services Pvt. Ltd, Pondicherry, India
v
Contents
Preface ix
About the Editors xi
List of Contributors xiii
Acknowledgements xv
Index 311
ix
Preface
A wide array of wastewater treatment alternatives are being investigated nowadays, and
this is owing to the increase in polluted wastewater generation because of the growth in
population and industrial activities. Advanced oxidation processes (AOPs) have become, in
the last few years, a selected alternative due to several advantages, such as their nonselec-
tive degradation of pollutants and their easy setup. Photo-based processes have always
been one of the most preferred AOP options, due to the possibility of using solar radiation
that may reduce the AOPs’ high elevated costs. Photocatalysis processes fall under the AOP
category, and it is studied worldwide for various applications. A photocatalyst is defined as
a “catalyst able to produce, upon absorption of light, chemical transformations of the reac-
tion partners” [1]. The excited state of a photocatalyst interacts repeatedly with the reac-
tion partners, resulting in the formation of reaction intermediates, and regenerates itself
after each cycle of such interactions. In effect, the photocatalyst is activated with radiation,
which brings about the separation of electrons and holes from, respectively, the valence
and conduction bands of semiconductor photocatalysts. This, in turn, starts a series of
chain reactions that lead to the generation of oxidants and, ultimately, to pollutant degra-
dation. However, even photocatalysis has limitations for future applications; for instance,
the electrons and holes are usually recombined, long treatment times are required, etc. As
a solution, the combination of photocatalysis with the application of an electrochemical
field (photoelectrocatalysis) has been contemplated.
On the other hand, electrochemistry, an interdisciplinary field of interfacial charge
transfer, has been introduced for the decontamination of both organic and inorganic pol-
lutants, and therefore has developed significant worldwide interest toward water remedia-
tion. In this connection, electrocatalytic oxidation and reduction usually work together to
decompose organic contaminants, and convert heavy metal ions from their toxic to non-
toxic form in electrocatalytic advance oxidation processes (EAOPs). Although this tech-
nique was elucidated long back in the 1970s, it is only in recent years that the electrocatalysts
have become highly encouraging materials toward water remediation. Electrocatalysts
degrade or convert the contaminants (organic or inorganic) through profound collision of
a very clean reagent – “the electron”; therefore, the technique is recognized as environmen-
tally benign. In addition, this technique has been found to be highly versatile toward deg-
radation of various contaminants, including dyes, pesticides and herbicides, phenolic
compounds, pharmaceuticals, etc., and is also able to convert heavy metal ions from their
x Preface
toxic to nontoxic forms. Moreover, the most attractive features of EAOPs toward water
treatment are high treatment efficiencies, accumulation of less toxic by-products, and envi-
ronmental friendliness.
The subject of this book has been meticulously designed to cover both the photo and
electrocatalytic water remediation aspects, starting from fundamentals to the applications.
This book describes the major functions of catalysts (photo-, electro-, and electrophoto-) in
the domain of water remediation, along with the involved chemical reactions, mecha-
nisms, challenges, and up-to-date developments. In addition, the scope of further research
on photo, electro, and electrophotocatalysts is also thoroughly discussed. Enriched with
critically analyzed and expertly opined contributions from several well-known researchers
around the world, this book is likely to serve as one of the most comprehensive and author-
itative pieces of literature that has ever been published in this field, and will undoubtedly
serve as a potent source of information for those interested in this field.
Prasenjit Bhunia
Kingshuk Dutta
S. Vadivel
Reference
1 IUPAC, (1997) Compendium of Chemical Terminology: The Gold Book. Oxford: Blackwell
Scientific Publications.
xi
Dr. Prasenjit Bhunia has obtained his Masters and Doctorate in Inorganic Chemistry
from Jadavpur University, Kolkata, India. In addition, he has done Post-Doctoral research
at National Taiwan University, Taiwan and Sungkyunkwan University, Suwon, South
Korea, and has gained prolonged experience in Graphene/Graphene Oxide and their func-
tionalization and applications. He has also served as an Institute Post-Doctoral Fellow in
the Department of Chemical Engineering, Indian Institute of Technology Kharagpur,
India, and has gathered significant experience in photocatalysis and electrocatalysis.
Furthermore, he has noticeable industrial experience from working at Hindustan Unilever
Limited, Bangalore and TCG Life Sciences, Kolkata, India. In addition, he has served as a
Principal Researcher at TATA Steel Limited, Jamshedpur, India, where he has gained out-
standing experience in the field of photocatalytic wastewater treatment. Now, he serves as
an Assistant Professor in the Department of Chemistry, Silda Chandra Sekhar College,
Jhargram, India (affiliated to Vidyasagar University, Paschim Medinipur, India). At this
time, he has 23 international peer reviewed journal articles, 7 book chapters and 5 patents
to his credit. His present research field is photocatalytic water treatment.
Dr. Kingshuk Dutta, FICS, is currently employed as a Scientist in the Advanced Polymer
Design and Development Research Laboratory of the Central Institute of Petrochemicals
Engineering and Technology, India. Prior to this appointment, he worked as an Indo–US
Postdoctoral Fellow at Cornell University, USA (2018–19) and as a National Postdoctoral
Fellow at the Indian Institute of Technology – Kharagpur, India (2016–17), both funded by
the Science and Engineering Research Board, Govt. of India. Earlier, as a Senior Research
Fellow funded by the Council of Scientific and Industrial Research, Govt. of India., he had
carried out his doctoral study at the University of Calcutta, India (2013–16). He possesses
degrees in both technology (B. Tech. and M. Tech.) and science (B. Sc.), all from the
University of Calcutta. He was also a recipient of the prestigious Graduate Aptitude Test in
Engineering (GATE) and National Scholarship, both from the Ministry of Human Resource
Development, Govt. of India. His areas of research interest lie in the fields of fuel cells
(including alcohol, bio/microbial, and hydrogen fuel cells), sensors, water purification,
polymer blends and composites, and biodegradable polymers. At this time, he has contrib-
uted to 54 experimental and review papers in reputed international platforms, 25 book
chapters, 1 patent application, and many national and international presentations. In
xii About the Editors
addition, he has edited/co-edited four books published by Elsevier and two books pub-
lished by the American Chemical Society. He has also served as a guest associate handling
editor for Frontiers in Chemistry and a peer-reviewer for over 180 journal articles, confer-
ence papers, book chapters, and research project proposals. He is a life member and an
elected fellow of the Indian Chemical Society, a life member of the International Exchange
Alumni Network (US Department of State) and a member of the Science Advisory Board
(USA). Earlier, he held memberships with the International Association for Hydrogen
Energy (USA), the International Association of Advanced Materials (Sweden), the Institute
for Engineering Research and Publication (India) and the Wiley Advisors Group (USA).
Dr. S. Vadivel is currently working as an Assistant Professor (Senior Grade) in the
Department of Electrochemistry, Saveetha School of Engineering, Saveetha Institute of
Medical and Technical Sciences, Tamil Nadu, India. He obtained his PhD in Chemistry
(2015) from the AC Tech Campus, Anna University, Chennai, and then successfully com-
pleted his postdoctoral fellowship tenure at the Tokyo Institute of Technology, Tokyo,
Japan, under the highly prestigious JSPS Fellowship. Furthermore, he received the highly
prestigious PIFI fellowship from the Chinese Academy of Sciences in 2019. His current
research involves the development of novel materials with graphene, graphitic carbon
nitride, in combination with metals, metal oxides, polymers, and carbon nanotubes for
energy conversion & storage, and removal of various toxic pollutants. His research results
have been documented in 66 peer-reviewed journals, including 5 review articles and 10
book chapters. He also has more than 2200 citations with an h-index of 25. He served as a
guest editor for a special issue of Frontiers in Chemistry, and is currently serving as an asso-
ciate editor for Heliyon journal and editing two books for reputed publishers. He is also
serving as a peer-reviewer for various high impact journals from Royal Society of Chemistry,
American Chemical Society, and Elsevier journals. He has supervised one PhD Scholar
under the DST-SERB (Early Career Research Award Scheme) and is currently guiding two
PhD scholars.
xiii
List of Contributors
Sin Ling Chiam School of Materials and Vineet Kumar Chemistry and
Mineral Resources Engineering, Universiti Bioprospecting Division, Forest Research
Sains Malaysia, Nibong Tebal, Malaysia Institute, Dehradun, India
xiv List of Contributors
Acknowledgments
Prasenjit Bhunia
Kingshuk Dutta
S. Vadivel
1
1.1 Introduction
Photocatalysts and Electrocatalysts in Water Remediation: From Fundamentals to Full Scale Applications,
First Edition. Edited by Prasenjit Bhunia, Kingshuk Dutta, and S. Vadivel.
© 2023 John Wiley & Sons Ltd. Published 2023 by John Wiley & Sons Ltd.
2 1 Fundamentals and Functional Mechanisms of Photocatalysis in Water Treatment
photodegradation. These reactive oxygen species have strong redox potential, which can
degrade almost all types of organic pollutants from water. Thus, ideal photocatalysts must
possess high light absorption ability, suitable bandgap value, low recombination process,
and large surface area.
The construction of an ideal photocatalyst cannot be accomplished easily, however, and
there are several infirmities such as wide bandgap, inappropriate separation, migration of
charge carriers, high recombination rates of excitons, and low light absorption ability that
hindered wider applicability. Especially for bare photocatalysts, these drawbacks are
more prominent. For efficient solar light harvesting, semiconductors with a small band-
gap are required; on the contrary, such semiconducting materials will speed up the recom-
bination process. These two conditions contradict each other, thereby eventually reducing
the overall quantum efficiency. Several modifications were thus done to overcome these
drawbacks.
Heterojunction formation is one of the most common and efficient techniques where the
different materials with suitable band edge potential and bandgap were fabricated together.
Such heterojunction-based photocatalysts provide good charge transfer ability with high
charge separation and better oxidation and reduction capability. This chapter, therefore,
summarizes the characteristic properties and heterojunctions of various metal oxides,
metal phosphides, carbonaceous materials, and other layered materials. Also, the funda-
mental and functional mechanisms of varied photocatalysts utilized in the water decon-
tamination process are briefly described [5, 9–13]. The mechanism of charge transfer in
different heterojunctions, specifically, type II, Z-scheme, and S-scheme are described in
detail. Different characterization techniques including X-ray photoelectron spectroscopy
(XPS), density functional theory (DFT) calculation, trapping experiments, and electron
paramagnetic resonance (EPR) are also elucidated to confirm the successful fabrication of
a heterojunction and charge transfer route. Finally, the applications of different metal
oxides, metal phosphides, and carbonaceous material based heterojunctions are consid-
ered; a summary is then appended.
as the reduction in particle size increases the surface-to-volume ratio and surface energy of
adsorbent. Furthermore, good recyclability is an advantageous characteristic of metal
oxides, which makes them persistent nanomaterials studied in applications from environ-
mental remediation to energy conversion; this is true specifically for transition metal
oxides owing to their good crystallinity, versatile surface characteristics, well-controlled
structure, nontoxicity, high stability, cost-effectiveness, and nature as an earth-abundant
material suitable for the formation of an ideal photocatalyst [14].
Typically, metal oxide semiconductors have a large bandgap value (Eg) of > 3 eV and are
extensively employed in photocatalysis. They also demonstrate great potential for the gen-
eration of both reducing and oxidizing species on irradiation. The valance band maximum
(VBM) and conduction band minimum (CBM) majorly consist of oxygen 2p and metal ns
or nd orbitals, respectively. When photons of energy equal to or more than the bandgap
value strike on the semiconducting surface, the photoexcited electrons accumulate on the
CB while the holes remain on the VB. Once these charge species are created, they are typi-
cally trapped on metal oxide surfaces and can oxidize or reduce the pollutant. The basic
photocatalytic mechanism is attained by following four steps: (i) light absorption and
charge separation, (ii) electron migration to acceptor, (iii) oxidation of donor, and (iv)
charge recombination. The dye photosensitization of metal oxide semiconductors occurs in
the following steps: (i) visible light absorption, (ii) electron transport from the dye (excited
state) to CB of the metal oxide semiconductor, (iii) electrons shifting to acceptor, (iv) charge
recombination, and (v) regeneration of sensitizer. Similarly, the ligand-to-metal charge
transfer (LMCT) photosensitization is accomplished by (i) visible light stimulated LMCT
shifting, (ii) electron transport to acceptor, (iii) charge recombination, and finally (iv)
regeneration of adsorbate or degradation of adsorbate in the presence and absence of elec-
tron donor. Despite several favorable features of metal oxide semiconductors, various prop-
erties should be precisely optimized for practical applications [14, 15].
Generally, wide bandgap and high recombination of excitons are the main drawbacks of
metal oxide semiconductors, which reduces their visible light absorption response and also
decreases the density of available charge carriers to carry photocatalysis. Wide bandgap
allows the absorption of light radiation under the UV region, which consists of only 3–4%
of the solar spectrum. Additionally, UV radiation possesses highly energetic photons that
can directly activate the chemical bonds of some organic substances and cause the forma-
tion of radical intermediates, initiating the nonselective reactions. Furthermore, the study
of UV light active metal oxide semiconductors in the laboratory needs specialized glass-
ware and high-cost UV light sources. Several modifications, therefore, such as doping, tun-
ing of surface, defects creation, and heterostructure formation, are commonly used to
enhance charge separation and visible light response of semiconductors. Crystallinity,
geometry, surface area, and conductivity are some other influencing factors that affect the
photocatalytic performance of metal oxide-based photocatalysts. These semiconductors
exhibit both n and p-type conductivity depending upon the interaction between oxides and
metal orbitals. Usually, O 2p orbitals are more localized whereas oxide orbitals are highly
dispersed, resulting in a smaller effective mass of electrons in comparison to holes. Since
carrier mobility is inversely proportional to carrier effective mass, most metal oxide semi-
conductors show higher mobility of electrons than holes and predominately exhibit n-type
conductivity.
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