REVIEW

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Recent Research Advancements in Carbon Fiber-Based

Anode Materials for Lithium-Ion Batteries
Mahmuda Akter,* Ibrahim Hossain, Maitree Howlader, Fahim Shahriar,
and Umme Habiba Saima

electrolyte salt.[1] Anode materials for LIBs

Energy consumption is a critical element in human evolution, and rapid advances include carbon-based materials, silicon-
in science and technology necessitate adequate energy. As human society based materials, as well as metals and
evades, the advancement of energy storage components has become critical in their oxides, nitrides, phosphides, and sul-
fides.[2] The development of innovative
addressing societal challenges. Lithium-ion batteries (LIBs) are promising can-
anode materials for improved LIBs has
didates for future extensive use as optimal energy storage devices. However, the received substantial attention.[3,4] LIBs are
current limitations of LIBs pose a challenge to their continued dominance. extensively studied due to their high energy
Researchers are constantly exploring new materials to enhance the performance densities, absence of memory effects,
of LIBs, and carbon fiber (CF) is a dominant contender in this pursuit. The high and comparatively low self-discharge rates,
electrical conductivity of carbon-based materials benefits the battery system enabling single-cell battery configurations
and extended operational lifespans.[5,6]
by facilitating efficient electron transfer and improving overall performance.
LIBs comprise four essential components:
CF-based materials provide enhanced energy storage capacity and cycling sta- anode (negative electrode), cathode (posi-
bility in LIBs. Progress in carbon-based materials has resulted in electrodes with tive electrode), separator, and electrolyte.
increased surface areas, enabling greater rates of charging and discharging. The operational idea is based on electro-
In addition, the exceptional corrosion resistance of CF ensures the durability and chemical processes occurring between
robustness of LIBs. A comprehensive review is carried out on the correlation isolated electrodes, facilitated by the elec-
trolyte serving as a conducting medium
between the material's structure and its electrochemical performance, with a
for lithium ions. During charging, lithium
special emphasis on the uses of pure carbon fibers, transition metal oxides, ions migrate from the cathode to the anode,
sulfides, and MXene carbon-based transition metal compounds in LIBs. facilitating the transmission of electrons
back to the cathode and completing the cir-
cuit. The opposite transpires during the
battery’s discharge.[7,8]
1. Introduction The existing LIBs face numerous challenges associated with
the traditional manufacture of active materials (anodes and
The demand for green energy materials and processes is growing cathodes) and the subsequent processing of electrodes. The tra-
due to the scarcity of fossil fuels, climate change, and environ- ditional synthesis and electrode processing necessitate numer-
mental degradation. Powering electrical engines with lithium-ion ous chemicals, extended processing durations, carbon coating
batteries (LIBs) is one environmentally friendly way to address of active materials, electrode fabrication through the amalgam-
energy storage issues. LIBs are extensively studied due to their ation of active materials with carbon black and binder, a slurry
elevated energy densities, absence of memory effects, and com- preparation involving hazardous reagents, application of slurry
paratively low self-discharge rates, enabling single-cell battery onto current collectors, and subsequent overnight vacuum dry-
configurations and extended operational lifespans. The majority ing in an oven. The amalgamation of two methods introduces
of modern LIBs commonly employ lithium metal oxide, specifi- numerous drawbacks, including excessive weight, elevated costs,
cally Li(Co, Mn, or Ni)O2, as the cathode and crystalline graphite environmental risks, expanded dimensions, and diminished
as the anode, exhibiting capacities of 160 mAh g
1 for LiCoO2 energy density, to the LIB system.[8] To resolve this issue, it is

1
and 340 mAh g for graphite, with LiPF6 serving as the necessary to manufacture additive-free components (anodes or
cathodes) by employing thin-film production techniques like
M. Akter, I. Hossain, M. Howlader, F. Shahriar, U. H. Saima as chemical vapor deposition (CVD) or physical vapor deposition.
Department of Apparel Engineering The electrodes of conventional LIBs are typically produced by
Bangladesh University of Textiles applying a slurry containing active materials, binders, and con-
Dhaka 1208, Bangladesh ductive materials onto the surfaces of current collectors, which
E-mail: [email protected]
are usually aluminum or copper foils. Metal foils exhibit signifi-
The ORCID identification number(s) for the author(s) of this article cant weight, low elastic limits, and inadequate adhesion with
can be found under https://doi.org/10.1002/ente.202401426. active materials, resulting in LIBs that lack sufficient flexibility
DOI: 10.1002/ente.202401426 and lightweight characteristics. When deformation applied to

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the battery exceeds the threshold, it may result in significant low conductivity, which restricts the nominal full cell voltage
structural damage and a decline in electrochemical performance, due to its higher lithiation voltages (≈1.5 V vs Li/Li+).[21] In con-
leading to failure.[2] trast, conversion-type anodes, including metal oxides, exhibit
Researchers have made significant progress in recent years in high capacity (≈1000 mAh g
1 for iron oxide-based materials);
the study of carbon-derived anode materials for LIBs. These however, their voltage hysteresis and limited reversibility hinder
materials exhibit impressive traits such as excellent structural sta- further advancements.[22] The primary reason for the limited
bility, a high specific capacity, reliable capacity retention, excep- practical application of conversion-type electrodes in LIBs lies
tional cycling stability, and impressive rate performances. For is that conventional electrode processing through slurry casting
this reason, carbon materials have drawn considerable scientific yields electrodes with suboptimal lifetimes.[23] This process is a
interest as next-generation electrode materials for energy storage. result of the methodology employed in slurry casting, which gen-
LIBs are the leading technological and market alternative for elec- erally yields electrodes composed of active particles combined
tric vehicles (EVs) and microchips. Also, LIBs have recently with a polymer binder (PVDF = poly(vinylidene fluoride)) and
emerged as the dominant power source for portable electronics, carbon additives in a high boiling point solvent (NMP = N-
unmanned aerial vehicles, power grid storage, and electric air- methyl-2-pyrrolidone). This mixture forms an ink that is subse-
crafts.[9,10] LIBs have been leading the portables electronic revo- quently cast onto current collectors and dried. This frequently
lution for about 30 years, mainly to their unique energy density results in inadequate control of the electrode microstructures
compared to other rechargeable technologies. The Nobel Prize in and, in some instances, significant mechanical instability.
Chemistry for 2019 was awarded to John Goodenough, Stanley Nonetheless, the slurry casting method, regardless of whether
Whittingham, and Akira Yoshino, emphasizing the important NMP or water is utilized as a solvent, demonstrates superior per-
role of LIBs in current and future eras.[11] formance for intercalation materials (e.g., graphite, lithium iron
Carbon fibers (CFs) have a high electric conductivity, which phosphate). In these cases, the issues related to volume expan-
helps to increase electron transfer in electrochemical reaction sion and stress-induced fracture of active particles are compara-
processes.[12] Carbon-derived materials can also improve the per- tively limited with each successive cycle; however, the method
formance of batteries in various ways, likely to optimize thermal remains inadequately suited for long-term cycling.[23] An appeal-
conductivity, mechanical strength, stability, energy storage, and ing alternative to slurry casting for battery electrodes is the pro-
discharge rates of electrodes. Additionally, they allow for the cess of electrospinning followed by carbonization, which has
design of batteries that are both lightweight and increase the been successfully employed to produce free-standing plain
volume density of the battery pack, which contributes to perfor- nonwoven carbon fabric electrodes.[24] Electrospun fabrics dem-
mance increase. It can both be used as an active material, con- onstrated over double the volumetric capacity after several hun-
ductive additives, current collectors, and a structural component dred cycles, in some instances, when compared to slurry cast
of batteries.[13–16] In the advancement of carbon materials for electrodes. This enhancement can be attributed to improved elec-
LIBs, 1D carbon materials have drawn interest due to their trical contact with the active particles facilitated by the CF net-
unique attributes such as excellent mechanical properties, com- work. The carbon fabrics were subsequently either adorned
parable electric conductivity, large surface area, with good chem- with battery-active particles or incorporated with active particles
ical stability. Silicon (Si) is a revolutionary anode material with a that were grown directly on the CFs or tubes.[25] Despite the
theoretical capacity of ≈4200 mAh g
1,[17] surpassing commer- enhanced functionality of these hybrid electrodes, their micro-
cial graphite anodes. The abundance of Si in nature makes it structural characteristics remain inadequate for sustaining LIB
an ideal material for the next generation of high-performance performance below 500 cycles at elevated C-rates. This limitation
LIB anodes. The low intrinsic electrical conductivity of silicon is attributed to the detachment of active particles from carbon
dioxide (SiO2) results in sluggish electrode kinetics, and its fibers and excessive electrolyte decomposition, which collectively
low initial Coulombic efficiency (CE) further limits its application contribute to increased internal resistance.[26] Due to their excep-
in LIBs.[18] The utilization of 2D graphene, a carbon derivative, tional conductivities, low densities, and abundant reserves,
has been recognized as an appropriate carbon species for improv- carbon-based materials are regarded as suitable host materials
ing the electrochemical properties of traditional silicon anodes. for lithium metal anodes.[27] Without appropriate surface treat-
However, silicon experiences a significant volume expansion of ment, the carbon surface may exhibit lithiophobic properties, lead-
≈300% during lithium intercalation and a substantial volume ing to uneven deposition of lithium and the potential growth of
contraction upon lithium removal.[19] During significant volume lithium dendrites during battery operation. To boost the lithiophi-
changes, silicon readily pulverizes, leading to a decrease in capac- licity of carbon materials, various strategies have been devised,
ity and coulomb efficiency. Furthermore, the silicon electrode including modifying the substrate composition and applying
may fracture, impeding electron transport and leading to a rapid heteroatom-doped, alloy stage, metallic NPs, transition metal
decline in capacity. To address the aforementioned issues, vari- oxides (TMOs), MXene carbon, metallic sulfides, metallic sele-
ous strategies have been developed, including the design of nide, and metal nitrides.[28,29] When deployed in combination with
nanostructures[19] to reduce the propensity for Si particle fracture lithiophilic structure approaches, these carbon-derived materials
and the embedding of Si nanoparticles (NPs) within a matrix often exhibit minimal nucleation overpotential, homogeneous
material.[20] Dispersing silicon particles in carbon materials, nucleation, and prevention of lithium dendrite formation.
including porous carbon, graphene, and carbon nanotubes A battery typically consists of five major components: an anode
(CNTs), represents an effective strategy. Commercial applica- (negative electrodes), cathode (positive electrodes), electrolyte,
tions utilize carbon-rich silicon composites to balance stability porous separator, and current collector. LIBs, as an assortment
and capacity, whereas lithium titanate oxide (LTO) exhibits of secondary batteries, operate by transferring Li+ ions from

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cathodes to anodes.[30] Throughout the process of battery charg- to grow, the demand for processes and technologies that can
ing and discharging, Li-ion moves back and forth across the keep up with the expansion becomes more crucial. The energy
anode and cathode. In charging, Li-ions are transferred from source in an EV is the rechargeable battery. A motor, a compo-
cathodes to anodes via the electrolyte, leaving the anode in a nent of the vehicle’s engine, converts electrical energy from the
lithium-rich state. This process is reversed upon discharge.[31] battery into mechanical energy. The emergence and widespread
The difference in electrical potential between the two electrodes adoption of technological products like solar cells, EVs, and
results in the LIBs functioning as an electrochemical cell. The hybrid electric vehicles represent significant advancements
equilibrium of the two electrodes is accomplished through anode toward an eco-friendly society. Consequently, research aimed
oxidation as well as cathode reduction. Electrochemical reactions at enhancing the properties and performance of LIBs has become
occur when electrons move from the anode to the cathode essential. This review focuses on CF materials and their possible
through a circuit. Lithium ions simultaneously demonstrate con- application in LIB. The relationship between the material’s
current mobility between the electrodes within the electrolyte. structure and its electrochemical performance is thoroughly
The process of converting chemical energy into electrical energy addressed, with a focus on the application of pure CF anodes,
facilitates energy storage within a battery. Figure 1 shows the MXene carbon composites, TMOs, sulfides, and selenides in
operational concept of a LIB, and Equation (1)–(3) show their LIBs. Furthermore, the advantages and disadvantages of each
chemical mechanism[32] type of electrode material, as well as the major challenges that
current technologies confront, are investigated.
Cathode ð+Þ chemical mechanisms : Li1
y CoO2 + yLi+
(1)
+ ye
↔ LiCoO2 2. The Technological Development Phases
Anode ð
Þ chemical mechanisms∶ Liy C ↔ C + yLi+ + ye
(2) of LIBs

Overall chemical mechanisms∶ Liy C + Li1
y CoO2 At present, LIB technology is inadequate to satisfy the increasing
(3) energy and power demands of EVs, as well as the energy storage
↔ C + LiCoO2 requirements for renewable sources such as solar and wind
energy. Extensive research has focused on advancing battery
In recent years, LIBs have become the predominant power technologies to address the increasing energy demands, empha-
storage technology utilized in laptops, mobile phones, and other sizing exceptional power density along with high gravimetric,
compact electronic devices. Despite the widespread acceptance and volumetric energy capacities. Figure 2 illustrates the early
and deployment of LIBs across various applications, there stages of LIB development, which started in the 1960s with
remains a need for further research, innovation, and develop- the significant intercalation compound research conducted by
ment. This necessity arises from the demand for batteries char- Robert Huggins and Carl Wagner.[34] Their research provided
acterized by higher energy density, extended lifespan, and rapid a solid foundation for comprehending the movement of ions
charging capabilities, which are essential for fulfilling the energy within solid materials, a crucial concept for understanding LIBs.
needs of extensive storage operations and applications, including In the 1970s, as responding to the oil crisis, Stanley Whittingham
solar cells and EVs, within the rapidly evolving electrical, elec- at Exxon started searching for innovative battery technology as a
tronics, and automotive sectors.[33] As the industry continues potential solution to explore alternative energy sources. In the

Figure 1. Schematic illustration of a) Chemical mechanisms of LIBs and b) The basic structure of LIBs.[211]

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Figure 2. The technological development phases of LIBs.

mid-1970s, he designed the first prototype of a rechargeable bat- the development of more advanced batteries in the future, which
tery.[35] While conducting research on superconductors, will possess enhanced capacity, extended lifespan, and reduced
Whittingham made an important breakthrough with titanium weight, hence pushing the boundaries of energy storage capaci-
disulfide (TiS2), a potent material that he later used to develop ties. LIBs are well-known for their capacity to store electrical
a revolutionary cathode for LIBs. He developed a rechargeable energy and transform chemical energy into electricity via an elec-
battery by combining the TiS2 cathode with a LiAl anode. trochemical reaction, leading to them as a sustainable energy
However, the metallic lithium anode could not be commercial- source. The performance of LIBs is greatly influenced by the
ized because of its highly reactive nature and instabilities.[35–37] characteristics and interconnection of their components.
In 1980, John Goodenough made a historic finding about cobalt The selection of the aforementioned components greatly
oxide (CoO2)-based lithium cathodes. He found that using these affects energy levels, voltage ratings, cycle life, safety, and costs.
cathodes instead of metal sulfides significantly increased their Maximizing the performance of these components and their
potential, allowing for an operational voltage range of 2.5 to over interactions is essential for unlocking the full potential of LIBs.
4 V. This marked a crucial achievement that would lead to sig- A battery generally comprises five primary components
nificantly enhanced battery performance. The first economically (Figure 1) an anode (negative electrodes), cathode (positive elec-
feasible LIB was introduced in 1985 by Akira Yoshino. It utilized trodes), electrolyte, a porous separator, and a current collector.
Goodenough’s cathode, petroleum coke as anodes capable
of intercalating lithium ions, and a metallic cobalt oxide
(LiCoO2)-based cathode. These batteries were incredibly light- 2.1. Cathode
weight and had a notable lifespan, allowing for hundreds of
charges before any decline in performance. The benefit of LIBs The voltage output of LIBs is greatly impacted by cathode mate-
is that they do not rely on electrode chemical degradation, but rials. The cathode materials produce the lithium ions (Li+), which
rather on the back-and-forth motion of Li ions between the posi- determine the performance of the LIBs.[43] Table 1 presents the
tive and negative electrodes.[38–40] The first modernization of LIB electrochemical properties of frequently used cathode materials
was successfully commercialized in 1991 by the Sony and Asahi and their performance for LIBs.
Kasei teams, directed by Yoshio Nishi.[41,42] Based on Table 1, it is readily apparent that LiCoO2 has a
Although advancements in battery technology have already led higher theoretical capacity, but its actual capacity is just roughly
to significant changes in electronic devices, researchers are still more than half of that. In addition, it shows structural instability
striving to achieve higher energy density and improved perfor- and thermal instability when exposed to high temperatures. Its
mance. This continuous effort has promising prospects for density is compact, measuring 4.2 cm
3[44] LiFePO4 offers a

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Table 1. A concise overview of the electrochemical properties of commonly used cathode materials.[46,214–228]

Characteristicsa) LiCoO2 LiFePO4 NMC 622 LiMnO2 NCA NMC 111

1
Theoretical capacity [mAh g ] 274 170 – 140 279 275
Actual capacity [mAh g
1] 140 150 182 120 155 160
Average discharge voltage vs Li+/Li [V] 3.9 3.8 3.78 4.0 3.7 3.8
CE 97% 95% 88% 94.69% 86.6% 85%
Energy density [Wh kg
1] 679 544 562 476 562 –
Cycle life 50 1000 50 3000 200 >3000

a)
LiNi0.8Co0.15Al0.05O2 = NCA, LiNi0.6Mn0.2Co0.2O2 = NMC 622, LiNi1/3Mn1/3Co1/3O2 = NMC 111.

unique combination of safety, stability, long-cycle life, and afford- ions (Liþ) to move through the separator’s small pores during
ability. However, it shows reduced lithium diffusion kinetics, charging and discharging operations. The separator plays a cru-
which affects its performance at high current densities, leading cial role in preventing short circuits and ensuring insulation
to slower charging or discharging. Thus, it might not be the best between two electrodes, hence greatly enhancing the safety of
choice for energy-intensive EVs.[45] Lithium nickel manganese LIBs. Glass microfibers are commonly used for small-scale tasks,
cobalt oxide (NMC), such as LiNi0.8Mn0.1Co0.1O2 has more capac- but carbon-based polymers, such as polyolefins, are more fre-
ity, making it appropriate for power-intensive applications. The quently found in bigger commercial products. Separators are fre-
thermal instability of the system arises from the interaction quently employed as a fail-safe mechanism in commercial
between highly delithiated NMC and the organic electrolyte, systems. When temperatures exceed a certain threshold, the
resulting in the release of oxygen and subsequent thermal run- polymer undergoes melting, impeding the movement of ions
away.[46] Lastly, LiMnO2 demonstrates excellent thermal stability, between the electrodes and ultimately leading to the shutdown
low cost, abundance, and environmental friendliness. However, of the battery.[49] A separator possesses several key characteris-
its capacity is considerably lower than that of most other cathode tics: first, it exhibits adequate wettability; second, it demonstrates
materials, which restricts its usefulness to high-performance chemically stable capabilities; and finally, it possesses notable
applications. Ultimately, the unique requirements of the applica- mechanical strength in both reducing and oxidizing conditions.
tion determine the most suitable cathode material. Furthermore, The material must exhibit thermal stability throughout a broad
ongoing research aims to create innovative cathode materials for temperature range. Additionally, the uniform thickness of the
future-generation LIBs to overcome these limitations. separators determines the life span of LIBs.

2.2. Anode 2.4. Current Collectors

The anode in LIBs serves as the negative electrode, facilitat- Each electrode affixes a thin metal foil, typically made of alumi-
ing the transfer of lithium ions from the cathode during dis- num or copper, to act as the current collector. It facilitates the
charge. The charging process functions in a reversible manner. movement of electrical current between the electrodes by control-
The selection of the anode material significantly influences the ling the flow of charge carriers (Li-ions) within the electrolyte. For
capacity, energy density, charging and discharging rates, and the cell to function properly, it is essential that the current collector
cycle life of LIBs, much like the choice of the cathode.[47] To max- has both conductivity and stability. It is crucial to carefully select
imize both specific and volumetric capacities, it was necessary to current collectors to avoid rapid corrosion, as they are exposed to
firmly pack the atoms within a confined space. Using a solid metal the electrolyte to some extent.[50] For lithium batteries to work effi-
structure is the most effective technique for arranging metal ciently, the current collectors need to have a large surface area,
atoms, which leads to the highest possible theoretical capacity. spacious pores, and be strong enough to handle the changes in
Table 2 shows a variety of contemporary anode materials for LIBs. volume of lithium metal during charging and discharging. One
However, using metallic anodes poses significant challenges. way to accomplish this is by introducing molten lithium metal into
While each metal possesses distinct features, its surface exhibits pre-constructed 3-D carbon frameworks like graphene films.
high reactivity, leading to various issues. Such issues include cor- A suitable current collector needs to have lithiophilic properties
rosion, dendritic formation, low cycling stability, and so on.[48] to meet this requirement.[51] Methods such as doping, deposition,
Surface modifications and composites are being used to over- and chemical group modification can be used to enhance the lith-
come these problems. Graphite, Li Metal, TMOs, silicon-based iophilic properties of carbon materials. This can lead to greater
compounds, are most commonly used as anodes in LIBs.[33] functioning as current collectors in battery technology.

2.3. Separator 2.5. Electrolyte

The mechanism of LIBs employs a separator to prevent direct Electrolytes serve the purpose of facilitating the transfer of
interaction between the cathode and anode. This enables lithium charges between electrodes within a cell. This ion/charge

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Table 2. A variety of contemporary anode materials for LIBs.

Active material Current Capacity Theoretical Cycles Voltage ranges [V] CE [%] References
density [mA g
1] [mAh g
1] capacity [mAh g
1]
CNT 530 1000 1116 300 1.0–3.0 95.3% [58,212,229–231]
Graphene 500 500–1718 744 250 0–3.5 87.6% [232–234]
Porous carbon-fiber monolith 500 650 – 100 1.5–3.0 – [235]
N-doped CF 500 870 – 300 0.01–0.8 – [236,237]
N-doped CNFWs 2000 943 – 600 0.01–3 – [60]
TiO2 500–2000 320 335 100 1.7 98% [212,238,239]
LiTi4O5 100 166 175 200 1.0–2.5 95.9% [240,241]
Si 400 600–3580 4200 100–200 0.4 72% [94,109,212,238,242]
Sb 100–2000 230–631 660 100–2000 0.1–3.0 99.6 [243]
Ge 1250 1623 1624 600 0.5–4.2 85% [244,245]
Sulfides 50–5000 500–1800 894 100–1500 0.8 95.1% [137,212,246,247]
TMOs 100–1440 500–1200 716 120–200 0.005–3.0 98% [212,248–250]

transport facilitates the electrical circuit, allowing for the smooth compared to graphite anode. However, it is crucial to thoroughly
flow of current and efficient energy exchange. The electrolyte comprehend and tackle the potential gassing issue that may arise
should maintain its chemical stability during operation. If the during the repeated charge–discharge cycles of this material. In
electrolyte interacts with the electrodes or other components, general, the selection of anode material plays a crucial role in
it could potentially impact the battery’s performance and determining the performance, power density, as well as security
safety.[52] The electrolyte works in conjunction with the separator, of LIBs. In recent years, there has been significant research on
so it needs to be compatible with the separator.[53] The electrolyte enhanced anodes, focusing on both carbon and noncarbon mate-
is a highly flammable element in batteries, which has a consid- rials. This research has included the study of many materials,
erable impact on the security, cost, and capacity. Research and such as CNTs,[54,58,59] carbon nanofibers (CNFs),[60] graphene,[61,62]
developments in this field are still ongoing to bring out the true porous carbon,[63] Si[64] and SiO,[65] Ge,[66–68] tin,[69–71] and
potential of a battery. TMOs,[72–74] metal sulfides,[75,76] metal phosphides,[77] and metal
nitrides.[78,79] Figure 3 illustrates the relationship between redox
2.6. Overview of Anode Materials of LIBs potentials and Li/Liþ, as well as the specific capacity of different
anode materials. This finding demonstrates that the selection of
LIBs are extensively utilized in a range of applications, spanning appropriate anode materials greatly enhances the energy density
from flexible electronic devices to EVs. The anode is a vital ele- of LIB cells. The review discusses various types of carbon-based
ment of a LIBs, as it has a pivotal function in the operation and anode materials, including pure carbon, metallic NPs,
efficiency of the battery. The anode in a LIB is responsible for the
storage and release of lithium ions during the process of charg-
ing and discharging. Usually, it consists of a material that may
intercalate or alloy with lithium, enabling the reversible insertion
and extraction of lithium ions. An effective anode for a LIBs
needs to satisfy the criteria of having a good reversible gravimet-
ric and volumetric capacity, minimal potential compared to cath-
ode, being able to charge and discharge at a rapid rate, a long
lifespan, inexpensiveness, exceptional tolerance to abuse, and
ecologic compatibility.
Graphite, silicon, and lithium titanate are frequently utilized
as anode materials. Graphite is a popular option for anode mate-
rial in LIBs due to its impressive theoretical capacity, exceptional
stability, reliable cycling performance, strong rate capabilities,
and cost-effectiveness. However, it is important to mention that
silicon has a higher capacity for lithium-ion storage compared to
graphite. However, it experiences notable volume fluctuations
during charging and discharging, which can result in mechanical Figure 3. Schematic illustration of active anode materials for LIBs.
deterioration and decreased cycling stability. In contrast, lithium Potential (V vs Li/Liþ) versus capacity density.Reproduced under terms
titanate (Li4Ti5O12, LTO)[54,55] and β-TiO2[56,57] have a lower spe- of the CC-BY license.[212] Copyright 2023, Hossain et al. Published by
cific capacity but boast notable safety and an extended cycle life, Elsevier B.V.

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carbon-based/TMOs, MXene carbon, metallic sulfides, metallic sele- distinct interconnected 3D structure and boast an impressive
nides, and metal nitrides. These materials are classified according surface area of around 2381 m2 g
1. The anodes based on
to their electrochemical lithiation/delithiation mechanisms and CNFWs demonstrate exceptional electrochemical performance,
features. The materials mentioned above have shown great poten- with the battery’s specific reversible capacity maintaining a high
tial in terms of electric conductivity and/or capacity retention, value of 943 mAh g
1 even after undergoing 600 cycles at a cur-
when compared to the traditional graphite anode. Unlocking rent density of 2 A g
1.[60] In a separate study, Kim et al.[83] found
their full potential requires significant research efforts in a variety that an anode made from CNFs showed several impressive prop-
of fields. The potential for developing advanced anode materials is erties. These included a significantly larger surface area, high car-
optimistic among researchers and industry experts, driven by bon purity without the need for a binder, excellent electrical
recent technological advancements and a better understanding conductivity, a strong structure, thin web micromorphology,
of the fundamentals. and a rate capability of 350 mAh g
1 at 100 mA g
1. In high-
energy applications, the voltage profile of the carbon material
shows a sloping pattern instead of a low-voltage plateau. This
3. Application of Carbon-Based Materials in LIBs suggests that it offers more stable anodes compared to graphite.
Wang et al.[84] had successfully developed anode materials for
Rechargeable batteries, such as LIBs, utilize the transfer of lith- flexible LIBs without the need for binder. The researchers initi-
ium ions (Li+) between the cathode and anode. During the charg- ated their study by developing spherical vanadium phosphate
ing and discharging process, Li+ moves between two electrodes. (VPO4), known as VP, on carbon fiber cloth (CFC), as depicted
Li+ is transferred from the positive electrode to the negative elec- in Figure 4a. They then utilized simple hydrothermal techniques
trode during the charging process through the electrolyte, which to fabricate VP/CFC composite anode materials. The findings
contains a significant concentration of lithium. Release is the from the field-emission scanning electron microscopy (FESEM)
opposite of discharge. This section provides a comprehensive analysis reported in Figure 4f–g show that the CF-rich CFC
summary of recent advancements in carbon-based anode mate- forms a 3D porous network. The CF has a diameter of ≈7 μm.
rials for LIBs. The CF surface was enriched with active oxygen groups through
the application of HNO3 pretreatment. These oxygen groups
3.1. Pure Carbon-Based Anodes played a crucial role in the formation of VPO4. Figure 4b,c
presents strong evidence indicating that the CF has been coated
LIBs have consistently been the preferred option for rechargeable by VP particles. Figure 4d presents a distinct perspective on the
energy storage for the past 20 years, specifically due to their spherical shape of the particles, exhibiting an average diameter of
exceptional energy densities and extended operational lifespans. ≈100 nm. The transmission electron microscopy (TEM) image
Graphite is commonly employed as the anode and LiCoO2 as the depicted in Figure 4e illustrates the spherical morphology of
cathode in commercial LIBs. Graphite is the material of choice the particles, exhibiting an average diameter of around 100 nm.
because of its reliable flow, good CE, comparatively lower oper- The synthesized VP specimens, which do not contain CFC,
ating electric tension, and significant capacity. To fulfill the exhibit an oval shape (Figure 4h,i) and have a diameter similar
future energy capacity demands of EVs and electric wire netting to VP@CFC composite electrodes. For the purpose of demon-
technology for storage, LIBs must undergo significant develop- strating the practical use of VP@CFC anode in flexible devices,
ments in terms of specific storage capabilities and cycling researchers opted to use the conventional LiCoO2 (LCO) coated
speed.[80,81] To achieve optimal performance in advanced LIBs, on CFC as the cathode. The VP@CFC/LCO/CFC composite was
it is crucial to have an anode material that exhibits improved formed to provide power to a white LED with a voltage of 3.0 V
reversible energy, rate capabilities, and battery stability. and power consumption of 0.1 W. The LED was tested under
Recently, Xia et al.[82] developed metal-free fluorinated carbon three bending conditions, and the outcomes are depicted in
fibers (FCF) specifically designed for lithium-ion secondary bat- Figure 4j–l. It is evident that the flexible full cell successfully illu-
teries. A straightforward fluorination process was used to create a minated the LED under three mechanical conditions, including
host material with good Li wettability, employing polyvinylidene flat, bending, and post-bending states, thereby exhibiting the
fluoride as a precursor of fluorine. It has been identified that a exceptional stability and flexibility of the full cell. Based on
precise and consistent LiF layer can develop naturally on the solid the findings, it appears that the VP@CFC electrode, in its current
electrolyte interphase (SEI) layer when the Li surface is deposited form, is highly compatible with portable electronic devices. The
on FCF. With this approach, Li electrodeposition becomes pos- study revealed that the VP@CFC hybrid electrode materials dem-
sible, ensuring efficient charge transfer between the electrode onstrated a reversible capacity of 541.2 mAh g
1 at 0.1 C, an
and the electrolyte. As a result, this specific type of LIBs, with impressive rate performance of 350.2 mAh g
1 at 1 C, along with
the FCF hosting Li, shows an impressive capability to consis- superior cycling stability. Recent findings have revealed that
tently cycle at a very high current density of 20 mA cm
2, while the electric conductivity of LIBs can be enhanced, resulting in
also keeping the voltage hysteresis significantly reduced. This a notable improvement in their electrochemical performance.
study showed the remarkable capabilities of CFs as an anode Furthermore, the optimization of electron and Liþ transit routes
material for lithium-ion metal batteries. In a distinct experimen- was minimized, consequently accelerating these advances.
tal study, researchers designed N-doped porous carbon nanofiber In another study, Tang et al.[85] applied a controlled carboni-
webs (CNFWs) for anodes in LIBs by chemically activating man- zation method to green synthesized CFs from a natural
ufactured polypyrrole nanofiber webs with KOH treatments. Tyromyces fissile (TF) fungus. The study employed synthesis
These CNF-webs are made up of porous CNFs that have a techniques at temperatures of 500, 800, and 900 °C for a duration

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Figure 4. a) Schematic representation of the VP@CFC composite anode, b–d,f–i) FESEM images of the VP@CFC composites; e) TEM image of the
VP@CFC composites, j–l) a white LED tests under voltage 3.0 V and power 0.1 W. Reproduced with permission.[84] Copyright 2020, Elsevier.

of 3 h in an inert argon atmosphere to obtain CF samples. interlayer spacing of 0.386 nm compared to graphite (0.335 nm),
Following that, the CFs were manual milling and were then refer TF derived in an amorphous structure.
employed as anode materials for LIBs. The experiment involved Based on the data presented in Figure 5e, the TF500_3 battery,
connecting a charged cell with a CF hybrid anode and a regular after undergoing 150 cycles at a C/5 rate, demonstrates a specific
LiCoO2 cathode, as shown in Figure 5a, to a 2 V yellow light- capacity of ≈300 mAh g
1. The initial irreversible capacity of
emitting diode and a 3 V green light-emitting diode. The cell ≈400 mAh g
1 effectively limits the first CE to 40%. Biomass-
also had 1 M LiPF6 electrolytes. Furthermore, multiple state half derived materials possess a significant abundance of functional
cells have been designed to investigate their electrochemical groups such as oxygen and hydrogen, resulting in the presence of
features. active functional groups on the surface of carbon derived from
The scanning electron microscopy (SEM) views of the hand- biomass.[86] This leads to the formation of an excessive SEI on the
milled TF800_3 CFs allowed for the measurement of the mor- carbon surface during the initial discharge in a half cell.[87]
phological characteristics. The milling process fragmented the Following the tenth cycle, the CE exhibits a rapid increase, sur-
long CFs into smaller pieces (Figure 5b,c). The fragments consist passing 99%, and remains constant throughout the subsequent
of solid fibers measuring 40–60 μm in length and tubular fiber cycles. The performance of TF500_3 was remarkable showing a
branches measuring 10–20 μm in length. The entangled and 93% capacity retention rate when comparing the first and 150th
branched CFs, when utilized as electrodes, create a network of charge capacities. According to the study, the TF500_3 anode
conductive routes that facilitate rapid transfer of electrons and performs better than the TF800_3 and TF900_3 anodes at differ-
lithium diffusion. X-ray diffraction (XRD) studies revealed that ent C-rates, as shown in Figure 5f. TF500_3 exhibited a specific
CFs have a disordered carbon structure Figure 5d, with a larger capacity of 350 mAh g
1 at a cycling rate of C/10, exceeding the

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Figure 5. a) Synthesis of rechargeable LIBs with TF-derived CF and their use in a full cell to power LEDs; b,c) SEM views of TF electrodes; d) XRD patterns;
e) cycling performance of TF500_3; f ) rate performances of TF electrodes; g) CV of a half-cell with TF anode for temperature 500 °C; and h) discharge–
charge profile. Reproduced with permission.[85] Copyright 2016, American Chemical Society.

specific capacities of TF800_3 and TF900_3 which were 250 and and ultrathin characteristics. The implementation of phosphorus
210 mAh g
1, respectively. Scientifically proven to efficiently (P) doping enables an increase of specific capacity with electro-
facilitate the transportation of significant quantities of charge chemical behaviors. A continuous conductive network is formed
in LIBs, the unique carbon composition of TF500_3 exhibits on the surface of CFs through the degradation of urea into
superior capacity.[88,89] g-C3N4, particularly when the CFs are exposed to a nitrogen
Cyclic voltammetry (CV) was employed for studying the elec- (N) atmosphere. This process facilitates the presence of high lev-
trochemical mechanism of the TF500_3 electrodes, as depicted els of nitrogen (8.5 at%) and phosphorus (2.8 at%) in both the
in Figure 5g. A single wide decrease peak from 0.8 to 0 V in the composite and g-C3N4. The huCF/g-C3N4 anode material
initial negative scan suggested the establishment of the SEI and demonstrates specific capacities of 1030 mAh g
1 considering
lithium intercalation into the carbon framework. The inverted pos- the current density of 1 A g
1 following 1000 cycles and
itive scan produces a single oxidation signal at 0.5 V, indicating 360 mAh g
1 for 10 A g
1 during 4000 cycles. This makes it an
lithium extraction from carbon. The succeeding scans showed sin- excellent choice for a flexible anode in LIBs. In addition, the
gle broad decrease peaks from 1 to 0 V. Due to the initial SEI layer researchers conducted an experiment where they pyrolyzed
inhibiting additional SEI generation,[60] the peak height was much Cap skin tissue (CST) derived from the Portobello mushroom
lower. The oxidation peaks observed at 0.5 V exhibited a slight (PM) at various temperatures. The goal was to create a carbon
increase while maintaining their respective forms and intensities. anode that is free of binders and additives. At temperatures above
Consistent cycling of the TF500_3 anode after fabrication was 900 °C, a network of hollow carbon nanoribbons is formed by the
observed through overlapping scans. Figure 5h displays the PM-CST anodes through pyrolysis. PM-CSTs demonstrated
discharge–charge patterns of TF500_3, which correspond to the excellent performance as a self-supporting anode for 700 cycles,
CV data. CF surface encapsulation begins with a peculiar dis- outperforming lithium. SEM analysis shows that PM-CSTs that
charge curve slope change at 0.8 V in the initial cycle. For better were heated to or above 900 °C have a hierarchical porous struc-
performance, they coated CFs with CoO NPs using solid-state mix- ture and their specific capacity goes up. This indicates that the
ing and thermal degradation to create a hybrid LIB anode. At a component undergoes self-activation, possibly due to its remark-
C/10 rate, the hybrid anode of CF and CoO with a 10 mol% loading ably high potassium concentration. PM-CSTs were tested after
had showed 530 mAh g
1 reversible capacity. The superior perfor- being heated at 1100 °C and soaked in a high-concentration KOH
mance was attained as a result of the interconnected CFs forming a solution. There was an initial increase in capacity for the first 50
conductive network, and the well-dispersed cobalt oxide nanoclus- cycles, but it decreased in comparison to nonwetted 1100 CSTs in
ters enhancing reaction kinetics. Fungi-derived carbon-based com- the following cycles. This research aims to investigate energy
pounds have the potential to serve as anodes in high-performance storage materials that are both high-performance and cost-
LIBs based on their performance characteristics. effective, while also being environmentally friendly. These mate-
Tao et al.[90] fabricated N, P dual-doped hollow CF/graphitic rials will be derived from biomass and will have a hierarchically
carbon nitride (huCF/g-C3N4) that possesses flexible, freestanding, structured design.[91] Table 3 provides an overview of the anode

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Table 3. Electrochemical properties of pure carbon-derived anode materials for LIBs.

Anode material Applied methods Reversible capacity Current density Cycle number References
[mAh g
1] [mA
1g]
N-doped CF Hydrothermal þ calcination process 870 500 300 [236]
Hollow carbon nanospheres (HCNs) Vacuum assistant Annealing Cu–C 400 186 100 [251]
Carbon-coated natural graphite TVD and impact milling 300 50 10 [252]
Porous carbon-fiber monolith Pyrolysis 650 500 100 [235]
Porous carbon spheres Template-free spray pyrolysis 365 37.2 100 [253]
Hollow CNT/CNF In situ CVD 1150 100 70 [254]
2D mesoporous CNSs and graphene nanosheets Solution deposition method 770 100 15 [62]
Porous graphene CVD 1718 37.2 – [232]
CNT from ambient CO2 Solar thermal electrochemical process 370 200 100 [255]
Accordion-like graphene oxide array (AGA) Freeze-drying 91 1860 400 [256]
Graphene nanosheets Soft-chemistry approach 460 161 100 [257]
Hollow carbon nanospheres Hydrothermal synthesis 137 100 – [258]
N-doped CNFWs Modified oxidative template assembly 943 2000 600 [60]
route þ chemical treatment
CNF Thermal treatment 450 30 – [83]
N-doped carbon photonic crystals on carbon papers In situ 900 186 1000 [28]
NCNT-coated carbon cloth one-step pyrolysis 143.4 1000 650 [259]
P-doped mesoporous carbon A multicomponent co-assembly process 500 186 200 [260]
Folded structured graphene paper Freeze-drying þ thermal reduction 568 100 100 [261]
Porous graphite KOH treatment 170 930 100 [262]
Carbon cloth and PNS-co-doped carbon net Li metal melt þ injection method 124 161 600 [263]
CNTs/CC film@Li Infusing molten methods 157 161 100 [264]
N-doped carbon photonic crystals on carbon papers Stirring solution 900 186 1000 [28]
N,P dual doped-CFs/graphitic-C3N4 Hydrothermal synthesis 1030 1000 1000 [90]

materials framework for LIBs derived from pure carbon. This element, because of its cost-effectiveness and impressive energy
table exhibits the electrochemical properties along with the tech- density. Understanding the intricate process of lithiation in this
niques applied techniques of pure carbon materials-based anode material relies on specific voltage thresholds and the initial mor-
electrodes of LIBs. phology and structure of silicon. Understanding the behavior of
silicon during the process of lithiation in a Li-ion cell at room
3.2. CF/Silicon (Si) Composites temperature can be quite intricate, as it is influenced by a multi-
tude of factors including particle size, shape, and rate.[92] A par-
Si exhibits a notable specific capacity of 4200 mAh g
1. However, ticular silicon electrode still faces challenges in terms of their
it has also experienced certain drawbacks, including reduced circulation capacity. During the delithiation process, the silicon
electric conductivity and considerable volume changes, which electrodes experience a significant volume change of over 300%.
surpass those of lithium by four times. These limitations have Structural breakdown occurs as a result of various factors, includ-
resulted in poor rate performance and significantly lower capac- ing material shattering, loss of electric link to the conductive
ity retention, hindering its further development. Additionally, agent and current collector, and the formation of irregular
these limitations have also led to the unrestricted growth of surfaces.[93]
the SEI and pulverization of the electrode material. Recently, As part of this study, a composite was created to deal with the
there has been a surge of interest in metallic anode materials problem of damage to structures caused by large changes in the
because of their promising ability to enhance energy, power den- volume of Si while still having excellent electrical conductivity. Si
sity, and security. The combination of silicon and carbon materi- NPs embedded in a gigaporous carbon microsphere, then cov-
als achieved a notable increase in performance. The carbonic ered by a carbon nanoshell, form the composite anode.
structure surrounding enables the silicon to expand in bulk Figure 6a presents a schematic illustration of the fabrication pro-
through honeycomb-like pores. Similar to a material chemist, cess. Figure 6b displays the structure of the hollow microspheres
this type of carbon shell enhances electric conductivity by con- prior to deployment with Si. The microspheres exhibit an average
tacting the fiber mesh, while also preventing an electrolyte from particle size ranging from 15 to 20 μm, while the pore diameter
passing into the core. Si plays a crucial role as an alloying exceeds 0.5–1 μm. The shape of the microsphere changed as the

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Figure 6. a) Schematic illustration of carbon-wrapped/Si anodes. SEM images of composites materials with u-Si contents of b) 0 wt%, c) 25 wt%, d) 50 wt%,
and e) 85 wt%. SEM images of f ) SEM views of PUF-covered microspheres of (d), g) carbonized product of (f ), h) magnification of (g), and
i) corresponding TEM image of (h); j) C, and k) Si is EDS mappings of (h); l) CE of @u-Si and u-Si cells, and m) CE of @n-Si and n-Si cells.
Schematics depicting the structural modifications of n) typical u-Si and n-Si electrodes, as well as o) @u-Si and @n-Si electrodes. Reproduced with
permission.[94] Copyright 2020, Elsevier Ltd. p) A 3D model of the whole structure showing the Si/po-C@C composite fiber's design; q) changes in
Si/po-C@C structure brought upon by treatment and cycling; r) SEM views of Si/po-C@C composite; s) TEM view of the electrode made of
po-C@C fibers; t) cycling performance of developed composite electrodes Si/po-C@C, pure Si NPs, and po-C@C. Reproduced with permission.[213]
Copyright 2015, Royal Society of Chemistry.

amount of micron-sized (0.8 μm) Si powder (u-Si) increased of the PUF shell into a carbon nanoshell, resulting in a signifi-
from 25% to 80% by weight, as shown in Figure 6c–e. After cantly lowered thickness of less than 40 nm. The composite elec-
Si implantation, a noticeable change in the hollow microsphere’s trode materials, denoted as @u-Si, exhibit a composition of
morphology was observed. Thermal treatment induces polymer 85 wt% Si. Figure 6g illustrates the presence of a 2 μm primary
decomposition within the microspheres illustrated in Figure 6c– pore situated beneath the nanoshell. In addition, the porous
e, resulting in carbon formation. The microspheres gradually microsphere was filled with Si nanopowder (n-Si) with a standard
attain Si contents of 80, 95, and 98 wt%, respectively, as time pro- size of 50 nm and a specified Si concentration of 25 wt% to achieve
gresses. To enhance the strength of porous microspheres, a complete encapsulation through PUF after carbonization.[94]
material containing 50 wt% Si was carefully selected and subse- The study evaluated the cycle performance of electrodes made
quently coated with 80 nm thick polyurethane (PUF), as depicted from different silicon variants during the charge/discharge pro-
in Figure 6d. Here, thermal treatment enabled the transformation cess. The voltage range used was 0.01 to 1.2 V, followed by a

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current density of 420 mA g
1. Figure 6l,m visually depicts the framework. The fundamental premise posits that the internal
findings. Extensive computations were undertaken to ascertain structure and external shell are inseparable and instead
the precise capacities of each individual cell, considering the constitute a cohesive carbon matrix. The idea is that the three-
mass of Si. dimensional network that is connected to each other could be
Figure 6l shows that after the first charge, LIBs with a u-Si a very good way for electricity to flow when the carbon matrix
anode have a remarkable initial capacity of 2891 mAh g
1, and Si NPs are close together.[100]
achieving a CE of 73%. The capacity exhibits a substantial decline Subsequently, additional studies were conducted by research-
after 20 cycles, reaching a range of less than 500–1000 mAh g
1. ers to further improve this outcome. Figure 6t effectively illus-
After 100 cycles, the capacity decreases to 206 mAh g
1, indicat- trates the relative specific capacity of Si/po-C@C regarding
ing a significantly low retention rate of only 7%. By using @u-Si the total weight of the Si/C composite. Assessing the Si capacity
as the anode material, a large initial capacity of 3236 mAh g
1 in the Si/C composite is of utmost importance. According to the
and an initial CE of 85% for LIBs are achieved. This battery has TGA results, the composite material contains 21.8% weight per-
an impressive capacity retention of 88%, yielding 2847 mAh g
1 cent Si. The initial charging specific capacity of the Si/po-C@C
even after 100 charge/discharge cycles. The porous structure of composite is 3612 mAh g
1 during the first cycle, and it declines
the @u-Si cell enhances its cyclability by effectively absorbing to 2528 mAh g
1 upon 150 cycles. The observed changes in spe-
and minimizing electrode damage as the volume of Si increases. cific capacity can be ascribed to the impact of the carbon matrix
The incorporation of a carbon nanoshell enhances the anode’s constituents. The Si/po-C@C combination exhibits a greater sil-
cyclability by improving its electrical conductivity. icon availability compared to the maximum reported capacity
Figure 6m compares the battery performance of n-Si and range. In Figure 6t, the electrode composed solely of Si exhibits
@n-Si. The initial specific capacity of the n-Si electrode is a discharge capacity of 3422 mAh g
1. The Si/po-C@C compos-
2780 mAh g
1, having an initial CE of 72%. These values approx- ite materials demonstrate an initial discharging capacity of
imate those of the u-Si electrode (Figure 6l). After 100 cycles of ≈4065 mAh g
1 when compared to Si composites. This compo-
charging and discharging, the capacity of n-Si cells decreases to site’s hollow carbon architecture promotes Si acquisition by
1220 mAh g
1, keeping 44% of its original capacity. In contrast, forming a 3D network of conductors within the fiber using
u-Si cells retain only 7% of their initial capacity. The literature[95–98]
Si NPs.[101,102]
suggests that n-Si electrodes exhibit superior retention compared
In a different study, Wu et al.[103] used interconnected hollow
to u-Si electrodes due to their smaller volume variation. @n-Si
structured carbon fibers (IHCFs) to create Si@IHCF hybrid
cells exhibited an initial capacity of 3320 mAh g
1 and demon-
composite electrodes using the electrospinning and a coaxial dual
strated enhanced stability, with a capacity of 2985 mAh g
1 and
nozzle technique. The electrodes consist of a honeycomb-like
90% retention after 100 cycles. Figure 6n shows how repeated
carbon architecture with silicon NPs embedded in the central
lithiation and delithiation can break down particles and anodes
region. Here, the hybrid core is surrounded by an interconnected
because of stress and bigger changes in volume. This pulveriza-
carbon shell that has a cobweb-like appearance. The electrode
tion can result in a decrease in electrical contact and capacity. The
made with Si@IHCFs demonstrates consistent cycling perfor-
hollow structure’s ability to accommodate the increased volume
mance, boasting high specific capacities, and enhanced rate
of Si explains the enhanced cyclability of @u-Si and @n-Si, as
capacities when compared to the Si@HCFs electrode featuring
shown in Figure 6l,m. Figure 6o illustrates how the carbon nano-
shell enables the hollow microspheres of Si to preserve their a disconnected carbon shell. The unique architecture of
firmness and prevent potential breakage. Si@IHCFs contributed to their superior electrochemical advan-
Additionally, we uncovered a different structure that employs tages. The core of the fiber has a porous carbon framework that
the dual coaxial electrospinning technique to wrap silicon nano- can effectively absorb the expansion of Si NPs by utilizing its
particles (Si NPs) within interconnected tubular CFs. The layered empty spaces. In addition, this framework enhances the move-
core-shell structure of silicon/carbon (Si/C) hybrid fibers leads to ment of electrons and ions, creating highly conductive pathways
enhanced performance. Figure 6p,q depicts the fabrication tech- within its intricate carbon structure that resembles a honeycomb
nique and the two-dimensional nucleus-shell architecture. The with complex pores. The cycling properties of various electrodes
fiber core embeds Si NPs into its carbon skeleton, encircling were examined under specific conditions, such as current density
them with a network of interconnected carbon shells. The strati- and voltage range. The electrodes tested included pure Si, Si/CFs,
fied core-shell structure enables this arrangement.[99] The versa- Si@IHCFs, and IHCF. Both the pure Si and Si/CFs electrodes
tile and layered structure of Si/po-C@C composites was analyzed show limited cycling capabilities. Similar to a physical chemist,
by obtaining CFs without silicon (po-C@C) through the corro- the reversible capacity of pure Si electrodes decreased from 2749
sion of silicon nanoparticles (Si NPs) in Si/po-C@C using a to 362 mAh g
1 after 50 cycles. In contrast, the Si/CFs electrodes
NaOH solution. The SEM and TEM images presented in exhibited a decrease in reversible capacity by 1076 mAh g
1 after
Figure 6r,s offer an exhaustive view of the morphology and com- the fifth cycle and 416 mAh g
1 after 100 cycles. Silicon NPs may
position of po-C@C. Therefore, the carbon matrix’s fundamental lose electrical contact with conductive additives in the pure sili-
and inherent structure is clearly exhibited. The image depicts con electrode when subjected to repeated significant volume
fibrous carbon matrices composed of two intersecting profiles: changes. Reduced electrical linkage caused by conductive addi-
an inner core with a porous carbon structure and an outer shell tions on the pure Si electrode can result in fleet capacity fading.
with a dense carbon layer. Figure 6r,s illustrates the uniform dis- The reduplicative big volume fluctuation in the Si NPs is respon-
tribution of mass in the spherical pores resulting from the sible for this phenomenon. Si NPs are incorporated into the CF
removal of Si NPs within the 3D interconnected carbon matrix, leading to enhanced electrical contact. Consequently,

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they demonstrate enhanced capacity retention in comparison to When a current density of 400 mA g
1 was applied, the reversible
Si/CFs throughout the first 30 cycles.[104–106] capacity after 100 cycles was found to be 1441.0 mAh g
1. The
The review discusses a novel electrode with a hierarchical findings are anticipated to have important implications for the
core-shell structure.[103] It highlights the advantages of incorpo- progress of Si/carbon composites in the research and develop-
rating freestanding membranes of Si/HCFs and Si/IHCFs as ment of advanced anode materials.
electrodes in the fiber network. This approach eliminates the Mu et al.[64] investigated the interaction between nitrogen and
need for a binder, conductive agent, and current collector, oxygen-codoped 3D vertical graphene nanosheet arrays (VGAs)
thereby enhancing the benefits of the interconnected framework. on Si/CNFs. Silicon content was regulated via electrospinning
The study observed that the resulting freestanding membrane and CVD methods. Figure 7a illustrates the fabrication methods
anodes have lesser specific capacities compared to the slurry- used to develop hybrid flexible VGAs/Si/CNFs electrodes. The
derived Si@HCF and Si@IHCF anodes. Additionally, the spe- direct synthesis of VGAs on Si@CNFs was achieved through a
cific capacities decrease over time as the mass, specifically the thermal CVD procedure. This involved infusing ethanol vapor as
thickness, increases. It is indicated that certain types of fiber indi- the carbon precursor into a custom-made apparatus (Figure 7b).
viduals are well-insulated within the conductive framework of the Uniform growth of VGAs was achieved by adjusting the propor-
membrane as a result of their nonwoven-like arrangement. It is tions of H2 and ethanol vapor in multiple Si@CNFs composites,
worth mentioning that the capacities of Si@HCF anodes exhibit as depicted in Figure 7c–f. The interconnected VGAs (Figure 7g–j)
a more rapid decrease during cycling in comparison to the slurry- form a 3D conductive network, facilitating the formation of effec-
derived anodes. As an illustration, the researchers noted that the tive conductive pathways. This study briefly examines the process
Si@HCFs initially had a reversible capacity of 703 mAh g
1, of vertical graphene formation through thermal CVD.[110,111] The
which then reduced to 437 mAh g
1 after 40 cycles. This indi- development of VG on a flat base is a time-consuming process due
cates a retention rate of 62%, which is lower than the 89% reten- to the frequent curling of carbon atoms. The addition of H2 causes
tion rate observed for the slurry-derived Si@HCF anodes. In the carbon atoms to form irregular phases and defects, resulting in
addition, it was noted that the charge–discharge graphs display graphene growing perpendicular to the base. The presence of
clear voltage plateaus around 0.7 V in the initial discharging larger curvatures in the 1D CNFs and 0D Si NPs of Si@CNFs
cycle. The occurrence of these processes is observed when a SEI facilitates the rapid development of graphene. The interconnected
is formed on the carbon matrix, causing the migration of water- architecture of this novel design enhances the mechanical proper-
soluble Liþ ions into the layers of graphene, and charge curves ties and electrode stability by leveraging electrochemical proper-
shift between 0.2 and 0.6 V as Li is released from the LixSi ties.[111,112] The VGAs exhibit a height of ≈150 nm, which can be
alloys.[107,108] As a result, the performance of the Si@HCF mem- precisely manipulated by varying the growth duration (Figure 7k–n).
brane deteriorates more quickly as the fibers form an insulative The observed relationship between VGA density, height, and
solid electrolyte interface layer. This process gradually dimin- deposition time is evident. When using CH4 as a carbon source,
ishes the overall structural conductivity of the membrane. Si@CNFs exhibit a significantly higher height of 50–300 nm in
Moreover, the capacity retentions of these two membranes 3 h compared to original CNFs, which take ≈6 h to reach a height
exhibit declining trends, with the Si@HCFs experiencing a grad- of 150 nm.
ual decline. Despite having a lower loading mass than Si@IHCF To assess the electrochemical efficiency of different electro-
materials, Si@HCFs exhibit enhanced performance over forty des, coin cells were designed with VGAs@Si@CNFs as anodes
consecutive cycles, often surpassing the material’s initial invert- and LCO as cathode electrodes. Figure 7o displays the CV pro-
ible capacity. In terms of performance and retention, Si@IHCFs files of the first four cycles for VGAs@Si@CNFs-1. The scan rate
outperform Si@HCFs for a comparable range of loading masses. used was 0.1 mV s
1, and the potential (V vs Li/Liþ) range was
Additionally, scientists attribute the observed decline in cycling 0.005–3 V. The first scan shows apparent cathodic peaks at 0.90
performance to the interaction between the carbon material and and 0.01 V for VGAs@Si@CNFs-1 electrode, which is due to SEI
a dense shell during the insertion and extraction of lithium.[72] on VGAs coating, as reported in the past.[113] The cycle function-
Cheng et al.[109] developed a hierarchical composite, termed ality of VGAs@Si@CNFs-X electrodes (X = 1–4) was evaluated
Si/S-doped carbon fibers (SCF)@rGO, to enhance the cycling using a current density of 0.1 A g
1, encompassing a voltage range
efficiency of the Si anode through in situ polymerization and of 0.005–3.0 V (Figure 7p). The electrode VGAs@Si@CNFs-1
chemical reduction technique. The study sought to establish reveals a notable reversible capacity of 2390.5 mAh g
1 throughout
the most effective concentration of sodium dodecyl sulfate 100 cycles. The VGAs@Si@CNFs-X with varying electrode values
(SDS), and the appropriate quantity of Si NPs required for the (X = 1–4) demonstrate reversible capacities of 2104.5, 1559.9, and
synthesis of uniformly distributed Si/SCF@rGO. They found 1451.5 mAh g
1 throughout 100 cycles, with capacity retentions of
that adding SCF and reduced graphene oxide (rGO) to a hierar- 68.9%, 73.3%, and 93.6% accordingly. The electrodes fabricated
chical sequential network made the Si/SCF@rGO composite from VGAs@Si@CNFs, with a Si content of 90.58%, demonstrate
electrode more stable and improved its electrochemical perfor- a decrease in capacity retention when operated at a lower current
mance. The layer of rGO combined with electrolyte NPs acts density. The observed behavior in lithiated LixSi at different cur-
as a protective barrier, effectively preventing direct interaction rent densities may be attributed to the discrepancy in x-values. A
with the electrolyte. Enhancing the formation of a stable SEI film decrease in current density can cause Si to fully lithification, lead-
leads to an improvement in CE. The interior of the SCF greatly ing to an increase in the x-value. Increasing the values of x pro-
improves the bonding properties of the active ingredients. LIBs motes the expansion of the volume of Si during the process of
tested the anode and demonstrated a strong ability to charge lithiation. This leads to a reduction in the stability of the electrode
quickly, with a capacity of 572.1 mAh g
1 at 3200 mA g
1. and the ability to retain its capacity. The benchmark electrode of

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Figure 7. a) The fabrication method of VGAs@Si@CNFs anodes using electrospinning and CVD, b) ethanol vapor as the carbon precursor into custom-
made apparatus; SEM images of controllable synthesis composites; c,g) VGAs@Si@CNFs-1, d,h) VGAs@Si@CNFs-2, e,i) VGAs@Si@CNFs-3, and
f,j) VGAs@Si@CNFs-2; k–n) growth of VGAs; o) the first four CV curves of the VGAs@Si@CNFs-1 anode at 0.1 mV s
1; p) the cycling performance
of the composite anode at a current density of 0.1 mA g
1; q) rate performance of the composite anode VGAs@Si@CNFs-X (X = 1, 2, 3, 4). Reproduced
under the terms of the CC-BY license.[64] Copyright 2022, The Authors. Published by Wiley-VCH GmbH.

Si NPs exhibits rapid capacity declines at 0.1 A g
1, primarily the unique VGAs that grow on the structure of the CNFs. The
caused by Si expansion during lithiation/delithiation. properties of CNFs and the prevalence of VGAs contribute to
The rate performance of the electrodes was assessed by eval- their long-term continuous framework. The carbon encapsula-
uating the kinetics of Li-ion storage, as shown in Figure 7q. The tion is crucial in enabling the significant volume expansion of
electrode VGAs@Si@CNFs-1 exhibits notable reversible capaci- Si NPs at both the charging and discharge processes. Table 4
ties across various current densities, spanning from 3331.9 to presents a summary of the electrochemical performance of
1378.3 mAh g
1. The device exhibits a notable reversibility of carbon–silicon composites.
1064.7 mAh g
1, even under the influence of a high current den-
sity of 10 A g
1. The rate performance of the VGAs with Si and 3.3. CF/Metallic Selenide(MSe) Composites
CNFs electrodes is remarkable. However, the capacity decreases
as the Si content increases. It is noteworthy that VGAs@CNFs Transition metal selenides have garnered significant attention
demonstrate remarkable rate capability and cycle stability in from researchers as electrode materials in electrochemical
the context of Li+ storage. The electrochemical properties of energy storage systems. Transition metal selenides consistently
the VGAs@Si@CNFs composite are primarily influenced by exhibit a sandwich structure, characterized by a metal atom

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Table 4. Electrochemical performance of carbon-based silicon composite materials in LIB anodes.

Anode materials Applied methods Reversible capacity Current density Cycle number References
[mAh g
1] [mA g
1]
C/SiNW/Li Molten Li infusion techniques 58 372 500 [265]
SiC/gradient decorates CC composite Bottom-up deposition 120 186 120 [266]
Si-coated graphite – 500 – 50 [267]
Si@MOF composites In situ mechanochemical 830 200 500 [93]
C–Si granule electrode CVD 1950 – 20 000 [268]
Si/porous-C Dual coaxial electrospinning 997 200 150 [213]
Si@IHCFs Dual coaxial electrospinning 903 200 100 [103]
Si/porous-C Dual coaxial electrospinning 603 500 300 [213]
Si/po-C@C Triple coaxial electrospinning 1210.7 50 100 [100]
Si@C-CNTs Blade-coating 803 500 100 [269]
2Si@C-CNTs Blade-coating 1140 500 100 [269]
Graphene-Si aerogels Freeze-drying 817 200 150 [270]
Si/C Centrifugal spinning 758 100 50 [31]
C-coated Si/SiO2/CNFs Electrospinning þ carbonization þ CVD 733 100 50 [271]
Si/rGO Magnesiothermic reduction 904 200 150 [272]
Si/SCF@rGO In situ polymerization þ chemical reduction 1441 400 100 [109]
Si/multilayer graphene sheets Electrochemical exfoliation 990 372 500 [273]
SiO2/NGA Hydrothermal techniques 1052 100 80 [274]
C/MnO/SiOC – 770 100 200 [65]
Graphite/Si/GO/C Spray drying 1212 200 100 [275]

positioned between two selenide layers. The atoms within these heterojunctions. The purpose of this section is to present a thor-
three layers are covalently bonded, while the sole interaction ough summary of the latest developments in MSe hybrid nano-
between the individual sheets is attributed to weak van der fibers. These advancements hold great promise in enhancing the
Waals forces.[114] The latter force is sufficiently weak to permit production of robust anode materials for LIBs. Our study in this
other atoms to intercalate reversibly in the interchain spaces, section of the review studied the successful development of one-
resulting in the formation of intercalation compounds or inter- dimensional CoSe@N-doped CNFs using electrospinning and
calates; consequently, energy can be stored in the layered conduc- annealing techniques. To facilitate CoSe synthesis, the research-
tors.[115] Other TMSs, such as ZnSe, Cu2Se, and CuSe, ers introduced a suitable quantity of selenium powders into the
predominantly exhibit semiconducting properties with compar- precursor solution. In addition, the CoSe@NCNFs material per-
atively higher conductivity. These materials have been utilized in formed annealing at different temperatures (550, 650, and
electrochemical energy storage due to their distinct electrical 750 °C) to produce the CoSe@NC-550 material. Throughout
properties. Transition metal selenides exhibit a significantly the cycling process, the improved material demonstrated
higher theoretical capacity than traditional graphite in LIBs. improved capacity and favorable rate potential.[116]
Certain selenides have the capacity to incorporate sodium and The surface properties of CoSe@NC materials were evaluated
magnesium ions. Additional advantages of transition metal sele- using SEM and TEM techniques, as shown in Figure 8. Both the
nides include their affordability, abundance in the earth’s crust, high-resolution SEM and low-magnification TEM images
and ease of fabrication; these characteristics significantly (Figure 8a–f ) demonstrate an even bond between the CoSe
enhance their utility in electrical device applications.[114] Metal NPs and the nanofibers. When the temperature increased from
selenides (MSe) have garnered considerable interest as anode 550 to 750 °C, the study observed a decrease in both the size and
materials in LIBs owing to their diverse range of species and density of NPs. The observed effect can be defined as the ideal
notable theoretically specific capacities. However, the electrodes growth conditions for CoSe NPs at higher temperatures.[117]
made of the core metal selenide have certain drawbacks that hin- Moreover, the reduced dimensions of the NPs facilitate a reduced
der their effectiveness for storage purposes. These include lim- diffusion path for Li+ and enhance their electrical conductiv-
ited ion movement, insufficient electrical conductivity, and ity.[118] In addition, the lattice spacing of CoSe@NC NFs samples
significant volume expansion during charging and discharging. remained consistent at 0.26 nm, as shown in the high-resolution
To address these challenges, a range of techniques are utilized to TEM (HRTEM) images (Figure 8g–i). The energy-dispersive
optimize storage efficiency. Possible advancements in this field X-Ray spectroscopy (EDS) analysis of CoSe@NC-550 (Figure 8j)
encompass the incorporation of carbon-based materials, the reveals the existence of C, N, Co, and Se, as depicted in
creation of precise nanostructures, and the formation of Figure 8j1–j4.

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Figure 8. a–c) SEM images of CoSe@NCNFs composite electrodes for temperature (550, 650, and 750 °C); TEM images of d,g) CoSe@NCNFs-550;
e,h) CoSe@NCNFs-650 and f,i) CoSe@NCNFs-750; j–j.4) EDS images of CoSe@NCNFs-550; k–m) CV profiles of CoSe@NC composite electrodes for
temperature (550, 650 and 750 °C); n) Cycling performances of CoSe@NC. Reproduced with permission.[116] Copyright 2020, Elsevier.

Figure 8k–n illustrates the electrochemical responses of the This creates hollow structures and multiple channels in NMCFs
anode composite in LIBs. CV curves displaying similar redox and polymethylmethacrylate and styrene acrylonitrile copolymers.[121]
peaks were presented (Figure 8k–m). During the initial cycle, The flexible anode materials NCFs/MoSe2, NMCFs/MoSe2, and
three reduction peaks were observed at 1.2, 1.0, and 0.6 V. NHMCFs/MoSe2 were synthesized utilizing a straightforward
These peaks indicate the presence of various chemical reactions hydrothermal and annealing process, as shown in Figure 9b–d.
and transformations occurring within the material. The oxidation Figure 9e,g,i shows SEM images of NCFs, NMCFs, and
peak voltage measured at 1.2 and 2.1 V provides confirmation of NHMCFs. The CNFs exhibit a 3D interconnected network struc-
Li+ de-intercalation to CoSe.[119] In the second and third curves, ture, enabling uninterrupted electron flow for the electrode.
the injection of Li+ resulted in a decrease in peaks at 1.4 and NCFs, NMCFs, and NHMCFs have an average diameter of
0.6 V. The oxidation peak aligned with the initial CV curve, sug- 400, 500, and 600 nm. NMCFs and NHMCFs have rough surfa-
gesting the effective performance of CoSe@NC electrodes in ces with many grooves, while NCFs have smooth surfaces
LIBs during charge/discharge. Figure 8n shows the electrode (Figure 9f ). NMCFs and NHMCFs in Figure 9h,j have many
cycling performance. After 100 cycles at a current density of holes in their cross sections. NMCFs and NHMCFs have several
1 A g
1, CoSe@NC-550, CoSe@NC-650, and CoSe@NC-750 nanochannels, which reduce volume growth during charge–
attained specific reversible capacities of 796, 671, and 574 mAh g
1, discharge. Furthermore, it has been confirmed by researchers that
respectively. These findings indicate that CoSe@NC-550 has a NHMCFs possess a hollow and nanochannel structure. This
higher degree of reversibility. increases the surface area, both inside and outside, available for
In addition, ultrathin MoSe2 and three different structures of loading the active material MoSe2, resulting in enhanced power.
CNFs (CFs), such as N-doped CFs (NCFs), multi-nanochannel The study also found that NHMCFs have specific surface areas
CFs (NMCFs), and hollow NMCFs (NHMCFs) were used to that are 2.65 and 1.56 times greater than NCFs and NMCFs,
develop anode materials for high-performance LIBs.[120] Figure 9 respectively. NCFs have pores of small size, while NMCFs and
demonstrates the three-step synthesis techniques of flexible NHMCFs have mesoporous structures with sizes ranging from
anode materials: NCFs/MoSe2, NMCFs/MoSe2, and NHMCFs/ 8–15 to 25–48 nm, respectively. This feature increases the surface
MoSe2. In the very first phase, a piece of flexible membrane area of contact between the active material and electrolyte, making
was generated using an electrospinning technique shown in it easier for lithium-ions to move.
Figure 9a. The as-spun fibers were subsequently preoxidized Figure 9k shows the cycle performance of three designed elec-
in air and carbonized in N2, yielding CFs with a variety of archi- trodes at 1 A g
1. The NHMCFs/MoSe2 exhibit a significantly
tectures. When heated to high temperatures, polymethylmetha- higher initial discharge specific capacity of 743 mAh g
1, over
crylate and styrene acrylonitrile copolymers break down into gas. the values of 602.4 mAh g
1 for NMCFs and 554.6 mAh g
1 for

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Figure 9. a–d) Schematic illustration of the electrode fabrications process; e,f ) SEM images of NCFs; g,h) SEM images of NMCFs; i,j) SEM images of
NHMCFs; k) the cycle performance of hybrid electrode materials at a current density of 1 A g
1; l) the rate performance of hybrid electrode materials at
varying current densities. Reproduced with permission.[120] Copyright 2021, Elsevier.

NCFs. During the initial 35 charge–discharge cycles, the elec- structure, effectively manages the volume changes of MoSe2 and
trode materials become active, resulting in an increase in the enhances the transfer of Li-ions during cycling.
capacity of all three electrodes. The maximum capacities of Figure 9l shows an analysis of the rate capacity of three electro-
NHMCFs/MoSe2 were found 805.2, 704.9, and 683.2 mAh g
1. des, covering current densities from 1 to 10 A g
1. When current
NMCFs/MoSe2 and NCFs/MoSe2 lose significant capacity after density increases, the specific capacity of NCFs/MoSe2 decreases
35 charge–discharge cycles, but NHMCFs/MoSe2 lose slowly and significantly compared to NMCFs/MoSe2 and NHMCFs/MoSe2.
remain almost constant after 220 cycles. After undergoing This finding confirms that the presence of multi-nanochannels
400 cycles, NHMCFs/MoSe2 exhibit a reversible capacity of in NMCFs and NHMCFs can effectively enhance electrode rate per-
582.5 mAh g
1 and a capacity retention of 78.4%, exceeding the formance. During the initial rating test, NHMCFs/MoSe2 demon-
performance of NMCFs/MoSe2 (235.7 mAh g
1, 39.13% reten- strated reversible capacities of 666.4 at a current density of 1 A g
1.
tion) and NCFs/MoSe2 (165.9 mAh g
1, 29.91% retention). In However, as the current density increased, the reversible capacities
addition, NHMCFs/MoSe2 electrodes exhibit excellent cycle stabil- decreased. At 10 A g
1, it exhibited reversible capacities of
ity, high CE, and reversible capacity, as a result of their structural 244.3 mAh g
1. Figure 9l demonstrates superior capacities com-
advantages. The NHMCFs/MoSe2 material exhibits a 3D hollow pared to the NCFs/MoSe2 and NMCFs/MoSe2 electrodes. After
structure composed of multiple nanochannels, resulting in a high undergoing 180 cycles of different current density testing,
surface area and excellent electrical conductivity. Additionally, the the NHMCFs/MoSe2 electrode has a remarkable capacity of
presence of perpendicular MoSe2 nanosheets on both the inner 570.7 mAh g
1 when the current density reaches 1 A g
1. The
and outer surfaces of NHMCFs enhances the number of active lith- results indicate that the NHMCFs/MoSe2 electrode has remarkable
ium-ion sites available for lithiation/delithiation processes. The rate capability as a result of its substantial specific surface area and
NHMCFs/MoSe2 electrode, with its hollow and multi-nanochannel distinctive hollow and multi-nanochannel structure of NHMCFs.

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In their study, Ni et al.[120] utilized the electrospinning efficacy of electrodes comprising carbon and metal sulfide in
approach to develop N-doped 3D flexible networks utilizing three LIB. Within the scope of our review, we reviewed a study by
distinct types of CNFs (CFs) such as NCFs, multi-nanochannel Dong et al.[130] that investigated the incorporation of CoS into
CFs (NMCFs), and hollow MNCFs (NHMCFs). In addition, they anionic N,S-dual-doped porous CNFs (CoS-NS-PCNFs) electro-
used a hydrothermal technique to vertically grow ultrathin MoSe2 des for LIBs. A high specific capacity was shown by the uniformly
nanosheets on both the inner and outer surfaces of the distributed CoS NPs. The CNFs also physically buffered the CoS
NHMCFs. The study’s findings suggest that the loading mass of NPs, so they couldn't swell to their full potential. The efficiency of
MoSe2 in hollow CFs can reach a substantially higher value of ultrafast cycling was improved by incorporating N and S atoms
71.55% compared to ordinary CFs. The NHMCFs/MoSe2 anode into the hollow structure, resulting in an enhanced ion-electron
demonstrates a remarkable capacity of 586.7 mAh g
1 after transfer rate. Figure 11a–h displayed the morphological charac-
400 cycles at 1 A g
1, indicating significant potential for use in teristics of newly developed hybrid electrode materials using low
LIBs. Additionally, the hollow structure of the MSe anode enhan- and high-magnification FESEM images, along with correspond-
ces its capacity for lithium storage. ing schematics. The size of the CoS2 particles ranged from ≈74.8
to 123.6 nm, and they exhibited a sphere-like form, as shown in
3.4. Transition Metal Dichalcogenides (TMDs) Figure 11a,e,i. Additionally, they found that the diameter ranges
for CoS2-CNF were ≈255.9–308.8 nm, and for CoS-NS-CNF, they
TMDs, inorganic compounds that possess the structural formula ranged from 198.5 to 238.6 nm. Similarly, CoS-NS-PCNF exhib-
MX2 (where M represents a transition metal and X denotes a ited a diameter range of 184.0–229.1 nm. The study also indi-
chalcogen), have garnered interest as anode materials for LIBs cated that networks with connected topologies facilitated the
owing to their remarkable physical, chemical, electrical, and movement of charge, particularly between ions and electrons
two-dimensional capabilities.[122] 2D TMDs are atomic-layered during cycling Figure 10b–d. Furthermore, the distribution of
binary compounds, including MoS2, WS2, MoSe2, and WSe2, CoS NPs within the CNFs was more uniform in the CoS-NS-
where van der Waals forces interconnect the individual sheets CNF and CoS-NS-PCNF samples, as compared to the CoS2-
in a layer-by-layer arrangement (Figure 10), but the atoms inside CNF sample when the cysteine polymer was not present.
the layers are held together by robust covalent bonds.[123–125] The In general, CoS NPs tend to aggregate due to their inherent
sandwich structure and increased interlayer spacing (≈0.65 nm) instability and high surface energy. However, when cysteine
facilitate the efficient diffusion of Li+ ions, which is crucial for an polymer was introduced to CoS-NS-CNF and CoS-NS-PCNF, it
anode material to accommodate Li+ ions at an accelerated rate. helped to enhance the dispersion of CoS NPs in carbon by
MoS2 and WS2, capable of inserting 4 mol of Li+ ions through the lowering their surface energy.[131] Figure 10g,k shows that the
charging–discharging process, frequently surpass their theoreti- surface of the CoS-NS-CNF is smooth, while Figure 11h–l dem-
cal capacities of 670 and 433 mAh g
1, respectively.[122,126,127] onstrates that the CoS-NS-PCNF has an uneven surface with
Lower electrical conductivity and unstable structure during bat- mesopores. The carbonization process led to the decrease and
tery cycling, coupled with inadequate rate performance and cycle evaporation of the ZnO particles, ultimately resulting in the
stability, hinder their practical deployment. Nonetheless, MoSe2 observed roughness.[132] In addition, according to the results, the
and WSe2 exhibit enhanced efficiency because to the superior presence of CoS NPs in CNFs was supported by weight reductions
electrical conductivity of Di selenide compared to sulfide of 33.5%, 33.8%, and 34.7% in the CoS2-CNF, CoS-NS-CNF, and
atoms.[128,129] Furthermore, TMDs nanosheets/nanoflakes CoS-NS-PCNF, respectively. With its distinctive mesoporous
enhance the diffusion paths for Li+ ions and provide additional structure, CoS-NS-PCNF boasts a well-distributed arrangement of
sites for ion storage and rapid electron transport due to their CoS NPs within the PCNFs. This design offers a multitude of
extensive surface area and broader interlayer spacing. These active sites and a reduced ion diffusion route, resulting in enhanced
exceptional qualities can be further augmented by integrating cycling performance with remarkable speed.
them into a 3D nanostructure. Over 100 cycles at 100 mA g
1 in the voltage range of
With these features, the combination of highly reactive carbon 0.05–3.0 V (vs Li/Li+), Figure 10m indicates the long-term stabil-
materials and active NPs shows great potential for increasing ity of charge/discharge performance. With a particular discharge
capacity and improving electrochemical feasibility. In Table 5, capacity of only 271.2 mAh g
1 and a capacity retention rate of
a succinct summary is presented regarding the electrochemical 36.1%, commercial CoS2 was shown to have poor cycling stability

Figure 10. van der Waals heterostructures for lithium intercalation. Reproduced with permission.[123] Copyright 2018, Springer Nature Limited.

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Table 5. Electrochemical performance of carbon materials/metal sulfide composite materials in LIB anodes.

Anode material Applied methods Reversible capacity Current density Cycle number References
[mAh g
1] [mA g
1]
WS2–CNF Tip-sonication þ Electrospinning 814 100 120 [276]
MoS2@FexOy@CNF Single nozzle-based electrospinning 723 500 300 [277]
MoS2/C Centrifugal spinning 250 100 100 [278]
TiS2/C Force spinning 250 50 100 [247]
SnS2/CNT sponge Solvothermal 502 100 100 [261]
MoS2@CNFs Tip-sonication þ Solution mixing 862.3 200 100 [279]
CoS-NS dual doped CNFs Electrospinning þ carbonization 748.6 100 100 [130]
In2S3/C Electrospinning 696.4 50 100 [136]
FeS2/WS2-CNFs Electrospinning þ sulfuration þ hydrothermal 422.6 500 500 [280]
MoS2@N-doped CNFs Electrospinning þ hydrothermal 1031.7 5000 1000 [137]
SnS/CNFs Electrospinning 548 500 500 [281]
Liquid metal coated CS fibers Facile coaxial electrospinning 603.9 1000 1500 [282]
MoS2–SnO2@CNF Solvothermal þ electrospinning 463 500 100 [283]
MoS2/C/CNFs Electrospinning þ hydrothermal 1275 200 150 [76]
MnS@MXene@CNFs Electrospinning 500 1000 1000 [284]
PCNF@MoS2 Hydrothermal 1255.8 100 450 [75]
Co1
xS/multichannel-CNFs In situ þ solution mixing 813 100 180 [285]

in the test. As a result of significant volume expansion, the capac- In a study, Yuan et al. developed In2S3/CNFs as anode mate-
ity diminished rapidly, leading to poor performance.[133] rials for high-performance LIBs through the processes of electro-
Therefore, incorporating carbon into CoS is needed for effec- spinning and thermal treatment. The anode exhibits exceptional
tively reducing volume expansion. Because of its distinct charac- lithium storage characteristics, such as a high capacity, extended
teristics, CoS-NS-PCNF had a greater specific capacity cycle life, and favorable rate performance. After undergoing 100
(748.6 mAh g
1) and superior retention (96.5%). This could be cycles at a current density of 50 mA g
1, the electrode composed
due to PCNF’s better CoS NP dispersion. of In2S3/CNFs demonstrated a capacity retention of 95.1% in
The cycling stability experiments of CoS2, CoS2-CNF, and LIBs. Furthermore, the In2S3/CNF electrode retains 80.5%
CoS-NS-CNF resulted in 60.5, 140.7, and 220.2 at a high current capacity after 600 cycles in LIBs at 1000 mA g
1. The superior
density of 2000 mA g
1 over 500 cycles, respectively, as shown in electrochemical behavior of In2S3/CNFs is mainly attributed
Figure 11o. The CoS-NS-PCNF electrode showed exceptional to the carbon encapsulation process, which effectively improves
cycling performance, maintaining a specific capacity of conductivity and minimizes the volume expansion resulting
514.6 mAh g
1 and retaining 93.5% of its capacity after 500 from the alloying reaction. The LIBs chemical reaction mecha-
cycles at a current density of 2000 mA g
1. Figure 11n illustrates nism comprises both the conversion and alloying reactions.
the rate performance for a range of current densities, from 100 to The highest theoretical specific capacity of In2S3 in LIBs was cal-
2000 mA g
1. Based on the rate performance figure, we observed culated to be 1205 mAh g
1. The researchers anticipate that the
a significant decrease in the specific capacity of commercial clarified Li/Na storage mechanism will accelerate the develop-
CoS2. In contrast, CoS-containing carbon exhibited a signifi- ment of In2S3 in the electrochemical energy storage area.[136]
cantly higher specific capacity. The low-rate performance of Ni et al.[137] employed a straightforward electrospinning and
CoS2-CNF can be attributed to the agglomerated CoS NPs within hydrothermal synthesis technique (Figure 12a) to fabricate a
the CNFs. However, CoS-NS-CNF and CoS-NS-PCNF demon- self-contained NCNFs/MoS2 hybrid composite. Notably, this
strate higher specific capacities in comparison to CoS2 and composite exhibited enhanced interlayer spacing for the anode.
CoS2-CNF. This can be attributed to the well-distributed CoS The structural characteristics of the NCNFs and NCNFs/MoS2
NPs in the N,S-dual-doped carbon. This distribution prevents vol- hybrid composite electrodes were examined using FESEM, as
ume expansion and enhances electric conductivity. The CoS-NS- shown in Figure 11b–e. Obviously, NCNFs (Figure 12b) and
PCNF electrode demonstrated excellent rate performance, NCNFs/MoS2 (Figure 12d) have unique 3D network morpholo-
achieving a range of 822.1–550.4 mAh g
1 across current densi- gies. Hybrid composites possess a 3D structure that reduces the
ties ranging from 100 to 2000 mA g
1. The experimental find- length of Li-ion diffusion channels and enhances the speed of
ings indicate that the mesoporous structure and anion dual electron transport during charge–discharge cycles.[138] The
doping of PCNFs effectively enhance the transport of Li ions surface of NCNFs exhibits a smooth texture, with an average
and facilitate electron transfer, resulting in enhanced electro- diameter of 300 nm, as depicted in Figure 12c. Furthermore,
chemical performance.[134,135] homogeneous MoS2 nanoflowers with a size of 100 nm were

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Figure 11. a–d) Low-resolution FESEM and e–h) high-resolution FESEM images, and i–l) schematic presentation of developed electrodes CoS2, CoS2-
CNF, CoS-N,S-dual doped-CNF, and CoS-NS-dual doped Porous CNF; m) cycling performance at current density of 100 mA g
1 following 100 cycles,
n) rate performance of electrodes at 100–2000 mA g
1; o) ultrafast cycling stability following at 2000 mA g
1 up to 500 cycles. Reproduced with
permission.[130] Copyright 2020, Elsevier.

observed on the outer layer of NCNFs, as shown in Figure 12e. of commercially available MoS2, which measures 0.62 nm. Based
The compact and homogeneous growth of MoS2 nanoflowers on on the chemical maps depicted in Figure 12h–l, it is evident that
NCNFs facilitates electrolyte/electrode interaction and prevents the MoS2 flowers exhibit a uniform distribution within the
agglomeration during the charge–discharge cycle.[139–141] The MoS2/NCNFs electrodes. Additionally, the resulting CNFs dem-
microstructure of the composite was analyzed using TEM images onstrate a properly proportioned hybridization with N. The inclu-
(Figure 12f ). The images reveal a uniform distribution of MoS2 sion of a uniform N-doped carbon in NCNFs/MoS2 in LIBs has
on the surface of NCNFs. These MoS2 nanoflowers are open-type the potential to decrease charge transfer resistance and improve
constructions made up of nanosheets (Figure 12f ). The porous conductivity, thereby bolstering the electrochemical properties of
nature of the MoS2 nanoflower facilitates the passage of ions, the system.[142]
reducing diffusion resistance and promoting better contact Figure 12m depicts the cycling results of the NCNFs/MoS2
between the electrode and electrolyte. The MoS2 nanoflowers and MoS2 electrodes at current densities of 5 and 10 A g
1,
exhibit a layer spacing ranging from 0.85 to 1.0 nm, as depicted respectively. After 1000 cycles, the discharge capacity of NCNFs/
in Figure 12g. This layer spacing is significantly greater than that MoS2 remains stable at 1031.7 mAh g
1, demonstrating an

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Figure 12. a) Schematic presentation for synthesis methods of MoS2 electrode materials; SEM views of: b,c) NCNFs and d,e) NCNFs/MoS2 composite
materials; f,g) TEM and HRTEM of NCNFs/MoS2 ; h–l) elemental mapping (C, N, S and Mo) of NCNFs/MoS2 ; m) cycle performance of the NCNFs/
MoS2 at current density of 5 and 10 A g
1; n) charge voltage profiles of freestanding NCNFs/MoS2 electrodes. Reproduced with permission.[137] Copyright
2020, Elsevier.

impressive capacity retention of 94.49% at 5 A g
1. After under- (Figure 12n) to uncover the underlying mechanism at work. The
going 1000 cycles with a current density of 10 A g
1, the capacity rise in charge capacity was divided into three stages: 0.01–1.2,
remains consistently high at 723.5 mAh g
1. When functioning 1.2–2.5, and 2.5–3 V, as analyzed by the CV curve. Polymeric
at current densities of 5 and 10 A g
1, the first-cycle efficiency gel-like films (PGF) is formed at low potentials, Mo is oxidized
can reach up to 76.2% and 79.6%, respectively. Due to their supe- to Mo4+/Mo6+, LiS2 is oxidized to sulfur or polysulfides, and PGF
rior structure, freestanding composites of NCNFs/MoS2 exhibit a grows at high potentials.[144,145] ΔC1, ΔC2, and ΔC3 represent the
high current density, resulting in a high reversible capacity and charge capacity difference between the 150th and 10th cycles
CE. Initially, NCNFs establish a network that allows for efficient with voltages of 1.2, 2.3, and 3 V. The significant positive values
movement of electrons between electrodes. In addition, the of ΔC1 (55 mAh g
1) and ΔC3 (155.6 mAh g
1) clearly show that
inclusion of perpendicular MoS2 nanoflowers on NCNFs PGF production and growth have the greatest influence on
increases the quantity of active sites which assists in the cluster- charge capacity.
ing of MoS2 during the charge and discharge process. The inter- Furthermore, we investigated a hybrid electrode made of
layer spacing of the MoS2 nanoflowers is increased, which in double-layer carbon-coated MoS2 and CNF, which was effectively
turn enhances the surface area for Li-ion interaction. This ulti- fabricated utilizing a simple hydrothermal and electrospinning
mately reduces barriers during the lithiation and delithiation process. Based on the study, the use of double-layer carbon (inner
processes.[140,143] amorphous carbon layers with outer CNFs layers) shells in this
The capacity of the NCNFs/MoS2 hybrid composite anode case has been found to be highly effective. The addition of these
materials exhibits a substantial increase within the initial layers improves the mobility of electrons, prevents the agglom-
150 charge/discharge cycles, which hold utmost significance. eration of MoS2 flakes, and helps to minimize changes in volume
Scientists have stated that the increase in capacity can be and loss of polysulfides during long periods of cycling. The devel-
explained by the formation and expansion of gel-like films, oped MoS2/C/C fiber electrode displayed an impressive capacity
mostly caused through electrolyte decomposition. To gain a com- of 1275 mAh g
1 during a current density of 0.2 A g
1. It also
prehensive understanding of the capacity increase during the ini- demonstrated an 85.0% first-cycle CE, along with enhanced rate
tial 150 cycles, we conducted an analysis of the CV profiles capability and cycling stability.[76] In addition, Zhang et al.

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proposed a multistep process for producing hierarchically struc- Peng et al.[150] has demonstrated significant advancements in the
tured polyacrylonitrile–metal–organic framework (PAN-MOF)- fabrication of a series of porous two-dimensional holey MTMO
derived porous CNF@MoS2 fibers. The template effect of nanosheets. This was achieved through the utilization of GO as
PCNFs was demonstrated by the uniform vertical assembly of sacrificial templates, allowing for the precise control of pore sizes.
ultrathin MoS2 nanoplates on their surfaces. Proper precursor This work presents a comprehensive two-step methodology for the
content resulted in minimal restacking of the nanoplates. controlled synthesis of holey 2D MTMO nanosheets, featuring
PCNF@MoS2 demonstrated improved cycle and rate perfor- adjustable pore sizes. The process utilizes GO as a sacrificial tem-
mance as an anode material in LIBs, highlighting the benefits plate, as illustrated in Figure 13. This method has been shown to
of employing PAN-MOF-derived 1D composites for semiconduc- effectively synthesis a range of 2D holey MTMO nanosheets. This
tor development platforms. It is important to mention that elec- includes both simple oxides, such as Fe2O3, Co3O4, and Mn2O3, as
trospinning is a significant part of flexible energy storage well as mixed oxides like ZnMn2O4 (ZMO), ZnCo2O4 (ZCO),
systems.[75] Another promising transition metal sulfide is anti- NiCo2O4 (NCO), and CoFe2O4 (CFO). Consequently, 2D holey
mony trisulfide (Sb2S3), which is a promising electrode material MTMO nanosheets demonstrate significantly enhanced rate capa-
with properties such as stability, low cost, and high specific bility and cycling stability for lithium and sodium ion storage. This
capacity, but it cannot be commercialized due to insufficient elec- improvement is attributed to the increased surface areas and inter-
tronic conductivity and significant volume change during dis- faces, along with efficient interfacial interactions. Scanning trans-
charge cycles. Additionally found another research of Yin mission electron microscopy (STEM) images of ZnMn2O4
et al. synthesized hybrid anode materials from N-doped Sb2S3 precursor/rGO and 2D holey ZMO nanosheets with intercon-
(NSS) and CFs using one-step eco-friendly electrospinning nected ZnMn2O4 nanocrystals are presented in Figure 13b,c.
and vacuum heating techniques, that could effectively increase The synthesized 2D holey ZnMn2O4 nanosheets demonstrated
atom use while reducing environmental pollution. The atom uti- a remarkable rate performance of 770 mAh g
1 at 200 mA g
1
lization of the NSSC source is close to 100%. The composites and an impressive capacity of 430 mAh g
1, achieving 56% capac-
made from NSSC exhibited a capacity of 490.3 mAh g
1 when ity retention at current density 1200 mA g
1. In contrast, the con-
exposed to a current density of 100 mA g
1 for a duration of trol spinel ZnMn2O4 exhibited only 32% and 6% capacity
1000 cycles. After 200 cycles, the cell’s capacity remained constant retention, respectively.[151]
at 600 mAh g
1 with a current rate of 0.5 C. This study introduces a The objective of the study was to encompass TMOs with vari-
thorough environmentally-friendly approach for sulfides, which has ous carbon materials, such as porous carbon, bio-mass-derived
the potential to support the advancement of various metal sulfides carbon, graphene carbon, and MXene carbon-based composites.
and metal selenides with efficient atom utilization and minimal We addressed the limited conductivity and volume expansion
waste.[146] issues associated with individual metal oxides. The materials
are currently being studied for their potential use as anode mate-
rials in LIBs.[74] Table 6 presents the electrochemical perfor-
3.5. CF/TMOs Composites
mance of various carbon-based transition materials in LIBs
anode applications.
TMOs materials, including Co3O4, NiO, Fe3O4, and MnO2, are
extensively studied as lithium-ion anodes due to their impressive
theoretical capacities (700–1200 mAh g
1) and comparatively 3.5.1. Iron Oxide
high-power density. However, TMOs run into various chal-
lenges: significant volume fluctuations, pulverization and clus- Fe3O4 has been thoroughly investigated as a promising candidate
tering of primary particles, and their insignificant electronic because of its affordable cost, environmentally friendly produc-
conductivities, which impede electrochemical reactions and tion methods, and impressive theoretical specific capacity of
result in restricted battery capacity. To overcome these chal- 924 mAh g
1.[152] Only the Fe3O4 anode exhibited structural deg-
lenges, metal oxides are developed into nanostructures with vary- radation. The lithiation/delithiation reaction caused a significant
ing dimensions, including the design of hollow and hierarchical volume change (93%) in Fe3O4, leading to rapid capacity attenu-
structures, coatings, or through the integration of conductive ation. As a result, it was not possible to establish an electrical
buffer materials (e.g., CNTs and graphene nanosheets) with joint between the anode material and current collectors.[153,154]
TMOs.[122,147–149] This study introduced an eco-friendly anode material derived
Recently, mixed-TMOs (MTMOs), which are ternary metal from green microalgae, thereby enhancing environmental sus-
oxides containing two distinct metal cations, have garnered tainability. The main steps in preparing α-Fe2O3@nitrogen-
increased interest as potential anode candidates. This is attrib- doped carbon (NC) anode materials for LIBs are illustrated in
uted to their mixed valence states and multiredox reactions, Figure 14a.[155] This innovative method presents promising
enhanced electrical conductivities resulting from lower activation opportunities for using green microalgae and enhancing the
energy for electron transfer between cations, and superior alloy- utilization of biotemplating and spray pyrolysis techniques to
ing capabilities with lithium ions when compared to physically generate electrochemically viable components for LIB anodes.
mixed and single metal ion oxides. Due to the benefits associated Figure 14b,c illustrates the microspheres of α-Fe2O3@NC com-
with 2D nanostructures, 2D holey MTMO nanosheets exhibiting posites, which exhibit a uniform form and particle sizes ranging
adjustable porosity and intrinsic mechanical stability are from 200 to 500 nm. The TEM image (Figure 14d) illustrates a
regarded as potential anode candidates for various emerging composite material composed of porous α-Fe2O3@NC and voids.
applications in energy storage. Recent research conducted by The TEM result, as shown in Figure 14e, displays distinct lattice

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Figure 13. a) Schematic illustrating the primary technique for synthesizing 2D holey TMOs nanosheets. Two transition metal cations are combined with
GO and subsequently affixed to the surfaces of rGO templates during a solution-phase process. 2D holey MTMO nanosheets, consisting of linked MTMO
nanocrystals, are generated following the removal of rGO templates during postcalcination. b) STEM image of ZMO precursor/rGO shows sheets-like
morphology. c) STEM image of 2D holey ZMO nanosheets shows holey nanosheets composed of interconnected ZMO nanocrystals. Reproduced under
the terms of the CC BY 4.0 license.[150] Copyright 2017, The Authors. Published by Springer Nature.

fringes with a spacing of 0.37 nm. This indicates the presence of carbon, and Fe2O3 improves the anode performances.
the (012) plane of α-Fe2O3 in the powder of α-Fe2O3@NC hybrid N-doping enhances electrochemical properties and increases
composites.[156] active sites, resulting in improved cycling performance, leading
In Figure 14j, the rate performance of α-Fe2O3@NC and to improved electrode performances. Microalgae serve as car-
bare α-Fe2O3 anodes was investigated over a current density bon support materials that possess exceptional electrical con-
(200–1000 mA g
1). Following 10 cycles, the α-Fe2O3@NC elec- ductivity and mesoporous properties. These qualities
trodes demonstrated a specific capacity of 843.6 mAh g
1 when contribute to improved electrochemical performance and aid
exposed to a current density of 1000 mA g
1. The aforemen- in the expansion of buffer volume during Li+ charge/discharge
tioned impressive capability is ≈3.6 times higher than that of reactions.
pure α-Fe2O3, with a value of 231.9 mAh g
1. When the current Combining nanostructured ZnFe2O4 with a flexible and con-
density was increased again to 200 mA g
1, the capacity quickly ductive carbon support framework is a highly effective method
returned to 954.9 mAh g
1. The α-Fe2O3@NC composite elec- for improving the electrical conductivity and structural stability
trode showed a marginal improvement in efficiency when of ZnFe2O4 electrodes. In accordance with the aforementioned
exposed to low current densities of 400 and 600 mA g
1. The effects, Tan et al.[158] employed a two-step procedure to create
observed outcome may be ascribed to the enhanced accessibility a three-dimensional porous ZnFe2O4/rGO electrode. The
of Li+ ions during cycling, facilitated by the hybrid structure.[157] α-Fe2O3ZnO/rGO composite was subjected to a 2 h thermal
Figure 14k depicts the discharge capacity of α-Fe2O3@NC and treatment at 500 °C in an argon environment using a tube fur-
pure α-Fe2O3 composites at a current density of 1000 mA g
1 nace. The anode is composed of ZnFe2O4, and rGO exhibits
over a specified duration. Following 100 cycles, the battery exhib- remarkable cycling stability and a high specific capacity.
ited a consistent current density of 603.8 mA g
1, indicating a Figure 12f displays the FESEM image of the ZnFe2O4/rGO
state of stability. The cycling CE of the α-Fe2O3@NC electrodes electrode, demonstrating that the ZnFe2O4/rGO composite
is high. The CE in the initial cycle is 70% and remains at 99% maintains a substantial level of structural integrity.
for the subsequent 20 cycles. The high CE indicates the possi- Furthermore, the rGO layers exhibit the ability to detect the
bility of reversible Li-ion insertion/extraction in α-Fe2O3@NC enclosed ZnFe2O4 NPs. The HRTEM analysis of the sample
hybrid composite electrodes. The incorporation of N-dopants, in Figure 12g reveals the presence of nanocrystals with diverse

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Table 6. The electrochemical performance of various carbon-based transition materials in LIBs anode applications.

Anode material Fabrication methods Reversible capacity Current density Cycle References
[mAh g
1] [mA g
1] number
Bimetal Se@N-CNFs Electrospinning þ selenization 826.1 1000 300 [286]
FeCo@N-doped CNFs Electrospinning þ thermal treatment 566.5 100 100 [287]
Fe3O4/C Force spinning þ carbonization 300 100 100 [288]
Fe3O4/C Solution combustion 470 100 100 [289]
Fe3O4/Fe3C/TiO2/C Dry-spinning method 702.1 100 400 [290]
GNSs/Fe3O4 Freeze drying þ solvothermal 1145 100 120 [291]
Fe2O3/SWCNT Floating catalyst CVD 1243 50 90 [292]
Fe3O4@Porous rGO Redox deposition 2136 500 100 [293]
Fe3O4@Bacterial Cellulose-CNFs Freeze-drying þ hydrothermal reaction 755 100 80 [294]
3D Graphene/Fe2O3 Ostwald ripening methods þ thermal treatment 1129 200 130 [295]
C/Fe3O4/rGO Solvothermal 832 200 300 [296]
ZnO/C Sol–gel þ calcination processes 790 100 100 [297]
CC@ZnO/N-doped C@Li In situ þ electrodepositing 135 372 400 [298]
MgZnO NPs/CNF In situ þ electrospinning 87 100 600 [299]
N-doped hollow CF/CNS/ZnO Electrospinning 153 186 500 [300]
ZnCo2O4/rGO Hydrothermal þ calcination 1203 100 70 [301]
Self-assembled ZnO/rGO Standard Schlenk line techniques >700 500 100 [302]
SnOx–ZnO/CNFs Electrospinning þ annealing 963 100 55 [303]
ZnO/ZnS@N-doped C/CNTs Molecular assisted 1020.6 100 200 [304]
ZnO/H-rGO In situ etching method 942 200 400 [305]
CoO/ZnO-N-doped rGO Solvothermal þ freeze-drying 600 2000 1000 [306]
Mo2C NPs@CCn Infiltration þ coprecipitation method 158 161 500 [307]
Li-Oxidized PAN fibers/ZIF-8@Cu In situ þ electrospinning 140.8 186 120 [308]
Al2O3 coated graphite Sol–gel 337.1 100 100 [309]
CoO@CC-Li Thermal infusion 121 100 500 [310]
Co3Sn2@Co-NG Hydrothermal 1615 250 100 [311]
Co3O4 nanoplates/rGO Hydrothermal þ thermal treatment 1566.5 1000 150 [312]
Sb/C Electrospinning þ carbonization 315.9 100 100 [313]
Peapod-shaped V2O3 NRs/CNTs Hydrothermal 186 100 125 [314]
MnO2 nanowires/MWCNTs Hydrothermal 350 100 100 [315]
MnO NPs/CNFs Electrospinning þ thermal carbonization 987.3 100 150 [316]
MnO nanocrystals/CNFs Electrospinning þ carbonization 778 123 90 [317]
Sn NPs/CNFs Electrospinning þ heat treatment 580 200 200 [318]
PCNFs@MoS2 NSs Electrospinning þ solvothermal reaction 690 50 50 [319]
SnO2/N-doped CNFs Electrospinning þ carbonization 754 1000 300 [320]
CuO NSs/rGO Vacuum filtration þ hydrothermal reduction 736.8 67 50 [321]
TiO2–grapheme Dipping þ hydrothermal 157 200 100 [322]
TiO2 QDs@C@ZnO Atomic deposition þ hydrothermal 1154 200 100 [323]
TiO2@SnO2@C Sol–gel coatings þ hydrothermal 484 200 300 [324]
TiO2/C Force spinning þ thermal treatment 228.9 100 100 [241]
TiO2/GA Template-free method 663.2 100 250 [325]
GE@Cu/TiO2 Electrochemical anodization process 223 200 50 [326]
TiO2/rGO-P Sol–gel method þ thermal treatment 291 100 100 [327]
MoO3–NiO @C Citric-assisted hydrothermal self-assembly process 944 100 2000 [328]
Co3O4 nanopore arrays/rGO/Ni foam Modified hummer’s 700 100 400 [329]
NiO@N-doped C NSs Hydrothermal synthesis 1036 50 30 [330]

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Table 6. Continued.

Anode material Fabrication methods Reversible capacity Current density Cycle References
[mAh g
1] [mA g
1] number
SnO2/NiO/C Scalable þ carbonization 633 400 100 [331]
NiO@Co3O4@GQDs Solvothermal treatment 1158 100 250 [332]
CNFs@NiS NPs Electrospinning þ thermal calcination 1149.4 100 100 [333]
NiO/rGO In situ ultrasonic agitation 825 100 50 [334]
NiO/Fe3O4/rGO Solvothermal route 647 500 200 [335]
N-doped MnO/rGO Hydrothermal þ calcination 1020 200 150 [336]
MnO/C Hydrodynamic induction 845 1500 100 [337]
MnO-graphene Hydrothermal 1185 50 500 [338]
MnO@N-doped C Hydrothermal þ In situ polymerization 784 500 200 [339]
MnO@C hollow nanospheres Hydrothermal 839 1000 900 [340]
MnO/C@rGO Solvothermal 1536.4 100 100 [341]
MnO@S, N-dual doped C One-step pyrolysis 955.5 500 500 [342]
MnO/Mn3O4/N-doped Graphene Laser-inducing process þ In situ 992 200 400 [343]

Figure 14. a) Schematic presentation of the synthesis of α-Fe2O3@NC electrodes; b,c) SEM images of the α-Fe2O3@NC electrodes; d,e) TEM images of
the α-Fe2O3@NC electrodes; j) rate performance of α-Fe2O3 and α-Fe2O3@NC electrodes, and k) cycling performance (discharge capacity). Reproduced
with permission.[155] Copyright 2019, Elsevier. f ) The FESEM images and g) the HRTEM images of ZnFe2O4/rGO composites; h) cycling performance of
ZnFe2O4/rGO composite anode at the current rate of 1 A g
1; i) cycling performance of ZnFe2O4/rGO, γ-Fe2O3@ZnO/RGO, and ZnO/RGO composite
anode. Reproduced with permission.[158] Copyright 2020, Elsevier.

lattice fringes. During the initial cycling, the larger ZnFe2O4 crys- According to Figure 14h, the electrodes’ cycle performance
tals undergo a transformation into smaller ZnO and Fe2O3 par- remains consistent after 500 cycles at 1.0 A g
1, exhibiting a
ticles. The nanocrystals exhibit multiple voids, which are easily reversible capacity of ≈1022 mAh g
1. The newly developed
discernible through yellow dash outlines. The voids observed can ZnFe2O4/rGO anode exhibits an initial discharge capacity of
be attributed to the successful immobilization achieved by the ≈1939 mAh g
1 and a charge capacity of ≈1285 mAh g
1 after
rGO structure. 300 cycles. This would result in a significant reduction in initial

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capacity, reaching up to 33.7%. We evaluated the cycle stabilities before it. To improve the electrochemical properties, the synthesis
of three electrode materials for the first 100 cycles using the iden- of composite materials called CFO@rGO involved the use of GO.
tical procedure, as depicted in the figure labeled Figure 14i, The layered 3D structure enables the efficient movement of Li+
which illustrates the composite electrode’s CE, which is ions and reduces changes in volume, resulting in improved cycle
≈66.5%. The material demonstrates a notable initial specific stability. The structural benefits of CFO@rGO lead to improved
charge capacity of 1410 mAh g
1 with an initial discharge capac- electrochemical characteristics for lithium-ion anodes, including
ity of upward of 1971 mAh g
1. After 20 cycles, the reversible better rate performance, higher specific capacity, and enhanced
capacity exhibits a marginal decrease to 1080 mAh g
1. After cycle stability. Following 100 cycles at a current density of
100 cycles, the current density slightly increases to 1282 mAh g
1. 100 mA g
1, the anode materials demonstrated a significant spe-
At different current densities, the ZnFe2O4/rGO sample demon- cific capacity of 933.1 mAh g
1.
strates varying reversible capacities. The ZnFe2O4/rGO material
exhibits a remarkable reversible capacity of ≈1022 mAh g
1 after 3.5.2. Cerium Dioxide
500 continuous cycles, highlighting its exceptional storage
performance. This study reviewed the unique structure of N-doped CF(NCF)
Another research effort utilized electrospinning and thermal hollow spheres containing cerium oxide (CeO2) (CeO2@NCF).
treatment to synthesize Fe3O4 NPs, which were then encapsu- The objective of this study was to create a robust interface
lated in porous carbon fibers (PCFs) to create Fe3O4@PCFs between the electrolyte and anode, which would lead to a longer
anode materials. The Fe3O4@PS/PAN composite precursor fibers battery life. The evaluated anode materials exhibited remarkable
are synthesized by combining a solution containing PAN and poly- performance. The implementation of a flexible framework effec-
styrene (PS) with Fe3O4 NPs. When PS and PAN undergo thermal tively mitigated the volume expansion of CeO2, thereby maintain-
breakdown, they form Fe3O4/carbon hybrid fibers that possess a ing the electrode’s structural integrity throughout the charging
porous structure. These fibers consist of an extremely strong car- and discharging processes. The utilization of one-dimensional
bon shell that wraps a carbon core with a unique honeycomb struc- conductive nanofiber improved electron supply efficiency by
ture including Fe3O4. When operating at 0.2 A g
1, the Fe3O4@PCF minimizing the electron’s movement path, facilitating rapid
anode possesses a reversible capacity of 1015 mAh g
1. It retains redox reactions. CeO2 hollow configuration enhances electrolyte
84.4% of its initial capacity after 80 cycles of operation. penetration, boosts Li-ion diffusion kinetics, and enhances Li
Additionally, this anode exhibits exceptional rate performance, as storage at a high current density. The integration of NCF and
the current density rises from 0.1 to 2.0 A g
1. Furthermore, it CeO2 led to improved discharge-specific capacity, advanced rate
sustains a capacity of 91% after undergoing 200 cycles at a cur- capability, and remarkable cycling stability in LIBs. Furthermore,
rent density of 2.0 A g
1. CFs possess excellent electrical conduc- the research demonstrates a clear correlation between pseudoca-
tivity and retain their structural integrity consistently. The pacitive and electrochemical properties.[166]
unique design of these buildings allows them to easily adjust
to changes in the volume of Fe3O4 inside. In addition, they serve
as efficient routes for the transportation of Li-ions and electrons, 3.5.3. Lithium Vanadate
resulting in a substantial improvement in the overall perfor-
mance of the anodes.[159] In a separate study, Park et al.[160] Amorphous lithium vanadate (LiV3Ox) is another TMO that has
employed a microalgae template spray drying technique to develop been effectively employed in the advancement of negative elec-
multilayer porous Fe3O4/C interconnected microspheres. The trodes for LIBs. Li et al. conducted a study where they utilized
microspheres were subsequently employed as anode materials electrospinning and postannealing techniques to create hybrid
in LIBs. Fe3O4/C composite microspheres exhibit improved elec- anodes of LiV3Ox and CNFs. The anode demonstrates great elec-
trochemical properties due to the combined effects of the carbon trochemical behavior, exhibiting consistent cycling and rate
matrix derived from microalgae, natural doping atoms, and lay- performance. The observed effect can be associated with the
ered porosity design. After undergoing 700 cycles, the composite encapsulation of amorphous LiV3Ox within conductive CNFs.
anode exhibits a discharge capacity of 1375 mAh g
1 and a current Encapsulation allows for the creation of larger electrochemically
density of 1 A g
1. The rice-shaped γ-Fe2O3@CNFs were reported active sites for lithium storage, enhances charge transfer, and
by Cho et al. The application of a thin carbon layer on the top layer efficiently controls volume changes that arise during the inser-
of γ-Fe2O3 resulted in a synergistic impact, encompassing stress tion and extraction of lithium. The study uncovered that the
reduction, inhibition of volume expansion, facilitation of electron LVO@CNF anode had a discharge capacity of 603 mAh g
1 after
mobility, and enhancement of Li+ conductivity. After undergoing 200 cycles at a current density of 0.5 A g
1 with higher current
200 cycles, a reversible capacity of 1252 mAh g
1 was attained at retention 90% and a rate capacity of 326 mAh g
1 after 400 cycles
10 A g
1.[161] Hu et al. employed gradient electrospinning for fab- at a current density of 5 A g
1. The CNF coating demonstrated
ricating finer, hollow FexOy NPs that were uniformly linked to improved electrochemical performance by facilitating charge
porous N-doped CNR (FexOy@PN-CNR).[162] Similar research transfer and minimizing volume changes, due to the presence
studies were carried out on Sb2O3@1D-MCNF[163] and GeO2/ of electrochemically active sites.[167]
MCNF.[164] Wang et al.[165] effectively produced layered bimetallic
oxides of CoFe2O4 (CFO) hollow spheres through the solvothermal 3.5.4. Cobalt Oxide
and subsequent calcination process. The CFO found on this study
retained the identical hollow structure and spherical shape as the Cobalt oxide (CoO) has gained significant interest as a TMO due
Co-based ferrocene coordination polymer (Co-Fc-CPs) that came to its remarkable theoretical capacity of 715 mAh g
1 and its

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economically efficient production methods. CoO NPs exhibit during the initial 100 cycles. This phenomenon is commonly
limited surface area, low electrical conductivity, and inadequate observed in electrodes based on TMOs[170] and can be attributed to
durability. Carbon materials possessing high conductivity and several factors. Composite materials undergo a gradual activation
durability are commonly employed to provide support for CoO process as the structure is reconstructed, resulting in the expo-
NPs, thereby addressing the aforementioned limitations.[168] sure of additional active sites and flaws, thereby enhancing their
Meng et al.[169] synthesized Co3O4@CNFs electrodes for LIBs capacity. The in situ production of TMO compounds would
by electrospinning using a nitrogen atmosphere, Figure 15a. The enhance the dissolution of electrolytes, leading to the formation
research focused on the utilization of graphitic carbon shells to of a polymer/gel-like film that provides additional capacity.
encapsulate transition metallic cobalt. The fabricated Co3O4@CNFs The Co3O4@CNFs electrodes exhibit an increased electrochemi-
electrode showed a large specific surface area, porosity, and N- cal capacity compared to the anticipated capacity of Co3O4
dopant concentration. The morphological characteristics of the (890 mAh g
1).[171] In addition, the study examines cycling
developed electrodes were studied using SEM and TEM. The behaviors at a high rate of 2 A g
1, as depicted in Figure 15f.
SEM images (Figure 15b) reveal the structure of the spindle-like After undergoing 500 cycles, the battery exhibits a notable revers-
Co3O4@CNFs, which is composed of spherical NPs and frac- ible capacity of around 500 mAh g
1, with the CE close to 100%.
tured shells. The arrangement of NPs in a spindle structure Figure 15g illustrates the rate performance of the resulting
and their even dispersion, without any aggregation, would greatly composite at various current densities ranging from 100 to
enhance the efficiency of charge transfer. Figure 15c,d reveals the 2000 mA g
1. Figure 13g illustrates a decrease in specific dis-
lattices of Co3O4 and graphitic carbon in the HRTEM image and charge capacities as current density increases. The figure illus-
selected-area electron diffraction (SAED) pattern, respectively. trates that when the current density is dropped to 100 mA g
1,
Co3O4@CNFs electrodes for LIBs were evaluated for their the specific capacity of the Co3O4@CNFs electrodes rapidly
electrochemical properties using cycling studies at rate of 100 increases to 940.5 mAh g
1, indicating the superior high-rate
(Figure 13e) and 2000 mA g
1 (Figure 13f ). Figure 13e high- performance of these electrodes. The results mentioned above
lights a significant increase in discharge and charge capacities demonstrate that the hybrid Co3O4@CNFs composite material

Figure 15. a) The synthetic procedure of Co3O4@CNFs electrodes; b) the SEM image; c) HRTEM image; d) SAED pattern; e,f ) cycling performance of
electrodes at current densities 100–2000 mA g
1; g) rate performance. Reproduced with permission.[169] Copyright 2021, Elsevier.

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exhibits high specific capacity, good cycling performance, and that facilitates electron and ion transmission, while also reducing
strong rate capability. This can be attributed to several factors. volume expansion during discharge. The composite electrodes
First, the spindle-like structures of the material minimize the dis- employed as a LIB anode exhibit notable specific capacity, excep-
tance for ion movement, promoting rapid reaction kinetics. tional stability, and outstanding rate performance. Hence, the
Additionally, the even dispersion of Co3O4 NPs contributes to researchers suggest that the electrode material derived from bulk
the high specific capacity. Furthermore, the presence of graphitic GC exhibits significant potential for lithium storage. In a related
carbon prevents structure collapse caused by volume change dur- study, Hu et al. employed hydrothermal and sulfurization meth-
ing cycling and enhances the electrical conductivity of the com- ods to create hierarchical S-doped CoO nanospheres enclosed
posite. Lastly, the addition of N-doping, particularly pyrrolic N, within graphene (CoOS0.1@G). Compared to a single CoO sam-
provides more active sites and accelerates mobility. ple, the hybrid microsphere electrode demonstrated enhanced
We conducted a review of a novel architecture that utilized the lithium storage capacities and cycle stability. Through certain
electrospinning-annealing technique to produce anode materials modifications in the lattice’s design and electronic structure,
composed of CoMoO4 NPs and porous CNFs. The formed hybrid the study found that S-doping enhances the rapid diffusion of
composites, CoMoO4/CNFs have large specific surface area and lithium-ions and optimizes the electronic conductivity. TMOs
outstanding electrochemical performance due to their porous, can be used as anode materials in advanced LIBs, which helps
interlinked nanostructure. The unique performance of the anode to broaden the notion of electrode design.[177]
materials was attributed as (I) The 1D porous CNFs with gra- Zhao et al. successfully synthesized the Co3O4@NGFs com-
phitic crystallization functioned as highly conductive matrices posite by electrospinning ZIF-67/PAN as a precursor and then
that buffered CoMoO4 volume changes following lithium inser- thermally treating it. Graphitic carbon completely encased the
tion/extraction, assuring electrode conductivity; (II) the CoMoO4 Co3O4 NPs in their study, increasing the electrode’s conductivity
NPs were able to enhance Li+ storage through generating larger and affinity for the electrolyte, while also acting as a buffer
active sites and reducing the gap for lithium diffusion; Finally, against Co3O4 volume changes. A 3D conductive CF network
ex situ TEM analyses revealed the effectiveness of this hybrid with a large specific surface area enabled electron transport.
design in reducing volume change-induced electrode pulveriza- This Co3O4@NGFs electrode worked as a LIBs anode without
tion. This method for producing mixed oxides within crystalline a conductive agent or current collector. It kept its charge for
carbon matrices shows promise as a powerful electrode material 750 mA h g
1 at 0.1 A g
1 and 98.5% of its charge after 100
for electrochemical energy storage.[172] cycles. Surface-controlled capacitive and diffusion-controlled pro-
In addition, we examined a study conducted by Zhang cesses were the key contributors to the quick Liþ diffusion kinet-
et al.[173] which developed nanostructured anode materials for ics and increased capacity. This electrode exhibited impressive
LIBs using Co3O4/Co NPs/N-doped CNF. These materials exhib- flexibility, suggesting potential applications in flexible energy
ited improved rate performance, extended cyclic lifetime, and storage devices.[178]
comparable reversible capacity. The reversible capacities after
350 cycles were 663 and 448 mAh g
1 at high rates of 500 and
1000 mA g
1, respectively. The enhanced lithium capacity can 3.5.5. Titanium Oxide
be attributed to the presence of high temperature-affected metal
Co, evenly distributed Co3O4/Co NPs, and N-doped porous Titanium dioxide (TiO2) has garnered significant interest due to
CNFs. Moreover, the nanohybrid architecture exhibits adaptabil- its abundant availability, nontoxic nature, minimum volume
ity to various other TMO anodes. Hierarchically designed change (<4%) throughout the (de)lithiation process, higher dis-
Co3O4@porous CFs were successfully synthesized by the charge/charge voltage, and cost-effectiveness. Although TiO2 has
researchers through the electrospinning of ZIF-67/PAN nano- its advantages, its practical application is limited by factors such
fibers. The distribution of Co3O4-NPs within the CNFs was deter- as its low electrical conductivity and inadequate Li+ diffusion.
mined through elemental mappings of carbon, nitrogen, oxygen, There are two main approaches to improve the storage efficiency
and cobalt, indicating an even distribution. The composite mate- of lithium (Li) in titanium dioxide: reducing the particle size of
rials’ hierarchical structure resulted in impressive specific capac- TiO2 to nanostructures and combining TiO2 with various highly
ities of 705 mAh g
1 at 1 A g
1 and 558 mAh g
1 at 5 A g
1 when conductive compounds.[179]
employed as LIB anode materials.[174] Also, Li et al.[175] synthe- Researchers have recently demonstrated and confirmed the
sized additional cobalt-based electrodes using a one-step, cost- feasibility of utilizing biomass carbon in LIBs. Mulberry leaves
effective pyrolysis process. They created a composite material possess a high cellulose content, making them an excellent car-
of Co3O4/N-doped porous carbon (Co3O4/NPC). The resulting bon source. The exploration of biomass as a potential carbon
product exhibits a high degree of Co3O4 particle embedding, source for energy storage materials is driven by its affordability
while the presence of NPC facilitates the creation of many active and extensive accessibility. Here, we report a work that blends
sites for the transmission of Li-ions. which in turn, enhances the Li4Ti5O12–TiO2(LTO–TO2) microspheres with mulberry leaf
efficiency of charge and discharge processes, while simulta- (ML) extract as a carbon (C) source precursor. MLC derived from
neously reducing electrode resistance. After 236 cycles, the anode ML biomass serves as a convenient and efficient channel for lith-
materials showed maximum reversible capacity 577 mAh g
1. ium ions, thereby increasing the specific surface area of the
The synthesis of nanoporous CoO nanowire clusters on 3D material. This phenomenon enhances the movement of Li-ions
porous graphene fabric (CoO-NW@GC) was investigated by across the interface connecting the electrolyte and electrode. In
Zhou et al.[176] using a hydrothermal approach and an annealing Figure 16a, a one-step hydrothermal fabrication method is
procedure. The clusters and GC exhibit a unique microstructure depicted for the production of flower-like LTO–TO2/C1

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Figure 16. a) Schematic illustration of the formation of LTO-TO2/C1; b,c) SEM images; and d) HRTEM image of electrode material LTO-TO2/C1; e) cycle
performances of electrodes and f ) charge–discharge profile of electrodes considering the voltage range of 1–2.5 V (vs Li+/Li) at current density 1 C.
Reproduced with permission.[180] Copyright 2020, Elsevier.

electrodes with a carbon content of 2.8%.[180] Figure 16b depicts Additionally, we also have found another watermelons seeds-
the particle radius of the LTO–TO2/C1 composite electrodes, like structure of anodes which was fabricated from TiO2 NPs
which is ≈700 nm, nearly equivalent to the radius of the pure (P25) and amorphous carbon (C).[179] The P25@C anodes showed
phase, which is 500 nm. Additionally, Figure 14c illustrates that superior electrochemical performance when used in a LIBs via
the LTO–TO2/C1 electrodes are composed of condensed nano- half cells. The performance was enhanced by the numerous
sheets. The incorporation of MLC in the composite did not alter micropores and mesopores present in the TiO2 NPs within the
the overall structure of the LTOTO2 materials. Figure 14d dis- carbon spheres. The pores facilitate the electrolyte’s penetration and
plays high-resolution TEM images that exhibit multiple lattice reduce the deformation stress on TiO2 during the (de)lithiation
fringes. These fringes have an average pitch of 0.48 nm and align phase. The P25@C anodes exhibit significant enhancements in
with the (111) plane of the spinel Li4Ti5O12. In addition, they Li storage capacity, rate performance, and cycling stability.
observed lattice fringes with a pitch of ≈0.35 nm, which can A study was performed to assess the electrochemical lithium
be attributed to the (101) plane of anatase TiO2. The sample storage capacity of the P25@C anode material utilizing half-cells.
exhibits a composition comprising both Li4Ti5O12 and TiO2 The study found that the rate performance of P25@C was exam-
phases. ined at various current densities, ranging from 0.5 to 200 C. The
Figure 16 displays the electrochemical outcomes of all electro- voltage window used was 1.0–3.0 V, and the experiment was con-
des. Figure 16e shows that LTO-TO2/C1 and C2 (with a carbon ducted over ten cycles. At a current density of 0.5 C, the anode
content of 2.8%) demonstrate better cycle performance and dis- demonstrated a discharge capacitance of 496 mAh g
1. At a cur-
charge capacity when compared to LTO-TO2. The figure illus- rent density of 2 °C, the capacitance gradually decreased and
trates a decline in the discharge capacity of LTO from 156.2 to eventually reached at 180 mAh g
1. P25@C exhibits exceptional
137.5 mAh g
1 after 500 cycles. Similar to that, LTO-TO2/C1’s electrochemical activity, demonstrated by its substantial dis-
discharge capacity dropped from 174.3 to 159.2 mAh g
1 while charge capacity at various current densities, particularly at
LTO-TO2/C2’s capacity dropped from 162.7 to 147.5 mAh g
1. 0.5 C. The P25@C composite electrode demonstrates remark-
The successful integration of MLC has led to remarkable out- able electrochemical activity, as evidenced by its significant dis-
comes by reducing the Li-ion diffusion route and improving the charge capacity at different current densities, especially at 0.5 C.
electrical thermal conductivity of LTO-TO2. Figure 16f illustrates Also, P25@C materials demonstrate remarkable stability and
the concurrent charge and discharge outputs of LTO–TO2/C1 at improved reversibility, as indicated by their discharge capacity
a current density of 1 C. The elevated voltage of around 1.55 V is of 399 mAh g
1 and impressive capacity retention ratio of
associated with the lithium insertion/delithiation mechanism of 95.9% upon restoring the current to 1 C. The discharge capacity
Li4Ti5O12. A small platform, measuring ≈1.75 V, is observed, of P25@C drops to 99, 49, and 25 mAh g
1, respectively, at cur-
indicating the delithiation process from LixTiO2.[181] The out- rent densities of 5, 10, and 20 °C, indicating superior rate capa-
come significantly enhances capacity while maintaining a com- bility. Reversing the current density to 1 C results in a discharge
paratively modest current rate. The higher charge and discharge capacity of 393 mAh g
1 and a capacity retention of 94.5% when
rates of LTO–TO2/C1 can be associated with the combined compared to the initial 1 C. During ultra-high-rate continuous
advantages of the MLC and the LTO–TO2 microsphere.[182] charge–discharge reactions, it is anticipated that the anode

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structure of P25@C, resembling a watermelon, will remain structured pore networks serve as vital for enhancing electrolyte
undamaged. P25@C exhibits improved reversibility and cycling wettability and facilitating the rapid diffusion of Li-ions.
stability. Furthermore, the carbon shell ensured efficient electronic move-
Furthermore, we performed a comprehensive evaluation ment and protected against the accumulation and dissolve of
of a newly developed anode consisting of a hybrid composite Mn-ion throughout the cycling process. Developed MnO/C elec-
material featuring a three-dimensional honeycomb structure. trodes offer higher reversible discharge capacity (981 mAh g
1 at
The honeycomb structure showcases porosity, exhibits notable 100 mA g
1), improved rate performance, and prolonged cycle life,
cycling stability, and encompasses a significant quantity of elec- making them ideal for practical applications as electrode materials
tron/lithium pathways. Deng et al.[183] employed the in situ tech- for LIBs.
nique to create a TiO2/GNs nanocomposite using anatase-TiO2 Furthermore, we found a novel structure of anode materials.
and rGO nanosheets (GNs) for the fabrication of honeycomb Figure 17h emphasizes a significant technological advancement:
design. The experimental specimen exhibits a notable specific a self-supporting MnO2 NS positioned on a CNF film.[187] The
capacity of 184 mAh g
1 after 10 000 cycles at a current density process involved applying a MnO2 NS suspension onto electro-
of 50 C when employed as the anode material in a LIB. The spun PAN nanofibers and then carbonizing them. These materi-
exceptional properties of TiO2 can be attributed to the robust als have the potential to significantly reduce the aggregation and
bond formed between TiO2 and rGO, which arises from the in decomposition of MnO2 NSs, resulting in improved electro-
situ manufacturing process and the unique nanoarchitecture chemical performance of electrodes. The integrated CNF matrix
enabled by rGO. Furthermore, the TiO2/GNs composite exhibits facilitates the movement of charge carriers and accommodates
a porous structure and a large surface area, enhancing the effi- changes in electrode volume during cycling. The morphological
ciency of Li-ion transfer and accommodating regional volume features of MnO2 NSs@CNFs indicate that the MnO2 NSs are
changes. This facilitates the distribution of electrolyte. evenly dispersed over the surface of CNFs. The lattice gap of
the nanosheets is 0.24 nm, aligning with the (111) plane of
3.5.6. Manganese Oxide MnO2. The composition along with crystallinity characteristics
of MnO2 NSs and CNFs were analyzed using Raman analysis
The theoretical specific capacity, tunable oxidation states, and low (Figure 17i). Two distinct bands, referred to as the D-band and
reduction potential of manganese oxide (MnOx) make it a highly G-band, are detected at wavenumbers 1344 and 1576 cm
1,
attractive anode material for next-generation battery technology. respectively. The MnO2 NSs@CNFs exhibit an ID/IG ratio of 1.02,
MnOx, similar to other TMOs, demonstrates nonconductive suggesting an amorphous carbon structure. This suggests that an
characteristics and undergoes substantial volume expansion after amorphous carbon anode holds significant promise for energy
lithiation. These attributes present difficulties in assessing their storage.[188]
prospective rate and cycle efficacy. To address the aforemen- The researchers employed CV as an approach to investigate
tioned issues associated with MnOx, various approaches have the electrochemical properties of MnO2 NSs@CNFs electrodes
been explored, primarily falling into two main categories: nano- and evaluate their efficacy in storing lithium. The CV curves
technology and carbon-compositing.[184] in Figure 17j show similar forms with increasing scan rates
Hierarchical pore designs in composite electrode provide (0.1, 0.3, 0.5, 0.7, 1.0, and 2.0 mV s
1), suggesting strong stability
significant benefits, such as more active sites for Li-ion transmis- and reversible principles of the charge/discharge response. The
sion, shortened ion diffusion routes, and faster Li-ion diffusion. peaks broaden, reduction peaks drop, and oxidation peaks rise.
These benefits enable the development of high rate as well as Two sets of peaks at 0.2/0.5 and 1.0/1.3 V versus Li/Li+ indicate
high-energy LIBs. Based on the structural benefits, Yu et al.[185] Mn3+/4+ to Mn2+ and Mn2+ to Mn reactions, respectively.
employed biomass fungus as a raw material for developing mul- Cathodic/anodic peaks are broad, indicating a nondiffusion-
tilayer porous MnO/C (PCM) electrodes using hydrothermal and limited pseudocapacitive Li-ion storage activity. Ion storage
subsequent chemical treatments, Figure 17a. The electrodes that capacity is high due to faradaic surface or near-surface redox pro-
were produced had a cocoon-like shape. cesses termed pseudocapacitance.[189] Figure 17k demonstrates
The morphological characteristics of the MnO/C composites that MnO2 NSs@CNFs-1% exhibited superior capacities with
were studied by SEM and TEM. SEM in Figure 17b demonstrates the stability compared to MnO2 NSs@CNFs-5% and CNFs for
that the MnO/C electrode materials show cocoon-like shape even all applied current densities. This finding suggests that the pro-
after being calcined at a temperature of 800 °C. A rough outer portion of MnO2 nanosheets significantly influences the perfor-
surface has been observed, indicating the presence of a signifi- mance of lithium storage. The MnO2 NSs@CNFs-1% composite
cant pore structure, involving macropores and mesopores, in the electrode demonstrates impressive performance, measuring
MnO/C electrodes, as illustrated in Figure 17c. The energy dis- 1053.0 mAh g
1 at first discharge and 683.1 mAh g
1 at maxi-
persive X-ray elemental mappings of MnO/C composite elec- mum reversible capacities at 0.01 A g
1. Research findings indi-
trode revealed a consistent distribution of carbon, oxygen, and cated a notable increase in capacity when the current density was
manganese elements, as depicted in Figure 17d. In addition, adjusted to 50 mA g
1. After 200 cycles at 50 mA g
1, the capacity
the TEM images in Figure 17e,f reveal a porous cocoon-like struc- enhances from 554.3 to 597.6 mAh g
1 (Figure 17l), indicating
ture, with MnO NPs intertwined within a carbon shell layer. the electrode’s excellent stability and reliability. The reduction
In Figure 17g, the lattice fringe spacing was determined to be in fading is due to the increased utilization of the reaction during
0.26 nm, which closely corresponds to the (111) diffraction conversion, resulting in the formation of improved surface layers
plane of the MnO.[186] The MnO/C composite’s rich and from the electrolyte.[190]

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Figure 17. a) Schematic demonstration of the construction of a MnO/C composite electrode, b,c) SEM images of rough surfaces, d) the element map-
ping representations for Mn, O, and C; e,f ) cocoon-like shape by TEM and HRTEM image, g) demonstrates the lattice fringe spacing. Reproduced with
permission.[185] Copyright 2019, Elsevier. h) Schematic illustration of the MnO2 NSs@CNFs electrodes; i) Raman spectra of MnO2 NSs@CNFs; j) CV
curves of MnO2 NSs@CNFs electrodes; k) rate capabilities; l) the cycling performance of MnO2 NSs@CNF. Reproduced with permission.[187] Copyright
2022, American Chemical Society.

3.5.7. Zinc Oxide Researchers are consistently endeavoring to identify appropri-

ate combinations. Xiong et al.[192] employed a hybrid composite
Zinc oxide (ZnO) is a highly suitable anode material because consisting of ZnMn2O4-graphene nanosheet (ZMO/G) synthe-
it is inexpensive, readily available, and has a significantly high sized using modified Hummers methods as the anode and a
theoretical specific capacity of 978 mAh g
1. Nonetheless, the LiFePO4 nanosheet as the cathode to develop a LIB with a full
material exhibits inadequate electrical conductivity, restricted nanosheet structure. In the study, STEM (Figure 18a) illustrates
Li-ion diffusivity, significant early irreversible capacity loss, the uniform distribution of ZMO nanocrystals on 2D graphene
and poor cycling stability due to substantial volume alterations nanosheets. Additionally, Figure 18b illustrates the results of gal-
during lithiation and delithiation processes.[191] To overcome vanostatic charge/discharge studies, indicating that the 2D struc-
these shortcomings, researchers are developing fabrication tured ZMO/G composite electrodes displayed greater specific
techniques as well searching suitable materials to combine capacity, enhanced rate performance, and higher cyclic stability
with ZnO. compared to conventional graphite electrodes. Flexible/bendable

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Figure 18. a) STEM images and b) cycling performances of 2D ZMO–G composite anode materials at 400 mA g
1; c–f ) the flexible pouch cell powered by
red LED (UT) logo with different states; g) cyclic performance of the pouch cell under four states. Reproduced with permission.[192] Copyright 2016,
Elsevier. h) Hydrothermal synthesis technique of ZnO/G hybrid electrode materials; i–k) SEM images of ZnO/G hybrid electrode materials based of
various G contents. Reproduced with permission.[191] Copyright 2016, Royal Society of Chemistry. l) Synthesis methods of NiO/GF anode materials;
m) cycling outputs and CE of composite anodes; and n) rate capabilities of NiO and NiO-2/GF. Reproduced with permission.[73] Copyright 2019, Elsevier.

full LIBs were designed by integrating the ZMO/G composite ZnO-graphene hybrid composites. The even distribution of
anode and LiFePO4 nanosheets cathode into the provided half- ZnO NPs on the graphene sheets suggests a strong bond that
cells. The electrochemical performance of this flexible battery links the ZnO NPs and the 2D graphene sheets. As the wt%
was observed to be exceptional, with no structural damage of graphene increases, the quantity of ZnO NPs decreases,
and minimal loss of capacity and CE under various mechanical resulting in their reduction to nanoscale dimensions. The inclu-
bending conditions (Figure 18c–g). To improve performance of sion of graphene sheets is thought to be responsible for the tran-
ZnO as a node of LIBs, Feng et al.[191] combined ZnO with GO. sition from small ZnO particles to NPs in ZnO-graphene
Figure 18h represents the hydrothermal synthesis technique of composites. Graphene sheets enhance the nucleation process
ZnO-graphene hybrid materials for high-performance LIB ano- of ZnO, resulting in the formation of ZnO NPs. During hydro-
des. The study produced three hybrid composites, ZnO-LG, thermal reduction procedures, the dispersion of ZnO NPs serves
ZnO-MG, and ZnO-HG, using GO with weight compositions to prevent the fracture and restacking of graphene sheets. It is
of 43.08%, 61.11%, and 71.45%, respectively.[191] important to note that during charge and discharge cycles, opti-
The SEM images presented in Figure 18i–k offer a compre- mal electron and Li-ion transport is largely dependent on the
hensive examination of the morphological properties of the close contact between the various components in the composites.

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ZnO-HG demonstrates a strong interaction with ZnO NPs and NiO-2/GF electrodes was 640 mAh g
1, which is similar to the
graphene, resulting in a reversible specific capacity of 749.2 mAh g
1, specific capacities of NiO-1/GF and Ni-3/GF. These were mea-
a high cycle stability over 100 cycles with 70.3% retention, and a sured at 424 and 232 mAh g
1, respectively. The specific capacity
commendable current density of 2 A g
1. of raw NiO decreased significantly to 66 mAh g
1 after 50 cycles,
Furthermore, we have conducted further investigations on in contrast to the composites. The charge/discharge patterns of
anodes composed of zinc and carbon materials. The carboniza- NiO and NiO-2/GF at varied current densities (100–2000 mA g
1)
tion process was successfully employed by Gao et al.[193] to syn- are illustrated in Figure 16n, offering insights into their rate per-
thesize self-assembled ZnO/porous carbon microspheres. The formance. NiO-2/GF specific capacities were ≈635 mAh g
1 for
even distribution of zinc oxide NPs (ZnO NPs) within porous 100 mA g
1, decreasing to 210 mAh g
1 for 2000 mA g
1.
carbon serves as a buffer layer. The composite electrode demon- Conversely, the specific capacities of raw NiO decreased signifi-
strates exceptional cycle capabilities and rate optimization capa- cantly, practically reaching zero at high current densities.
bilities. Composites with a microsphere structure improve NiO-2/GF has a considerably higher rate capacity than NiO after
structure stability of electrode and reduce capacity fading. In integrating the conductive GF substrate. The superior strength
addition, the porous carbon structure supports Li+ charge/dis- and stability of NiO/GF anodes are due to the positive relationship
charge, adapts to large volume fluctuations, and enhances elec- among GF and NiO components, as shown in the above results.
trochemical performance. In a separate study, Wang et al.[194] First, conductive GF may elastically buffer volume variation and
employed a spray drying technique to coat ZnO particles with accelerate electron transport, boosting integrated electrode cycle
graphene, resulting in the development of composite electrodes and rate performances. Second, the hollow pattern reduces NiO
(ZnO/rGO). This method enhances the electric conductivity of particle volume change and shortens lithium-ion diffusion.
the electrode materials, minimizes the volume growth of ZnO Third, the elastic GF base prevents NiO particle formation, and
NPs during the entire charge/discharge cycle, and facilitates effi- the huge surface interfacial surface stores more lithium ions.
cient electron transport. When used as an anode in LIBs, the The combining effect of these elements makes NiO/GF anodes
developed ZnO/rGO electrodes exhibited better electrochemical better electrochemically than GF and NiO.
performance compared to traditional ZnO composite electrodes.
To overcome the limitations of ZnFe2O4-based anode materi-
als, Li et al.[195] developed and synthesized GO-coated ZnFe2O4 3.6. MXene Carbon-Based Anode Materials
hollow spheres using a simple self-assembly technique. The
h-ZnFe2O4/GO composite electrode demonstrates excellent elec- Recently, there has been growing interest in MXene, a novel 2D
trochemical performance and features a durable and flexible hol- transition metal carbide/nitride. MXene comprises transition
low structure, rendering it a suitable choice for anode materials metal carbides, nitrides, and carbonitrides. The general formula
in LIBs. In comparison to pure ZnFe2O4, it exhibited improved for MXene is Mn+1XnTx, where M represents a transition metal,
reversibility, improved cycle stability (829 mAh g
1 at a current X denotes carbon and/or nitrogen, and Tx indicates surface func-
density of 200 mA g
1 after 500 cycles), and a higher rate poten- tional groups such as ─O, ─OH, and ─F.[200] MXene stands out
tial (463 mAh g
1 at a high current density of 1000 mA g
1). This due to its special surface chemistry, customizable composition,
article introduces a feasible method for improving the Li-ion and unique physicochemical properties. This has made it a sub-
storage capacity of future LIBs. Paloma et al.[196] Hyeongwoo ject of great interest in the field of energy storage. In 2011,
et al.[197] Xiao et al.[198] and Wang et al.[199] also developed various Gogotsi et al. achieved a significant breakthrough by synthesiz-
anode materials based on GO and TMOs. ing the first Ti3C2-Tx (MXene). The researchers achieved this by
A pioneering study demonstrated the successful growth of employing a 50% concentrated hydrofluoric acid solution at
hollow microspheres of a Nickel (Ni) and MOF on a graphene room temperature to selectively eliminate aluminum from
foam (GF) substrate through a straightforward solvothermal Ti3AlC2.[201] MXene is mostly used combined with oxides based
technique. The study utilized Ni-MOF/GF as precursors for on titanium, cobalt, and iron to fabricate composites that serve as
synthesis of NiO/GF binder-free anode materials for high- lithium substitute anodes for ion batteries, revealing great poten-
performance LIBs, as shown in Figure 18l.[73] The anode materi- tial, Table 7 provides a concise overview of the electrochemical
als composed of NiO/GF demonstrated higher specific capacities performance of various carbon-based MXene composite materi-
and improved cycling stability when compared to the individual als used as anodes in LIBs.
components of pristine NiO and GF. The remarkable electro- Xiao et al.[202] employed a straightforward method to deposit
chemical performance can be credited to the combined proper- TiO2 NPs onto delaminated few-layer MXenes, which produced
ties of the NiO and GF components. The GF matrix enhances Ti3C2Tx/TiO2 composites. Following 200 charge–discharge
electrode conductivity and offers a flexible platform for incorpo- cycles, a composite material with a 1:4 mass ratio of MXene
rating active materials, thereby preventing the release and diffu- to TiO2 demonstrates enhanced reversible capacity as a negative
sion of NiO NPs into the electrolyte throughout the cycle. electrode for LIBs. Hybridizing multiple layers of MXene during
The cycling performance of NiO, GF, and NiO/GF was lithium-ion insertion and extraction enhances the structural sta-
assessed at 100 mA g
1, as shown in Figure 16m. The initial CE bility of the composite material. Recent research indicates that
of NiO-2/GF in the first cycle was 67.8%, which was attributed to Ti3C2Tx MXene serves as a suitable substrate for the creation
an irreversible reaction and the formation of a SEI. During the of oxidative TiO2. When utilized as an anode in a rechargeable
second cycle, the specific capacity experienced a decrease from LIB, TiO2 derived from Ti3C2Tx has a low lithium-ion diffusion
903 to 628 mAh g
1. Subsequently, it remained constant for a coefficient, inadequate conductivity, and limited capacity. A
total of 50 cycles. After 50 cycles, the specific capacity of the doping method utilizing alternative elements or oxides has been

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Table 7. Electrochemical performance of several carbon-based MXene composite materials in LIBs anode.

Anode materials Applied methods Reversible capacity Current density Cycle number References
[mAh g
1] [mA g
1]
C@Fe3O4/Ti3C2 Hydrothermal þ calcination treatment 231.5 100 200 [344]
h-Co3O4@rGO Solvothermal treatment þ annealing process 1154.2 500 100 [345]
N-doped Ti3C2@TiO2 In situ þ hydrothermal 302 200 500 [204]
Co3O4/Ti3C2Tx Hydrothermal þ ultrasound treatment 999.3 500 900 [207]
Ti3C2Tx/ZnFe2O4 Ultrasonication þ freeze-drying 436 – 100 [346]
Fe3O4@Ti3C2 Ultrasonication 278.3 – 800 [347]
Ti3C2@Si/SiOx@TiO2 Sol–gel 1051 100 100 [348]
s-Ti3C2Tx/Fe3O4 Ultrasonication þ freeze-drying 326.6 2000 1000 [349]
CNTs@Ti3C2Tx In situ þ microwave irradiation 175 10 000 500 [350]
Ti3C2Tx/CNFs CVD 320 372 295 [351]
Ti3C2Tx MXene/CNF A facile spin steaming technology 140 74.4 1000 [352]
S/N co-doped Nb2C MXene – 140 50 100 [28]
2DSi@MXene Solution mixing 835 5000 3000 [353]
Ti3C2 MXene aerogel scaffold Template methods 110 372 100 [354]
Single layer Zn-MXene (Ti3C2Clx) Rolling-to-rolling þ spray coating 110 1700 500 [355]
Li5Cr7Ti6O25/MWCNTs Sol–gel method 123.8 1020 400 [230]
C/TiO2@Li||LiFePO4 One-step green in situ oxidation 128 170 250 [356]
CoO/Ti3C2 Hydrothermal þ calcination 313 100 100 [205]
N-doped Ti3C2@TiO2 MXene In situ þ hydrothermal 302 200 500 [204]
N-Ti3C2/Fe2O3 Thermal decomposition 549 200 400 [210]
Co3O4-NPs/MXene composite Solvothermal 1005 372 300 [357]
Ti3C2Tx/TiO2 Dissolving þ Rolling 143 500 200 [202]
TiO2@NC/Fe7S8 In situ polymerization 516 100 100 [203]
CoO/Ti3C2 Hydrothermal method 313 100 100 [205]
N-Ti3C2/Fe2O3 Solventless thermal decomposition 1065 100 400 [210]
C-Fe3O4/Ti3C2 Solvothermal Technique 997 1000 2000 h[209]

suggested. In addition, a 3D TiO2@nitrogen-doped carbon based on N-doped Ti3C2@TiO2 MXene. The hybrid material
(NC)/Fe7S8 composite was synthesized using a simple hybrid exhibits a significant reversible capacity of 302 mAh g
1 at a cur-
approach, which involved the in situ polymerization of pyrrole rent density of 0.2 A g
1 after 500 cycles and 154 mAh g
1 at a
monomer with alkalized Ti3C2Tx, followed by vulcanization at current density of 2 A g
1 following 1500 cycles, rendering it a
700 °C. Upon assessment as an anode material for LIBs, the potential anode material for LIBs. The sustainable nature of this
TiO2@NC/Fe7S8 exhibits a substantial reversible capacity of LIB anode can be attributed to its notable capacitive impact, excel-
516 mAh g
1 after 100 cycles at a current density of 0.1 A g
1, lent electrical conductivity, and the formation of high-capacity
exceptional rate capability of 337 mAh g
1 at 1 A g
1, and nanoscale TiO2 in situ. Furthermore, the N-doped Ti3C2@TiO2
impressive long-term cycling stability of 282 mAh g
1 after exhibits an interlayer-expanded structure that significantly
1000 cycles at 4 A g
1. The remarkable electrochemical perfor- improves its efficacy.[204]
mance is attributed to the distinctive architecture of Another TMOs compound, cobalt oxide, including Co3O4 and
TiO2@NC/Fe7S8, wherein the 3D urchin-like TiO2, exhibiting CoO, were recently employed as anode materials for LIBs owing
excellent structural stability, offers sufficient space to enhance to their high theoretical capacities (Co3O4: 890 mAh g
1, CoO:
the contact between the electrode and electrolyte, reduces the 715 mAh g
1) and synthesis methods. The process is straightfor-
lithium-ion diffusion path, and mitigate volume changes; the ward, eco-friendly, and has garnered significant attention.
NC shell layer enhances electrical conductivity, promotes elec- Consequently, it is anticipated to emerge as a viable alternative
tron transport, and inhibits the aggregation of Fe7S8; Fe7S8 pro- anode material. In contrast to graphite anodes, cobalt oxide
vides a high specific capacity during the charge/discharge cycle. exhibits significant irreversibility and inadequate cycle stability
The hybrid approach in this study elucidates the investigation of owing to substantial volume expansion during lithiation and deli-
combining MXene-derived oxides with other metal sulfide for thiation, as well as suboptimal rate performance resulting from
potential applications in energy storage.[203] Li et al. employed sluggish reaction kinetics and low intrinsic conductivity.
a hydrothermal technique to synthesize composite materials Drawback constrains the practical utilization of sophisticated

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LIB. It was found that the combined structural strategy is a viable high-energy-density batteries. In a study conducted by Zhang
approach for improving the electrochemical performance of et al.[210] a nanocomposite was synthesized using a solvent-free
LIBs. The perfect anode material, along with a unique structure, thermal decomposition technique. The nanocomposite consisted
can significantly improve the electrochemical performance of of well-dispersed iron oxide NPs (N-Ti3C2/Fe2O3) that were
LIBs. Thereby, Li et al.[205] employed a simple hydrothermal attached to a highly conductive N-doped MXene nanosheet.
approach to synthesize CoO/Ti3C2 composites. The CoO/Ti3C2 The study found that nitrogen-doped Ti3C2 nanosheets have mor-
composite material, owing to its synergistic effect, serves as the phological characteristics that indicate the presence of well-
anode material for LIBs, enhancing the storage capacity of Li+. anchored Fe2O3 NPs with a diameter of ≈30 nm. Additionally,
The initial discharge capacity recorded is 1389 mAh g
1, with the analysis of image mapping revealed that the distribution of
a CE of 61 at 100 mAh g
1. Following 100 cycles, the reversible Fe and O elements in the hybrid composite aligns with the evenly
capacity remains at ≈313 mAh g
1, significantly surpassing that dispersed Fe2O3 NPs on the N–Ti3C2 matrix. The distribution of
of pure Ti3C2 and pure CoO. Furthermore, Zhao et al.[206] oleic acid molecules, which possess long carbon chains and func-
employed three distinct techniques: alternating filtration, spray tion as surfactants, is responsible for the observed equal distribu-
coating, and in situ wet chemical synthesis to facilitate the tion. These molecules serve as effective caps for the NPs,
hybridization of 2D Ti3C2TxMXene with Co3O4 or NiCo2O4. The impeding their aggregation during the thermal disintegration
MXene/TMO hybrid membrane electrode, developed through phase. According to the electrochemical results, the N-Ti3C2/
these three methods, demonstrates a high reversible capacity that Fe2O3 electrodes demonstrate a significant reversible capacity
surpasses 1200 mAh g
1, making it a promising candidate as a of 1065 mAh g
1 at 100 mA g
1 when used as the anode in
LIBs anode material. All films demonstrated remarkable long- LIBs. Furthermore, the device exhibits fast charge and discharge
cycle stability and outstanding rate performance. In another capabilities, along with robust cycle performance, maintaining a
work, the sandwich-like CO3O4/Ti3C2Tx hybrid composite was sustained value of 549 mAh g
1 after 400 cycles at 2 A g
1.
fabricated by Zhang et al. by applying a simple ultrasonic treat-
ment. When employed as the anode material of LIBs, CO3O4/
Ti3C2Tx shows higher electrochemical properties. With its 4. Conclusion
impressive large surface area as well hollow structure, the
Co3O4/Ti3C2Tx material is able to efficiently absorb electrolyte As stated above, there has been notable progress in the scientific
and provide sufficient active sites. As a result, it exhibits out- study and development of LIBs that utilize carbon as a vital mate-
standing electrochemical performance. Following 900 cycles at rial. In summary, the article focuses on the applications of CFs
a current density of 500 mA g
1, the Co3O4/Ti3C2Tx
3 composite and their influence on LIBs. This study mainly highlights their
exhibited a sustained discharge capacity of 999.3 mAh g
1. The striking advantages, such as electrochemical behavior, superior
composite’s economical production process and exceptional electrical conductivity, efficient electron transmission, and mini-
performance indicate its potential as a promising electrode mal volume fluctuation. In addition, CFs have demonstrated
for LIBs.[207] In addition, Sun et al. conducted a study exploring excellent reversibility, minimal charge-transfer impedance, and
a scalable bottom-up approach to synthesize a variety of exceptional stability throughout charging and discharging.
Co3O4@monolayer Ti3C2Tx (s-Ti3C2Tx) hybrids. This 2D hybrid Furthermore, CFs possess qualities that make them both afford-
material emphasizes remarkable structural and compositional able and effective, making them highly advantageous for cost-
benefits when used as a negative electrode material for LIBs. effective technical production. Currently, flexible LIBs widely
This material demonstrates an impressive high-rate capacity of employ carbon derivatives as the anode. CFs offer superior effi-
223 mAh g
1 after being subjected to an ultrahigh current den- ciency and produce minimal reactions compared to alternative
sity of 10 A g
1. In addition, the composite material exhibits an materials used as anodes in flexible batteries and other applica-
impressive cycle life of 550 mAh g
1 at 1 A g
1 even after under- tions that require both high intensity and exceptional electro-
going 700 successive cycles.[208] Li et al.[209] designed a hybrid chemical performance. As a result, the combined effect of
composite electrode (C-Fe3O4/Ti3C2) with a 3D spring coil archi- CFs and batteries yields unique electrochemical performance.
tecture, consisting of Ti3C2-wrapped carbon-coated Fe3O4. The However, the performance of pure CF falls short of expecta-
3D C-Fe3O4/Ti3C2 electrodes, used as an anode for LIBs, exhibit tions. In light of the current circumstances, an increasing num-
both the strong electrochemical activity of Fe3O4 and exceptional ber of academics are working on overcoming hurdles in the hunt
electrical and ionic conductivity. f-Ti3C2, a compound with phys- for new and acceptable materials. Developing a unique combina-
ical properties, can improve the electrical and ionic conductivity tion of pure CF and other materials appears to be a compelling
of C-Fe3O4. Furthermore, it is advantageous to control the sub- and effective option. This strategy not only overcomes the con-
stantial volume fluctuations of Fe3O4 that arise during the Li+ straints of pure CF, but also incorporates the benefits of other
insertion/extraction procedures. Furthermore, the compound materials into the compounds. Fortunately, tremendous prog-
C-Fe3O4 effectively inhibits the self-restacking of f-Ti3C2 by ress has been made in the development of these compounds, par-
increasing its surface area and generating a higher quantity of ticularly CF coupled with TMOs, metal sulfides, metal selenides,
active sites. The C-Fe3O4/Ti3C2 anode demonstrates superior MXene, and other materials, in recent years. According to recent
electrochemical performance and a prolonged cycle lifespan at research, TMOs, sulfides, MXene, and allied materials have dem-
high current density. The battery exhibits a reversible capacity onstrated exceptional performance. Combining these materials
of 997 mAh g
1 at 1 A g
1, even after undergoing 2000 cycles. eliminates many of the disadvantages of pure CFs. For example,
The results indicate that the composite material developed rate performance, cycling stability, and electron conductivity
exhibits promising characteristics as an anode for long-lasting, were thoroughly investigated, ensuring that the composite

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materials exhibit distinct features in a variety of applications. The valuable materials while also reducing carbon emissions to
research study indicates that fabrication processes for CF-based address the environmental challenges posed by used LIBs;
materials have made tremendous progress, providing new oppor- and 9) To properly identify Li ion plating behavior, it becomes
tunities to enhance their performance in many applications. essential to develop novel in situ or operation methodologies that
Furthermore, we found that the application of carbon materi- can correctly monitor the process within a functioning cell.
als to LIBs offers additional benefits. 1) Carbon-based materials Because Li is reactive and deposition and stripping of Li have its
with porous and large surfaces have the potential to create a own unique properties, different ex situ characterizations can
strong and conductive structure that allows active materials to change its basic properties and give false results. Studying the
strongly bond. Also, the carbon framework has the ability to with- actual Li-ion plating/stripping behavior in a working cell will help
stand repeated deformation and facilitates the transportation of us better understand the process of dendritic development and
both ions and electrons, effectively improving electrochemical growth. It is strongly advised to do operation characterization of
kinetics. 2) The remarkable characteristics of carbon materials, operating Li metal anodes in pouch or winding-type cells.
including their lightweight nature, low interface resistance, and The specific capacity remains low in comparison to the theo-
plentiful active sites, contribute to the enhancement of energy retical capacity. Additionally, capacity diminishes rapidly follow-
density when used in LIBs. 3) The excellent electrochemical sta- ing cyclic deformations. The mass of active materials loaded on
bility of carbon materials improves both rate and cyclic perfor- carbon-based electrodes is restricted, which adversely affects vol-
mance with the specific capacity of LIBs. According to the current umetric and area energy densities. Furthermore, there is a scar-
research, there are several challenges that must be addressed in city of strategies and devices for the large-scale, reproducible
future advancement: 1) First, it is necessary to design novel synthesis of carbon materials with specific structures and mor-
anode materials for LIBs with high efficiency. New materials, phologies at a low cost. Consequently, the development of flexi-
such as high-entropy and zero-strain materials, are now being ble carbon-based anode materials characterized by superior
improved and adjusted for their application as battery anodes; flexibility, high energy capacity, scalability, and cost-effectiveness
2) As active materials interact with conductive components to will be a primary focus of future research. Finally, CFs have sig-
facilitate ongoing electrochemical reactions. Therefore, it is nificant potential for future use in energy storage devices such as
important for conductive materials to be easily deposited with LIBs. To enhance the electrochemical properties, it is necessary
active materials. In addition, a strong interfacial strength plays to develop more effective ways. Although there are numerous
a crucial role in enhancing both the electrochemical and mechan- challenges to address, composites made from CF materials show
ical performance; 3) The formation of metal meshes, or nano- significant potential for expanding the use of CF-based anode
wires, is ideal for developing versatile electrodes that are materials in LIBs.
free-standing and binder-free. Furthermore, controlling the level
of porosity in mesh, nanowires, or foam-based electrodes is impor-
tant for improving overall battery capacity; 4) Applying different Acknowledgements
carbonaceous materials or conductive polymers to the metal
current collectors is an effective way to enhance their electro- The authors would like to express their gratitude to Md. Haris Uddin for
chemical and mechanical performance while also protecting providing them with insightful guidance and suggestions that helped them
improve the content of the article.
them against corrosion; 5) Anode-free lithium metal batteries
(AFLMBs) require further development of carbon materials col-
lectors. AFLMBs are currently used in limited applications due to
their low initial CE, unstable SEI, and dead Li generation. Carbon Conflict of Interest
substrates with high mechanical strength provide a large surface The authors declare no conflict of interest.
area that effectively mitigates Li plating and stripping, reducing
the production of Li dendrites and inactive Li. By combining
other techniques, such as a suitable electrolyte, the interfacial
environment can be improved to produce a more robust SEI Keywords
layer, resulting in better Li utilization. Nonetheless, significant anodes, carbon fibers, carbon materials, electrodes, energy storage,
challenges remain in the development of carbon-based collectors lithium-ion batteries
that must be overcome to achieve the commercialization criteria
for AFLMBs; 6) Currently, the primary focus of the study is on Received: July 25, 2024
Revised: October 4, 2024
material synthesis, with a deficiency in research on the underly-
Published online: October 30, 2024
ing mechanism. To study the battery operating procedure and
dendrite formation, thorough modeling and simulation are
required. Furthermore, there is a need to broaden the scope
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Mahmuda Akter has been working as an associate professor at the Bangladesh University of Textiles. She
has completed her Ph.D. from Erciyes University, Turkiye, under the prestigious CoHE (Council of Higher
Education) Ph.D. Fellowship. Prior to that, Dr. Mahmuda obtained her B.Sc. and M.Sc. in textile
engineering from the Bangladesh University of Textiles (BUTEX). Before becoming a faculty member of
BUTEX, she had professional and industrial experience in textile factories. Her major fields of study and
research interests are wearable technology, smart textiles, graphene, energy storage materials, fiber-
reinforced polymer composites, nanocomposites, technical textiles, and sustainable materials.

Ibrahim Hossain attained his bachelor of science (B.Sc.) in textile engineering from the Bangladesh
University of Textiles (BUTEX). He possesses profound expertise in material science and polymer
science. His research delves into the evolution and implementation of conductive textiles in signal-
sensing technologies. His research interests encompass smart textiles, energy storage materials,
supercapacitors, graphene, textile composites, and additive manufacturing. Ibrahim also explores the
application of silver nanoparticles for antimicrobial purposes in textiles. His overarching objective is to
identify novel materials and pioneering solutions that effectively address emerging challenges across
various sectors.

Maitree Howlader is a graduate student who has completed her B.Sc. in apparel engineering from the
renowned Bangladesh University of Textiles. Her field of work interest is textile design where she desires
to leave her mark. She has also worked on wearable supercapacitors, nano-based textile printing and
dyeing, and the application of enzyme in textile processing. She shows profound research interest in
wearable and sustainable textile design with a vision of bringing remarkable distinction in this field.

Fahim Shahriar earned his bachelor of science (B.Sc.) in textile engineering from the Bangladesh
University of Textiles. His research interests lie in material science, textile technology, and advanced
materials, with a focus on developing innovative solutions for industrial applications and sustainable
energy storage. While Fahim has explored carbon fiber and composite materials for energy-related
technologies, his broader passion remains in material science and its related fields. He aims to continue
advancing research at the intersection of textiles and advanced materials to foster sustainable
innovations across multiple sectors.

Umme Habiba Saima is a graduate of the Bangladesh University of Textiles (BUTEX), with a degree in
textile engineering specializing in apparel engineering. She has excelled as a research assistant while
maintaining exemplary academic performance. Her research interests include graphene, wearable
technology, smart textiles, functional textiles, advanced materials, nanoparticles, sustainable textiles, and
industrial engineering. Saima is committed to advancing her academic journey and contributing to
innovations and sustainable solutions in advanced materials, functional textiles, smart textiles, and
sustainable textiles.

Energy Technol. 2025, 13, 2401426 2401426 (42 of 42) © 2024 Wiley-VCH GmbH