Available online at www.sciencedirect.

com Current Opinion in

ScienceDirect Electrochemistry

Review Article

Boron-doped diamond electrodes for the

mineralization of organic pollutants in the real
wastewater
Ansaf V. Karim1, Puthiya Veetil Nidheesh2 and
Mehmet A. Oturan3

Abstract vitally important for sustainable development [1]. The

The presence of recalcitrant organic compounds in wastewater release of these industrial effluents containing higher
poses a serious threat to the ecosystem and human health. chemical oxygen demand (COD) load and recalcitrant
Electrochemical advanced oxidation processes constitute a organic pollutants without proper treatment can
promising way for the mineralization of persistent organic adversely affect the ecosystem [2,3]. The reliability,
compounds. They are commonly used for the transformation of cost, and effectiveness of conventional wastewater
organic pollutants into more biodegradable compounds or their treatment processes to degrade these persistent/toxic
complete removal from water. In this review, we present the organic pollutants are not feasible [4]. Suitable treat-
recent advances in the use of boron-doped diamond (BDD) ment technologies are required to meet the discharging
electrodes in the anodic oxidation process for the mineraliza- standards for these complex effluents.
tion of real wastewater. First, the characteristic properties of
BDD electrodes are discussed followed by the degradation Electrochemical advanced oxidation processes based on
mechanism. In addition, an overview on the application of BDD the in-situ generation of oxidant species have been
electrodes for mineralization of real wastewater is provided. extensively studied to remove persistent organic pollut-
ants from water owing to their wider application range and
Addresses environment-friendliness [5e11]. Selecting suitable
1
Environmental Science and Engineering Department, Indian Institute
electrode material is crucial for electrochemical advanced
of Technology, Bombay, India
2
CSIR-National Environmental Engineering Research Institute, oxidation processes as it governs the process efficiency,
Nagpur, Maharashtra, India selectivity, and energy consumption for the oxidative
3
Université Gustave Eiffel, Laboratoire Géomatériaux et Environne- degradation process [12e14]. Boron-doped diamond
ment (LGE), EA 4508, 77454, Marne-la-Vallée, France (BDD) electrodes are nonactive electrodes with unique
Corresponding authors: Oturan, Mehmet A. (mehmet.oturan@univ-
characteristics possessing wide potential window, high O2-
eiffel.fr); Nidheesh, P. V. ([email protected]), evolution overpotential, electrochemical stability, exten-
([email protected]) sive application for low detection of species, and so on that
qualifies them as an optimal electrode material for elec-
trochemical mineralization of organic compounds [15e
Current Opinion in Electrochemistry 2021, 30:100855
20]. Compared with other electrodes, BDD anodes have
This review comes from a themed issue on Diamond Electrochemistry powerful oxidation capacity under mild operating condi-
(2021)
tions and can also be used as cathodes in the electro-
Edited by Guohua Zhao, Nianjun Yang, Carlos A. Martínez-Huitle chemical oxidation process for generating extra reactive
For complete overview about the section, refer Diamond oxygen species in the system [21e23]. Overall, the use of
Electrochemistry (2021) BDD electrodes in the treatment of complex wastewater
Available online 8 October 2021 effluents seems to be of great interest. Therefore, the
https://doi.org/10.1016/j.coelec.2021.100855 present review is focused on the application of BDD
2451-9103/© 2021 Elsevier B.V. All rights reserved.
electrodes for the mineralization of real wastewater
covering the works published mainly during the last four
years in this field. The governing structural characteristics
Keywords
of BDD electrodes for oxidation of organics and its appli-
Electrochemical oxidation, Boron-doped diamond electrode, Anodic
oxidation, Wastewater, Mineralization.
cation for the treatment of real wastewater are discussed.

Introduction Structural characteristics of boron-doped

The presence of toxic and/or persistent organic com- diamond for electrochemical oxidation
pounds in real wastewater is a major concern as the As the material of the electrode is a deciding factor in
water crisis continues to grow, and its recycling becomes the effectiveness of anodic oxidation, the characteristic

www.sciencedirect.com Current Opinion in Electrochemistry 2021, 30:100855

2 Diamond Electrochemistry

properties of BDD such as corrosion resistance, chemi- (3D) microporous BDD electrodes with uniformly
cal inertness and stability, high overpotential, and high distributed pores reduced electron transfer resistance,
current efficiency make it a versatile electrode for and the interconnected network exhibited excellent
electrochemical oxidation of organic pollutants in an electrochemical activity owing to their enhanced surface
aqueous medium [24,25]. BDD anode materials are area and mass transfer rate. Although BDD electrodes
chemically inert with higher O2 evolution overpotential outperform other electrodes, their fabrication cost,
when compared with Pt and dimensionally stable power consumption, and poor machinability are major
anode electrodes and therefore are beneficial to drawbacks [31,33,34]. Although electrodes such as
generate more ,OH physically adsorbed on the surface PbO2, carbon felt, and so on are cost-effective elec-
(BDD [,OH]) [26,27]. In addition, as the O2 evolution trodes with good mechanical strength, their service life
potential of electrodes increases, the energy consump- and electrochemical performance are less when
tion by the electrodes decreases, and degradation effi- compared with BDD [22,35].
ciency increases [26]. Furthermore, the highly
remarkable corrosion stability of BDD anodes under Electrocatalytic oxidation mechanism using
extreme acidic solutions and its ability to produce boron-doped diamond
weakly adsorbed ,OH makes it efficient anode materials The electrocatalytic oxidation of organic compounds by
for faster oxidation of organic compounds [28]. BDD electrodes takes place typically through direct,
indirect, and mediated oxidation by the oxidants
The electrochemical mineralization efficiency of BDD generated as shown in Figure 1 [13,21,22]. In the direct
electrodes also depends on the sp3/sp2 ratio on the oxidation process, electron transfer from the BDD sur-
surface of the BDD film electrode, a higher sp3 con- face directly reacts with organic compounds [23]. The
centration (diamond) over sp2 (graphite) is preferred for water discharge on the BDD anode leads to the forma-
more generation of radicals on the electrode surface. tion of the BDD (,OH) for indirect oxidation of organic
However, conversely, with lower diamond content, the compounds [36,37]. The interaction between the ,OH
evolution of molecular O2 is more favored promoting the and the anode surface has a significant effect on the
direct oxidation of organic compounds on the BDD chemical reactivity as the weaker physisorption of radi-
surface [29]. The sp2 carbon on the BDD electrode acts cals onto the BDD surface rather than chemisorbed
as impurities for promoting electrochemical conversion radicals as in the case of active anodes (Pt, dimension-
and results in more O2 production [29]. Furthermore, ally stable anode, PbO2, and so on) makes it easily
the boron-doping level is an important parameter available for oxidation of organic compounds at its vi-
determining the charge transfer, the width of the po- cinity [27,33]. Furthermore, these quasi-free weakly
tential window, and electroanalytical performance in the adsorbed radicals [BDD (,OH)] react with organic
BDD electrode. Higher loading of boron may increase compounds and form degradation intermediates under
the sp2 impurity level in the electrode. However, mild operative conditions [21]. Because the oxygen
beyond an optimum level of boron doping, the number evolution reaction occurs at a high overpotential on the
of charge carriers for conduction decreases and reduces surface of the BDD anode, the mass transfer of organic
the oxidation potential of electrodes [13,26,30]. compounds toward the surface of the electrode should
be high. Indirect oxidation involves the generation of
Moving forward, the surface roughness of the electrodes reactive oxidant species such as O3, H2O2, and other
increases the effective electroactive surface area, which radical species in the aqueous solution [6]. Furthermore,
could help improve the contact area between organic mediated oxidation is the process of generation of active
compounds and BDD electrodes, and further increases species such as active chlorine species, persulfate, and
the reaction sites for degradation of organic compounds, sulfate radicals on the BBD anode surface resulting in
producing more ,OH. Depending on the surface modi- the degradation of organic compounds [3,12,38].
fication techniques such as surface etching or
nanotemplate deposition, the effective electroactive Enhancement of boron-doped diamond
surface area of the electrodes may vary, and some of activity for degradation of organic
them may produce irregular nanopores, adding impu- compounds
rities or low mass transfer, and so on. Improving the The operational performance of BDD anodes for organic
catalyst surface by nanoparticle etching on BDD elec- pollutant removal may vary with the structural modifi-
trodes can enhance the surface area of the electrode, cations of electrodes or with the presence of electrolytes
which concurrently improves the contact area of the in the solution. Surface modification of the BDD anode
electrode for more adsorption of organic compounds by surface termination, doping, nanofabrication, and so
[31]. Furthermore, the porous nanostructures (square on can overcome the drawback associated with the cost
and triangular holes) of BDD electrodes can improve the and productivity of BDD electrodes for wastewater
roughness of the electrode and also enhance the transfer treatment [39]. Improving the surface area of the BDD
of electrons through the nano surface [31]. In a study anode can enhance the production of more ,OH.
conducted by Mei et al. [32], the three-dimensional Furthermore, modifying the electrochemical reactor
Current Opinion in Electrochemistry 2021, 30:100855 www.sciencedirect.com
 BDD for wastewater mineralization Karim et al. 3

Figure 1

Possible BDD-based electrochemical degradation mechanism of organic compounds. Reprinted with permission from the study reported by McBeath
et al. [20]. Copyright The Royal Society of Chemistry 2019. BDD, boron-doped diamond.

configurations from static to flow cell systems can resulted in obtaining a 3D material that exhibits high
overcome the diffusion limitations and enhance the surface area and high active site density in a homoge-
mass transport to the anode, ensuring the efficient uti- neous porosity distribution and exhibited high electro-
lization of current density [40,41]. In a study conducted catalytic oxidation resulting in a higher degradation rate
by Brito et al. [41], higher degradation of an azo dye was and lower energy consumption during the degradation of
observed with a perpendicular inlet-outlet flow reactor brilliant green dye [43]. Surface pretreatment of the
system which enhanced the contact time between the BDD electrode to control the H2 and O2 evolution can
electrode and pollutant and improved the cur- influence the electrochemical activity of the electrode
rent efficiency. including the surface redox processes and surface
wettability [44].
The use of BDD electrode layers grown on other sub-
strates such as Si, carbon fiber, Ti, and so on can also The use of different electrolytes, oxidants or external
enhance electrocatalytic performance. In a study con- energy sources in the system can generate more reactive
ducted by Morda
cı́ková et al. [42], the use of the BDD oxidant species in the solution such as H2O2, Cl,, SO-, 4
layer grown on structured Si substrates led to a signifi- [16,45]. Depending on the electrolyte used, BDD
cant increase in the removal efficiency of a mixture of anodes are capable of generating active oxidizing species
pharmaceuticals owing to the enhancement in surface such as ozone, H2O2, chloro-oxidant species, persulfate,
area of the electrode. Further in another study, the use and so on [46]. The addition of supporting electrolytes
of carbon fiber as a substrate for the BDD electrode such as NaCl or sodium sulfate can enhance the

www.sciencedirect.com Current Opinion in Electrochemistry 2021, 30:100855

4 Diamond Electrochemistry

electrochemical process efficiency via the generation of current density, pH, reaction time, and so on, higher
active chlorin species and persulfate/sulfate radical, mineralization can be achieved by electrochemical ap-
respectively, to achieve higher degradation rates [36,47]. plications using BDD electrodes. A mixture of industrial
Photo assistance (ultraviolet [UV]) and visible light) for wastewater collected from the chemical manufacturing
electrochemical degradation processes using BDD industry containing polyfluoroalkyl and perfluoroalkyl
electrodes can enhance radical species production and substances was successfully mineralized into shorter
improve the mass transfer limitations to improve overall chain perfluorocarboxylic acids using a BDD anode-
degradation efficiency [46]. based electrochemical process [48]. Experiments con-
ducted on the effluents resulted in 99.7% perfluoroalkyl
Electrochemical mineralization of real substance removal with more than 90% total organic
wastewater using boron-doped diamond carbon (TOC) reduction at a current density of
The electrochemical oxidation processes with BDD 50 mA cm
1 for 10 h. A summary of BDD-based elec-
electrodes with higher potential to generate BDD trochemical treatment of real wastewater is shown
(,OH) on the surface by water discharge can effectively in Table 1.
mineralize real complex wastewater. Furthermore, with
the characteristic properties of the BDD anode and The selection of suitable anode material determines the
controlling the operational parameters such as the efficiency of electrochemical treatment processes,

Table 1

Wastewater mineralization by the BDD anode.

Wastewater Reactor Cathode Optimized conditions Highlights of the study References

configuration

Petrochemical Electrochemical flow Ti disc 40 mA cm−2 current density, BDD anode-based [56]
cell in a single temperature 25  C, 8 h treatment enhanced the
compartment reaction chemical oxygen demand
(COD) removal with less
power consumption when
compared with the Pt
anode in an
electrochemical flow cell
reactor
Textile effluents Electrolytic cells with BDD electrodes 60 mA cm−2 current density, Complete COD removal [3]
two parallel flow- supported on Si 3.0 g L−1 NaCl, pH 2.0 was observed in 3 h
by compartments substrates electrolysis
Pharmaceutical Single-compartment Stainless steel 30 mA cm−2 current density, Among the 60 samples of [57]
electrochemical temperature 25  C, pH real pharmaceutical
flow cell 6–6.5 effluents, efficient
mineralization for 80% of
the samples were
observed with
electrochemical process
compared with Fenton’s
oxidation
Winery Electrochemical Stainless steel plate 50 mM Na2SO4 and NaCl as Complete mineralization of [58]
oxidation in an electrolytes, 60 mA cm−2 wastewater was observed
undivided open current density in the presence of salts
cell owing to the production of
SO-4 and oxidative
chlorine species
Washing machine Prepilot plant parallel Ti 7 g L−1 Na2SO4, 66 mA cm−2 88% COD removal [49]
effluent disc in a single current density, 6 h efficiency was observed
compartment reaction with BDD electrodes
electrochemical when compared with 71%
flow reactor for Ti/Pt anode
Woodworking Electrochemical Stainless steel sheet 45 mA cm−2 current density, Addition of electrolytes [59]
wastewater oxidation in an pH 7, 2 g NaCl/500 mL, significantly reduced the
open-comparted 8 h reaction time energy consumption and
cylindrical glass resulted in 93%
reactor mineralization

BDD, boron-doped diamond.

Current Opinion in Electrochemistry 2021, 30:100855 www.sciencedirect.com

 BDD for wastewater mineralization Karim et al. 5

especially, the efficiency of the anodic oxidation process. electrochemical means reacted with sulfate and chlo-
The electrochemical process efficiency of BDD and Ti/ rides to generate SO,- ,
4 and Cl and selectively reacted
Pt electrodes for the treatment of real washing machine with organic compounds to enhance the TOC removal
effluents was compared at a prepilot plant scale study of wastewater. Higher contents of organics in real
[49]. The increase in applied current density and the wastewater may require a significant amount of radicals
presence of electrolytes improved the mineralization to mineralize it. In a study conducted by Olvera-Vargas
process. However, significant performance was observed et al. [2], the contribution of homogeneous and heter-
while using the BDD electrode with less energy con- ogenous BDD-based electro-Fenton for the mineraliza-
sumption and resulted in 88% COD removal when tion of pharmaceutical wastewater was analyzed. As
compared with 71% for the Ti/Pt electrode owing to the shown in Figure 2, they concluded that a synergy be-
enhanced production of active chlorine species. In tween the homogenous ,OH and the heterogeneous
another study, when BDD and a dimensionally stable BDD (,OH) accelerated the mineralization in the initial
electrode (Ti/SnO2eSb) were used for the electro- stages. Later, the short-chain carboxylic acids were
chemical pretreatment of vinasse from wine distillery predominantly mineralized by electron transfer reaction
wastewater, BDD performed better with higher COD from the BDD surface resulting in 97.1% of TOC
removal at lower energy consumption [50]. The better removal in 6 h reaction time. Although BDD electrodes
performance observed for BDD electrodes was attrib- are efficient in the mineralization of organic pollutants
uted to the higher stability and better selectivity of in wastewater, the cost associated with it is a major
oxidation compounds. Although comparing the perfor- hurdle. An electro-Fenton study conducted by Mousset
mance of BDD electrodes with Ti/IrO2 and Ti/Pt anodes et al. [55] for the mineralization of real effluents from an
for the mineralization of biologically pretreated landfill electronic industry reported that higher mineralization
leachate, higher COD removal of 87% was observed with was observed with BDD electrodes when compared with
BDD electrodes owing to their nonactive nature gen-
eration of BDD (,OH) on its surface [51]. Figure 2

The use of oxidants or external energy sources can

improve the process efficiency of BDD-based electro-
chemical mineralization processes [52]. Enhanced
mineralization of industrial effluent polluted with
metoprolol and caffeine was observed for the photo-
assisted BDD-based electrochemical oxidation process.
The UV irradiation resulted in the generation of highly
oxidizing sulfate and chloride radicals from the real
wastewater and improved the overall mineralization
process. The real wastewater coming from the pharma-
ceutical industry and municipal wastewater treatment
plant containing pharmaceutical compounds was treated
using a UV and ultrasound irradiation-assisted electro-
chemical degradation process [53]. Both the irradiations
enhanced the mineralization of organic compounds;
however, the higher energy consumption of ultrasound
irradiation made their combination less attractive when
compared with UV irradiation. The combination of
Fenton and UV irradiation with BDD anode electro-
oxidation improved the mineralization of real olive oil
mill wastewater owing to the enhanced production of
BDD (,OH) in the solution [52]. The photolytic action
of UV on the photoactive by-products and Fe(OH)2þ to
Fe2þ improved the production of BDD (,OH) in the
system, and the biodegradability of the wastewater was
improved from 0.334 to 0.6 after 6 h of treatment [52].

The organic matrix may have a significant effect on the

electrochemical mineralization of wastewater. The
Schematic representation of the removal of organics in pharmaceutical
presence of chloride and sulfate ions in biologically
wastewater by the electro-Fenton process involving homogenous (OH)
pretreated pharmaceutical wastewater enhanced the and heterogenous BDD (OH) hydroxyl radicals. Reprinted with permis-
mineralization during a BDD-based electrochemical sion from the study reported by Olvera-Vargas et al. [2], Copyright © 2020
oxidation process [54]. The BDD (,OH) generated by Elsevier B$V.

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6 Diamond Electrochemistry

the carbon-PTFE cloth. However, the economic analysis This study evaluated the efficiency of homogeneous and heteroge-
neous electro- Fenton process for the treatment of real pharmaceutical
of the study concluded that affordable materials with wastewater and explaned the mechanism of simultaneous radical
low energy requirements such as the carbon-PTFE generation during the process.
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8 Diamond Electrochemistry

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