sustainability

Review
Synthesis and Characterization of Nanomaterials for
Application in Cost-Effective Electrochemical Devices
Hosam M. Saleh * and Amal I. Hassan

Radioisotope Department, Nuclear Research Center, Egyptian Atomic Energy Authority, Cairo 11787, Egypt
* Correspondence: [email protected] or [email protected]; Tel.: +20-1005191018;
Fax: +202-37493042

Abstract: Nanomaterials have gained significant attention as a remarkable class of materials due to
their unique properties and the fact that they encompass a wide range of samples with at least one di-
mension ranging from 1 to 100 nm. The deliberate design of nanoparticles enables the achievement of
extremely large surface areas. In the field of cost-effective electrochemical devices for energy storage
and conversion applications, nanomaterials have emerged as a key area of research. Their excep-
tional physical and chemical properties have led to extensive investigations aimed at improving the
performance and cost-effectiveness of electrochemical devices, including batteries, supercapacitors,
and fuel cells. The continuous development and enhancement of these high-performance materials
are driven by the demand for enhanced productivity, connectivity, and sustainability at a reduced
cost. This review focuses on the electrochemical performance of electrodes, energy storage, and
electrochemical sensors (ES) based on nanotechnology. It discusses the application of nanotechnology
in electrochemistry for water purification and the fate of substances in water, while also introducing
green nanotechnology and cost-effective, high-fidelity product creation through electrochemical meth-
ods. The study emphasizes the synthesis of novel nanomaterials, such as metal–organic frameworks
(MOFs), covalent organic frameworks (COFs), and MXenes, with applications in electrochemical
devices. Furthermore, it explores the integration of nanostructures with electrochemical systems in
economically significant and future applications, along with the challenges faced by nanotechnology-
based industries. The paper also explores the interplay between nanomaterials and biosensors, which
play a vital role in electrochemical devices. Overall, this review provides a comprehensive overview
Citation: Saleh, H.M.; Hassan, A.I.
of the significance of nanomaterials in the development of cost-effective electrochemical devices for
Synthesis and Characterization of
energy storage and conversion. It highlights the need for further research in this rapidly evolving field
Nanomaterials for Application in
Cost-Effective Electrochemical
and serves as a valuable resource for researchers and engineers interested in the latest advancements
Devices. Sustainability 2023, 15, 10891. in nanomaterials for electrochemical devices.
https://doi.org/10.3390/
su151410891 Keywords: nanomaterials; green nanotechnology; electrochemical devices; cost-effective; biosensors;
energy storage
Academic Editor: Changhyun Roh

Received: 25 May 2023

Revised: 24 June 2023
Accepted: 3 July 2023 1. Introduction
Published: 11 July 2023
The development of cost-effective electrochemical devices is crucial for efficient energy
storage and conversion, which is essential for sustainable development. Nanomaterials
have demonstrated great potential in enhancing the performance of electrochemical devices,
Copyright: © 2023 by the authors.
but the synthesis of these materials for large-scale applications remains a challenge [1]. Sev-
Licensee MDPI, Basel, Switzerland.
eral synthesis methods have been developed to address this challenge, including solution-
This article is an open access article based, template-based, and microwave-assisted synthesis. These methods have shown
distributed under the terms and promise in producing high-quality nanomaterials in large quantities, and they have the
conditions of the Creative Commons potential to reduce production costs. Integrating nanomaterials into electrochemical devices
Attribution (CC BY) license (https:// is also a significant challenge, as the properties of nanomaterials differ significantly from
creativecommons.org/licenses/by/ those of their bulk counterparts [2]. The interface between the nanomaterials and other
4.0/). components of the electrochemical device is critical, and it can significantly influence device

Sustainability 2023, 15, 10891. https://doi.org/10.3390/su151410891 https://www.mdpi.com/journal/sustainability

Sustainability 2023, 15, 10891 2 of 52

performance and efficiency. Therefore, optimizing the integration of nanomaterials into

electrochemical devices is crucial for realizing their full potential.
The synthesis of nanomaterials on a large scale for practical applications remains a chal-
lenge. However, significant progress has been made in developing various synthesis meth-
ods, such as solution-based methods, template-based methods, and microwave-assisted
synthesis [3,4]. These approaches show promise in producing high-quality nanomaterials
in large quantities while also potentially reducing production costs.
Integrating nanomaterials into electrochemical devices presents another significant
challenge. The properties of nanomaterials differ significantly from their bulk counterparts,
necessitating careful consideration of their integration with other components of the de-
vice. The interface between nanomaterials and the device’s other constituents critically
influences device performance and efficiency [5]. Therefore, optimizing the integration of
nanomaterials is crucial to fully exploit their potential in electrochemical devices [5].
One key aspect that distinguishes nanomaterials in electrochemical applications is
their electrical properties. Nanomaterials can be broadly classified as conductive, semi-
conductive, or insulating based on their ability to conduct electricity. Conductive nanoma-
terials, such as carbon nanotubes and graphene, exhibit high electrical conductivity and
find extensive use as current collectors, electrodes, and catalysts [6]. Semi-conductive nano-
materials, such as metal oxides and sulfides, possess moderate electrical conductivity and
can serve as active materials for energy storage and conversion. Insulating nanomaterials,
including metal–organic frameworks (MOFs) and covalent organic frameworks (COFs),
offer low electrical conductivity but provide high surface area and large pore volumes,
making them suitable support materials for electrochemical devices [7].
Moreover, the composition of nanomaterials also affects their electrical properties. In-
novative nanomaterials like MOFs, COFs, and MXenes have gained considerable attention
due to their tunable electrical properties and high surface areas, making them promising
candidates for electrochemical device applications [7].
Overall, the unique properties of nanomaterials make them attractive for use in electro-
chemical devices, and their potential for cost-effectiveness makes them even more appeal-
ing. By understanding the different types of nanomaterials and their properties, researchers
can continue to develop new and improved electrochemical devices with enhanced per-
formance and cost-effectiveness. Therefore, this review will highlight electrochemical
techniques, energy storage, as well as electrochemical sensors based on nanotechnology. As
well as the integration of nanostructures with the electrochemical system in applications of
economic interest. It will shed light on the future of these applications and the challenges of
environmental sustainability. Moreover, innovative sustainable materials have been used in
nuclear applications such as cellulosic waste in treatment [8,9] or cement mixed with plant
waste [10,11], natural clay [12,13], bitumen [14,15] or with asphaltene and polymer [16],
cement waste [17], and glass [18–20] for waste stabilization and radiation shielding.

2. Classification of Nanomaterials
Nanomaterials can be classified based on their dimensions, such as 0D, 1D, and 2D
structures. Zero-dimensional (0D) nanomaterials are spherical nanoparticles and are the simplest
type of nanomaterials. Examples of 0D nanomaterials include metal nanoparticles like gold and
silver, semiconductor nanoparticles like quantum dots, and oxide nanoparticles like titanium
dioxide [21]. These nanomaterials have unique physical and chemical properties compared to
their bulk counterparts, such as a high surface-to-volume ratio and quantum confinement effects.
Moving on to one-dimensional (1D) nanomaterials, they have one dimension in
the nanoscale range. Examples of 1D nanomaterials include nanowires, nanotubes, and
nanorods. Carbon nanotubes, silicon nanowires, and zinc oxide nanorods are some com-
mon examples of 1D nanomaterials. These nanomaterials are appealing for use in a wide
range of electrical, photonic, and energy storage applications because of their excellent
mechanical, electronic, and optical capabilities that result from their one-dimensional struc-
ture. Finally, two-dimensional (2D) nanomaterials have two dimensions in the nanoscale
 norods. Carbon nanotubes, silicon nanowires, and zinc oxide nanorods are some com-
mon examples of 1D nanomaterials. These nanomaterials are appealing for use in a wide
range of electrical, photonic, and energy storage applications because of their excellent
mechanical, electronic, and optical capabilities that result from their one-dimensional
structure. Finally, two-dimensional (2D) nanomaterials have two dimensions in the na-
Sustainability 2023, 15, 10891 3 of 52
noscale range. Examples of 2D nanomaterials include graphene, transition metal dichal-
cogenides (TMDs) like MoS2 and WS2, and black phosphorus [22]. These nanomaterials
have unique electronic, mechanical, and optical properties that make them promising
range. Examples
candidates of 2Dapplications,
for various nanomaterials include graphene,
including transition
sensors, energy metal and
storage, dichalcogenides
electronic
(TMDs)
devices. like MoS 2 and WS 2 , and black phosphorus [22]. These nanomaterials have unique
electronic,
Nanomaterials can also be classified based on their electric properties, such as insu-for
mechanical, and optical properties that make them promising candidates
various applications, including
lating, semiconducting, sensors,
and metal-like energy storage,
properties. and electronic
Insulating devices.
nanomaterials do not con-
Nanomaterials can also be classified based on their electric properties,
duct electricity and have a wide band gap. Examples of insulating nanomaterials such as insulating,
include
semiconducting,
metal and metal-like
oxides like titanium dioxide,properties. Insulating
zinc oxide, nanomaterials
and aluminum oxide.do not conduct
These electricity
nanomaterials
and
are have aused
widely wideinband gap. applications,
various Examples of insulating
including nanomaterials include
catalysis, energy metaland
storage, oxides
envi-like
titanium dioxide,
ronmental remediation.zinc oxide, and aluminum oxide. These nanomaterials are widely used in
various applications, including catalysis, energy storage, and environmental
Scheme 1 and Table 1 summarize the use of nanomaterials in various types of elec- remediation.
Scheme 1 and Table 1 summarize the use of nanomaterials in various types of electro-
trochemical devices.
chemical devices.

Scheme 1. 1.
Scheme Nanomaterials in in
Nanomaterials various types
various of of
types electrochemical devices.
electrochemical Made
devices. byby
Made authors.
authors.

Table 1. 1.
Table Nanomaterials Used
Nanomaterials inin
Used Various Electrochemical
Various Devices.
Electrochemical Devices.

Electrochemical
ElectrochemicalDevice
DeviceNanomaterials Used
Nanomaterials Used Applications
Applications References References
Batteries Nanostructured metals, metal ox- Electrode materials to improve [20,21]
Electrode materials to improve performance,
Nanostructured metals, metal
increase surface area, improve conductivity,
Batteries oxides, and carbon-based [20,21]
and provide higher energy and
materials, MOFs, COFs, MXenes.
power densities
Carbon nanotubes, graphene, and Electrode materials to increase surface area,
Supercapacitors other carbon-based materials, improve conductivity, and provide high power [22–26]
MOFs, COFs, and MXenes. and energy densities
Platinum, gold, and other metal Catalysts to improve the efficiency of
Fuel Cells nanoparticles, MOFs, electrochemical reactions that [27]
COFs, MXenes. generate electricity
Sustainability 2023, 15, 10891 4 of 52

Table 1. Cont.

Electrochemical Device Nanomaterials Used Applications References

Sensing elements to improve sensitivity and
Metal nanoparticles, metal oxides,
selectivity due to their high surface area, high
Sensors and carbon-based materials, MOFs, [28]
catalytic activity, and unique optical and
COFs, MXenes
electrical properties

Semiconducting nanomaterials have intermediate electrical conductivity, and their con-

ductivity can be tuned by doping or changing their size. Examples of semiconducting nano-
materials include quantum dots, carbon nanotubes, and TMDs [29]. Various electrochemical
devices can benefit from the use of certain nanomaterials because of their distinctive electrical
and optical capabilities in the fields of electronics, photonics, and energy conversion. For
example, metal nanoparticles like gold and silver have been used in electrochemical sensing
and catalysis. Carbon nanotubes have shown potential as electrodes in batteries and fuel
cells, while graphene has shown promise as a material for supercapacitors. Some studies
focused on the use of graphene as a means of stabilizing the interface between silicon-based
electrodes and electrolytes to achieve a stable cycle life. While coating graphene on the surface
of nanostructured silicon electrodes is an effective approach, most of the graphene-supported
anode reports involve silicon nanoparticle structures. The study by Yang et al. [30] suggested
that coating graphene layers on silicon nanowires could be a viable option for stabilizing the
interface between silicon-based electrodes and electrolytes. After 500 charge–discharge cycles,
the resultant silicon nanowires showed excellent Coulombic efficiencies of over 99% and a
huge reversible capacity of 1650 mA h g1. The nanowires were composed of silicon carbide
nanocrystals and surrounded by a homogenous graphene shell. Furthermore, Si nanowires
were formed in situ by a gold-catalyzed procedure (Figure 1). These nanowires, when backed
by graphene, showed an initial reversible lithium extraction capacity of 2009 mA h g1, and
after 30 cycles at 420 mA g1, a reversible capacity of 1400 mA h g1 was achieved. These
findings demonstrate the potential of graphene-supported silicon nanowires and suggest a
promising avenue for further research in this area. Furthermore, insulating nanomaterials like
titanium dioxide have been used as anodes in lithium-ion batteries, while semiconducting
nanomaterials like quantum dots have been used in solar cells [2].
To better understand and categorize the different types of nanomaterials that can be
used in electrochemical applications, a classification based on different classes of materials
has been proposed. These classes include carbon-based nanomaterials, metal oxides, and
hydroxides, conducting polymers, and hybrid materials. Carbon-based
Sustainability 2023, 15, x FOR PEER REVIEW
nanomaterials such
5 of 55
as graphene, carbon nanotubes, and fullerenes have been extensively studied and show
great potential for improving the performance of electrochemical devices, particularly in
energy storage applications such as batteries and supercapacitors [31].

Figure 1. GNS-supported Si nanowires: (a) SEM image and (b) TEM image. Reprinted with permis-
sion from
Figure ref. [32] license
1. GNS-supported 5535970520510.
Si nanowires: Copyright
(a) SEM image and (b) Elsevier in Reprinted
TEM image. 25 April with
2023.per-
mission from ref. [32] license 5535970520510. Copyright Elsevier in 25 April 2023.

3. Applications of Nanomaterials in Electrochemical Devices

Metal oxides and hydroxides, including titanium dioxide, zinc oxide, and iron ox-
ide, have also shown promise in electrochemical devices due to their high surface area
Sustainability 2023, 15, 10891 5 of 52

3. Applications of Nanomaterials in Electrochemical Devices

Metal oxides and hydroxides, including titanium dioxide, zinc oxide, and iron oxide,
have also shown promise in electrochemical devices due to their high surface area and
redox properties [33]. Conducting polymers such as polyaniline and polypyrrole offer
unique properties such as high conductivity and tunable redox potential, making them
suitable for a range of electrochemical applications. Hybrid materials, which combine two
or more classes of nanomaterials, have also been investigated and offer the potential for
improved performance and functionality. When electroactive materials are nanostructured,
significant alterations are made to the devices’ electro-chemical characteristics. Assembled
from quasi-zero-dimensional structures or building blocks (nanoparticles), two- and three-
dimensional nanometer-sized structures like dye-sensitized solar cells (DSSC) are one
example. Moreover, 0D nanoparticles and nanodots have attracted significant attention for
their potential use in batteries due to their small size and high surface area. In particular,
0D nanoparticles and nanodots exhibit unique physical and chemical properties that
make them promising candidates for electrode materials in batteries. These materials can
significantly improve the performance of batteries by providing high capacity, fast charging
and discharging rates, and a long cycle life [34].
One advantage of 0D nanoparticles and nanodots is their high surface area, which
provides numerous active sites for electrochemical reactions. This property can enhance
the capacity of batteries by increasing the amount of active material available for electro-
chemical reactions [35]. Additionally, the small size of 0D nanoparticles and nanodots
enables fast diffusion of lithium ions, leading to faster charging and discharging rates.
More efficient ion transfer and enhanced electrochemical performance are two benefits of
using 0D nanoparticles and nanodots in batteries, which benefit from their high surface
area-to-volume ratio [35].
Research has been conducted on various types of 0D nanoparticles and nanodots,
including metal oxide nanoparticles, carbon nanodots, and quantum dots. For instance,
studies have shown that tin oxide nanoparticles can improve the cycling stability and rate
capability of lithium-ion batteries, while carbon nanodots have been proven to enhance the
capacity and rate performance of sodium-ion batteries [36]. Quantum dots have also been
investigated for their potential use in next-generation batteries because of their unique
electronic and optical properties [36]. Moreover, 0D nanoparticles and nanodots have
unique properties that make them attractive for use in various electrochemical devices
beyond just batteries. For instance, their high surface area-to-volume ratio and tunable size
and shape make them ideal for use in sensors, catalysts, and supercapacitors. Addition-
ally, their small size can facilitate electron transfer and enhance ion diffusion, improving
overall device performance. Recent research has focused on developing novel synthetic
methods for producing highly uniform and monodisperse 0D nanoparticles and nanodots,
as well as exploring their electrochemical properties and potential applications in various
electrochemical devices [37].
Extensive research has been carried out on 1D nanowires and 2D nanosheets for
their applications in various electrochemical devices, such as supercapacitors and fuel
cells [38]. These materials exhibit high specific capacitance and fast charge/discharge rates
in supercapacitors due to their large surface area and excellent conductivity. In fuel cells,
1D nanowires and 2D nanosheets have been used as catalysts to improve reaction kinetics
and reduce the cost of electrochemical reactions. The unique properties of 1D and 2D
nanomaterials, such as their mechanical strength, flexibility, and transparency, make them
attractive for various electrochemical device applications [39].
Three-dimensional (3D) nanometer-sized structures, also known as nanoarchitectures
or nanostructures, have also been investigated for their potential use in electrochemical
devices. These structures can offer a high surface area and unique porosity, which can
enhance electrochemical reactions and improve the performance of electrochemical de-
vices [40]. Examples of 3D nanostructures include nanocubes, nanorods, and mesoporous
silica. Researchers have explored their use in batteries, supercapacitors, and fuel cells with
Sustainability 2023, 15, 10891 6 of 52

promising results. However, challenges remain in synthesizing and integrating 3D nanos-

tructures into practical electrochemical devices, and more research is needed to overcome
these challenges and fully exploit the potential of these materials.
Definite analytical techniques are used for nanoparticle detection and characterization.
Advanced technologies include electron microscopes for scanning or transmission (SEM,
TEM) [38,39,41,42]. Different optical procedures can provide various types of physico-
chemical information for nanoparticles, but their usefulness depends on the technology
and particular material properties, such as composition and scale [43]. Electrochemical
technologies can address some problems, such as low-cost, easy-to-use portable controllers
and self-powered devices [44]. As many nanoparticles can generate electrical signals, have
high biocompatibility and stability, and are simple to operate, nanotechnology may be a
promising solution for many electrochemical technologies [45].
Quantitative techniques are required to quantify exposure to foreign organisms to
support the creation and implementation of biomonitoring programs. The electrochemical
phenomenon has many technological applications, such as chemical synthesis, electroextrac-
tion, metal refining, batteries, fuel cells, sensors, and surface modification by electrostatic
precipitation, separation, and corrosion. Recent studies have emphasized the importance
of nanotechnology in constructing promising electrode materials for high-performance
supercapacitors [43–47]. The synthesis of nitrogen-rich activated nanosized carbon with
hierarchical micro/mesoporous and ultra-high specific surface area was greatly simplified
and chemical waste was reduced when Zheng et al. [48] revealed a template-free and one-
step carbonization–activation technology. Activated carbon with a high nitrogen content
and strong electrochemical characteristics was obtained by synthesizing chitin nanoparticles
in a NaOH/urea solvent using a mechanically driven sol–gel transition process.
In Table 2, we compare different types of nanomaterials used in various electrochem-
ical devices. Metal oxides and hydroxides, such as titanium dioxide, zinc oxide, and
iron oxide, offer high surface area and redox properties, making them suitable for elec-
trochemical applications. Conducting polymers like polyaniline and polypyrrole exhibit
high conductivity and tunable redox potential, providing versatility in electrochemical
devices. Hybrid materials, which combine different nanomaterial classes, offer improved
performance and functionality due to synergistic effects. Furthermore, nanomaterials de-
signed for electrode materials in electrochemical devices demonstrate tailored properties for
high-performance devices. By understanding the distinctive characteristics and synthesis
methods of these nano-materials, researchers can develop cost-effective electrochemical
devices with enhanced performance.

Table 2. Comparative Analysis of Morphological Features and Properties of Nanomaterials Synthe-

sized via Different Methods.

Nanomaterials Synthesis Method Morphological Features Properties References

Metal oxides and High surface area, redox Suitable for electrochemical
Various [46,47,49,50]
hydroxides properties devices
Conducting polymers (e.g., High conductivity, tunable Versatile for electrochemical
Various [51]
polyaniline, polypyrrole) redox potential applications
Combination of
Improved performance and Enhanced properties
Hybrid materials nanomaterial [52]
functionality through synergy
classes
Promising for batteries,
0D nanoparticles and Various synthesis
Small size, high surface area sensors, catalysts, [53]
nanodots methods
supercapacitors
Suitable for supercapacitors,
1D nanowires and 2D Various synthesis Large surface area, excellent
fuel cells, and other [54]
nanosheets methods conductivity
electrochemical devices
Sustainability 2023, 15, 10891 7 of 52

Table 2. Cont.

Nanomaterials Synthesis Method Morphological Features Properties References

3D nanostructures
Various synthesis High surface area, unique Potential for batteries,
(nanocubes, nanorods, [55]
methods porosity supercapacitors, fuel cells
mesoporous silica)
Nanomaterials for Various synthesis Tailored properties for Potential for cost-effective
[56]
electrode materials methods high-performance devices electrochemical devices

4. Morphology and Properties of Nanomaterials Prepared by Different Synthesis Methods

Both top-down and bottom-up methods are employed in the production of nano-
materials. Top-down methods reduce raw materials to their nanoscale building blocks.
Mechanical milling, laser ablation, etching, sputtering, and electro-explosion are all ex-
amples of top-down processes. Manufacturing phase blends and nanocomposites can
benefit greatly from mechanical milling as it is a low-cost method for developing nanoscale
products from bulk materials [57]. Nanocomposite materials, such as those enhanced by
oxides and carbides, wear-resistant spray coatings, and nanoalloys of aluminum, nickel,
magnesium, and copper, have all been made using this technique. Carbon nanoparticles
that have been ball-milled are a special kind of nanomaterial that has applications in
environmental remediation, energy storage, and energy conversion [2]. To produce nanos-
tructured materials, such as nanofibers, from a variety of materials, most notably polymers,
electrospinning is a commonly used top-down approach. By using two coaxial capillaries
and either two viscous liquids or one viscous liquid as the shell and one non-viscous liquid
as the core, core–shell nanoarchitectures may be constructed in an electric field [58]. The
generation of carbon-based nanomaterials relies heavily on bottom-up approaches, such as
chemical vapor deposition techniques. This technique may be used to create a wide range
of carbon-based nanomaterials by chemically reacting vapor-phase precursors to generate
a thin coating on the surface of the substrate.
Despite these limitations, top-down techniques have several advantages, such as the
ability to produce well-defined, monodisperse nanoparticles with precise control over
size and shape. These techniques are also scalable and can produce large quantities of
nanoparticles. Recent research has focused on improving the efficiency of top-down
techniques and reducing their environmental impact, making them more sustainable for
industrial-scale production [59]. Top-down and bottom-up methods of creating graphene
have both recently been developed. Bottom-up manufacturing converts carbon precursors
including carbon-bearing gases, aromatic hydrocarbons, and polymers into graphene
by processes like chemical vapor deposition (CVD), laser and heat pyrolysis, epitaxial
growth, and direct organic synthesis. These processes are challenging because they often
need sophisticated equipment and elaborate surroundings. Graphite may be converted
to graphene via a variety of top-down methods, including chemical oxidation–reduction,
liquid-phase exfoliation (LPE), electrochemical exfoliation, solid-phase exfoliation, and
arc discharge.
It is not unexpected that the majority of commercially available graphene is made
using top-down methods due to its ease of usage and reduced production costs. However,
because of its high production cost, graphene is not yet widely produced across the world.
Successful commercialization and industrial adoption of graphene, therefore, remain criti-
cally dependent on the development of novel methodologies and improvements in existing
top-down procedures. The remarkable acceleration of graphene preparation progress over
the past several years is emphasized in Figure 2. This has allowed for the commercial
production of various types of graphene in metric ton quantities.
 ments in existing top-down procedures. The remarkable acceleration of graphene prep-
aration progress over the past several years is emphasized in Figure 2. This has allowed
for the commercial production of various types of graphene in metric ton quantities.

Sustainability 2023, 15, 10891 8 of 52

Figure 2. Timeline of main events in the research and development of graphene preparation, begin-
ning with the isolation of graphene in 2004. Reprinted with permission from [59]. Copyright year,
Elsevier, 15 April 2023. License Number 5530201217040.
Figure 2. Timeline of main events in the research and development of graphene preparation, be-
Table
ginning 3 provides
with a comprehensive
the isolation of graphene in comparison of different
2004. Reprinted classesfrom
with permission of nanomaterials,
[59]. Copyright
highlighting their relevant properties and performance
year, Elsevier, 15 April 2023. License Number 5530201217040. characteristics.

Comparative
Table 3.Table Analysis
3 provides of Nanomaterial
a comprehensive Classes: Properties
comparison and Performance
of different Characteristics.
classes of nanomaterials,
highlighting their relevant properties and performance characteristics.
Properties/Performance Carbon-Based Metal-Based Metal Oxide Semiconductor Composite
Characteristics Nanomaterials Nanomaterials Nanomaterials Nanomaterials Nanomaterials
Table 3. Comparative Analysis of Nanomaterial Classes: Properties and Performance Characteris-
High electrical conductivity ✓tics.
Large surface area
Proper- ✓ ✓
Carbon-Based Metal-Based Na- Metal Oxide Na- Semiconductor Composite Nano-
ties/Performance
Excellent mechanical
✓
Nanomaterials nomaterials nomaterials Nanomaterials materials
strength
Characteristics
High
Unique electrical
catalytic properties ✓
✓
conductivity
High surface-to-volume
✓
ratios surface area ✓
Large ✓
Excellent mechan- ✓ ✓
Semiconducting behavior✓
ical strength
Diverse functionalities
Unique catalytic ✓
✓
Size-dependent optical and
properties ✓
electronic properties
Enhanced conductivity ✓
Tunable bandgap ✓
Efficient charge separation ✓
Improved photocatalytic
✓
activity
High electrocatalytic activity ✓
Fast charge transport ✓
High stability ✓
Efficient light absorption ✓
Mechanical strength ✓

Note: ( ✓ ): The sign refers to a specific characteristic that indicates the desired function of nanomaterial.

To create nanostructured materials, the hydrothermal process is one of the most well-
known and commonly utilized techniques. The hydrothermal method involves carrying
out a heterogeneous reaction in an aqueous medium at high pressure and temperature close
to the critical point in a hermetically sealed tank, resulting in nanostructured materials.
The solvothermal strategy is functionally equivalent to the hydrothermal one. The only
 Sustainability 2023, 15, 10891 9 of 52

difference is that it is performed in an organic solvent rather than water [60]. Closed systems
are typically utilized for hydrothermal and solvothermal processes. The sol–gel process
is a common wet-chemical strategy for fabricating nanomaterials [61]. This method is
employed to fabricate a wide range of superior metal-oxide-based nanomaterials. Because
the liquid precursor is first transformed to a sol before the metal oxide nanoparticles are
synthesized, this procedure is referred to as the sol–gel technique.
Morphology control is a promising and successful technique for changing surface
atomic active sites and thereby increasing intrinsic electrocatalytic activity and selectivity.
A change in morphology might result in the appearance of new physical and chemical
characteristics in the same material [62]. Because of the varied atom distribution, the
form of the nanomaterial might influence the electroanalytical properties. The intrinsic
morphology, crystal morphology, and aspect ratio of 1D transition metal oxides strongly
influence their electrochemical performance. Studies aimed at optimizing the electrochem-
ical performance of supercapacitors by controlling the aspect ratio and morphologies of
1D nanomaterials are being conducted on transition metal oxides used in supercapaci-
tor electrodes [63]. Mao et al. [64] manufactured core–shell CuCo2 S4 /CoMoO4 nanorods
by a hydrothermal and calcination process. Core–shell-structured CuCo2 S4 /CoMoO4
nanorods were generated on nickel foam using a combination of the hydrothermal tech-
nique and calcination in this work. The hydrothermal method was employed to grow the
CuCo2 S4 /CoMoO4 nanorod heterostructure on the NF substrate (Scheme 2). In Figure 3,
the morphologies of CuCo2 S4 , CoMoO4 , and CuCo2 S4 /CoMoO4 are displayed. CuCo2 S4
exhibits a porous cluster structure with interlaced nanowires, as depicted in Figure 3a,b.
During the hydrothermal reaction, CoMoO4 forms a nanosheet on the NF, as shown in
ability 2023, 15, x FOR PEER REVIEW Figure 3c,d. Meanwhile, Figure 3e–h display the SEM images of CuCo2 S4 /CoMoO 11 of 55 4 , which
demonstrate that it has highly uniform nanorods with a diameter of approximately 100 nm.
Interestingly, this is in stark contrast to the morphologies of CuCo2 S4 and CoMoO4 .

Scheme 2. Illustration
Scheme 2.ofIllustration
the synthesis of synthesis
of the the CuCoof2Sthe
4/CoMoO
CuCo24Snanorod
4 /CoMoO array on the
4 nanorod NF substrate.
array on the NF substrate.
Reprinted with permission
Reprinted withRef. [64] withRef.
permission permission
[64] withlicense 5536080833324.
permission Copyright Elsevier.
license 5536080833324. 25 Elsevier.
Copyright
April 2023. 25 April 2023.

The electrochemical
The electrochemical performance performance of the
of the CuCo CuCo2 S4 /CoMoO
2S4/CoMoO 4 heterostructure
heterostructure is en- is en-
hanced. The CuCo S
hanced. The CuCo2S4 nanorods 2provided4 nanorods
pathways for quick electron transport andtransport
provided pathways for quick electron effi- and
efficiently disseminated CoMoO
ciently disseminated CoMoO4 particles, while particles, while the outer CoMoO
4 the outer CoMoO4 shell hindered shell hindered
4 the inner the
inner CuCo2 S4 nanorods’ expansion during the redox reaction and boosted the composite’s
CuCo2S4 nanorods’ expansion during the redox reaction and boosted the composite’s
stability [64,65].
stability [64,65].
Titania nanostructures with low dimensions (such as 0D, 1D, and 2D structures)
have intriguing properties, including a high surface-to-volume ratio, clearly defined
surfaces in terms of structure and geometry, small curvature radii, and enhanced elec-
trical, thermal, and chemical stability. Electrochemical capacitors, photocatalysis, sensors,
and energy storage devices are just some of the many surface-related and interfacial ap-
plications that might benefit from TiO2 nanostructures because of their unique features
[66]. Incorporating 0D and 2D materials into a composite may be performed in four
 employed to grow the CuCo2S4/CoMoO4 nanorod heterostructure on the NF substrate
(Scheme 2). In Figure 3, the morphologies of CuCo2S4, CoMoO4, and CuCo2S4/CoMoO4
are displayed. CuCo2S4 exhibits a porous cluster structure with interlaced nanowires, as
depicted in Figure 3a,b. During the hydrothermal reaction, CoMoO4 forms a nanosheet
on the NF, as shown in Figure 3c,d. Meanwhile, Figure 3e–h display the SEM images of
Sustainability 2023, 15, 10891 CuCo2S4/CoMoO4, which demonstrate that it has highly uniform nanorods with a diam- 10 of 52
eter of approximately 100 nm. Interestingly, this is in stark contrast to the morphologies
of CuCo2S4 and CoMoO4.

Figure
Figure3.3.SEM
SEMimages
images of of
CuCo 2S4 (a,b); CoMoO4 (c,d); and CuCo2S4/CoMoO4 nanorod structures
CuCo 2 S4 (a,b); CoMoO4 (c,d); and CuCo2 S4 /CoMoO4 nanorod structures
(e–h). Reprinted with permission from Ref. [64] with permission license 5536080833324. Copyright
(e–h). Reprinted with
Elsevier. 25 April 2023.
permission from Ref. [64] with permission license 5536080833324. Copyright
Elsevier. 25 April 2023.

Titania nanostructures with low dimensions (such as 0D, 1D, and 2D structures) have
intriguing properties, including a high surface-to-volume ratio, clearly defined surfaces in
terms of structure and geometry, small curvature radii, and enhanced electrical, thermal,
and chemical stability. Electrochemical capacitors, photocatalysis, sensors, and energy
storage devices are just some of the many surface-related and interfacial applications that
might benefit from TiO2 nanostructures because of their unique features [66]. Incorpo-
rating 0D and 2D materials into a composite may be performed in four different ways
(Figure 4a–d): The 0D component is used as decoration for the bottom surface of the 2D
material (Figure 4a). The 0D part is placed around the boundaries of the 2D substance
(Figure 4b). A 2D substance encloses the nanoparticle (Figure 4c) [67]. as Additionally,
the dopants can be incorporated into the 2D material (Figure 4d) if the zero-dimensional
component consists of single atoms. In a composite where the particle is located on the
basal plane (as shown in Figure 4a), the nanoparticle or fullerene must be securely attached
to the two-dimensional material host to maximize catalytic activity, prevent nanoparticle
Sustainability 2023, 15, 10891 11 of 52

ripening, or at the very least reduce the likelihood of the zero-dimensional component
detaching from the composite under practical conditions. By understanding the interaction
processes between the zero-dimensional and two-dimensional components and properly
capping the nanoparticle or treating the two-dimensional material host in advance, we
can better design our materials. Engineering functional groups for the zero-dimensional
component and/or the two-dimensional material that take advantage of one of four types
of interaction (Figure 4e–h) may improve its adherence, including van der Waals attrac-
tion (Figure 4e), hydrogen bonds, electrostatic repulsion, and dipole–dipole interactions
(Figure 4f), as well as p interaction with aromatic molecules (Figure 4g) or a covalent bond
(Figure 4h) [68].
In metal oxide supercapacitors, the charge storage mechanism is generally governed
by faradaic processes (reversible redox reactions) at the electrode surface [69]. Non-faradaic
Sustainability 2023, 15, x FOR PEER REVIEW 12 of 55
supercapacitors, which are dominated by electrostatic charge diffusion and accumulation
at the electrode–electrolyte interface via an electric double-layer capacitor formation, can
be integrated into the metal oxide matrix to significantly improve hybrid supercapacitors’
TiO 2 demonstrates
capacitive performanceelectrochemical double-layer
[69]. In terms capacitance
of electrochemical (non-faradaic)
performance, TiOwith signifi-
2 demonstrates
cantly lower specific
electrochemical capacitance
double-layer values than(non-faradaic)
capacitance standard carbonaceous non-faradaic
with significantly capac-
lower specific
itors. Because
capacitance titaniathan
values is semiconducting, its conductivity
standard carbonaceous is limited,
non-faradaic and the
capacitors. interfacial
Because titania is
states/defects
semiconducting, between the titania isand
its conductivity metaland
limited, electrodes slow down
the interfacial charge transport,
states/defects between the
preventing
titania and themetalelectrodes
electrodesfrom achieving
slow down chargetheir full electrochemical
transport, preventing potential [70]. Thefrom
the electrodes
hydrothermal
achieving their procedure, which is simple
full electrochemical and inexpensive,
potential is widely used
[70]. The hydrothermal to create which
procedure, var- is
ious titania/titanate nanostructures [71]. In particular, the alkali-controlled hydrothermal
simple and inexpensive, is widely used to create various titania/titanate nanostructures [71].
treatment of the
In particular, titania is extremely hydrothermal
alkali-controlled effective in controlling
treatment the surface
of titania shape of tita-
is extremely effective
nia/titanate nanostructures. However, the Schottky barrier, which
in controlling the surface shape of titania/titanate nanostructures. However, the is expressed bySchottky
the
Fermi level mismatch between the semiconducting titania and the metallic
barrier, which is expressed by the Fermi level mismatch between the semiconducting titania electrode, is
typically characterized by the interfacial contact between the nanostructured titania and
and the metallic electrode, is typically characterized by the interfacial contact between the
the metal electrode for electrochemical device applications.
nanostructured titania and the metal electrode for electrochemical device applications.

The
Figure 4.4.The
Figure different
different morphologies
morphologies and and potential
potential interaction
interaction mechanisms
mechanisms for hybrids.
for 0D-2D 0D-2D hybrids.
(a)
Nanoparticles are arranged
(a) Nanoparticles on the
are arranged on basal plane.
the basal A TEM
plane. image
A TEM of CoS
image nanoparticles
of 2CoS decorating
2 nanoparticles a
decorating a
reduced
reducedgraphene
grapheneoxide
oxide(r-GO)
(r-GO)nanosheet
nanosheet [72]. (b)(b)
[72]. Nanoparticles
Nanoparticlesare are
preferentially situated
preferentially alongalong
situated
the nanosheet edge. A TEM image of triangular MoS2 with Au nanoparticles along their edges [73].
the nanosheet edge. A TEM image of triangular MoS2 with Au nanoparticles along their edges [73].
(c) Nanoparticles encapsulated in 2D sheets. A TEM image of a Pt nanoparticle encapsulated in
several graphene layers. Scale bar 2 nm [74]. (d) Single-atom sites within, on top of, or along the
edge of the nanosheet. High-angle annular dark-field (HAADF) scanning-mode transmission elec-
tron microscopy (STEM) image of Pt substitutions in MoS2 [75]. (e) A van der Waals interaction,
such as between graphene and a ligand-free nanoparticle. (f) Electrostatic dipole–dipole interac-
tion, such as between a hydroxyl functional on GO and a citrate ligand on a nanoparticle. (g) An
Sustainability 2023, 15, 10891 12 of 52

(c) Nanoparticles encapsulated in 2D sheets. A TEM image of a Pt nanoparticle encapsulated in

several graphene layers. Scale bar 2 nm [74]. (d) Single-atom sites within, on top of, or along the edge
of the nanosheet. High-angle annular dark-field (HAADF) scanning-mode transmission electron
microscopy (STEM) image of Pt substitutions in MoS2 [75]. (e) A van der Waals interaction, such as
between graphene and a ligand-free nanoparticle. (f) Electrostatic dipole–dipole interaction, such as
between a hydroxyl functional on GO and a citrate ligand on a nanoparticle. (g) An aromatic/p-p
interaction, such as between graphene and a phenylethanethiol-capped nanoparticle. (h) A covalent
bond is typically formed between a functional group on GO and a ligand. Permission from Elsevier,
License Number 5527170984812. 13 April 2023.

The self-sourced Ti surface is directly modified into titania nanostructures in situ and
then used as-is as an electrochemical microelectrode, which is novel [71]. As a result, the
transition between metallic Ti and semiconducting TiO2 is greatly enhanced. The near-
defect-free interfacial feature of the Ti-TiO2 microelectrode has demonstrated outstanding
super-capacitive performance for enhanced charge storage devices, demonstrating the
importance of interfacial states and defects in controlling the charge transport characteristics
of electronic and electrochemical devices.
To create hollow carbon nanocages, scientists use graphene microcrystals as building
blocks to enclose curved carbon nanosheets with sub-micrometer gap space. A large num-
ber of sub-nanochannels (1 nm) or purpose-built nanopores (1–10 nm) connect the inside
and outside of carbon nanocages [76]. This unique carbon nanocage material has a number
of advantages over previously developed nanocarbon materials, including a readily accessi-
ble inner cavity, the coexistence of micropores, mesopores, and macropores, a high specific
surface area, and the ability to be easily doped and modulated. Also, the arch arrangement
of carbon layers in the cage-like carbon nanomaterials’ curved nanosheet structure may sig-
nificantly reduce anisotropy by obstructing interlayer sliding and guaranteeing structural
stability [76]. Designing interfacial composites based on hollow carbon nanocages may be
conducted in two ways: (a) by constructing metal or metal compounds enclosed by hollow
carbon nanocages and (b) by generating hollow carbon nanocages coated with metal or
metal compounds. Furthermore, the electrochemical energy storage capabilities of hollow
interfacial materials may be improved by the compact interfacial effect of carbon nanocages’
metal compounds. Molybdenum phosphide nanoparticles and nitrogen-doped carbon
(MoP-NC) complex hollow nanocages were successfully synthesized by Liu et al. [77]
by combining non-template and annealing techniques with both organic and inorganic
composite precursors. The findings suggest that there is a complementary relationship
between nitrogen-doped carbon and hydrogen production in alkaline electrocatalysis. The
use of hollow nanocages and molybdenum phosphide nanoparticles (metal-carbon) can
further enhance this relationship, resulting in faster hydrogen production. Therefore, these
materials can improve the performance of electrocatalysis for hydrogen production by
optimizing the interaction between nitrogen-doped carbon and the hydrogen production
process [77].

5. Nanotechnology-Based Electrochemical Sensors

The synthesis and characterization of nanomaterials have opened up new opportuni-
ties for the development of cost-effective electrochemical biosensors. These biosensors have
the potential to revolutionize various fields, including healthcare, environmental monitor-
ing, and food safety. Biosensors that detect analytes with high sensitivity and specificity
have been made possible by the use of nanomaterials due to their unique characteristics
and high surface-to-volume ratio.
The use of nanomaterials in biosensors has led to the development of various novel
sensing mechanisms, such as surface-enhanced Raman scattering (SERS), localized surface
plasmon resonance (LSPR), and electrochemical impedance spectroscopy (EIS). These
mechanisms offer several advantages, including improved detection limits, enhanced
selectivity, and reduced analysis time. Moreover, the use of nanomaterials in biosensors has
Sustainability 2023, 15, 10891 13 of 52

enabled the development of portable, low-cost, and disposable devices, which are highly
desirable in resource-limited settings.
Electrochemical sensors are based on enzymes, such as oxidation and reduction en-
zymes, that stimulate chemical reactions that produce or consume electrons. The sensor
consists of three electrodes: the reference electrode or signal, the precipitation, and the re-
serve electrode [78]. The target analyte participates in the reaction on the active electrode’s
surface, and the ions produced generate an electrical potential from that electrode to trigger
a signal. The electron flow rate can be measured in proportion to the analyte concentration
when the voltage is constant, or it can be measured at the zero point (this provides the
logarithmic response). It should be noted that a sensitive charge capacitance is used in the
working voltage or active electrode. Direct electrophoresis of small peptides and proteins
may be made possible by their intrinsic charges used for bio-functionalized ions in the
influencing field of the transistor. The potentiometer is a type of position sensor that works
as an adjustable voltage divider. The sensors are print screens, cabling embedded polymers,
and open circuit sensors that rely on conjugated polymers for immunoassays [79]. These
appliances have only hypersensitive and long-lasting electrodes. The alleles can only be
detected by HPLC, LC/MS, and without preparing a simple model at existing levels. The
signal is generated by electrochemical energy and physical alterations to the conductive
polymer layer due to variations on the sensor surface [80]. These changes are attributed
to ionic force, water pH, and redox reactions as the latter bends the enzyme around the
base. An existing measurement detector estimates the current when a solvent is actively
in contact with a working electrode, which is fixed to a constant tension for a reference
electrode [81].
An electrode solution is used to determine the voltmeters that produce a characteristic
electrode signal, called waveforms, which are then expressed. Electrode current data are
quantified over time using voltmeter and ammeter detectors. Reversible pulse potentials
between high and low values are useful for voltmeter measurements because they provide
the distinctive current response for inverse interactions. In order to measure the voltage
flowing through the electrode during its lifetime, the signal must be pulsed with extra
voltage at short intervals between high and low values. An oxidized or reduced product can
be created on the electrode surface, resulting in a positive or negative current by applying
pulses of potential voltage between high and low voltage levels, respectively.
Recent technological developments have made it easier to design electrodes that are
sensitive to certain analytes while still being cost-effective, dependable, and selective.
Electrodes with screen printing, integrated nanomaterials, and EC immunoassays are three
examples of how these advancements might be used together to create electrical sensor
(EC) technology. These new technologies have led to the creation of heterogeneous systems
that combine their best features [81]. Chemical exposure analysis has several potential
uses in modern environmental and biological monitoring thanks to the development of
low-cost and selective EC sensors. Chemicals, metabolites, proteins, metals, inorganic ions,
organic compounds, and more may all be identified using these methods in a wide range
of biological matrices [82].
Nanomaterials provide several advanced analysis technologies, including more sensi-
tive, selective, and biomonitoring electrochemical sensors.
Carbon nanomaterials are favored in enhancing the performance of electrochemical
sensing [83]. Carbon nanomaterials can increase electrode surface area, accelerate electron
transfer, and act as catalysts, enhancing electrochemical processes such as detection, adsorp-
tion, and removal. Several carbon nanomaterials, including graphene, mesoporous carbon,
carbon nanotubes, and carbon dots, have demonstrated strong adsorption and detection
capacities (Figure 5). Electrochemical methods using anodic stripping voltammetry with
modified carbon electrodes are commonly used for detecting heavy metals due to the
excellent electrocatalytic properties of carbon and its derivatives. Surface modification of
the working electrode (GCE) increases the sensitivity of metal electrode detection. Electro-
 Sustainability 2023, 15, 10891 14 of 52

Sustainability 2023, 15, x FOR PEER REVIEW 15 of 55

chemical sensors can be made much more effective by first coating the working electrode
with a layer of active electrocatalytic species.

Differenttypes
Figure5.5.Different
Figure types of carbon nanostructures
nanostructuresininzero,
zero,one,
one,and two
and dimensions.
two dimensions.Reprinted with
Reprinted
permission
with fromfrom
permission Ref.Ref.
[84][84]
withwith
permission license
permission 5537630623042.
license Copyright
5537630623042. Elsevier.
Copyright 29 April
Elsevier. 2023.
29 April
2023.
Electrochemical platforms with enhanced electrical conductivity and sensitivity can
be designed and fabricated
Electrochemical platformsusing CNPs dueelectrical
with enhanced to their conductivity
excellent characteristics.
and sensitivity Incan
this
context, establishing a stable modifier coating on the electrode’s surface is
be designed and fabricated using CNPs due to their excellent characteristics. In this con-crucial. Electrode
surface
text, modification
establishing using
a stable CNPs coating
modifier has beenonaccomplished
the electrode’s in surface
differentisways,
crucial.asElectrode
illustrated
schematically
surface in Figure
modification using6.CNPs
Drop-casting
has beenmodification
accomplished is in
a quick andways,
different simple as approach
illustratedto
creating customized
schematically in Figureelectrodes. When a CNP
6. Drop-casting suspension
modification is aisquick
droppedandover the surface
simple approach of bare
to
electrodes, stable films are generated due to the CNPs’ strong dispersibility
creating customized electrodes. When a CNP suspension is dropped over the surface of in water. This
method
bare is practical
electrodes, stablefor carbonaceous
films electrodes
are generated due to like glassy strong
the CNPs’ carbon dispersibility
electrodes (GCE) due to
in water.
the strong contacts between the electrode surface and CNPs or CNP composites
This method is practical for carbonaceous electrodes like glassy carbon electrodes (GCE) with other
carbon nanomaterials (such CNTs and graphene). However, the modifier
due to the strong contacts between the electrode surface and CNPs or CNP composites film’s stability
with other carbon nanomaterials (such CNTs and graphene). However, the modifier
film’s stability might be a problem for non-carbonaceous electrodes. Carbon paste elec-
Sustainability 2023, 15, x FOR PEER REVIEW 16 of 55
Sustainability 2023, 15, 10891 15 of 52

trodes (CPEs) are fabricated using a similar process, except that a combination of carbon
might be a problem for non-carbonaceous electrodes. Carbon paste electrodes (CPEs) are
(microparticles) powder and an appropriate binder (such as Nujol or ionic liquids (ILs))
fabricated using a similar process, except that a combination of carbon (microparticles)
is used to create an electrode. Carbon nanoparticle (CNP) composites can be used as
powder and an appropriate binder (such as Nujol or ionic liquids (ILs)) is used to create an
modified carbon paste electrodes for electrochemical platforms. CNPs have excellent
electrode. Carbon nanoparticle (CNP) composites can be used as modified carbon paste
characteristics for surface functionalization, and their composites with hydroquinone,
electrodes for electrochemical platforms. CNPs have excellent characteristics for surface
sodium dodecyl sulfate (SDS), and halloysite nanoclay (HNC) have been proposed for
functionalization, and their composites with hydroquinone, sodium dodecyl sulfate (SDS),
modified electrodes due to their low background current, large potential window, low
and halloysite nanoclay (HNC) have been proposed for modified electrodes due to their low
cost, ease of current,
background preparation, electrodewindow,
large potential surface low
renewal, andofpotential
cost, ease for miniaturization.
preparation, electrode surface
The layer-by-layer
renewal, (LBL)forassembly
and potential approachThe
miniaturization. haslayer-by-layer
been used to(LBL)
manufacture
assemblymultilayer
approach
uniform
has beenthin
usedfilms with regulated
to manufacture architecture
multilayer and thin
uniform composition,
films withwhich can address
regulated sta-
architecture
bility difficulties related to the drop coating method. The LBL method involves
and composition, which can address stability difficulties related to the drop coating method. alternat-
ing
Theadsorption
LBL method of involves
polyelectrolytes and/or
alternating nanomaterials
adsorption onto a charged
of polyelectrolytes substrate
and/or with an
nanomaterials
opposing charge.
onto a charged substrate with an opposing charge.
The
Theelectrode
electrode surface
surface modification with the
modification with the LBL
LBLtechnique
techniquehashasbeen
beenused
usedtotoassemble
assem-
ble negatively charged phenyl sulfonated carbon nanoparticles onto positively
negatively charged phenyl sulfonated carbon nanoparticles onto positively charged sub- charged
substrates,
strates, suchsuch as chitosan,
as chitosan, poly (diallyldimethylammonium
poly (diallyldimethylammonium chloride)
chloride) (PDDAC), (PDDAC), im-
imidazolium
idazolium salt ionic liquid (IL) precursor, and sol–gel-processed functionalized
salt ionic liquid (IL) precursor, and sol–gel-processed functionalized silicate. silicate.

6. Schematic
Figure 6.
Figure Schematic representation
representationofofvarious methods
various methodsfor for
electrode surface
electrode modification
surface usingusing
modification CNPs.
CNPs. Reprinted
Reprinted with permission
with permission from
from Ref. Ref.
[84] [84]
with with permission
permission license 5537630623042.
license 5537630623042. Copyright
Copyright Elsevier.
Elsevier.
28 April 28 April 2023.
2023.
Sustainability 2023, 15, x FOR PEER REVIEW 17 of 55
Sustainability 2023, 15, 10891 16 of 52

The modification of carbon nanoparticle (CNP) electrodes with organic compounds

The modification of carbon nanoparticle (CNP) electrodes with organic compounds
significantly improves their electrochemical sensitivity to both organic and inorganic
significantly improves their electrochemical sensitivity to both organic and inorganic
analytes. Electrochemical polymerization of conducting polymers (CPs) is an effective
analytes. Electrochemical polymerization of conducting polymers (CPs) is an effective
method for creating modified electrodes with excellent electrical conductivity. One such
method for creating modified electrodes with excellent electrical conductivity. One such
method involves the electro-polymerization of CNPs/pyrrole aqueous solution on the
method involves the electro-polymerization of CNPs/pyrrole aqueous solution on the
surface of a glassy carbon electrode (GCE) by cycling the voltage between 0 and 0.8 V.
surface of a glassy carbon electrode (GCE) by cycling the voltage between 0 and 0.8 V. This
This process creates a sensing platform where the synergistic impact of polypyrrole (PPy)
process creates a sensing platform where the synergistic impact of polypyrrole (PPy) and
and CNPs enhances electrochemical performance beyond the sum of their separate sur-
CNPs enhances electrochemical performance beyond the sum of their separate surface
face area effects.
area effects.
CNPs are responsible for high electrochemical activity because they can act as liq-
CNPs are responsible for high electrochemical activity because they can act as liquid–
uid–liquid interface stabilizers and interfacial conduits for electrons. Another method for
liquid interface stabilizers and interfacial conduits for electrons. Another method for the
the formation
formation of CNPs
of CNPs on surface
on the the surface of electrodes
of electrodes is through
is through the cyclic
the cyclic voltammetry
voltammetry (CV)
(CV) technique, which was used to achieve surface nanocrystallization of carbonaceous
technique, which was used to achieve surface nanocrystallization of carbonaceous surfaces
surfaces
like like
glassy glassy
carbon carbon electrodes
electrodes in anhydrous
in anhydrous N, N-dimethylformamide
N, N-dimethylformamide (DMF)
(DMF) containing
containing tetra-n-butylammonium
tetra-n-butylammonium bromide
bromide (TBAB) [85].(TBAB) [85].inAs
As shown shown
Figure in situ
7, in Figure 7, in situ
synthesis of
synthesis of CNPs on the surface of GCE occurred due to redox reactions
CNPs on the surface of GCE occurred due to redox reactions and the insertion of Bu and the inser-
+
4N
tion of Bu 4N+ ions and electrolytes into the surface layer of the GC electrode during con-
ions and electrolytes into the surface layer of the GC electrode during continuous cathodic
tinuous
and cathodic
anodic and anodic scanning.
scanning.

Figure Mechanismofofinin
7. Mechanism
Figure 7. situ
situ formation
formation of CNPs
of CNPs on surface
on the the surface
of GCofelectrode
GC electrode by surface
by surface nano-
nanocrystallization process
crystallization process usedused for investigation
for investigation of direct
of the the direct electrochemistry
electrochemistry of glucose
of glucose oxidase
oxidase en-
zyme (GOD),
enzyme (GOD), Reprinted
Reprinted with
withpermission
permissionfrom
fromRef.
Ref.[85].
[85].With
With permission
permission license
license 5537631494458.
5537631494458.
Copyright Elsevier.
Copyright Elsevier. 28
28 April
April 2023.
2023.

Biosensors are analytical devices that combine a biological biological component, such as an
enzyme or antibody,
antibody, with a physicochemical transducer to
with a physicochemical transducer to convert
convert a biological
biological response
into a measurable
measurable signal. Electrochemical biosensors,
signal. Electrochemical biosensors, in in particular, have emerged as a
promising tool for healthcare
healthcare applications,
applications, as they can detect
detect biomarkers
biomarkers in bodybody fluids
fluids
such as saliva, interstitial fluid, and sweat.
sweat. By functionalizing carbon nanomaterials with
chemical and biological components,
components, biosensors
biosensors cancan be
be made
made to to work
work at the same scale as
natural biological processes, providing
providing high sensitivity and specificity for the detection of
high sensitivity and specificity
target analytes.
target analytes.
Electrochemical
Electrochemical sensors
sensors are
are used
used in
in the
the medical
medical sector;
sector; for
for instance,
instance, aa glucometer
glucometer
(glucose meter) is used to monitor blood levels of glucose in
(glucose meter) is used to monitor blood levels of glucose in diabetic diabetic patients [86].
patients Modern
[86]. Mod-
electrochemical
ern electrochemicalbiosensors are promising
biosensors toolstools
are promising for the
for healthcare
the healthcare sector, because
sector, theythey
because can
detect
can detect biomarkers in body fluids such as saliva, interstitial fluid, and sweat. Blood is
biomarkers in body fluids such as saliva, interstitial fluid, and sweat. Blood is
the standard biofluid
the standard biofluidforforglucose
glucosemonitoring.
monitoring. ForFor example,
example, the the
bloodblood glucose
glucose levellevel is
is well
well
knownknown
to betoused
be used for warning
for warning patients
patients withwith diabetes.
diabetes. Blood Blood glucose
glucose levelslevels are about
are about 4.9–
4.9–6.9 mM, while patients can have a high (even 40 mM) or a low glucose
6.9 mM, while patients can have a high (even 40 mM) or a low glucose level (2 mM) level (2 mM)[87].
[87].
Sustainability 2023, 15, x FOR PEER REVIEW 18 of 55
Sustainability 2023, 15, 10891 17 of 52

Two types of electrochemical glucose sensors are available, enzyme and

Two types
non-enzyme. of electron
The electrochemical glucose sensors
redox mediators are available,
are organic enzyme and non-enzyme.
and organometallic compounds
The ferrocene
like electron redox mediators
derivatives, are organic
ferrocyanide, and organometallic
organic salt conductingcompounds
agents, andlike ferrocene
quinones. In
derivatives,
contrast, the ferrocyanide,
electrochemical organic salt conducting
properties of glucose agents,
sensorsand
stillquinones.
depend onInGOx
contrast, the
proper-
electrochemical
ties, properties
and it has been of glucose sensors
more complicated still depend
to manufacture on GOx
glucose properties,
sensors [87]. and it has
beenThe
more complicated to manufacture glucose sensors [87].
schematic and operational mechanisms of glucose detection utilizing single
The schematic
nanomaterial and operational
and nanocomposite mechanisms
sensors of glucose
are depicted detection
in Scheme utilizing single nano-
3 [88].
material and nanocomposite sensors are depicted in Scheme 3 [88].

Scheme 3. Mechanics of sensing glucose using single nanomaterial and nanocomposite glucose
Scheme 3. Mechanics of sensing glucose using single nanomaterial and nanocomposite glucose
biosensors. Reprinted with permission from Ref. [88], with permission license 5537761217387.
biosensors. Reprinted with permission from Ref. [88], with permission license 5537761217387. Copy-
Copyright Elsevier 28 April 2023.
right Elsevier 28 April 2023.
The
The third
third generation
generation ofof glucose
glucose sensors
sensors has
has lower
lower detection
detection features
features and
and aa smaller
smaller
linear
linear range compared to the first- and second-generation sensors. Non-enzymaticglu-
range compared to the first- and second-generation sensors. Non-enzymatic glu-
cose
cose sensors
sensors are
are based
based onon direct
direct glucose
glucose oxidation
oxidation on
on the
the electrode
electrode surface
surface and
and can
can use
use
methods
methods such
such asas potentiometry
potentiometry and and amperometry
amperometryto to measure
measure thethe electrode’s
electrode’s potential.
potential.
Certain
Certain metals
metals such
such as
as Pt,
Pt, Au,
Au, Cu,
Cu, Ni,
Ni, and
and Co,
Co, metal oxides like
metal oxides like CuO
CuO andand CO
CO33O
O44,, and
and
carbon materials are
carbon materials arepromising
promisingcandidates
candidatesforfor non-enzymatic
non-enzymatic glucose
glucose sensors
sensors due due to
to their
their electrocatalytic
electrocatalytic activity.
activity. An glucose
An ideal ideal glucose
sensorsensor
shouldshould be selective
be selective for glucose
for glucose and haveanda
sensitivity of more than 1 µA/mMcm2 . Additionally, the sensor should remain stable for at
least 6 months during application.
Sustainability 2023, 15, 10891 18 of 52

Bare carbon electrodes have inadequate sensitivity and an excessive level of electro-
chemical insulin detection. To improve electrode sensitivity, various types of nanoparticles
such as SiO2 NPs, NiONPs, SiCNPs, CNTs, RuOCNTs, Ni (OH)2 , and GO have been used for
electrode surface modification. The electrocatalytic activity towards insulin has been found
to increase when nanoparticles are modified with metal and graphene oxide. Researchers
have used a chemical method and polyaniline conductance polymer as a support holder
to develop a flexible glucose sensor that can be synthesized and deposited into the cotton
material substrate using nickel phosphide (NiP) and copper oxide (CuO) nanoparticles [89].
Scientific studies can use additional electronic measurements for glucose detection
besides resistance- and conductance-based methods. In the existence of glucose, the
ConA dextran displacement, immobilized with gold-coated nanostructures on an electrode,
changes capacity throughout the electrode. Potentiometrically, ion-selective electrodes can
measure free silver ions (Ag+ ), which in GOx-generated hydrogen peroxide are released
from silver nanoparticles. After glucose oxidation, it can be detected in nanotubes that
function on palladium, although it is several orders of magnitude below physiological
blood glucose with a linear range of detection [90].
To improve the sensitivity of electrochemical flavonoid sensors, modified materials
such as carbon nanomaterials, metal nana-particles, and the liquid combination of these
materials were employed [91]. The sensing elements could deliver more active sites, in-
crease the active electrical surface area, and improve mass transport rates and the speed
of electron transfer rates. A new electrochemical platform based on ionic nanocomposite
nanoparticles CoFe2 O for the analysis showed an excellent result because the ionic liquids
have high conductivity and quick mobilization The electrochemical flavonoid biosensors
have attracted attention because of their outstanding electric conductance, biocompatibility,
and significant stability. Electrochemical sensor construction with carbon-based nanomate-
rials has substantial properties, such as high chemical stability, large thermal and electrical
conductivity, and a high surface-to-volume ratio [92]. The carbon set as C6-C3-C6 is derived
from 2-phenyl chromone as the core of the flavonoid compounds.
The natural flavonoid compound mother’s core has hydroxyl, methoxy, oxygen hy-
drocarbon, isoprene oxygen, and other substitutes. Because of the location and difference
between substituents, flavonoids are divided into six subunits of isoflavone, flavonols, and
anthocyanin. The flavonoid structure has a powerful linkage to its redox characteristics [93].
Nanomaterials are significant to the sensor for the functionality of biological systems,
subject to fluctuating conditions. Nanomaterials can be developed to adjust the desired
electrocatalytic activity and improve the sensor’s stability. Non-enzymatic glucose sensors
have reported materials based on copper oxide, tin oxide, or titanium dioxide [94].
Table 4 shows some sensors based on nanomaterials, such as CNTs, and their methods
of manufacturing are chemical vapor deposition, arc discharge, laser ablation, and gas-
phase catalytic growth [95]. It also shows polymer nanowires with their methods [96],
graphene nanostructures [97], metallic nanowires [98], and silicon (Si) nanowires [99].
Avoiding drift and fouling, developing reproducible calibration methods, applying
preconcentration and separation methods to achieve a proper analyte concentration that
avoids saturation, and integrating the nanosensor with other elements of a sensor package
in a reliable manufacturable manner are all challenges for nanosensors [100]. Because
nanosensors are a new technology, there are numerous unsolved problems with nanotoxi-
cology, which restricts their usage in biological systems for the time being [100].
Table 5 provides a summary of the most common types of nanomaterials used in
electrochemical biosensors. Carbon nanotubes are highlighted for their high surface area,
good electrical conductivity, and excellent mechanical properties. These properties make
them a popular choice for detecting biomolecules such as glucose, cholesterol, and DNA.
Graphene is also used in biosensors to detect biomolecules such as glucose, dopamine,
and DNA. Metal nanoparticles are then described for their high surface area and excellent
catalytic activity. This property makes them useful in the detection of biomolecules such as
glucose, cholesterol, and DNA. Quantum dots are highlighted for their unique optical and
Sustainability 2023, 15, 10891 19 of 52

electronic properties. They are used in biosensors to detect biomolecules such as proteins
and DNA. By functionalizing these nanomaterials with chemical and biological components,
biosensors can be made to work at the same scale as natural biological processes, providing
high sensitivity and specificity for the detection of target analytes.

Table 4. Nanosensors and methods of manufacture with one-dimensional materials.

Nanostructure Method of Manufacture References

Chemical vapor deposition
Arc discharge
Carbon nanotubes [95]
Laser ablation
Gas-phase catalytic growth
Electrochemical deposition
Polymer nanowires Template filling [96]
Reactive ion etching
Exfoliation
Graphene nanostructures Chemical vapor deposition [97]
Epitaxial growth
Template-assisted electrodeposition
Electrochemical deposition
Metallic nanowires [98]
Electroless deposition
4- Template filling
Reactive ion etching
Si nanowires [99]
Photolithography

Table 5. A summary of the nanomaterials commonly used in electrochemical biosensors.

Nanomaterials Properties Application References

High surface area, good electrical conductivity,
and excellent mechanical properties
The development of (bio)sensors capable of
tackling future biosensing challenges in clinical
Detection of glucose,
diagnostics, environmental monitoring, and
Carbon nanotubes (CNTs) cholesterol, and DNA [101]
security control represents a very good
alternative when the special properties of CNTs
are combined with the potent biomolecule
recognition properties and the known benefits of
the electrochemical techniques.
With high sensitivities, broad linear detection
ranges, low detection limits, and long-term Detection of glucose,
Graphene (GR) [102]
stabilities, GR-based biosensors displayed dopamine, and DNA
exceptional performance.
Metal Detection of glucose,
High surface area and excellent catalytic activity [103]
nanoparticles cholesterol, and DNA
Detection of biomolecules
Quantum dots Unique optical and electronic properties [104]
such as proteins and DNA
Detection of glucose,
Metal oxide nanoparticles High surface area and excellent catalytic activity [105]
cholesterol, and DNA

6. Nanostructured Materials for Enhanced Electrochemical Performance in Energy

Storage Devices
Providing robust electrochemical energy conversion and storage systems is one of
our society’s most difficult issues [103,104,106,107]. Because of their nanoscale size impact,
nanomaterials have numerous attractive features for electrochemical energy storage de-
vices that are considerably different from bulk or micron-sized material [108]. Constrained
Sustainability 2023, 15, 10891 20 of 52

dimensions, in particular, play crucial roles in regulating the attributes of nanomaterials,

including ion transport kinetics, strain/stress magnitude, and active material consump-
tion. Because they can sustain electron transport along the longitudinal plane and have a
confinement effect throughout the diameter, nanowires, as one of the characteristic one-
dimensional nanomaterials, offer significant potential for realizing a range of applications
in the disciplines of energy storage. Using renewable energy and avoiding conventional
fossil-fuel-related environmental issues has become critical for achieving a globally sus-
tainable energy future. Electrochemical conversion and storage methods for “clean energy”
(e.g., fuel cells, electrolyzers, photo-electrolyzers, metal–air batteries, metal-ion batteries,
and supercapacitors) have played critical roles in this regard [109]. To rival existing fossil-
fuel-based energy supply systems, the performance of renewable energy devices must
be greatly increased. Electrochemical energy conversion and storage typically involve
many intricate chemical reactions and physical interactions at the surface and inside of
electrodes/electrolytes, and the kinetics and transport behaviors of different carriers (e.g.,
electrons, holes, ions, molecules) are closely associated with the electrode materials and
electrode structures [110].
To qualify nanostructures as excellent electrodes for energy conversion and storage
that meet industry standards for device applications, it is essential to achieve well-defined
nanostructures with accurately controllable geometries of four key structural parameters:
size, structure, hetero-architectures through combining different nano-units, and spatial
arrangement [111].
Non-rechargeable primary batteries are essential in various applications, including
wristwatches, remote controls, and electronic keys, as they store energy for a long time, up
to ten years, and self-discharge less than rechargeable batteries [112].
Several types of batteries have been marketed for practical electrochemical appli-
cations [113]. The first portable, non-spill battery was the zinc dioxide and manganese
dry cell, which made light bulbs and other devices more convenient. However, mercury
batteries of zinc and mercury oxide, which had a higher energy level, were phased out due
to potential contamination and widespread mercury from discarded batteries. Lead–acid
batteries were the first practical rechargeable batteries that could be recharged from an
external source, and their reversible electrochemical reaction allows for the exchange of
electrical and chemical energy. They contain sulfuric acid and water, as well as lead plates,
with the most commonly used blending being 30% acid. However, if the acid remains
unchanged, it can crystallize inside the battery’s lead plates and render it useless. The
average lifespan of these batteries is around three years [114]. They are widely used in cars,
but their electrolytes of water limit the maximum voltage for each cell, and freezing water
can limit their performance in low temperatures [115]. In comparison, lithium batteries
do not use water in their elements. Rechargeable lithium-ion batteries are an essential
factor in many mobile devices. Experimental flow batteries provide a wider option to
regenerate reactants from external tanks [116]. Fuel cells have much greater efficiency than
any combustion process and can convert the chemical energy of hydrocarbon gases into
electric power. They are used to power spacecraft and for public energy grid storage [117].
A flow battery system generates energy using an electrochemical cell and electrically
active solutions, typically mineral salts [118]. This non-metallic material with electric
activity provides large-scale energy storage, which is crucial for utilizing renewable and
intermittent energy sources like solar and wind energy, which can account for over 20%
of the total energy capacity when paired with storage systems for electrical power. These
applications are used in electrical grids and remote generating stations that require inex-
pensive and flexible storage systems [119]. There are options for using water pumping
from a reservoir to high elevations as a power source, but these can be expensive and lim-
ited to specific geographic locations, such as conventional batteries and superconducting
electromagnetic storage [120]. Flow batteries, on the other hand, require two active and
dissolved components—compounds that can participate in the electrochemical reaction
that occurs at the electrode [115]. In the electrochemical cell, chemical energy is transformed
 of the total energy capacity when paired with storage systems for electrical power. These
applications are used in electrical grids and remote generating stations that require in-
expensive and flexible storage systems [119]. There are options for using water pumping
from a reservoir to high elevations as a power source, but these can be expensive and
limited to specific geographic locations, such as conventional batteries and supercon-
Sustainability 2023, 15, 10891 ducting electromagnetic storage [120]. Flow batteries, on the other hand, require two 21 of ac-
52
tive and dissolved components—compounds that can participate in the electrochemical
reaction that occurs at the electrode [115]. In the electrochemical cell, chemical energy is
transformed
into into electrical
electrical energy and viceenergy andanvice
versa via ionicversa via an membrane.
conducting ionic conducting membrane.
Electrically active
Electricallyare
substances active substances
pumped throughare
thepumped
cell intothrough the kept
a fluid and cell into a fluid tanks
in separate and kept in sepa-
outside the
rateas
cell, tanks outside
opposed the cell, as opposed
to conventional to conventional
electroactive electroactive
materials (Figure materials
8). This (Figurefor
design allows 8).
This design
optimum allows for
separation optimum
of the energyseparation of the energy
stored, depending on thestored,
size ofdepending on the size
the electrochemical of
cell
the
or theelectrochemical cell or the cell group [121].
cell group [121].

Figure8.8.Illustration
Figure Illustrationof
ofFlow
FlowBattery.
Battery.Adapted
Adapted from
from [122].
[122]. with
with permission
permission license
license 5583830752137,
5583830752137,
Copyright Elsevier 7 July 2023.
Copyright Elsevier 7 July 2023.

Nanostructuredmaterials
Nanostructured materialsare areof
ofinterest
interestforforelectrochemical
electrochemicalenergy energyconversion
conversionand and
storagedevices
storage devicesdueduetoto their
their large
large surface
surface area,
area, newnewsizesize effects,
effects, and increased
and increased kinetics
kinetics and
and other properties. Two types of nanoscale size effects have been discovered
other properties. Two types of nanoscale size effects have been discovered in these materials: in these
materials:
“trivial size “trivial
effects,”size
whicheffects,” whichonrely
rely solely thesolely
increasedon the increased surface-to-volume
surface-to-volume ratio, and “truera-
tio, and “true size effects,” which also require changes in local material
size effects,” which also require changes in local material characteristics [123]. The field of characteristics
[123]. The field
“nanoionics” has of “nanoionics”
established has established
a significant place in athis
significant place in this
area, comparable area, compara-
to nanoelectronics
ble
in to nanoelectronics
semiconductor in semiconductor
physics, and its advancementphysics,may and lead
its advancement may lead of
to future generations to future
clean
generations
energy of clean energy devices.
devices.
Tosignificantly
To significantlyimprove
improvethe theelectrochemical
electrochemicalefficiency
efficiencyof ofelectrode
electrodematerials,
materials,their
their
dimensionscan
dimensions canbebedecreased
decreasedto toaananoscale
nanoscalelevellevelto tobenefit
benefitfrom fromthe
thenanoparticle
nanoparticleeffect,
effect,
whichresults
which results in
in a higher surface
surface area
area and
andshorter
shorterion ionspreading
spreadingtime time[124]. Various
[124]. Variousna-
noparticle materials
nanoparticle materialswith
withimproved
improvedelectrochemical
electrochemical performance
performance have been been fabricated,
fabricated,
although controlling
although controlling the
the size,
size, especially
especially when
when itit isis less
less than
than 10 10nm,
nm, can
canbebeaadifficult
difficult
problem
problem[125].
[125].
Some studies have developed the nano-molecule flow battery, which can store electric and
hydrogen gas for supplying hybrid energy storage systems. This battery adopts a nano-battery
design, “hybrid hydrogen energy flow,” to store energy and release on-demand electricity or
hydrogen gas for use as fuel [126]. When a condensed liquid containing nanoparticles is used,
the volume of stored energy is increased by around ten times. This system allows for flexible
operation of the equipment, requiring either fuel or electricity [125].
Rechargeable batteries must meet several main parameters to be useful in hybrid
electric vehicles and electric vehicles, including cost, higher energy capacity, longer cycle
life, safety, and environmental viability [125].
Nanometer-sized electrode materials may improve electroactivity toward Li insertion
and high rate capability, enabling high power performance [127]. The high rate capacity
results directly from the transport benefits of tiny particle sizes, such as shorter transport
Sustainability 2023, 15, 10891 22 of 52

lengths for both e- and Li+ transport and a greater electrode/electrolyte contact area due to
the higher surface area [128]. The former allows for complete Li diffusion in a short storage
period, i.e., at high charge/discharge rates, while the latter considerably lowers the specific
current density of the active material [128]. In addition to the “conversion” mechanism,
an interfacial Li storage mechanism has recently been proposed to explain the additional
Li+ storage capacity in nanometer-sized transition metal oxides at low potential. Li surface
storage may play a key role in total capacity in nanostructured devices. This technique may
be more energy-efficient for nanometer-sized particles than for bulk insertion.
In recent years, metal oxide nanostructures have been investigated for various appli-
cations such as sensors, energy-efficient coatings, and semiconductor devices [129]. These
nanowires are covered with a gold–palladium alloy that functions as an existing conductor.
Manganese oxide is deposited on the alloy surface in the electrochemically active form [130].
The result is a hundred-fold increase in the surface area of the brush-like layer compared
to the copper cable because the broad surface is an essential factor for storing energy. The
nanowire acts as the sheath that covers the copper wire and is the supercapacitor’s first
electrode. Some researchers have investigated environmentally friendly batteries that can
provide cars and mobile phones with the necessary energy, using nanotechnology and
genetically modified viruses. These viruses infect bacteria, do not harm humans and have
been used to build the two charged terminals (poles) of lithium-ion batteries, which have
the same power, capacity, and performance as the latest rechargeable models [131]. As
a result, they operate hybrid energy cars and personal electronic devices. When tested
in laboratories, the new cathode material could be charged and discharged more than a
hundred times without losing any part of its capacity or electrical capacity. This technology
enables lithium-ion batteries to charge in seconds, not hours. This achievement will lead to
smaller, faster-charging batteries for mobile phones and other devices.
The incorporation of nanoscale silicon in lithium-ion batteries can increase their energy
density by up to 10 times due to the high surface area of the silicon nanoparticles, which
can store more lithium ions. Similarly, the use of nanostructured sulfur as the cathode
material in lithium–sulfur batteries has been shown to improve their energy density and
cycle life.
Lithium–sulfur batteries offer three times higher energy density than standard lithium-
ion batteries, thanks to the low atomic weight of lithium and moderate weight of sul-
fur [132]. During discharge, lithium dissolves from the cathode layer and reverses this
process on the anode surface during charging. Lithium–sulfur batteries can be refilled
at a temperature of 60 ◦ C and exhibit good cold–hot discharge characteristics. However,
they face challenges such as limited cycle life (40–50 charge/discharge cycles) and poor
stability at high temperatures [133–135]. Despite these challenges, lithium–sulfur tech-
nology shows promise for use in battery experiments with nanowires. Researchers have
developed a new high-performance lithium battery anode–electrode structure using carbon
and silicone nanomaterials. This material contains potent and durable silicon circuits with
irregular channels that increase molecular mass–lithium battery receptivity [131,132]. The
research has shown stable performance and capacity with graphite cathodes five times
larger than regular lithium batteries. Manufacturers tout it as a simple, cost-effective, safe,
and widespread technology [136]. However, structural problems limit the cycle life and
extraction of lithium at higher volumes. When compared to the more traditional method of
oxidizing and reducing organic molecules in organic synthesis, organic electrophoresis is a
more eco-friendly and reliable option. Electro-oxidation processes have various advantages
over conventional reagent-based reactions [137], including functional tolerance, moderate
conditions, scalability, and sustainability. Careful applications of electrochemical oxidation
to electrophoresis have been made [138]. Sustainable methods and tactics including oxida-
tion mediators for direct re-operation of anabolic and inactive C-H in massive industrial
contexts have also been created by researchers [139]. Some researchers have conducted
electrochemical anodic oxidation using the galvanizing method without catalysts and
oxidation. Recent studies have also focused on anode/cathode electrodes modified with
 Sustainability 2023, 15, 10891 23 of 52

electrolytic oxidation/reduction nanomaterials [140]. Using electrodes can expand the

electrode synthesis range and improve electrode synthesis efficiency. Therefore, developing
modified electrodes with special electrical synthesis functions is essential [141].
Nanotechnology provides new opportunities for designing, synthesizing, and modify-
ing cathode materials to overcome capacity limitations and significantly improve battery
performance. The nano-template approach allows the creation of nanostructure materials
with complicated morphology in a single step while maintaining high control over size and
form, which would otherwise be challenging to achieve [142]. Solvothermal/hydrothermal
and coprecipitation synthesis techniques are widely used, easy, and low-cost approaches
for producing cathode nanostructures with high yield, but they lack control over the final
nanostructure size and form [143]. The nanostructural fabrication of cathode materials
has resulted in improved battery performance due to their enhanced structure and shorter
Li+ diffusion route lengths, allowing for faster Li+ insertion/extraction processes [144].
Advances in nanosynthesis processes have led to precise control over size, form, and
repeatability at low to medium processing costs, and the limitations are quickly closing.
Supercapacitors, on the other hand, rely on the fast charge–discharge of ions at the
electrode–electrolyte interface, making them ideal candidates for nanomaterials. Nanoma-
terials such as graphene, carbon nanotubes, and metal oxides have been used as electrode
materials in supercapacitors to enhance their energy and power densities, as well as their
cycle life [145]. The use of these nanomaterials can increase the specific capacitance of
the electrodes by several orders of magnitude, due to their large surface area and high
conductivity. Supercapacitors can store a lot of energy and charge quickly; their working
voltage is between 1 and 3 V, which is suitable for both organic and aqueous electrolytes.
Batteries have a high energy density so our gadgets may be used all day, but they might
take a long time to charge. Electrochemical capacitors known as supercapacitors are utilized
for quick power supply and recharging (i.e., high power density). Nanomaterials are par-
ticularly well suited for use in supercapacitors because of their high surface area-to-volume
ratio, which provides a large interface area for ion adsorption and desorption. The fast
charge–discharge rate of supercapacitors is dependent on the rapid transfer of ions at the
electrode–electrolyte interface, and nanomaterials with their large surface area and short
diffusion distance are ideal for facilitating this process. Unless basic performance parame-
Sustainability 2023, 15, x FOR PEER REVIEW 25 of 55
ters are carefully considered, the fuzziness between these two electrochemical techniques
might lead to misunderstanding and even inappropriate claims (Figure 9).

Figure
Figure9.9. Comparing
Comparing batteries and supercapacitors.
batteries and supercapacitors.(A,D)
(A,D)The
The different
different mechanisms
mechanisms of capacitive
of capacitive
energy
energy storage are illustrated. Double-layer capacitance develops at electrodes comprising (A) carbon (A)
storage are illustrated. Double-layer capacitance develops at electrodes comprising
carbon particles
particles or (B) carbon.
or (B) porous porous The
carbon. Thelayer
double double layer
shown shown
here ariseshere
fromarises from the of
the adsorption adsorption
negative of
negative ions from the electrolyte on the positively charged electrode. Pseudocapacitive
ions from the electrolyte on the positively charged electrode. Pseudocapacitive mechanisms include
mecha-
nisms include (C) redox pseudocapacitance, as occurs in hydrous RuO2, and (D) intercalation
pseudocapacitance, where Li1 ions are inserted into the host material. (E,H) Electrochemical char-
acteristics distinguish capacitor and battery materials. Cyclic voltammograms distinguish a capac-
itor material where the response to a linear change in potential is a constant current (E), as com-
pared to a battery material, which exhibits faradaic redox peaks (F). Galvanostatic discharge be-
havior (where Q is a charge) for a MnO2 pseudocapacitor is linear for both bulk and nanoscale
material (G) [146,147], a LiCoO2 nanoscale material exhibits a linear response while the bulk mate-
Sustainability 2023, 15, 10891 24 of 52

(C) redox pseudocapacitance, as occurs in hydrous RuO2 , and (D) intercalation pseudocapacitance,
where Li1 ions are inserted into the host material. (E,H) Electrochemical characteristics distinguish
capacitor and battery materials. Cyclic voltammograms distinguish a capacitor material where the
response to a linear change in potential is a constant current (E), as compared to a battery material,
which exhibits faradaic redox peaks (F). Galvanostatic discharge behavior (where Q is a charge)
for a MnO2 pseudocapacitor is linear for both bulk and nanoscale material (G) [146,147], a LiCoO2
nanoscale material exhibits a linear response while the bulk material shows a voltage plateau (H).
Permission from Elsevier, License Number 5526570094637. 12 April 2023.

Table 6 provides an overview of the best-performing materials in various electro-

chemical devices, highlighting their material class, synthesis method, performance pa-
rameters, and applications. These materials play a crucial role in advancing the field
of electrochemistry by offering enhanced performance and enabling the development of
high-performance devices.

Table 6. Best-Performing Materials in Electrochemical Devices.

Material Name Material Class Synthesis Method Performance Parameters Application References
Lithium Cobalt High specific capacity, Lithium-ion
Metal Oxide Solid-state reaction [148,149]
Oxide (LiCoO2 ) good cycling stability batteries
Lithium Iron High energy density, long Lithium-ion
Metal Phosphate Sol–gel method [150]
Phosphate (LiFePO4 ) cycle life batteries
Silicon/Graphene Chemical vapor High specific capacity, Lithium-ion
Composite [151]
Composites deposition (CVD) enhanced stability batteries
Sodium-ion
Hydrothermal Good rate capability, low Sodium-ion
Intercalation Metal Oxide [152]
synthesis cost batteries
Materials
Carbon-based Mechanical High specific capacitance,
Graphene Supercapacitors [153]
Material exfoliation fast charge–discharge rate
Carbon-based Chemical High energy density, long
Activated Carbon Supercapacitors [154]
Material activation cycle life
Conductive Chemical High capacitance, good
Polyaniline Supercapacitors [155]
Polymer oxidation stability
Carbon-based Chemical vapor High power density,
Carbon Nanotubes Supercapacitors [156]
Material deposition (CVD) excellent cycling stability
Polymer
Proton Exchange Polymer High proton conductivity,
Solution casting electrolyte fuel [157]
Membrane (PEM) Electrolyte Low permeability
cells
Polymer
Platinum-based Wet chemical High catalytic activity,
Noble Metal electrolyte fuel [158]
Catalysts synthesis good durability
cells
High ionic conductivity,
Solid Oxide Solid-state Solid oxide fuel
Ceramic stable at high [159]
Electrolyte sintering cells
temperatures
Good oxygen reduction Solid oxide fuel
Perovskite Oxides Metal Oxide Sol–gel method [160]
reaction, thermal stability cells
Metal Oxide Chemical vapor High sensitivity, selective
Metal Oxide Gas sensors [161]
Semiconductors deposition (CVD) detection
Enzyme High specificity, rapid
Enzymes Biocatalyst Biosensors [162]
immobilization response
Nanomaterials (e.g.,
Various synthesis High sensitivity, versatile
Carbon nanotubes, Various Biosensors [163]
methods applications
Graphene)
Sustainability 2023, 15, 10891 25 of 52

In the realm of lithium-ion batteries, Lithium Cobalt Oxide (LiCoO2 ) demonstrates

high specific capacity and good cycling stability, while Lithium Iron Phosphate (LiFePO4 )
excels in energy density and cycle life. Silicon/graphene composites exhibit a high specific
capacity and enhanced stability. These materials have found significant applications in
lithium-ion batteries due to their favorable electrochemical properties.
For alternative energy storage systems, sodium-ion intercalation materials have gained
attention for their good rate capability and low cost, making them promising candidates for
sodium-ion batteries. Additionally, supercapacitors, which offer rapid charge–discharge
capabilities, find valuable materials in graphene, activated carbon, polyaniline, and car-
bon nanotubes.
Polymer electrolyte fuel cells rely on Proton Exchange Membranes (PEMs) with high
proton conductivity and low permeability, while platinum-based Catalysts provide ex-
cellent catalytic activity and durability. In the realm of solid oxide fuel cells, solid oxide
electrolytes with high ionic conductivity and stability at high temperatures, along with
perovskite oxides with good oxygen reduction reaction and thermal stability, contribute to
their efficient operation.
Metal oxide semiconductors find applications in gas sensors due to their high sensi-
tivity and selective detection capabilities. Enzymes, immobilized for enhanced stability,
offer high specificity and rapid response in biosensor applications. Nanomaterials like
carbon nanotubes and graphene exhibit versatile applications and high sensitivity in biosen-
sor technology.
The mentioned materials are synthesized using various methods such as solid-state
reactions, sol–gel methods, chemical vapor deposition (CVD), and solution casting. These
synthesis techniques play a crucial role in tailoring the properties and performance of
the materials.
However, there are still some challenges that need to be addressed in the application
of nanomaterials to energy storage devices. One of the key challenges is the scalability
of the production of nanomaterials, which can be a complex and expensive process. In
addition, the stability and durability of nanomaterials in harsh operating conditions need
to be improved to ensure their long-term stability and performance. Furthermore, the
cost-effectiveness of using nanomaterials in energy storage devices needs to be evaluated
against traditional materials. Despite these challenges, the potential of nanomaterials for
improving the electrochemical performance of energy storage devices makes them an
important research area for the development of advanced energy storage technologies.
There are various factors that contribute to the performance of materials in electro-
chemical devices. Understanding these factors is crucial for optimizing the design and
performance of these devices. The composition of the material plays a critical role in its
electrochemical performance. Different materials exhibit varying chemical and physical
properties, which directly impact their charge storage capacity, energy density, and stability.
For example, in lithium-ion batteries, materials like lithium cobalt oxide (LiCoO2 ) and
lithium iron phosphate (LiFePO4 ) are widely used due to their high specific capacity and
long cycle life.
The method of synthesis greatly affects the structural characteristics and performance
of materials. Various synthesis techniques, such as sol–gel, hydrothermal synthesis, chem-
ical vapor deposition (CVD), and solid-state reactions, result in materials with different
morphologies, crystal structures, and surface areas. These factors influence the electro-
chemical properties, including specific capacitance, energy density, and power density.
The surface area and porosity of materials significantly impact their electrochemical
performance. Materials with high surface areas provide more active sites for electrochemical
reactions, leading to improved charge storage capacity and faster reaction kinetics. The
porosity of materials affects ion diffusion and electrolyte accessibility, influencing the
overall device performance.
The morphology and nanostructure of materials play a vital role in determining their
electrochemical properties. Nanomaterials, with their unique size-dependent properties,
Sustainability 2023, 15, 10891 26 of 52

offer enhanced electrochemical performance due to their large surface-to-volume ratio

and shortened diffusion paths for ions and electrons. Materials with well-defined nanos-
tructures, such as nanowires, nanotubes, and nanoparticles, exhibit improved electrical
conductivity, ion diffusion, and stability.
The interaction between the electrode and electrolyte interface significantly impacts
the performance of electrochemical devices. A well-designed interface with good electrode–
electrolyte compatibility, minimized interfacial resistance, and effective charge transfer
enhances the device’s overall performance. Surface modification techniques and the use
of specific electrolytes can improve the electrode–electrolyte interface and boost device
performance. Understanding these factors and their interplay is essential for tailoring
material properties to meet specific device requirements. By optimizing composition,
synthesis methods, morphology, and interface characteristics, researchers can develop
high-performance materials for electrochemical devices with improved energy storage
capacity, cycling stability, power density, and overall efficiency.

7. New Types of Nanomaterials for Electrochemical Devices

Recent advances in nanotechnology have led to the development of new nanomate-
rials designed specifically for electrochemical devices. Among these emerging classes of
nanomaterials are metal–organic frameworks (MOFs), covalent organic frameworks (COFs),
and MXenes, which hold tremendous promise for the next generation of electrochemical
devices. COFs are a type of crystalline porous material composed of light components
bonded reversibly via covalent bonds in two to three dimensions. These materials have
gained attention due to their unusual characteristics and wide range of potential uses [164].
Previously, it was challenging to create organic polymer networks with distinct pores of
varying sizes, but the advent of reticular chemistry changed this. Reticular chemistry
was initially used to manufacture MOFs, which are also porous materials. MOFs with
very small dimensions, known as micro/nano MOFs, have better conductivity, a shorter
diffusion distance for guest transport, and more accessible surface-active sites compared to
bulk MOFs, without sacrificing any fundamental features of MOFs [165]. The structure of
MOFs can vary depending on the reaction duration, particle size, yield, and morphology,
even when using the same reactive combination (metal source, organic ligand, and sol-
vent). Some approaches of synthesis lend themselves particularly well to implementation
on a massive scale. Conventional solutions, diffusion synthesis, solvothermal synthesis,
microwave synthesis, sonochemical synthesis, electrochemical synthesis, and iono-thermal
synthesis are all employed to create MOFs, as shown in Figure 10. In addition, specific struc-
tural designs of micro/nano MOFs may confer novel functionalities and characteristics on
conventional MOFs [165]. For instance, MOF nanowires oriented in a particular direction
offer advantages for catalytic applications due to improved reactant and electron transport
and the exposure of surface locations. When utilized as electrode materials, ultrathin
metal–organic framework (MOF) nanosheets with high surface area-to-volume ratios may
assure electrolyte penetration and improve the performance of energy storage devices [166].
Micro/nano MOFs have desirable features that make them attractive as electrode materials
and high-performance catalysts for use in energy conversion and storage devices (such as
rechargeable batteries, supercapacitors, and catalysis) [167]. The coordination modulation
method allows for the expansion of MOF frameworks in specific directions by selectively
coordinating modulators on particular crystal planes. This results in the formation of
MOFs with different shapes, such as nanocubes, nanorods, and nanosheets. Researchers
Sikdar et al. discovered that lauric acid can be used as a modulator to control the size
and morphology of Zn-MOF. Without lauric acid, the MOF has an irregular shape due
to metal ions combining with organic ligands. However, with the addition of lauric acid,
the balance between the ligand and modulator coordination changes, leading to growth
along a specific crystal plane and resulting in an anisotropic shape (as shown in Figure 10a).
Varying concentrations of lauric acid enhance the competitive coordination, leading to
 Sustainability 2023, 15, 10891 27 of 52

Sustainability 2023, 15, x FOR PEER REVIEW 29 of 55

the formation of hexagonal nanoparticles, 1D nanorods, and 2D nanosheets (as shown

in Figure 10b–d).

Figure 10. Different methods of MOF synthesis, (a) sonochemical synthesis method, (b) conven-
Figure 10. Different methods of MOF synthesis, (a) sonochemical synthesis method, (b) conventional
tional solution method, (c) diffusion synthesis method, (d) iono-thermal process method, (e) mi-
solution method, (c) diffusion synthesis method, (d) iono-thermal process method, (e) microwave syn-
crowave synthesis method, (f) electrochemical synthesis method, and (g) solvothermal synthesis
thesisReproduced
method. method, (f) electrochemical
from Ref. [168] synthesis method,from
with permission and Elsevier,
(g) solvothermal
April 25,synthesis method.
2023. License Repro-
Num-
ber duced from Ref. [168] with permission from Elsevier, April 25, 2023. License Number 535901430300.
535901430300.

With 4-methoxy benzoic acid (MBA) as a modulator, Cu-MOF nanosheets were pro-
With 4-methoxy benzoic acid (MBA) as a modulator, Cu-MOF nanosheets were
duced by Zhou et al. [169]. The MBA and BDC competed synergistically to generate highly
produced by Zhou et al. [169]. The MBA2+and BDC competed synergistically to generate
distributed CuBDC-MBA-X when a Cu and MBA combination was dripped into a mixture
highly distributed CuBDC-MBA-X when a Cu2+ and MBA combination was dripped into
containing terephthalic acid (BDC). Two-dimensional nanosheets had their homogeneity
a mixture containing terephthalic acid (BDC). Two-dimensional nanosheets had their
altered by MBA. MOFs were created by the synthesis of a network of clusters containing
homogeneity altered by MBA. MOFs were created by the synthesis of a network of clus-
polyatomic inorganic metal atoms connected by polytopic linkers [170]. Wang et al. [171]
ters containing polyatomic inorganic metal atoms connected by polytopic linkers [170].
successfully synthesized a new hexagonal MOF nanoplate by using pyridine as a modulator.
Wang et al. [171] successfully synthesized a new hexagonal MOF nanoplate by using
This MOF is composed of two Ni2+ cations, four BDC anions, and the nitrogen-containing
pyridine as a modulator. This MOF is composed of two Ni2+ cations, four BDC anions,
terminals of 1,4-diazabicyclo[2.2.2]octane (DABCO) molecules. A paddlewheel secondary
and the nitrogen-containing terminals of 1,4-diazabicyclo[2.2.2]octane (DABCO) mole-
construction unit (SBU) is generated when pyridine and DABCO molecules fight for coor-
cules. A paddlewheel
dination, secondary
and this SBU construction
subsequently unit (SBU)
self-assembles is generated
into whenBecause
2D nanoplates. pyridine and
pyridine
DABCO
replacesmolecules
some offight for coordination,
the DABCO and this
on the crystal’s SBU subsequently
surface, self-assembles
a robust 2D growth trend is into
seen in
2D its
nanoplates.
presence. As concentrations of pyridine were lowered, changes occurred insurface,
Because pyridine replaces some of the DABCO on the crystal’s the shapea of
robust 2D growth trend is
the nanocrystals and hexagons. seen in its presence. As concentrations of pyridine were low-
ered, changes
Using occurred in the shape of
polyvinylpyrrolidone the nanocrystals
(PVP) and
as a regulator, hexagons.
Zheng et al. [172] synthesized Co-
Using polyvinylpyrrolidone (PVP) as a regulator,
MOF of varying sizes. While both Co-MOFs had identical chemical Zheng et al.and
[172] synthesized
physical character-
Co-MOF of varying sizes. While both Co-MOFs had identical chemical
istics, the ultrathin 2D Co-MOF NS demonstrated superior performance in supercapacitor and physical
characteristics,
tests due to the ultrathinexposure
its greater 2D Co-MOF NS demonstrated
of active sites and fastersuperior
electronperformance
transport. inInsu-
addi-
percapacitor
tion, high-performance energy storage and conversion applications (such as transport.
tests due to its greater exposure of active sites and faster electron rechargeable
In addition, high-performance energy storage and conversion applications (such as re-
chargeable batteries, supercapacitors, and fuel cells) rely heavily on materials having
hybrid micro/nanostructure. These multicomponent structures are difficult, yet they can
Sustainability 2023, 15, 10891 28 of 52

batteries, supercapacitors, and fuel cells) rely heavily on materials having hybrid mi-
cro/nanostructure. These multicomponent structures are difficult, yet they can potentially
outperform their simpler single-component analogues. Because of its hybrid nature and the
wide range of components available, the performance of any given application may be fine-
tuned [173]. To date, several different synthesis methods have been developed to generate
micro/nano hybrid structures; these approaches often include the use of precursors and
sacrificial templates to build the complicated hybrid structures. Because the surface energy
plays a role in the thermodynamic and kinetic processes of various re-actions happening at
the interface of micro/nanocrystals, the design and management of different morphologies
of MOF nanocrystals has been a popular issue in recent years [174].
Metal–organic frameworks (MOFs) are crystalline porous materials that are con-
structed from metal ions or clusters, which are linked together by organic ligand molecules.
The modular approach used to create MOFs allows for the production of three-dimensional
(3D) frameworks of varying topologies. MOFs are distinguished from their less-ordered
counterparts such as activated carbon, metal oxide, and silica by their well-defined pore
system [175]. MOFs have a wide variety of potential uses, including catalysis, the capture of
greenhouse gases, and electronic device manufacturing, among others, which are enabled
by their well-defined crystal structure. The storage and transformation of energy are among
the many possible applications for metal–organic frameworks. Redox-active metals are
particularly promising for electrochemical energy applications as they provide better charge
transfer between the ligand and metal nodes. In the field of electrochemistry, MOFs have
recently garnered much attention due to their high specific surface area, tunable shape,
numerous pores, and adaptability. Publications on the energy-related uses of MOFs have
increased significantly in the past two years [176]. Researchers have employed MOFs as
building blocks to create nanomaterials with a wide range of shapes and sizes, including
nanosheets, nanoparticles, nanospheres, and nanorods. However, the use of metal–organic
frameworks (MOFs) in electrochemical devices poses several challenges. One significant
challenge is their relatively low electrical conductivity, which can limit their use as electrode
materials in electrochemical devices. This can be addressed by incorporating conductive
materials into the MOF structure or by designing MOFs with higher intrinsic conductivity.
Another challenge is the stability of MOFs in the presence of moisture, which can cause
their structure to degrade and their performance to deteriorate. Researchers are working
on developing MOFs with improved moisture resistance or implementing protective coat-
ings to address this issue [177]. Additionally, the synthesis of MOFs can be complex and
time-consuming, which can hinder their commercial application. Therefore, efforts are
underway to develop simpler and more scalable synthesis methods for MOFs to overcome
this challenge. Furthermore, although MOFs have exhibited potential in electrochemical
devices, their electrochemical properties remain partially understood, and further research
is necessary to optimize their utilization in practical applications.
COFs, which are the initial form of porous organic frameworks (POFs), have been suc-
cessfully developed to incorporate organic building blocks into a systematically arranged
structure [178] and may be created utilizing the principle of dynamic covalent chemistry,
which involves linking together organic building blocks [179]. Through reversible ther-
modynamic bond formation, COF crystallization is facilitated via error correction and
self-healing, whereby structural abnormalities are dynamically rectified [180]. Due to their
composition of light elements linked via robust covalent bonds, COFs have exceptional
thermal stability and possess low mass densities and permanent porosity [180]. COFs may
be produced utilizing various energy sources, including heat, mechanical agitation, light
irradiation, ultrasound, electron beams, and microwaves. Microwave-assisted synthesis
has garnered significant attention due to its beneficial reaction features, such as reduced
energy consumption, faster reaction speeds, and increased yields [181]. COF-5, a Boronate
ester-linked COF, was synthesized in under 20 min at 100 ◦ C under microwave irradiation
by condensing 2,3,6,7,1,11-hexahydroxytriphenylene and 1,4-benzenediboronic acid, two
hundred times quicker than the standard solvothermal method [182]. Compared to the
Sustainability 2023, 15, 10891 29 of 52

solvothermal synthesis, COF-5’s Brunauer–Emmett–Teller (BET) surface area is higher at

2019 m2 g1 , whereas the solvothermal synthesis yielded only 1590 m2 g1 [183]. Addition-
ally, Bein’s team utilized microwave-assisted synthesis to produce mesoporous Boronate
ester-linked COF (BTD-COF), yielding a highly crystalline BTD-COF with a BET surface
area of 1000 m2 g1 after two successive heating periods of 40 min [184]. Sonochemical
synthesis drastically reduced the synthesis time by avoiding the induction phase, using
less energy and, as a result, less money, and generating higher pressures and temperatures
(>1000 bar and >5000 bar, respectively) due to the accelerated crystallization rate [185].
Sonochemically synthesized COF-5’s yield is better, with a BET surface area of 2122 m2 g1 ,
than a solvothermally manufactured equivalent [186]. While mechanochemical synthesis
(MS) has been employed to create a wide range of porous materials, including metal oxides,
porous carbon, metal–organic frameworks, and graphene derivatives, COFs remain a work
in progress in terms of MS synthesis. MS is a low-cost, simple, and environmentally friendly
technique. The photochemical synthesis method is useful for generating various functional
materials, and Choi, Lim, and their colleagues established a photochemical method for
synthesizing COF-5 (UV-COF-5) at room temperature in the presence of UV light, resulting
in a 48-fold increase in growth rate and a BET surface area of 2027 m2 g1 .
The production of functional materials was achieved by utilizing high-energy radia-
tion, where Imine-based covalent organic framework EB-COF-1 was synthesized in just
160 seconds. This was accomplished by condensing 2,4,6-tris-(4-formylphenoxy)-1,3,5-
triazine and TAPB at room temperature in the presence of a 1.5 MeV electron beam. The
rapid synthesis of the EB-COF-1 framework demonstrates the potential of high-energy
radiation as a powerful tool for producing advanced materials with specific properties
and functionalities [129]. This technology has opened up avenues for industrial-scale COF
production and ensures their rapid synthesis.
Covalent organic frameworks (COFs) also face several challenges in their application
in electrochemical devices. One significant challenge is their low electrical conductivity,
which can limit their use as electrode materials in electrochemical devices. This can be
addressed by incorporating conductive materials into the COF structure or by designing
COFs with higher intrinsic conductivity [187].
Another challenge is the limited stability of COFs under acidic or basic conditions,
which can cause their structure to degrade and their performance to deteriorate. This can
be addressed by developing COFs with improved stability under harsh conditions or by
implementing protective coatings.
The practical use of COF materials in energy-related devices is hampered by their
poor stability or limited endurance. The collapse of COF structures in high aqueous
acidic/alkaline electrolytes may make active centers inaccessible and hinder mass and
charge transfer. Because most COFs are synthesized by solvothermal reactions of precursors
in sealed glass tubes at elevated temperatures, resulting in completely insoluble powders
comprised of randomly aggregated crystallites, poor process ability may be another major
issue for their applications in electrocatalysis. This complicates the use of COF materials in
energy-related equipment.
Consequently, it is preferable to create synthetic processing methods for building
COFs with improved stability and process ability, which allows shaping, positioning, and
orienting COFs as required, while integrating them with other components of the devices
for stable functioning. Improving COFs’ electrical conductivity is further required for
enhancing their electrocatalytic performance and energy storage performance. One way
to do this is to grow oriented COF thin films on a conducting support or to produce com-
posites [188]. Finally, employing the novel stable and completely conjugated COFs made
of cyanovinylene or olefin linkages would be beneficial for improving charge transport
characteristics, which are required for electrochemical applications, and for increasing the
recyclability (robustness) [188]. Additionally, the synthesis of COFs can be complex and
time-consuming, which can limit their commercial application. Efforts are underway to
develop simpler and more scalable synthesis methods for COFs to overcome this challenge.
Sustainability 2023, 15, 10891 30 of 52

Moreover, while COFs have shown promise in electrochemical devices, their electro-
chemical properties are not yet fully understood, and more research is needed to optimize
their use in practical applications [189].
MXenes are a new type of 2D material composed of transition metal carbides, nitrides,
or carbonitrides. They exhibit impressive electrochemical properties such as rapid specific
capacitance, rapid charge–discharge rates, and great cycle stability [190]. Due to their high
conductivity, MXenes are suitable as electrodes in electrochemical devices [107].
Despite graphene’s significant contributions to scientific and technological advance-
ments, its basic structure and chemistry limit its further development compared to other 2D
materials. MXenes are a class of novel materials that have recently gained attention across
various disciplines due to their many layers and adjustable features, which allow for a wide
range of applications such as energy storage devices, catalysts, sensors, and biomedical
applications [191,192]. Recent studies have shown that, like graphene, MXenes’ surface
functional groups can be fine-tuned to alter their electrical and electrochemical properties.
MXenes exhibit high electrical conductivity, electrochromic behavior, antimicrobial charac-
teristics, and transparency, making them attractive for various applications [189,190]. The
exfoliation of the layered transition metal carbide Ti3 AlC2 to produce MXenes using the
top-down method involves immersing Ti3 AlC2 powders in 50% hydrofluoric acid (HF).
During exfoliation, OH and F groups are added to the surface, while Al layers are selec-
tively scratched away [193]. MXenes can be broken down into ML powder by exploiting
their inherent limitations. However, the search for inexpensive, environmentally friendly
alternatives to traditional metals and plastics for use in high-capacity batteries and superca-
pacitors is ongoing. MXenes have exceptional electrical and electronic properties, such as
a large specific surface area, a low energy barrier for electron transport, and a short ion-
diffusion route due to their atomic thickness, crystalline nature, and layered structure [194].
MXenes’ electrical properties can be tuned by adjusting their surface terminations [194].
To develop effective energy storage devices in the future, researchers have been exploring
novel applications of MXenes and MXene-based materials. MXenes face challenges in
their application in electrochemical devices, including the difficulty of large-scale synthesis,
susceptibility to oxidation in air, and sensitivity to the pH of the electrolyte, which can limit
their electrochemical performance in certain devices.
At high current densities, the rate capability of MXene-based electrode materials is
severely limited by the extremely high ionic diffusion resistance in the vertical direction
that arises from stacking the layers of MXenes [195]. A possible way to improve MXenes’
electronic conductivity, stability, and ion/electron transport is to structure them and cre-
ate hybrid materials based on them. Improved electrochemical performance may result
from the increased interlayer distances, which allow for the rapid passage of ions and
electrolytes. Accordingly, further research has to be conducted to strike a good compro-
mise between high-rate electrochemical performance and high-volume capacitance [196].
The influence of surface termination on the functional characteristics of MXene is poorly
understood [197]. The optimization of the MXenes’ surface terminations has great promise
for controlling their characteristics, but a thorough study is needed to demonstrate the
necessary relationships [198].
The key obstacles for MXene manufacturing and the limiting constraints for commer-
cial development are the availability and expense of MAX phase powders and the usage
of a significant volume of intrinsically dangerous high concentrated HF [199]. To reduce
the environmental impact of MXene-based products, a concerted, multifaceted effort is
necessary and desired [199].
The oxidation rate of MXenes may be slowed by removing the dissolved oxygen with
dry nitrogen and storing the compound at low temperatures. Thus, the electrochemical
charge storage mechanism of MXene-based electrode materials has been significantly
impacted by aggregation of the produced MXene and impacts of MXenes’ structural
properties like basal spacing, surface chemistry, etc. [197].
Sustainability 2023, 15, 10891 31 of 52

One of the biggest obstacles to making flexible supercapacitor devices is striking a

compromise between the mechanical features of MXenes (such as mechanical strength,
toughness, flexibility, etc.) and their electrochemical properties [196].
Colloidal MXenes created by solvent sonication or by applying extensive mixing/shaking
durations are widely employed in most research studies, although neither method demon-
strates a viable technology with practical application [200]. To actualize the achieved and
predicted property advantages, colloidal MXenes must be avoided; otherwise, the industrial
adoption of MXene into the electrodes of energy storage devices would run into the same
problems seen with graphene. For MXene to be used in industrial settings, the current high
cost of manufacture must be reduced [196].
Despite these obstacles, the outlook for pure MXenes and MXene-based materials
is brightly promising in not only the energy storage and energy conversion fields but
also in a wide range of other fields including catalysis, environmental protection, and
biomedicine. Specifically, improved performances may be achieved by a deeper knowledge
of the electrochemical charge storage mechanism of MXene-based materials, but this
requires extensive effort, novel concepts, and the application of cutting-edge research and
investigation techniques.

8. Nanotechnology through Electrochemistry in Water Purification

Nanotechnology has the potential to address critical challenges in developing coun-
tries, particularly the significant public health hazard posed by waterborne pathogens in
underdeveloped nations, which claim millions of lives each year. To minimize the risk
of waterborne diseases, it is essential to remove and/or inactivate viruses, bacteria, and
protozoa through point-of-use technologies [201]. Past research has mainly focused on
the electrochemical production of active chlorine species (>2.5 V; HOCl, Cl2 3− ) or electro-
chlorination, which may generate hazardous disinfection byproducts [202]. Interestingly,
studies have reported the successful elimination of bacteria and viruses by microfilters
based on single-walled and multi-walled carbon nanotubes, which also possess antibac-
terial properties. Furthermore, carbon nanotubes have shown potential as substrates for
photovoltaic and fuel cell applications. Hence, CNT-based microfilters may be employed
in an electrochemical manner similar to carbon anodes for pathogen inactivation [203,204].
Boron-doped diamond anodes, which do not create effective chlorine species and
are believed to be efficient for bacterial inactivation, might be a solution. Electrochemical
processes are versatile and provide technologies for cleaning. Desalination in most countries
is based on a technique called the reverse osmosis technique, and this method depends on
the osmotic property [205]. The pressure exerted on the surface of the membranes is used
to overcome the natural osmotic pressure of water. So, if a semi-permeable membrane is
placed between two solutions of equal concentration under equal temperature and pressure,
no water passage occurs through the membrane because of reciprocal chemical effort on
both sides. If we add a soluble salt, the two solutions decrease pressure, so an osmotic
flow of water occurs from the less salty side to the saltier one until the chemical voltage
returns to its equilibrium state. This equilibrium occurs when the pressure difference in the
saltier volume liquid becomes equal to the osmotic pressure [206]. Organic, inorganic, and
biological contaminants may be water contaminants. Specific contaminants are toxic and
carcinogenic and harm people and ecosystems. Highly toxic water pollutants are famous
for some heavy metals. Arsenic is one of the deadliest elements in history. Cadmium,
chromium, mercury, lead, zinc, nickel, and copper are other heavy metals and water
pollutants with significant toxicity [207].
The population increase combined with the exploitation of water resources for domes-
tic, industrial, and agricultural purposes has resulted in a shortage of freshwater supplies
in many parts of the world [208]. Seawater desalination and brackish water treatment
have become alternatives to freshwater resources. Different membrane processes are used,
such as nanofiber and reverse osmotic pressure membranes, to extract potable water [209].
However, the limitations associated with existing membranes (i.e., dirt, biological de-
Sustainability 2023, 15, 10891 32 of 52

composition, physical and mechanical change of membrane properties) result in reduced

membrane productivity because of high energy requirements and the cost of cleaning
procedures and regular replacement membranes [210]. In contrast, ultrafine nanofilms are
less expensive and require fewer operational requirements than reverse osmotic pressure
films. Despite their high productivity levels in water flow, their efficiency in filtering some
saline ions is lower than that of osmotic pressure membranes. Additionally, they differ
in terms of diffusion and distribution of pore size. Wastewater is defined as any water
contaminated with organic or bacterial pollutants or microorganisms, whether from an
industrial source or not, and can be divided into wastewater and industrial wastewater.
Wastewater treatment includes primary and secondary procedures and a triple technique
to remove residual protein from organic and inorganic materials and pathogenic microor-
ganisms through filtration and sterilization. To improve water treatment, nanomaterials
are used, such as nano-titanium oxide [211]. Nanoparticles of TiO2 have become a new gen-
eration of advanced materials, with a diameter of 100 nm, and their various environmental
applications, including gas sensors, are of great interest.
Recent studies have confirmed the importance of activated carbon in removing water
pollutants. Granular activated carbon has numerous uses, particularly in aqueous solutions,
and has increased in demand for various industrial applications [212]. The use of these
GACs for water treatment has shown considerable promise, sometimes outperforming
commercial carbons depending on the target pollutant [212].
The electrochemical method has been used to produce titanium dioxide nanoparticles.
Inorganic mediums such as tetrahydrofuran and acetonitrile in a 4:1 ratio and a stabilizing
agent increase the current density. Tetra-propyl bromide salt is a commonly used organic
medium. Solvent polarity, electrode distance, and stabilizer concentration are used to
control nanoparticle size. Electrochemical methods are applied to synthesize titanium diox-
ide nanoparticles for small-sized metal nanoparticles [213]. The overall process involves
oxidizing the bulk metal on the anode, migrating the metal cations to the cathode, and
decreasing them in a null-oxidation state by forming a metal or oxide. An ammonium
stabilizer prevents agglomeration by creating unwanted metal powder [213]. The electro-
chemical deposition approach is therefore discovered to be innovative and very effective in
suppressing microorganisms. Shashikala et al. [214] discovered that this approach delivers
silver immediately in metallic form, unlike conventional ways of preparing silver catalysts.
It is particularly cheap in recovering hydrogen by eliminating its usage in the process of
catalyst manufacturing. Hydrogen is the most recent energy supplier, with several social,
economic, and environmental benefits, including its use in chemical industries, which
accounts for up to 30% of its usage. This implies the value of H2 and its great demand in
the world today and in the future [215].
Nanoparticles can be emitted into the environment from point sources, such as pro-
duction plants and wastewater treatment plants, or non-point sources, such as washing
machines, garbage, or other nanoparticle materials [216]. Due to their high specific surface,
most nanoparticles accumulate and absorb immediately after water contact, losing their
nanoscale characteristics. The surface configuration of polymers influences the agglomera-
tion of nanoparticles in aqueous systems, such as polyethylene, providing interaction with
different proteins [217]. Besides polymer nanoparticles, different proteins like fetal bovine
serum can also interact.
Nanoparticles can be placed in natural water (lakes or rivers) and industrial storage
systems for a long time as agglomerates or adsorbed with macro-molecules. The nanoparti-
cles are bound to be “inactive” but not harmless because a changing environment, such
as an increase in temperature or a decrease in pH, may cause nanoparticle dissolution.
Different studies have calculated environmental concentrations of nanomaterials to esti-
mate their impact on the environment. Gottschalk et al. [218] concluded that there is a
risk associated with nanosilver, nano-TiO2 , and nano-ZnO when used for waste purposes
in the USA, Europe, and Switzerland. The risk quotient is defined as the predicted con-
centration of the environment and the predicted no-effect concentration. Nanoparticles
Sustainability 2023, 15, 10891 33 of 52

can be degraded and sedimented through biological treatment by interacting with the
microbiological community [219]. Due to their high specific surface, nanoparticles can form
large particles or absorb larger particles, aiding in their separation. If the particles do not
aggregate naturally, adequate flocculation surfactants can be added to cause larger clusters
to form. For example, this process can easily remove colloidal C60 aggregates.

9. Green Nanoscale and Electrochemical Methods in High-Precision Economical Products

Recently, there has been growing interest in the natural synthesis of nanoparticles
and the use of electrochemical methods to produce them [220]. This trend aligns with the
concept of green nanotechnology, which aims to create safe, environmentally friendly, and
energy-efficient products and processes while minimizing waste, greenhouse gas emissions,
and reliance on non-renewable resources [221]. By integrating nanotechnology with other
fields such as materials science, environmental science, electronics, and computing, green
applications are emerging that leverage various technological advancements. For example,
a study has shown that green cars with energy storage and release systems benefit from
nanotechnology-enabled batteries, which improve their efficiency and use a natural mineral
called lithium ferrophosphate (LiFePO4 ) as an electrode component [222]. However, while
nanotechnology plays a small role in the final product, green nanotechnology has significant
potential to enhance sustainability and economic benefits while reducing risks and costs.
Nevertheless, there are still concerns about the environmental and health implications of
some green nanotechnology applications [223,224].
Nanostructures can be categorized according to their size and structure, and they can
be synthesized using different atoms such as copper, calcium, magnesium, protein, and
DNA [225–227]. Each of these formulas serves a specific purpose: Copper nanoflowers
are used for efficient drug delivery, cell imaging, biosensing, and various medical appli-
cations [105]. Calcium nanoflowers improve the function of proteins in the environment,
while nano-magnesium acts as a catalyst for better drug delivery and high-resolution imag-
ing of cells. Researchers have also developed AuPt bimetallic nanoflowers using a one-step
electrochemical reduction method [207,208]. To accomplish electrochemical reduction at
low temperatures, this approach makes use of a unique mechanism involving the addition
of 10% water to eutectic solvents. Glassy carbon electrodes (GCEs) modified with nanoma-
terials (AuPt NFs/GCEs) were made available for the first time by the researchers to be
used as the anode in the electrical oxidation of XT to XO [228,229]. XO was synthesized by
electrical oxidation of XT with a high yield of XO (Figure 11). The researchers achieved a
high yield of XO through the electrical oxidation of XT with significantly lower applied
potentials (0.80 V versus Ag/AgCl) in the modified reaction and electrode system, making
Sustainability 2023, 15, x FOR PEER REVIEW 36 of 55
the system safer than other oxidation potentials. In addition to oxidizing XT to XO, the
system also had a low ability to cause side reactions.

Figure 11.
Figure 11.AAglassy
glassy carbon electrode
carbon (GCE)(GCE)
electrode modified with nanomaterials
modified (AuPt NFs/GCE)
with nanomaterials (AuPtasNFs/GCE)
the as the
anode for the electrical oxidation of XT to XO. Adapted from [228].
anode for the electrical oxidation of XT to XO. Adapted from [228].
Bimetallic nanoparticles possess unique properties and have shown promise as cat-
alysts with various applications [225,226]. The electrostatic deposition reduction method
is a green, controllable, and efficient approach to synthesizing alloy nanoparticles com-
pared to conventional methods [230]. Deep eutectic solvents, a new generation of green
solvents, exhibit remarkable physical and chemical properties, making them useful in
Sustainability 2023, 15, 10891 34 of 52

Bimetallic nanoparticles possess unique properties and have shown promise as cata-
lysts with various applications [225,226]. The electrostatic deposition reduction method is
a green, controllable, and efficient approach to synthesizing alloy nanoparticles compared
to conventional methods [230]. Deep eutectic solvents, a new generation of green solvents,
exhibit remarkable physical and chemical properties, making them useful in nanoparticle
synthesis, electrochemistry, and biochemistry, besides ionic fluids. These natural products
have significant biological and pharmaceutical properties, such as antibacterial, anti-cancer,
and anti-viral properties [231].
In electrochemical oxidation reactions, potential control is critical to achieving safe
electrical oxidation or avoiding unwanted side reactions [232]. Gold nanowires have
been found to enhance the performance of cobalt oxide microelectrodes in electrochemical
biosensors, which are widely used in clinical, environmental, industrial, and agricultural
applications [233]. The catalytic activity of glucose oxidase (GOx) is sensitive to environ-
mental conditions, such as temperature, humidity, pH, and toxic chemicals. The controlled
use of nanostructured metal oxides can overcome the limitations of costly enzymes like
GOx, thereby improving the sensitivity and stability of glucose detection [234].
The correlation between biosensing performance and the electrochemical and struc-
tural properties of electrodes has led to significant efforts to optimize charging and elec-
tronic transmission processes in advanced materials, thereby reducing primary resistance
in bioanalysis [235]. Metal oxides with nanostructures offer promising applications as
non-enzymatic catalysts in miniature glucose sensors due to their low cost, high bio-
compatibility, electrical catalytic activity, and enhanced electron transfer and adsorption
capabilities [236]. Researchers have focused on simpler and more manageable methods to
fine-tune pore size and np-Au ligaments for various applications. Electrochemical methods
provide proper control over pore and ligament sizes, making np-Au electrodes an efficient
and easy-to-handle option for electrochemical biosensing [237].
The surface morphology, pore size, and ligament size of np-Au can be determined
using scanning electron microscopy (SEM) [238]. For higher resolutions, transmission
electron microscopy (TEM) can be used to study thin np-Au films. X-ray energy dispersive
spectroscopy can offer information on mineral composition, aiding in the validation of the
exclusion of metals from np-Au.
Electrochemical techniques are significant for assessing the surface area and kinetics
at the np-Au interface. The method of choice for determining the np-Au electrode surface
area is cyclic voltammetry (CV). In CV, a particular scan rate is used to generate a triangular
waveform and calculate the resulting current [238]. In the reverse scan, the Au-electrode
immersed in diluted H2 SO4 is treated with an anodic scan to form a gold oxide layer. The
charge beneath the cathodic peak is measured, and the surface area of np-Au is calculated
based on the required charge to extract gold oxide from a square centimeter of the gold
surface. However, due to the double-layer charging, the contribution from other faradaic
processes, and variation in the metal’s crystal face, there is always the possibility that this
value will be lost. The geometric surface area is divided from tens to thousands, depending
on the preparation methods, the number of materials, and the size of the pores, and it is
possible to determine the roughness factor of np-Au against a planar surface [239].
Silver nanoparticles have attracted researchers’ attention due to their appropriate ap-
plications in various domains, including electronic science, physical sciences, and medicine.
Nanotechnology occupies a prominent place among innovative approaches to developing
agricultural processes and food production. The wide variety of methods for prepar-
ing nanoparticles in materials science, energy, medicine, and life sciences research has
contributed to the use of nanotechnology and the expansion of its fields [240].
Moreover, from its applications in genetically changed crops and agricultural chemical
production techniques, silver nanoparticles show potential antimicrobial effects against
infectious organisms such as Escherichia coli, Bacillus subtilis, Vibrio cholera, Pseudomonas
aeruginosa, Syphilis typhus, and Staphylococcus aureus [240]. More recently, Ag-NPs have
Sustainability 2023, 15, 10891 35 of 52

been used in a wide range of applications in fields such as mechanics, optics, biomedical
sciences, chemical industries, and electronics.
Different electrochemical techniques, thermo-destructiveness, laser ablation, and mi-
crowaves have been used in manufacturing silver nanoparticles [241]. To reduce the
electrochemical silver, a galvanostatic method (electrolysis) was used in this proposal. A
simple system of three silver anodes (50 × 10 × 0.2 mm3 ) and two silver wires (0.8 mm
diameter) as cathodes was placed at the half-distance between the anodes. Anodes were
positioned perpendicular to the direction in which the electrodes were placed. The dis-
tance between neighboring electrodes was 15 mm [242]. The electrolysis was performed
at 323 K with a current frequency of 0.5 mA cm−2 . A Phillips CM20 TWIN microscope
operating at 200 kV was used to investigate the size, morphology, and composition of the
obtained nanoparticles using transmission electron microscopy (TEM) (Figure 12A), energy
dispersive X-ray analysis (EDX) (Figure 12B), and electron diffraction. Silver oxidation is
noticeable above 0.4 V in the previous work on rising current densities in the anode curve.
This silver anode dissolution process proceeds on a surface with a one-electron reaction.
The nanoparticles form a polarization of silver in an ethanol solution, either potentiostat-
ically or galvanostatically. In the presence of ethanol, the proposed process mechanism
assumes anodic silver oxidation and dissolution. Aldehyde was obtained simultaneously
with the anode during ethanol oxidation to reduce Ag2 O in the last step. The presented
Sustainability 2023, 15, x FOR PEER REVIEW 38 of 55
method is simple and ecological, does not require costly tools, and there will be no need for
surfactants or other reduction agents.

Figure12.
Figure (A)TEM
12. (A) TEMassessment
assessmentwas wasconducted
conductedon onthe
theparticles
particlesobtained
obtainedbybythe
the galvanostatic
galvanostatic
method. (B) The
method. (B) The EDX EDX spectrums of particles obtained through the galvanostatic method
of particles obtained through the galvanostatic method indicate the
indicate
the characteristic
characteristic X-ray
X-ray lineslines
of theofobserved
the observed elements.
elements. Ref.permission
Ref. [242], [242], permission from 28
from Elsevier, Elsevier, 28
April 2023.
April 2023.
license license
number number 5533131415449.
5533131415449.

Anotherstudy
Another studydescribed
describedan anefficient
efficientelectric
electricapproach
approachfor forcolloidal
colloidalAgNP
AgNPsynthesis
synthesis
usingbulk
using bulksilver,
silver,bidistilled
bidistilledwater,
water,trisodium
trisodiumcitrate,
citrate,and
andan anapplied
applieddirect
directcurrent
current(DC)(DC)
voltagesource
voltage source[243].
[243].AAsubstantial
substantialmajority
majorityofofcolloidal
colloidalAgNPs
AgNPscan canbebederived
derivedininone one
processwith
process withaahigh
highantibacterial
antibacterialeffect,
effect,asassynthesized
synthesizedAgNPs AgNPscouldcouldbe beused
usedfor fordifferent
different
biomedicinaluses.
biomedicinal uses. This
This way,
way, the magnet
magnetstirrer
stirrerwaswasconnected
connectedasasanan electrode
electrode in in
thethe
500500
mL
glass beaker to two silver bars parallel to the direct
mL glass beaker to two silver bars parallel to the direct voltage voltage source. The two electrodes
The two electrodes
were6.5
were 6.5 cm
cm apart, and
and bidistilled
bidistilledwater
waterwaswasfilled
filledininwith
with silver electrodes
silver electrodesupup to 7tocm. The
7 cm.
magnetic mixing was performed for 0.016 percent (wt%) of trisodium
The magnetic mixing was performed for 0.016 percent (wt%) of trisodium citrate. For a citrate. For a further
2 h under
further 2 h magnetic revolution
under magnetic and room
revolution and temperature, it supplied
room temperature, a 12 V DC
it supplied a voltage
12 V DCto
the silver
voltage bars.
to the The bars.
silver stirring
Thewas still in
stirring operation
was for half anfor
still in operation hour
halftoanprevent
hour tothe scattering
prevent the
scattering of the residue produced during synthesis. The solution beaker was kept in the
dark for 24 h to complete the AgNP formation. At 2000 RPM, the AgNP solution was
decanted and sediment-free before use and measurements at 2000 RPM for 10 min. The
colloidal AgNP solution for Gram-positive and -negative bacteria achieved high anti-
bacterial effectiveness. The advantages of the above method show the simplicity of
Sustainability 2023, 15, 10891 36 of 52

of the residue produced during synthesis. The solution beaker was kept in the dark for
24 h to complete the AgNP formation. At 2000 RPM, the AgNP solution was decanted and
sediment-free before use and measurements at 2000 RPM for 10 min. The colloidal AgNP
solution for Gram-positive and -negative bacteria achieved high antibacterial effectiveness.
The advantages of the above method show the simplicity of preparation, high efficiency,
uniformity, and purity of colloidal ANPs. A recent study illustrated evaluating photo and
electrocatalytic activities in Iso-AgNPs using isoimperatorine, a furanocoumarin-natural,
as a significant decrease in the synthesis of synthesizing isoimperatorin mediated silver
nanoparticles (Iso-AgNPs) [244].
Iso-AgNPs, which were spherical particles ranging from 79–200 nm in size, exhibited
catalytic activity for sunlight-induced degradation (increased yield). This suggests that
Iso-AgNPs hold potential as effective catalysts for environmental remediation applications
that require sunlight-induced degradation. Compounds contained 4-chloro-fluorescein,
methylene blue, erythrosine B, and new fuchsine. Degradation rates for MB, NF, ER,
and 4-CP with iso-AgNPs were 96.5%, 96.0%, 92.0%, and 95.0%, respectively. Iso-AgNPs
showed an excellent electrocatalytic activity towards H2 O2 in many biological systems
without additional binder and conductive additives. There is a wide range of catalytic
applications for synthesized nanoparticles. A dropping method has been developed as
Iso-AgNPs can change glassy carbon electrodes (GCEs).
The working electrode was polished with alumina powder to achieve a mirror-like
surface. A 5 µL volume of an aqueous solution of Iso-AgNPs was directly applied to a
cleaned area of the glassy carbon electrode (GCE) and allowed to dry at room temperature,
resulting in the formation of Iso-AgNPs/GCE. This process ensures the uniform and
controlled application of Iso-AgNPs to the GCE surface, which is critical for accurate and
reliable electrochemical measurements.
The electrocatalytic activity, stability of Iso-AgNPs, and the decrease in H2 O2 in
0.1 M PBS was assessed using cyclic voltammetry and differential pulse voltammetry. The
PBS buffer was purged with ultra-pure nitrogen for 10 min to remove dissolved oxygen
before measuring.

10. A Fusion of Nanostructures with the Electrochemical System in Applications of

Economic Importance
Nanoscale working techniques have become essential in electronics, and nanoscale ma-
terials are emerging in consumer products, although it may take decades to develop small
usable devices [245]. For example, millions of nano-lines are molecularly applied to natural
and synthetic fibers to impart resistance to clothing and other fabrics at a scale of around
10 nanometers. Zinc oxide nanocrystals are used to create invisible sunscreens that block
UV rays, and silver nanocrystals are added to dressings for killing and preventing bacterial
infections [246]. The future scope for nanotechnology is vast. It is possible to manufacture
lightweight, robust, and programmable materials that require less energy to build than
traditional materials, which produce less waste and increase fuel efficiency in land, ship,
and aircraft transport compared to conventional manufacturing. Additionally, electronic,
magnetic, and mechanical devices and data processing systems can be manufactured for
human and environmental conservation, as well as chemical, optical, and biological sensors.
Innovative photovoltaic materials will make efficient solar panels possible, and molecular
hybrid semiconductors will drive the next revolution in the information age. There is
enormous potential for improvement in health, safety, quality of life, and conservation, and
we must address these opportunities to reap the benefits of nanotechnology [247].
Hierarchical assemblies of nanoscale materials, or their incorporation into devices,
provide a basis for the radical design of new materials and machines, even those intended
for large structures. This advance in structural materials benefits the automotive industry
because reduced weight leads to improved fuel efficiency [248]. Additional improvements
can improve safety or reduce the environmental impact of manufacturing and recycling.
Sustainability 2023, 15, 10891 37 of 52

Further advances, such as active materials showing impending failure or even being capable
of self-repairing faults, may be possible.
For almost every modern control system, sensors are critical. Multiple sensors, for
example, are used in automobiles for various tasks, such as motor control, emission con-
trol, safety, convenience, vehicle monitoring, and diagnostics [249]. Nanosensors exhibit
unexpected speed and sensitivity because of their small size and sometimes extend to the
detection of individual particles. Nanowires made of carbon nanotubes, silicon, and other
semiconductor materials, for example, have an extraordinary sensitivity to chemical species
or biological substances. The charging-induced changes in current can detect different
species on the nanowire surfaces coated with sensor molecules, which selectively bind
species. Many classes of sensor systems have adopted the same strategy [250]. There will
be several applications for new kinds of highly sensitive and specific sensors. When com-
posed of a few cells, sensors that can detect tumors are a significant development. Various
nanostructure fabrication technologies are becoming significant in sensors. Nanostructured
materials have sparked great interest in many sensor applications because of their superior
physical, chemical, and plasmonic properties [251]. Although there are many applications
for these nanostructures in sensor applications, certain limitations can restrict their use.
Gas sensors made of carbon nanotubes, for example, are nonselective. For example, there
was a lack of selectivity for gas sensors based on carbon nanotubes [252]. This lack of
selectivity is an essential factor that can prevent the further use of these CNT-based devices,
which can be reduced by the combination of CNT with other materials. There are also
technical problems in the manufacturing of nanostructures and serious concerns concerning
toxicity of nanostructures that could vary in the quality of each new type of particle’s phys-
ical characteristics [252]. Many sensors, such as electrochemical sensors, enzyme-based
biosensors, genetic sensors, immune sensors, and cellular sensors, are available. Rele-
vant electrochemical sensor developments open new avenues and strategies for research
into the future [253]. The high specificity of enzymes is combined with the sensitivity
of electrochemicals in the electrochemical enzyme-based sensor. Enzyme electrodes are
electrochemical samples on the surface of the working electrode with a thin layer of immo-
bilized enzyme. Because it provides selectivity for the sensor and catalyzes the formation
of the electroactive substance for detection, the enzyme is the most significant part of the
enzyme electrode. The production of various materials, techniques, and applications of
electrochemical enzyme-based biosensors has been the subject of several studies in the last
two years [254]. Nanoforms of minerals such as silver, titanium, and zinc and their oxides
are used in several kinds of toothpaste, cosmetics, sun protection, paint, clothes, and food.
Carbon nanotubes (graphene) also have exceptional properties. They are stronger than
steel, conduct electricity better than copper, and have a higher thermal conductivity than
diamond [255]. In a recent study, nanosynthesis, characterization, and implementation
of zinc oxide-graphene oxide (ZnO/GO) in the electrochemical system have been carried
out. Because of its exceptional properties, for instance, large area size proportions and
low production costs, graphene oxide has been given considerable attention in science
and engineering. It has emerged as a new carbon-based nanomaterial that provides an
alternative route to graphene. Graphene oxide (GO) is a feedstock for graphene, and it has
unique properties from its analog.
The general structure of graphene oxide can be described as a hexagonal carbon lattice
in which some carbon atoms exhibit sp2 hybridization and others exhibit sp3 hybridization
due to the presence of oxygen functional groups. These oxygen groups can be found
attached to both two- and three-hybridized carbon atoms, resulting in a highly functional-
ized graphene lattice.These oxidative functions give it fluctuation properties by being at
the hydrophilic boundary and hydrophobic level. Zinc oxide (ZnO) is an inorganic and
non-toxic semiconductor compound. Its chemical and thermal properties are stable; as an
inexpensive material, this makes it a significant material for research. A unit crystal cell
 Sustainability 2023, 15, 10891 38 of 52

with constants a = 3.2499A0 and c = 5.2060A0 where the u-coordinate is from creates the
following relationship [256]:

u = 1/4 + a2 /3c2 = 3/8 = 0.375 Wurtzite

The compact formation of the ZnO/GO nanocomposite was stated by microscopy

of electric field scans, HRTEM, X-ray diffractive, and reduced overall reflectance spec-
troscopy [257]. Compact ZnO/GO nanocomposites are also confirmed (Scheme 4). The
efficiency of direct electron transfer was therefore confirmed and was used for hydro-
gen peroxide amperometric detection. In another analysis, the GO/ZnO nanocomposite
was produced with ZnO nanoparticles synthesized by decorating expanded and oxidized
graphite oxide nanosheets. Photocatalysts were used to degrade basic fuchsin (BF) color.
The production process was based on the deposition of a two-step sol–gel process. A two-
dimensional structure with 0.54Go/0.46ZnO (w/w) composition and an average ZnO parti-
cle size of 25–30 nm was developed by the GO/ZnO nanocomposite. The GO nanosheet
ZnO nanoparticles have 3.25 eV bandgaps, while the bulk ZnO nanoparticles have a 3.70 eV
bandgap [140]. This research could lead to the growth of structurally engineered and 41 of 55
Sustainability 2023, 15, x FOR PEER REVIEW
efficient composite catalysts by providing detailed technical details for catalyst synthesis,
characterization, and testing of performance issues [258].

Scheme4.4.AAdiagram
Scheme showing
diagram the ZnO/GO
showing nanocomposite
the ZnO/GO preparation
nanocomposite and the electrode
preparation and themanufac-
electrode manu
ture of the
facture of sensor. Adapted
the sensor. from [259].
Adapted from [259].

At the bench level, global efforts are still working on developing desired materials
At the bench level, global efforts are still working on developing desired materials
that can treat water supplies. The principal trustworthy applicant suffered from many
that can treat water supplies. The principal trustworthy applicant suffered from many
challenges considering adsorbent and photocatalytic materials that limit its large-scale
challenges considering
application. adsorbent
Magnetic activated carbon,and photocatalytic
nanotubes (CNT), materials
graphene (G),thatquantum
limit itsGO,
large-scale
application.
carbon Magnetic
nanotubes activated
and reduced carbon,oxide
graphene nanotubes
(RGO), (CNT),
zeolite, graphene
silica, and (G), quantum GO
clay-based
carbon nanotubes
nanomaterials and reduced
are recently advanced graphene oxide Materials
water treatments. (RGO), zeolite, silica,in and
are available clay-based
various
nanomaterials are recently advanced water treatments. Materials are available in various
countries [260]. Thus, water-treating techniques have been developed.
The adsorption
countries andwater-treating
[260]. Thus, photocatalytic techniques
properties ofhave
thesebeen
nanomaterials
developed. make them a
promising option for the removal of heavy metals and organic dyes.
The adsorption and photocatalytic properties of these nanomaterials make Additionally, their them a
photocatalytic properties enable the degradation of pollutants under light irradiation,
promising option for the removal of heavy metals and organic dyes. Additionally, their
further enhancing their potential for environmental remediation applications. The main
photocatalytic properties enable the degradation of pollutants under light irradiation
features of these materials make them suitable to treat wastewater even in a low pollutant
further enhancing
concentration their potential
in combination for environmental
with higher remediation
kinetics of adsorption applications.
or decomposition [260].The main
features of these materials make them suitable to treat wastewater even in a low pollutan
11. Future and Challenges
concentration in combination with higher kinetics of adsorption or decomposition [260].
Nanomaterials have shown great potential in electrochemical devices. However,
11. Future
several and Challenges
challenges and limitations need to be addressed before their widespread adoption
can take place.
Nanomaterials have shown great potential in electrochemical devices. However
One of the key challenges is the synthesis and scalability of nanomaterials. The
several challenges and limitations need to be addressed before their widespread adop
synthesis of nanomaterials can be challenging due to their small size and complex structures
tion can take place.
One of the key challenges is the synthesis and scalability of nanomaterials. The
synthesis of nanomaterials can be challenging due to their small size and complex
structures and may require specialized equipment and expertise. Scaling up the produc
Sustainability 2023, 15, 10891 39 of 52

and may require specialized equipment and expertise. Scaling up the production of
nanomaterials to meet commercial demands can also be difficult, especially if the synthesis
process is complex and expensive [261].
Another challenge is the stability and durability of nanomaterials. Nanomaterials
can be susceptible to degradation over time, especially under harsh operating conditions.
This can limit the lifetime and reliability of electrochemical devices that incorporate these
materials. Developing new synthesis methods and surface modification strategies that
can protect the materials from degradation will be critical to improving their stability and
durability [262].
Nanomaterials also have the potential for toxicity and environmental impact. Some
nanomaterials are toxic to living organisms, especially at high concentrations. In addition,
the environmental impact of nanomaterials is not yet fully understood, and their potential
effects on ecosystems and human health need to be carefully evaluated [263]. Rigorous
testing and evaluation will be necessary to address the toxicity and environmental impact
of nanomaterials before they can be safely used in electrochemical devices.
Integration and compatibility with existing device components are other challenges
for nanomaterials. Nanomaterials may not always be compatible with certain electrode
materials or electrolytes and may require specialized equipment or conditions that may not
be compatible with existing device manufacturing processes. Developing new integration
strategies and improving compatibility with existing device components will be critical for
the successful incorporation of nanomaterials into electrochemical devices [264].
Finally, cost-effectiveness is a limitation of nanomaterials in electrochemical devices.
While some nanomaterials can be synthesized at a low cost, others may require more
expensive production methods. Additionally, the cost of incorporating nanomaterials into
electrochemical devices can be higher than traditional materials, which can limit their
commercial viability [265]. Developing new synthesis methods and improving scalability
will be critical for reducing the cost of nanomaterial production. Identifying applications
where the performance benefits of nanomaterials outweigh the additional cost will also
be important for maximizing their commercial potential. According to some studies,
nanoparticles may cause symptoms similar to those induced by asbestos fibers. The
inhalation of TiO2 particles of an elemental particle size between 2 and 5 nm has resulted in
pneumonitis at a concentration of 8.8 mg per metric m3 , as confirmed by other authors [266].
Carbon nanotubes (CNTs), including nanocrystals and quantum dots, have a lot in
common in creating more sophisticated and powerful solar cells [267]. Today, we can obtain
multiple groups of these advanced nanotubes and control the change in the shapes and
sizes of their grains. In nano-energy, significant work has been conducted to develop an
all-in-one system made up of multiple components that, when integrated, could produce
synergistic effects and meet all the criteria for a successful solar-to-fuel conversion [268].
Silicon electrodes now stand out because they have nearly ten times the power of a
graphite anode. Intelligent structural designs aim to combat instability caused by massive
volumetric changes. Nanowires, porous and core–shell structures, and surface change
composites produced with CNTs and graphene have been documented to have a low
specific ability compared to theoretical values [269].
Scientists are adjusting their research methodologies to create renewable energy from
readily available resources at a low cost. Because of its large surface area, optical characteristics,
and catalytic nature, they discovered that Nanoparticles (NPs) are the optimum contender
for this purpose. Therefore, NPs are used to generate energy from photoelectrochemical and
electrochemical water splitting, particularly in photocatalytic applications [270].
Green nanotechnology applications can clean polluted surroundings such as air and
water and prevent climate change by lowering gas emissions and hazardous waste. It is
still not clear how green nanotechnology will achieve environmental sustainability in the
future. The progress of green nanotechnology solutions must mitigate these risks [271].
As part of a comprehensive initiative toward green nanotechnology, research is per-
formed to produce safe and non-toxic nanomaterials to minimize potential risks.
Sustainability 2023, 15, 10891 40 of 52

The properties of nanostructures that lead to increased sensor selectivity are a sig-
nificant downside of electrochemical sensors. Furthermore, the shape of nanoparticles is
particularly important in identifying their applications. Recently, the tip-head ellipticity in
gold nanoparticles (AuNPs) has been identified as a physical parameter that directly affects
electromagnetic radiation scattering [272].
Intensive research using nanotechnology and electrochemical methods holds promise
for making desalination more efficient. Much of this research focuses on improving the
efficiency of the membranes used in reverse osmosis and other membrane desalination pro-
cesses [273]. Nanotechnology-based membranes have been shown to achieve productivity
gains of up to 20%. Using packed carbon nanotubes in reverse osmosis membranes can
reduce the costs of desalination to the level of technology [274]. For water technology to
be sustainable and cost-effective, we need to invest more in best practices that promote
efficiency and sustainable energy. In hard water and seawater, nanoparticles appear to
accumulate, and the type of organic matter or other natural particles (colloids) present in
freshwater has a significant impact [275]. Dispersion affects ecotoxicity, but several abiotic
factors that influence it, such as pH, salinity, and organic matter, have yet to be thoroughly
investigated in ecotoxicological studies [276].
The issue is how to implement new technology on a small scale and then scale it up to
commercial use on a large scale, and there is no single new technology that can solve this
problem. Performance, cost, safety, compliance with regulations, and lower environmental
impacts are some of the barriers that can prevent new technology from being used on a
large scale. Novel solutions in large-scale research can help identify current obstacles and
develop solutions that enhance efficiency, cost, safety, environmental acceptability, and
customer satisfaction [277].
Titanium dioxide has recently gained popularity as a large-scale semiconductor mate-
rial used in the fields of energy conversion due to its low cost, zero contaminants, relatively
high performance, and excellent chemical stability. However, it faces challenges such as
reduced carbon dioxide absorption and fast electron–vacuum recombination [278]. Carbon
materials, in addition to suitable metals and metal oxides, are a viable option. The electro-
chemical reactor system was designed and innovated to convert carbon dioxide from the
solid electrochemical state to chemicals with benefits [279]. We recommend that nanoparti-
cles be used carefully, especially for unknown toxic materials. Some authors consider the
risk of nanotoxicity to be superficial in terms of concentration volume and nanoparticles.

12. Conclusions
The conclusion drawn from the extensive analysis and findings presented in this
manuscript highlights the significant role of nanomaterials in shaping the future of various
industries and scientific domains. The demand for new devices capable of manipulating
materials at the nanoscale underscores the need for continuous advancements in the field of
nanotechnology. Computer simulations of atomic and molecular structures have emerged
as crucial tools in realizing the full potential of nanomaterials.
Nanomaterials have demonstrated their exceptional utility in enhancing electrochem-
ical performance, thanks to their unique properties such as large surface areas, distinct
structures, and abundant active sites. Their application extends beyond performance en-
hancement, with an emphasis on cost reduction in the development of nanotechnology
products. This pursuit of improved efficiency and affordability opens up new avenues for
widespread adoption and commercialization of nanomaterial-based solutions.
Looking ahead, the future of nanomaterials appears incredibly promising. These
materials are poised to play a vital role in addressing the increasing energy needs of
the future by powering next-generation devices. Additionally, they are anticipated to
revolutionize biosensors and nanomedicine, with far-reaching implications for diagnostics
and medical treatments. The ongoing advancements in nanomaterial research will continue
to drive innovation and contribute to addressing global challenges.
Sustainability 2023, 15, 10891 41 of 52

In essence, the exploration and application of nanomaterials present remarkable op-

portunities for scientific and technological advancements. By harnessing their exceptional
properties and leveraging advanced computational tools, we can unlock transformative pos-
sibilities in material design, energy technologies, and healthcare. The remarkable potential
of nanotechnology ensures a future characterized by sustainability, enhanced performance,
and groundbreaking innovations.

Author Contributions: Conceptualization, H.M.S. and A.I.H.; Methodology, H.M.S. and A.I.H.;
Software, H.M.S. and A.I.H.; Validation, H.M.S.; Formal Analysis, A.I.H.; Investigation, H.M.S. and
A.I.H.; Resources, A.I.H.; Data Curation, H.M.S.; Writing—Original Draft Preparation, H.M.S. and
A.I.H.; Writing—Review and Editing, H.M.S. and A.I.H.; Visualization, H.M.S.; Supervision, H.M.S.;
Project Administration, H.M.S. and A.I.H.; Funding Acquisition, H.M.S. All authors have read and
agreed to the published version of the manuscript.
Funding: This research received no external funding.
Conflicts of Interest: The authors declare no conflict of interest.

Abbreviations

1D One-dimensional
2D Two-dimensional
3D Three-dimensional
AgNPs Silver nanoparticles
Au Gold
AuPt Gold–platinum
BET Brunauer–Emmett–Teller
BF Basic fuchsin
BTD-COF Boronate ester-linked COF
CNTs Carbon nanotubes
CNTs Carbon nanotubes
Co Cobalt
CO3 O4 Cobalt tetraoxide
CoFe2 O Cobalt ferrite
COFs Covalent organic frameworks
Cu Copper
CuO Copper oxide
CV Cyclic voltammetry
EB Erythrosine B
EDX Energy dispersive X-ray
ES Electrical sensors
GCE Glassy carbon electrode
GO Graphene oxide
GOX Glucose oxidase
HPLC High-performance liquid chromatography
Iso-AgNPs Isoimperatorin-mediated silver nanoparticles
LC/MS Liquid chromatography–mass spectrometry
Li Lithium
LiFePO4 lithium ferrophosphate
MA Methyl-ammonium
MB Methylene Blue
MOFs Metal–organic frameworks (MOFs)
MoP-NC Molybdenum phosphide nanoparticles and nitrogen-doped carbon
MS Mechanochemical synthesis
NaOH Sodium hydroxide
NF New Fuchsine
NFs Nanoflowers
Ni (OH)2 Nickel(II) hydroxide
Sustainability 2023, 15, 10891 42 of 52

Ni Nickle
NiONPs Nickel oxide nanoparticles
NiP Nickel phosphide
NPS Nanoparticles
POFs First covalent organic frameworks
Pt Platinum
RGO Reduced graphene oxide
SEM Scanning electron microscope
Si Silicon
SiCNPs Silicon carbide nanoparticles
SiO2 NPs Silicon Dioxide Nanoparticles
TEM Transmission electron microscope
TiO2 Titanium dioxide
XO Xanthone
XT Xanthene
ZnO Zinc oxide

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