Composites Part C: Open Access: Zulfiqar Ali, Saba Yaqoob, Jinhong Yu, Alberto D'Amore

Composites Part C: Open Access 13 (2024) 100434
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Composites Part C: Open Access

journal homepage: www.sciencedirect.com/journal/composites-part-c-open-access
Critical review on the characterization, preparation, and enhanced

mechanical, thermal, and electrical properties of carbon nanotubes and
their hybrid filler polymer composites for various applications
Zulfiqar Ali a, Saba Yaqoob a, Jinhong Yu b, Alberto D’Amore c, *
a
Department of Mathematics and Physics, Università degli Studi della Campania “Luigi Vanvitelli”, Caserta 81100, Italy
b
Key Laboratory of Marine Materials and Related Technologies, Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials
Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
c
Department of Engineering, Università degli Studi della Campania “Luigi Vanvitelli”, Via Roma 29, Aversa 81031, Italy
A R T I C L E I N F O A B S T R A C T
Keywords: Carbon nanotube (CNT) reinforced hybrid polymer composites offer multi-functional and sustainable materials
Carbon nanotube due to fascinating mechanical, electrical and thermal properties. However, many studies reported the impact of
Hybrid polymer composites CNTs orientation and synergistically enhanced properties of hybrid polymer composites but only a few review
Synergistic effects
literatures are published. This review provides a comprehensive overview of published research by addressing
Mechanical properties
Thermal-electrical conductivity
CNT classification, preparation methods, mechanical, thermal, and electrical properties, and potential applica
Applications tions, as due to high strength, high young’s modulus, higher thermal and electrical conductivity these nano-
dimensional hybrid composites find many applications in aerospace, automotive, electronics, energy storage,
sensors, electromagnetic interference (EMI) shielding, engineering, and biomedical fields.
1. Introduction CNTs, being a one dimensional (1D) cylindrical, rolled up single-

layered sheet of carbon atoms, are an ideal candidate for polymer
With the increasing technology, the demand for multi-functional, composites due to high tensile strength, high chemical stability, higher
smart, lightweight, flexible, and cheaper materials is increasing elastic modulus, good thermal and electrical conductivity, stiffness and
rapidly. This is why traditional materials, e.g., metals, cannot serve in light weight [8–10]. The excellent mechanical, thermal and electrical
the industries. However, polymers are in abundance and able to replace properties of CNTs are due to their strong sp2 bonds between carbon
traditional materials with fascinating properties, e.g., low specific atoms, providing an accurate self-supporting atomic structure with
weight, high corrosion resistance, low cost, easier molding, smart opti exceptional phonon-dominated thermal conductivity and high tensile
cal properties, and good electrical and thermal insulation, but due to strength in axial direction [11]. Currently, CNTs reinforced hybrid filler
amorphous structure, low mechanical, thermal and electrical properties polymer composites have greatly attracted researchers due to adapt
are the bottleneck to their industrial applications. Thus, researchers ability with multiple fillers (e.g., graphene, carbon fiber, silica, carbon
presented polymer composites as a replacement with desired properties. black, fullerene etc.), impressive network structures, and synergistically
Composite is a different materials (filler and matrix) amalgamation with enhanced interfacial strength, electrical and thermal properties. Carbon
unique properties without losing the individuality of constituent mate nanomaterials, with high aspect ratios and lower density of CNTs (1D)
rials in the combination. Usually, three types of polymer matrix are used added with graphene (2D) deliver well-organized 3D structured
in making polymer composites, i.e., thermoplastic, thermosetting poly nano-sized hybrid filler and offer highly conductive polymer composites
mers, and elastomers [1–4]. Fillers are specific materials mostly used to with high tensile strength [12].
enhance the stiffness and strength of polymers. Among others, Carbon Indeed, when considering CNT hybrid filler polymer composites,
fillers, e.g., Carbon fiber (CF), Carbon nanotubes (CNTs), and Graphene which involve the presence of multiple fillers alongside carbon nano
(G), efficiently enhanced the desired properties in polymer matrices tubes (CNTs) in polymers, it is essential to examine the potential limi
[5–7]. tations of cost, scalability, safety, and regulatory challenges that are
* Corresponding author.
E-mail address: [email protected] (A. D’Amore).
https://doi.org/10.1016/j.jcomc.2024.100434
Available online 6 January 2024

2666-6820/© 2024 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Z. Ali et al. Composites Part C: Open Access 13 (2024) 100434
specific to this composite type. Due to CNTs production cost and in study, Zhou et al. developed polyamide 6 (PA6)/ functionalized gra
clusion in polymers with exotic fillers can considerably raise the mate phene (FG)/functionalized (FCNTs) composites by electrospinning and
rial cost. Thus, balancing the expenditure is crucial to achieving high- at loading of FG (0.2 wt%)/FCNTs (0.3 wt%) the mechanical properties
performing complex filler combinations. These complex combinations were increased unto 2.4 times of pure PA6, with 132 % enhanced
refer to ambiguities to maintain consistent quality at a larger scale with Young’s modulus. Additionally, there are many references to disclose
new safety risks and regulatory challenges associated with using mul the potential of CNT composites and methodologies employed [22–27].
tiple reinforcing fillers. Specialized equipment, effective regulatory This study encapsulates the classification of CNTs and mainly focuses
policies, and material optimization could help resolve these issues. on currently adopted techniques and preparation methods for CNTs and
Fig. 1 shows key features and advantages of CNTs as a hybrid filler hybrid polymer composites. The impacts of filler aspect ratios, disper
with multiple fillers to produce polymer composites with highly con sion effects, and geometrical configurations on mechanical, electrical,
nected structural configurations. In another study, MWCNTs/Epoxy and thermal properties reported in published research are discussed in
composites were produced with ultrahigh filler aspect ratios 10–68 wt.% detail. Moreover, to better introduce the multifunctionality of CNTs
by hot-press infiltration technique. The MWCNTs were wrapped around hybrid filler polymer composites, applications in macro-level industries
a semi-permeable membrane and epoxy resin was injected during the (aerospace, automotive, electronics, energy storage devices, and wind
processing. The aligned and randomly orientated CNTs composites were turbine blades) are also reviewed. In the last part, the conclusion and
produced, and the results were analyzed. The characterization results prospects will be briefly discussed.
revealed that at ultrahigh aspect ratio (68 wt.%), aligned CNTs com
posites showed higher Young’s modulus (36 GPa) with enhanced elec 2. Classification of CNTs
trical conductivity [17].
The efficiency of CNTs-reinforced polymer composites is highly CNT is a hollow 1D carbon tube with a nanometer diameter range,
related to the distribution of CNTs through polymer solutions. Pristine obtained by rolling a 2D graphite sheet into a cylindrical shape. These
CNTs are highly rigid, chemically inert, and have strong π–π in structures were accidentally discovered by Japanese physicist Sumio
teractions, resulting in difficulties in obtaining advanced reinforced Iijima (1991) during the fullerene synthesis by the electric arc discharge
composites with homogeneously dispersed CNTs. However, size, shape, method [28,29]. Based on structure, CNTs are classified into two major
and high surface area highly aid CNTs’ distribution and adjustment of categories: single-walled carbon nanotubes (SWCNTs) and multiwalled
polymers on CNTs’ surface, but high loading of CNTs leads to higher carbon nanotubes (MWCNTs). SWCNTs, also called graphene nanotubes
viscosity due to high surface area and agglomeration phenomena. Ag (GNTs), consist of only one graphene layer rolled cylindrically with
gregation and solvent chemistry regulate the CNTs particle size distri one-atom thickness, two micrometers length, 0–2 electron volts (eV)
bution and dispersion to resolve the above issue. For this purpose, CNTs bandgap, and a diameter of two nanometers. While synthesis, the
are chemically functionalized, which highly intrigues homogeneous cap-like closed-end SWCNTs are obtained with C-C bond, forming a ring
dispersion, adsorption energy, and interfacial adhesion between CNTs at both corners. Due to the variable arrangement of carbon atoms,
and polymer matrices by hydrogen bonding interaction [18]. SWCNTs possess three configurations: armchair, zigzag, and chiral
It can be concluded that the performance of CNTs relies on geometry structure. Depending upon the arrangement of chiral vectors, SWCNTs
(size, shape) and fabrication techniques to attain adequate dispersion show exceptional electronic properties and can also be employed as
and sufficient bonding through polymer matrices [19]. Li et al. [20] semiconductors, like in transistor applications [30–32]. Fig. 2 shows the
fabricated CNT–graphene nanoplatelet GNP/epoxy composite via CVD formation of CNTs and the classification of SWCNTs and MWCNTs.
method and achieved ~40 % increased tensile modulus and ~36 % However, MWCNTs are based on multiple (2–10) concentric gra
enhanced tensile strength at merely 0.5 wt.% hybrid filler loading. Wu phene layers, cylindrically rolled into a tube shape with one atom
et al. [21] prepared micro-structured MWCNTs-CFs/ methylphenyl sil thickness, 0.5–50 µm length, and internal diameter of more than ten
icone resin (MPSR) composites by chemical grafting with enhanced nanometers. Based on structural arrangement, MWCNTs can be
interfacial properties, impact toughness, and heat resistance. In another described by two main models. First, the Russian doll model, where
Fig. 1. Key features of CNTs as a hybrid filler to fabricate polymer composites. Reproduced with permission from Refs. [13–16].
2
Fig. 2. Overview of SWCNTs’ and MWCNTs’ formation and different configurations of both types of CNTs. Reproduced with permission from Refs. [33–35].
individually rolled graphite sheets are settled in concentric cylinders. is the easiest and most used method to attain CNTs with fewer structural
Secondly, the Parchment model, where a single graphite sheet is rolled defects than other techniques. This technique is based on a vacuum
around itself consistently like a jellyroll or rolled newspaper. Third, chamber with two water-cooled graphitic electrodes detached by 1–2
mixed MWCNTs based on the Russian doll and Parchment models mm, with a diameter (6–12 mm), and the chamber filled with an inert
[30–32,35–37]. MWCNTs come in different complex arrangements in gas Helium (He) or Argon (Ar) at high pressure about 500 torr (inert gas
which each concentric tube can have different sequential structures and can also be replaced by methane or hydrogen) [39,40]. During the
thus possess unique properties. Hence, MWCNTs have high aspect ratios process, the two graphite electrodes (anode, cathode) approach each
and are far stronger than SWCNTs, so practically, these are preferred for other, making an arc, and temperature increases (3000–4000 ◦ C) suffi
high mechanical applications [32]. cient to sublimate the carbon-contained anode. This vaporized carbon is
accumulated at a 1 mm/min rate on the cathode (negative electrode) in
3. Preparation methods for CNTs the form of a black soot, and the remaining carbon is deposited (hard
gray shell) on the chamber’s walls. The scanning electron microscopy
Many impurities and side reactions always accompany the synthesis (SEM) images showed the formation of MWCNTs and also fullerene,
of CNTs, while the type and amount of these impurities rely on the amorphous carbon, and graphite sheets [38,40].
adopted preparation technique. Hence, purity is a crucial factor in The arc discharge method can be employed to obtain both SWCNTs
determining a material’s actual ability and properties; thus, much and MWCNTs. The key difference between both types of synthesis is the
research was made to explore innovative preparation methods for CNTs use of a catalyst, as in the synthesis of MWCNTs, there is no need for a
to attain maximum purity with the least side reactions. Several tech catalyst precursor, while SWCNTs can be achieved by using metallic
niques to develop CNTs are reported in different literature listed below catalysts, e.g., Nickel (Ni), Cobalt (Co), Iron (Fe), Silver (Ag), Palladium
[38]. (Pd), Platinum (Pt) and alloys. The catalyst (metal powder) is packed
into a hole in the anode, and thus, small-diameter SWCNTs are achieved
3.1. Electric/plasma arc discharge method using a complex anode. However, a Nickel-Yttrium (Ni-Y) graphite
mixture is mostly used to get a high yield (about 90 %) of SWCNTs with
Electric arc discharge is an extreme temperature (>1700 ◦ C) based an average diameter of 1.4 nm [41]. Fig. 3 represents the schematic
technique first employed for CNTs synthesis by Sumio Iijima in 1991. It framework of the arc discharge method.
3
Fig. 3. Schematic electric/plasma-arc discharge technique setup for CNTs synthesis. Adopted with permission from Ref. [42].
The main advantages of this technique are the ability to produce indicates the working setup of the laser ablation method.
CNTs in large quantities, the simple procedure, and the lack of need for This method is advantageous for producing CNTs with fewer metallic
multi-step purification. The disadvantages are a high-temperature impurities and thus less need for purification processes. However, it is
requirement, the need for a metallic catalyst, purification of the ob not beneficial for the economical production of CNTs because of the
tained product, and no control over the alignment (chirality) of pro need for high-purity graphite rods and high laser power. Moreover, the
duced CNTs [41,43]. Moreover, this method primarily consumes a produced CNTs are not necessarily uniform, and high-temperature
substantial amount of energy, so high-power levels are used, resulting in control is needed because the structure obtained below 1200 ◦ C has
increased carbon emissions. Also, the reliance on inert gases, e.g., heli many defects, and below 200 ◦ C, CNTs are not produced [40,41].
um or argon, waste generation and use of catalyst materials in this Additionally, the high-energy laser used in this method results in
process can cause serious environmental issues. Greener gases can be significant energy consumption and carbon emissions. Also, operating in
explored to address these concerns, and effective strategies for catalyst an inert gas environment and using metal nanoparticles as catalyst
recycling and waste reduction can be developed to boost energy effi materials with waste production can emit airborne nanoparticles,
ciency and prevent environmental and health hazards. causing severe environmental impact. Thus, using greener gases, recy
cling catalysts, employing waste reduction and management policies,
and ensuring safety measures can improve energy efficiency and reduce
3.2. Laser evaporation method environmental concerns.
The laser ablation/evaporation process is like an electric arc

discharge method in many aspects e.g., high temperature, inert gas- 3.3. Chemical vapor deposition method (CVD)
filled chamber, water-cooled surface, and use of metallic catalyst
(mostly Ni or Co in this method) for SWCNTs synthesis. The key dif Chemical vapor deposition (CVD) is the most used technique
ference is that unlike producing a graphite electrode arc by electric commercially producing CNTs. The key difference between CVD and
current, a pulsed and continuous laser beam (Nd: YAG) with wavelength other methods is that, here, the CNTs are obtained by the decomposition
(355 or 1064 nm) is used to evaporate the graphite target [44]. In this of carbon-containing compounds, while in prior methods CNTs were
method, a quartz tube containing the graphite block is placed in the produced by sublimation of graphite. However, researchers currently
chamber filled with He or Ar gas and high-power laser vaporizes the employ many CVD types, e.g., catalytic CVD, plasma enhanced oxygen
graphite billet at the temperature (1200 ◦ C), and CNTs are obtained with assisted CVD, radiofrequency assisted CVD, water-assisted CVD, mi
few impurities. It was also observed that the diameter of produced CNTs crowave plasma-enhanced CVD, and hot filament CVD. Moreover, the
is highly dependent on laser power, i.e., by increasing the power of the CVD method may vary based on reactor pressure (high, low or atmo
laser, smaller diameter CNTs can be attained [45]. Fig. 4 briefly spheric), reactor type (hot wall or cold wall CVD), and carbon source
Fig. 4. Schematic representation of laser evaporation/ ablation method. Adopted with permission from Ref. [46].
4
(solid, liquid or gas) [47–49]. reactor designs and recycling of precursor gases and catalyst materials
Apart from others, catalytic chemical vapor deposition (CCVD) is can reduce the energy requirements and help mitigate the CVD process’s
currently popular for highly pure and large-scale CNT production of environmental effect.
CNTs. In this method, a gaseous precursor reacts and makes a solid In conclusion, there are challenges in the traditional production
coating on a heated (500–1000 ◦ C) substrate placed in the reactor, methods of CNTs. Although different approaches e.g., arc discharge in
producing CNTs. The schematic process is as follows: a substrate with a liquid media (water or ionic liquids lowers the requirement of inert
catalytic metal (Ni, Co, Fe, or combined) layer is placed and heated in gases), bacterial synthesis (micro-organisms used to produce CNTs,
the reactor, and a gaseous precursor (usually consisting of inert gas and lowering the demand for high temperatures and toxic chemicals), solar
hydrocarbons) enters the chamber at room temperature [50,51]. The gas thermal synthesis (CNT synthesis using solar energy, reduces carbon
is heated as it approaches the heated substrate, chemical reactions emissions and the need for traditional energy sources, green solvents,
occur, and CNTs start growing at the corners of catalytic metal particles hydrothermal synthesis, and plasma enhanced CVD offer environment-
on the substrate (based on adhesion between catalytic particles and friendly production of CNTs but lack in commercial production.
substrate, the catalytic metal particles can be on the top or bottom of
growing CNTs). In contrast, waste gases are removed by gas outlets. This 4. Preparation methods for CNTs/Polymer composites
technique can produce both MWCNTs and SWCNTs. However, the type
of CNTs (MWCNTs, SWCNTs) production is based on temperature and The processing method, orientation, and CNTs dispersion signifi
gas precursor. Usually, MWCNTs are produced at 600–800 ◦ C and cantly impact the performance of CNT/polymer composites. Thus, many
SWCNTs at 900–1000 ◦ C. The diameter of CNTs depends on the size of techniques have been adopted in practice to integrate CNTs into the
catalytic metal particles [52,53]. polymer matrix, and CNTs’ dispersion was a major issue. Without
The advantages of the CVD technique are more significant control of appropriate dispersion the CNTs tend to accumulate and, as a structural
CNTs production parameters, no need for expensive graphite rods, lower defect, restrict composites’ mechanical and physical properties. How
temperature requirement (500–1000 ◦ C), and highly pure large-scale ever, the alignment of CNTs through the polymer composites provides
production of CNTs [54]. The disadvantages are structural defects in effective routes for phonon transmission. Thus, orientation improves the
CNTs, chances of non-compatibility of materials for chemical reaction, thermal and electrical properties of CNT/polymer composites [57–59].
and chemical and safety threats due to toxic, combustible, explosive, Traditionally, there are three major techniques for preparing CNT/
and corrosive gas precursors used in some cases [55]. Reactor configu polymer composites.
rations for CVD synthesis typically include a reaction chamber with
tubes containing an inert gas and specific hydrocarbons, as shown in 4.1. Conventional approaches
Fig. 5(a). SWCNT production commonly employs methane, while
MWCNTs use ethylene or acetylene. The process involves heating the 4.1.1. Solution blending
substrate to temperatures between 850 and 1000 ◦ C (for SWCNTs) or Solution mixing is a versatile technique for large-scale production of
550 and 700 ◦ C (for MWCNTs). During thermal decomposition, carbon is nanocomposites without losing the properties of nano-sized fillers. It is
generated from the hydrocarbons and dissolves into the metal nano also a widely used for fabricating CNT/polymer composites in labora
particle catalyst. A semi-fullerene cap forms once a critical carbon tories [57,60]. In this method, CNTs and polymer matrix are dispersed
concentration is reached, serving as the initial structure for cylindrical separately in (similar or different) solvents with good miscibility and
shell nanotube growth (Fig. 5b and c). This growth occurs through a then mixed. The process is followed by intensive agitation, e.g.,
continuous flow of carbon from the hydrocarbon source to the catalyst ultra-sonication, magnetic stirring, strong shaking, and high-speed ho
particle. The schematic steps of the CVD process are shown in Fig. 5. mogenization. Finally, a CNT/polymer composite film is formed by
However, the CVD method often relies on hydrocarbon gases, and solvent vaporization (with or without vacuum assist).
maintaining high temperatures for CNT growth may result in green However, CNT/polymer composite can also be produced by directly
house gas emissions and air pollution. To break the limit, research is mixing CNTs into the polymer solution, followed by intense ultra-
ongoing to develop sustainable precursor gases, like methane from sonication and shear homogenization for a long time. However, it
renewable sources or captured carbon dioxide. Additionally, efficient damages the CNTs (shortening of length), causing the lower
Fig. 5. Schematic process of catalytic chemical vapor deposition (CCVD) (a) Representation of CVD process and CNTs growth (b) CNT base growth mechanism (c)
CNT tip growth mechanism. Adopted with permission from Ref. [56].
5
performance of resultant composites. However, surface functionalized g., CNTs and polymer chains may be disrupted, and thus, intrinsic
CNTs offer better dispersion and interfacial bonding with polymer ma properties might diminish due to high shear forces and temperature [58,
trix, improving composites’ mechanical, thermal, and electrical prop 70].
erties. The selection of solvent is also an essential parameter for the
production of composites. Usually, low boiling point solvents are 4.1.3. In situ polymerization/ reaction processing
preferred because evaporation of high boiling point solvents is complex, In situ polymerization is another efficient approach for CNT distri
and it may get trapped during the solidification of composites, causing bution in insoluble and unstable polymers that cannot be handled by
structural defects. The low-viscosity solvents allow better dispersion solution blending and melt processing methods. During its processing,
[61–64]. dispersed CNTs are first mixed with a monomers solution, and finally,
The main advantage of this method is the probability of de-bundling CNT/polymer composites are achieved followed by certain conditions
of CNTs to provide quality dispersion [65]. Nevertheless, this technique [62,71,72]. The polymerization of thermosetting material, e.g., Epoxy,
has some disadvantages, such the possibility of leaching of added con unsaturated polyester (PET) is initiated by a curing agent/hardener as a
stituents and possible environmental contamination due to the large catalyst. Polymerization occurs in thermoplastics by temperature raising
amount of solvent, and it provides no solution for insoluble polymers or adding an initiator [60].
[58]. This technique is beneficial for homogenous and uniform distribu
tion and compatibility of filler-matrix and provides a strong interaction.
4.1.2. Melt blending However, there are some disadvantages, as this processing involves
Melt blending is a simple, environmentally friendly, low-cost alter expensive equipment and requires a large volume of solvent [58].
native method for insoluble thermoplastic polymers to produce com
posites. Thermoplastic polymers become soft when heated at elevated
temperatures and hard when cooled. Thus, polymer pellets are melted in 4.2. Modern approaches
this method, and viscous liquid is mixed with additives, e.g., CNTs,
followed by shear forces using Banbury mixer and extruder machines. At 4.2.1. Layer by layer (LBL) assembling method
the end, the sample is air dried or passed by a water bath to solidify and The LBL is a simple, cheap, and effective technique to fabricate
cut into desired dimensions and shapes. In this way, a high sample molecular assemblies of multi-functional tailored materials with nano
volume can be produced [58,60,66,67]. meter thickness, which can be used in high-scale production of highly
This method is fast and industrially friendly, and no solvent is needed integrated micro-sensors.
for processing [68,69]. However, this technique has some drawbacks, e. The processing of this method, Fig. 6(a) and (b), is followed by
dipping a substrate into the dispersed solution of CNT and
Fig. 6. (a) Schematic representation of the LBL film-deposition. Steps 1 and 3 show the adsorption of polyanion and polycation, steps 2 and 4 represent washing
steps. (b) Two adsorption paths, LBL deposition for polymers and polymers with nanoparticles. Adopted with permission from Ref. [73].
6
polyelectrolyte. A thin composite film is created on the substrate and substrates by thermal rolling at 130 ◦ C. Remarkably, a 100 μm thick
washed with pure water to remove weakly bonded polyelectrolytes. The composite membrane showed a specific shielding efficiency of 13,734
substrate is first dipped into the positively charged polyelectrolyte so dB cm2 g− 1, surpassing previous MWCNT/polymer composites. Several
lution and later into the negatively charged polyelectrolyte solution to studies have reported excellent mechanical, electrical, and thermal
achieve a double-layered composite film [74,75]. This approach can also properties of polymer composites produced by the BP-based approach
be employed in the fabrication of inorganic nanoparticles (nano-wires [82–86]. Fig. 7 shows the whole schematic process of the experiment.
and nano-sheets) into organic polymers, and it is easier to control the However, conventional and current preparation methods of CNTs
CNT ratio and thickness of prepared composites [73,74]. hybrid polymer composites suffer significant limitations concerning
scalability, advanced apparatus requirements, and expenditure. For
4.2.2. Swelling method example, traditional methods like solution blending, melt blending, and
The swelling technique is an efficient approach to producing high- in situ polymerization are effective at smaller scales but do not suffice for
strength and robust CNT/polymer composites. It allows us to intro industrial production. Ensuring bulk production with greater control
duce CNTs in temperature-sensitive and insoluble polymer products. over quality requires specialized equipment, which results in extended
This approach allows CNTs to be dispersed even in very small-thickness costs and compact practicality. While modern techniques, e.g., LBL
polymer film and produce composites with high mechanical, thermal, assembling, swelling method, and BP approach, are effective but
and electrical properties. Ian et al. [76] produced CNT-reinforced Kevlar complicated and laborious. Such issues can be resolved by advanced
composites using the swelling method. While processing, MWCNTs and automation and process optimization. Thus, there is a need to explore
commercially available Kevlar fiber-based suspension was produced cost-effective equipment by recognizing sustainable material resources.
using N-methylpyrrolidone (NMP) as solvent under ultra-sonication.
The Kevlar fiber swells, and CNTs diffuse into the fiber during the pro 5. CNTs hybrid filler polymer composites
cess. Finally, the sample was dried and characterized, resulting in
improved mechanical properties of Kevlar-CNT composite. In another CNTs are a promising candidate for fabrication of polymer compos
report, conductive CNT-based polyethylene (PE) composites were pre ites due to higher strength, high elastic modulus, surface area, stiffness,
pared by utilizing the same strategy i.e. MWCNTs were dispersed into porosity, corrosion resistance, mechanical and chemical stability, and
the swelled thin PE film using tetrahydrofuran (THF) as a solvent and remarkable mechanical, thermal, and electrical properties [87]. Due to
the process was followed by ultra-sonication [74]. exceptional nanostructure and properties, CNTs are an ideal precursor
for polymers, metal/alloys, and ceramic composites [88]. The bulk
4.2.3. Bucky paper (BP) based method production of composites by using primary filler, e.g., CNT, is inflated.
Bucky paper (BP) is a porous and very thin sheet of CNTs incorpo Thus, secondary filler is introduced to reduce the cost.
rated by filtration of CNTs dispersed in a suitable solvent. In this However, due to the nano-sized structure and reacting ability of
approach, the BP is filled with a polymer matrix or introduced between CNTs, there is a higher probability of health risks during the production
laminates and polymer composites, producing excellent mechanical and and execution of nanocomposites. Mainly, handling the airborne and
electrical properties [74,77,78]. Besides Buchner filtration, BP can also disposal of CNTs is problematic, and it causes severe toxic effects if
be produced by the domino-pushing effect. The MWCNTs are vertically inhaled, e.g., lung cancer, pleural malignant mesothelioma, and respi
aligned in this method on a silicon substrate (10 cm diameter). Later, a ratory issues. Research is ongoing to make CNTs ecologically sustainable
microporous membrane is placed on the top and pressed by constant and reduce harmfulness through surface modifications.
pressure. This process is repeated several times, and finally, the silicon Currently, graphene oxide [89], silica [90], carbon black (CB) [91],
substrate is detached, and BP is peeled off from the porous membrane by zinc oxide (ZnO) [92], nano-clay (NC) [93], conductive carbon black
ethanol. This BP is strong and flexible with improved electrical (2.0 × (CCB) [94] and graphite [95] are used as secondary filler to produce
104 S/m) and thermal (153 W m− 1 K− 1) properties [79]. CNT hybrid filler. Graphene has incredible properties, e.g., flexibility,
Teotia et al. [80] prepared BP-based phenolic resin composites. The lightweight, fire resistance, exceptional electrical and thermal conduc
MWCNTs were dispersed in acetone and then added to phenolic resin. tivity, higher modulus, and strength. CNT and Graphene particles (GP)
The suspension was stirred for 5 min by a high-speed mixer (3000 rpm) hybrid filler-based natural rubber (NR) composites were prepared, and it
to get a homogeneous amalgamation. Later, the mixture was filtered by was observed that a combination of 3 phr CNT and 30 phGP showed
a specially designed filtration system. The filtered material was dried excellent performance in relaxation modulus and thermal stability of
and compression molded, resulting in BP-phenolic resin composite CNT/GP-NR composites as compared to CNT-NR and GP-NR composites.
paper. In another study, Kim et al. [81] introduced MWCNT BP and The characterization showed that CNT networks improved GP disper
electro-spun polyacrylonitrile (PAN) nanofibers based ultrathin, light sion and prevented agglomeration, facilitating electron tunneling. Due
weight composite membranes using electrospinning, thermal-rolling, to the connected filler network, the conductive properties and dielectric
and vacuum filtration. As a result, smooth surfaces, high surface en constant of NR composites was significantly improved [96].
ergy, and impressive mechanical strength of 19 MPa were achieved with Luo et al. [97] introduced pristine CNTs and functionalized f-CNTs in
an enhanced interfacial network between the buckypaper and nanofiber polymethyl methacrylate (PMMA)/GNP composite to produce a hybrid
Fig. 7. Schematic representation for synthesis of BP-based nanofiber (BP/NF) composite. Adopted with permission from Ref. [81].
7
composite (PMMA/GNP/f-CNT) with three-dimensional (3D) structure Dehrooyeh et al. [105] fabricated glass fiber/CNT/epoxy hybrid
with different ratios. The investigation of these composites showed 3D composite to obtain higher mechanical properties. The experiment was
networks inside, and due to synergistic effects, the thermal and electrical carried out in two significant steps. Firstly, the CNT/Epoxy composites
conductivity was significantly improved in the perpendicular direction. were prepared using CNT aspect ratios 0.1, 0.5 and 1.0 wt.% by solution
Skórczewska et al. [98] prepared poly-vinyl chloride, carbon blending method and tested for mechanical properties. It was observed
fiber/multiwalled-carbon nanotube (PVC/CF/MWCNT) hybrid com that a composite with 0.5 wt.% of CNT showed higher Young’s modulus
posites with hybrid filler ratios 1 wt.%, 5 wt.% and 8 wt.%, respectively. of 1.8 GPa and a tensile strength of 61 MPa.
The Processing of composites was followed by coating of CNTs onto CFs In the second step, the glass fiber/CNT/epoxy hybrid composite was
using polyvinyl acetate (PVAc) as an adhesive for better dispersion. It prepared by a hand-layup approach using a 45:55 filler-to-matrix ratio.
was demonstrated that with increase of filler content the electrical The investigation showed that hybrid composite followed the same
properties improved, while elastic modulus, rigidity and impact strength trend, i.e., at 0.5 wt.% CNT loading the ultrahigh Young’s modulus of
of composites was significantly increased and thermal stability slightly 24.9 GPa and a tensile strength of 300 MPa were achieved.
enhanced. Nabinejad et al. [99] developed pristine MWCNTs and oil Fig. 8(a) shows SEM images for CNT dispersion in the epoxy with
palm shell (OPS) powder-based unsaturated polyester (UP) composites various ratios of 0.1, 0.5, and 1.0 wt.% and at 0.1 wt.% there are few
using a solvent mixing technique with ultrasonication. Initially, the CNTs with uniform distribution and no agglomeration. Moreover, at 0.5
MWCNTs were precisely dispersed in four different solvents, e.g., wt.%, the structure is more organized, and dispersion is homogeneous
acetone, styrene, ethanol, and methanol. Secondly, polyester resin was with no accumulation of CNTs. Meanwhile, with 1.0 wt.%, the viscosity
added by shear mixing and ultrasonication. Later, the solution was increases, and CNT agglomeration causes structural defects and abnor
heated to evaporate the solvent. Lastly, the natural filler OPS was added malities, decreasing the mechanical properties. Fig. 8(b) shows stress-
and prepared composite solution was passed through molding and strain curves of CNT/Epoxy composite with CNT aspect ratios (0.1,
casting process. The investigation of these hybrid composites revealed 0.5 and 1.0) wt.%, and Fig. 8(c) shows stress-strain curves for glass
that, increasing the MWCNTs content (0.2–0.4) phr leads to maximum fiber/CNT/epoxy hybrid composite with CNT loading (0, 0.5 and 1.0)
tensile and flexural strength, while increasing the MWCNTs content (> wt.%.
0.4 phr) the viscosity increases, and tensile modulus starts decreasing In another research, Xu et al. [106] fabricated Graphene oxide/
due to structure abnormalities. carbon nanotube aerogel-based polystyrene (GOCA/PS) hybrid com
Liu et al. [100] introduced CNT/CF hybrid filler to prepare epoxy posites by hot pressing and in-situ polymerization processes and
composites for industrial scale. While preparing, the CNT was initially explored the compressive, flexural, tensile, and impact strengths with
functionalized with an amine monomer by a chemical modification different filler loadings (0, 0.8, 0.9, 1.0, 1.1 and 1.2) wt.%. In the
process to achieve better dispersion in a sizing agent. Later, the CNT fabrication process, the GOCA large-size sheet was prepared and sub
accompanying sizing agent was uniformly dispersed on the CF surface. merged in a solution containing a 40 g PS mixture and 0.18 g of azo
After drying, the epoxy-containing hardener was infused through a bisisobutyronitrile (AIBN) (analytical reagent). Later, the samples were
hybrid filler. The process was followed by solution blending and soni passed through different temperature ranges for 12 h, hot pressed, and
cation methods. FTIR and XPS characterized the specimen, and it was molded. Finally, the prepared GOCA/PS composites were tested for
observed that integration of CNT at the interface highly improved the mechanical properties.
interfacial shear strength of the prepared material. As shown in Fig. 9, all four properties improved with increasing filler
CNT hybrid composites offer many real-world industrial applica content. The calculated increased values compared to pure PS were as
tions, such as in the automotive sector, utilization of CNT composites in follows: tensile strength (103.29 %), flexural strength (60.30 %),
Ford’s GT supercar wheels greatly enhanced fuel efficiency and perfor compressive strength (177.03 %) and impact strength (611.38 %).
mance. CNT composites are applied in tennis rackets HEAD and Babolat However, in Fig. 9(a) at loading 0.8 wt.%, the curve line followed the
to achieve rigidity and reduced vibration. In electronics, CNT-based 3D same trend as pure PS. This is due to a very low aspect ratio, and the
printed filaments offer electrically conductive components, which assist GOCA was probably destroyed during the in-situ polymerization process.
in the prototyping of electrical devices. In textiles, CNTs are utilized in The results were excellent at 1.1 wt.% compared to 1.2 wt.% due to
smart fabric brands, e.g., Under Armour, for moisture, odor, and per increased density and porosity with increasing content ratio causing
formance control of sportswear. Moreover, CNT composites are used in structural defects and deprivation of mechanical properties. Fig. 9(b)
Boeing 787 Dreamliner for reduced weight and enhanced fuel efficiency. presents flexural stress-strain curves, Fig. 9(c) impact strength, and
Fig. 9(d) compression stress-strain curves. These graphs provide concise
6. Mechanical properties of CNT hybrid filler polymer and essential information about the material’s mechanical behavior
composites under different loading conditions.
CNTs own high mechanical properties, e.g., higher modulus 7. Thermal properties of CNTs hybrid polymer composites
(270–950) GPa, higher tensile strength (11–63) GPa, and lower density
(2.1) gcm− 3, due to unique structure with regular arrangement of sp2 With the increasing demand for multi-functional and smart mate
covalently bonded carbon atoms making it suitable filler for polymer rials, overheating of devices is inevitable, and thus, the fabrication of
composites. Moreover, CNTs synergize with other potential fillers and high thermal conductive, heat dissipative polymer composite materials
provide extraordinary mechanical properties [62,101–103]. Effective can resolve this issue. CNTs possess unique and strong configurations
distribution and homogeneous dispersion of CNTs through the polymer with high in-plane thermal conductivity (3000–3500 Wm− 1 K− 1) [107],
matrices play a key role in constructing interconnected 3D structures, which makes them ideal fillers for polymer matrices. CNTs are highly
which lead to outstanding mechanical properties [104]. effective in the thermal conductivity enhancement of hybrid polymer
Park et al. [103] reported MWCNTs and CFs hybrid filler-based composites due to synergistic behavior with other fillers by the forma
alkali-activated slag (AAS) composites using a solution blending tech tion of 3D bridge networks, which facilitates phonon transmission [108,
nique. The investigation results revealed synergistic effects due to the 109].
formation of bridging structures. The hybrid composite formation was Li et al. [110] designed hexagonal boron nitride (h-BN), reduced
followed by diverse proportions (0, 0.1, 0.5, 1.0, and 2.0) wt.% of hybrid graphene oxide (rGO), and CNTs based epoxy (EP) composite using a
fillers, and it was noted at 0.5 wt.% of MWCNTs and CFs, a highly layer-by-layer technique. In the fabrication process, the h-BN was
connected structure was produced which showed enhanced mechanical modified with tannic acid (TA) for better dispersion in EP coatings and
and electrical properties. later blended with rGO and CNTs. The prepared TA@BN-rGO-CNT/EP
8
Fig. 8. (a) Dispersion of CNTs in epoxy matrix at 0.1 wt%, 0.5 wt%, and 1 wt%. (b) Stress-strain curve of CNT/epoxy nanocomposites at different CNT weight
percentages. (c) Stress-strain curve of glass fiber/CNT/epoxy hybrid composites. Adopted with permission from Ref. [105].
Fig. 9. Mechanical properties (a) typical stress-strain curves, (b) stress-strain curves of flexural, (c) impact strength, (d) stress-strain curves of compression. Adopted
with permission from Ref. [106].
composite were investigated for higher thermal conductivity. It was reported the role of CNTs as a hybrid filler in the thermal conductivity
demonstrated that a well-defined interconnected hybrid structure was enhancement of polymer composites [111–114]. However, some refer
produced and at 46 Vol% filler loading the thermal conductivity reached ences are added and explained in this study.
5.65 Wm− 1 K− 1 (22.6 times higher than pure EP). Numerous articles Wang et al. [115] successfully developed siloxane (SiO) and
9
MWCNTs core-shell hybrid epoxy resin (EPR) composite to attain high nucleation effects in the crystallinity of the PVDF matrix. However, it
thermal conductivity. In the preparation process, initially, MWCNTs was observed that the addition of CNT into the PVDF/GNP composite
were treated with several surfactants and reagents, Cetyl exhibited excellent 3D conductive pathways rather than the addition of
trimethylammonium bromide (CTAB) to achieve surface polarity and GNP into PVDF/CNT composite. Thus, due to the higher synergistic ef
later reacted with tetraethoxysilane (TEOS) via hydrolysis condensation fect, the thermal conductivity of PVDF/CNT/GNP composite was highly
reaction and other saline coupling agents; 3-methacryloxypropyl tri enhanced. Fig. 11(a) shows the improvement in thermal conductivity
methoxy silane (MPS), 3-glycidoxypropyltrimethoxysilane (GPTMS) to with increasing filler loading. The thermal conductivity of all
produce core-shell hybrids. Finally, these core-shell hybrid fillers are PVDF/CNT/GNP-x specimens is higher than PVDF/GNP-x with the same
impregnated with epoxy resin to produce SiO/MWCNT/EPR composite. GNP loading. At 20 wt.%, the PVDF/GNP-20 composite presented only
The characterization results showed precise dispersion through the 1.64 W m− 1 K− 1 thermal conductivity, while PVDF/CNT/GNP-20
structure, and it was observed that with 1 wt.% content loading showed 1.92 W m− 1 K− 1. Fig. 11(c) shows the thermal conductivity
SiO/MWCNT/EPR achieved 0.55 Wm− 1 K− 1 thermal conductivity. enhancement for PVDF/CNT-x and PVDF/GNP/CNT-x specimens with
Figure shows different graphs related to thermal variations. Fig. 10(A) increasing filler loading. The graph shows that at CNTs loading 20 wt.%,
shows that the thermal conductivity of each composite is enhanced with the thermal conductivity of PVDF/CNT-20 was 0.56 W m− 1 K− 1 and
increasing filler content. Fig. 10(B) represents the thermal conductivity PVDF/GNP/CNT-20 achieved 0.69 W m− 1 K− 1. Fig. 11(b) and (d)
enhancements (TCE%) for all prepared composites, and core-shell hy represent the thermal enhancement factor (%) related to filler aspect
brids with saline coupling agents showed enhanced thermal conduc ratios.
tivity as compared to MWCNT/EPR composite. Fig. 10(C) shows the Besides the increased thermal performance, inspecting the long-term
surface temperature variations for SiO/MWCNT-MPS/EPR and stability and aging effects of CNT hybrid composites cannot be over
MWCNT/EPR composites in the 20–80 ◦ C temperature range, captured looked. To address this issue, the precise control over CNT loading,
via infrared camera. Fig. 10(D) represents a brief comparison of thermal particular selection, and processing parameters plays a decisive role in
conductivity enhancement with increasing filler volume (%) between the assembly of a characteristic composite material. After fabrication,
virgin MWCNT/EPR (red) and SiO/MWCNT-MPS/EPR (black) com the composite behavior over time and performances were analyzed by
posites. The improved thermal conductivity is due to connected surface various characterization techniques such as thermogravimetric analysis
and inter-links between core-shell hybrid fillers. (TGA), differential scanning calorimetry (DSC), dynamic mechanical
In another article, Xiao et al. [116] introduced poly (vinylidene analysis (DMA), and infrared spectroscopy (FTIR). Herein, TGA reveals
fluoride) (PVDF)/GNP and PVDF/CNT composites to produce further the shifts in decomposition temperature and weight loss and shows the
ternary PVDF/CNT/GNP and PVDF/GNP/CNT composites. The process composite aging process. Meanwhile, mechanical properties, e.g., ten
was carried out using a solvent method using N, N-dimethylformamide sile strength, flexural properties, and impact resistance, can affect the
(DMF) as a solvent, and the solution was passed through sonication and composite’s ability to conduct heat effectively. Moreover, the study in
stirring for 2 h at 55 ◦ C for homogeneity. Finally, the specimens were hot volves ecological influences, like UV radiation, moisture, and chemical
compressed and molded for investigation. The investigation results exposure, which can stimulate degradation in CNT-polymer composites.
revealed that the addition of CNT and GNP greatly enhanced the
Fig. 10. (A) Thermal conductivities and (B) thermal conductivity enhancements of different MWCT/EPR composites as the functions of filler contents. (Black:
MWCT/EPR, red: MPS/MWCT/EPR, blue: GPTMS/MWCT/EPR, olive: SiO/MWCT-MPS/EPR, pink: SiO/MWCT-GPTMS/EPR) (C) The surface temperatures of
MWCT/EPR and SiO/MWCT-MPS/EPR composites vary over time under the heating state. (D) EMA model fitting results of experimental data for MWCT/EPR (red)
and SiO/MWCT-MPS/EPR (black) composites at different filler loadings. Adopted with permission from Ref. [115].
10
Fig. 11. (a and c) Variations of thermal conductivity versus the content of fillers in the PVDF composites, and (b and d) the comparison of the thermal enhancement
factor between binary and ternary composites as indicated in the graphs. Adopted with permission from Ref. [116].
8. Electrical properties of CNT hybrid filler polymer composites Incorporating f-G-f-CNTs in PES composites significantly enhanced
electrical conductivity compared to composites filled with individual f-G
CNTs are ideal electrical conductors with high current carrying ca and f-CNTs fillers, owing to the synergistic effect. Fig. 12(a) illustrates
pacity due to high bonding strength between carbon atoms in the the experimental data, showing a notable peak at a f-G:f-CNT filler ratio
nanostructure. High electrical conductivity 106–107 Sm− 1 [117], lower of 1:3. Notably, the electrical conductivity of σf-G-f-CNTs (Wf-G/Wf-CNTs =
density, and other excellent properties make it a perfect reinforcing 1:3) was 3.45 times higher than σf-G and 10.6 times higher than σf-CNTs.
material for polymer composites. Fig. 12(b) portrays the variation in electrical conductivity of f-G-f-CNTs
Saleh et al. [118] developed CNT and carbon black (CB)/polystyrene (Wf-G/Wf-CNTs = 1:1)/PES composites as a function of f-G-f-CNT content
(PS) nanocomposites via melt mixing technique. During preparation while maintaining a fixed Wf-G:Wf-CNTs ratio of 1:1 in the mixed fillers.
CNT/PS, CB/PS and CNT: CB/PS composites were produced and inves The conductivity behavior of this composite, combining a conductor and
tigated for electrical conductivity enhancement. It was observed that an insulator, can be effectively elucidated through the application of the
CNT: CB/PS composite with CNT: CB (75:25) showed excellent electrical modified classical percolation theory.
conductivity as compared to other composites due to synergistic effects
σ = σ0 [(Φ − Φc )/(1 − Φc )]t (1)
through the well-organized structure.
Yu et al. [119] reported expanded graphite (EG)-CNT/EP hybrid The symbol σ represents the composite’s conductivity, while the
composites with enhanced electrical conductivity. In the preparation filler material’s conductivity is denoted by “σ0”. The volume fraction of
process, the EG was loaded with a metal catalyst, and hybrid EG/CNT the mixed filler is expressed as “Ф” and “Фc” refers to the volume
filler was produced by direct CNT growth onto EG via modified com percolation concentration. Moreover, the parameter “t” corresponds to
bustion and thermal chemical vapor deposition (CVD) technique. Then, the universal critical exponent. The conductivity behavior of the f-G-f-
EG/CNT filler was impregnated with EP resin, and the prepared com CNTs (Wf-G/Wf-CNTs = 1:1)/PES composites exhibited excellent agree
posite was hot pressed (80 ◦ C) and molded for 2 h. The characterization ment with the predicted percolation characteristics described by Eq. (1).
results revealed that EG-CNT/EP achieved remarkable electrical con The log-log plot of σ versus (Ф− Фc) in the inset figure displayed the best
ductivity compared to separate EG and CNT or simply mixed EG-CNT linear fit, yielding Фc = 0.22 vol%, t = 3.36, and a correlation factor R =
fillers. There are many references to demonstrate the fabrication of 0.972. Notably, the volume percolation concentration for these com
hybrid polymer composites with increased electrical properties using posites was significantly lower than that of the f-G/PES composite.
CNTs as reinforcing material [120–122]. Here, we report a detailed Hu et al. [124] synthesized CNTs and graphite (Gr) hybrid
analysis of a few articles. filler-based polypropylene (PP) composites via Pickering emulsion
Zhang et al. [123] prepared and investigated the synergistic effects in technique with different wt.% filler loadings. During the experimenta
poly (ether sulfone) (PES) composites reinforced with functionalized tion, three different network structures PP@Gr, PP@(CNTs/Gr), and
multiwalled carbon nanotubes (f-CNTs) and functionalized graphene (CNTs/PP) @Gr were fabricated and characterized to investigate elec
(f-G) for electrical conductivity enhancement. Composite preparation trical conductivity. The investigation revealed that (2 wt.%-CNT/PP)
was followed by solution casting and sonication techniques. The char @Gr at 13.01 wt.% Gr presented the maximum electrical conductivity
acterization results showed that the electrical conductivity of hybrid (1.45 Sm− 1) compared to all other composites. The structural analysis
composite with merely 5 wt.% of f-G-f-CNTs /PES was 2.2 and 8.9 times demonstrated that CNTs performed as a bridge, and a dense 3D structure
higher than 5 wt.% of f-G/PES and f-CNTs/PES composites. was produced, resulting in superior electrical conductivity. Fig. 13(a and
11
Fig. 12. (a) The DC conductivity of the f-G-f-CNTs/PES composites as a function of the weight ratio of f-G and f-CNTs in the mixed fillers at a mixed filler loading of 5
wt%. (b) Log (DC conductivity) as a function of the f-G-f-CNT content for the f-G-f-CNTs (Wf-G/Wf-CNTs = 1:1)/PES composites. The inset shows a log–log plot of the
conductivity σ as a function of Ф− Фc with an exponent t = 3.36 and a critical volume content Фc = 0.22 vol.% with a correlation factor of R = 0.972. Adopted with
permission from Ref. [123].
Fig. 13. (a) TGA thermograms of PP@Gr microparticles, (a1) the residual mass of the microparticles, and (b) the conductivity of composites. Adopted with
permission from Ref. [124].
a1) represents the TGA results for thermal stability of PP composites with 9. Applications
different Gr content and shows PP decomposition starts at 380 ◦ C and
completely decomposes at 800 ◦ C, but Gr is not decomposed. Fig. 13(b) In recent eras, the need for multi-processing and smart materials has
compares electrical conductivity enhancement for different composites been increasing rapidly, which is a bottleneck to traditional materials.
with different CNTs loading related to increasing Gr content (wt.%). Polymer composites are good alternatives. However, multi-functional
Owing to terrific electrical properties, CNT composites find wide operations require all good properties on the same page, and some in
spread employment in electronics. Conversely, the attributes come with dividual filler composites still have limitations. Consequently, extensive
safety challenges mainly linked with long and rigid airborne CNTs cause studies were conducted, and hybrid polymer composites were found
skin and eye irritation, and breathing of these nanoparticles can result in outstanding with multiple properties fit for aerospace applications due
lung infections. Moreover, the toxic behavior of CNT triggers oxidative to synergistic 3D structures, easy Processing, low density, strength-to-
damage in biological systems and affects the central nervous system. weight ratio, and inexpensive. CNT hybrid polymer composites offer
Careful safety procedures involving engineering controls to monitor the high mechanical, thermal, and electrical properties using structural
airborne CNT levels, worker training, and personal protective equip geometry, making them suitable for multi-functional operations and
ment are essential to tackle these concerns. Moreover, risk management engineering applications [102,125]. This article summarizes some
strategies, emergency response procedures, and regular safety assess top-notch applications of CNT polymer composites.
ments are essential to utilize the potential of CNTs in industrial appli
cations fully. 9.1. Aerospace
Beyond the realization of synergistically enhanced electrical con
ductivity, the large-scale production of CNT hybrid composites is highly Aerospace industries design, produce, and maintain aircraft, engines,
influenced by cost-effectiveness, scalability, and quality control. Pro space vehicles, missiles, and other propulsion units at large scale and
duction of CNTs and integration into polymer matrices can significantly thus require very high strength and durable materials. Due to easier
increase the overall cost of the composite materials. Thus, finding cost- molding, substantial strength, stiffness, and reduced weight, CNT
effective methods is crucial to make these composites commercially polymer composites are preferred for aerospace applications. Much
feasible. Furthermore, maintaining consistent quality and properties at a research was conducted to explore the properties and usage of CNT/
large scale is a complex assignment that demands sensible control and polymer composites in aerospace industries [126–129].
optimization of various factors. Composite quality and performance Zhang et al. [130] developed ultrathin CF-reinforced CNT/EP com
depend highly on CNT dispersion variations, polymer/CNT bonding, posites by ultrasonic tow-spreading technique for aerospace applica
and homogeneity. Thus, the execution of strict quality control measures tions. The composites were prepared with different CNT loadings, and it
is essential to validate the reliability of the final product. was observed that, at 0.2 wt.% CNT and 24 wt.% CF loading, the
CF/CNT/EP composite achieved high tensile strength, compressive
strength, and interlaminar shear strength with improved electrical,
12
thermal, and electromagnetic interference (EMI) shielding efficiency. approximately 50 % of the weight of automobile and fuel utilization.
Bellucci et al. [131] designed Gr-CNT/EP composites and examined Moreover, CNT/polymer composites are used in fuel consumption fields,
the electrical resistivity at different pressure and temperature ranges. It braking systems, exhaust systems, vehicle carcasses, and body parts
was demonstrated that even a small change in CNT content highly [136]. In traditional vehicles, the fuel system is mainly based on metal
changes the resistivity values suitable for circuits used in aerospace parts, and it was risky to replace them with plastics due to the possibility
applications. CNT/ polymer composites are effective in weight reduction of electrostatic discharge. It is estimated that future vehicles will operate
and thus preferably used in aircraft manufacturing. Most parts in Boe via hydrogen fuel cells. A hydrogen fuel cell is a fuel system with
ings 767 and 747 are CNT and aluminum alloy composites, e.g., eleva renewable compressed hydrogen that operates the vehicle by conversion
tors, flaps, tips, rudders, and spoilers. of chemical energy to electrical energy without emitting hazardous CO2
Along with other challenges, weight reduction is essential in space gas. Currently, CNT composites are utilized to improve the efficiency of
vehicles, commercial and military aircraft, and considerable cost is hydrogen fuel cells, and their availability is expected soon in developing
devoted to quick and safe travel. During flights, there is a considerable countries [137]. CNTs are flexible, anti-corrosive, more transparent and
risk of lightning strikes, and the weight of aircraft also considerably less brittle, making it a suitable coating material for automobile surfaces
increases due to ice accumulation on aircraft surfaces for long flights. compared to traditional and expensive Indium Tin Oxide. CNT coating
Alemour et al. [132] demonstrated that lightning strikes and ice accu shows higher resistance against rust and extreme weather conditions
mulation on aircraft during flights reduce aircraft efficiency and cause and attributes higher strength and stiffness to the surface. The me
serious accidents. Thus, high thermal conductive CNT/polymer com chanical properties of materials for vehicle manufacturing are crucial in
posites are used to modify aircraft surfaces to resolve the ice accumu automobile industries. For a long time, steel alloys served for vehicle
lation issues and reduce weight and fuel consumption. Fig. 14(a) shows body manufacturing and other parts despite their heavier weight and
the lightning strike in and out of the mechanism through the aircraft corrosivity. Then, industries preferred aluminum because of its lighter
structure and the significance of using composite materials in the weight and corrosion resistance to replace steel. However, the usage of
aircraft exterior. Fig. 14(b) shows the effect of lightning strikes on aluminum is expensive and non-economical. Thus, CNT and its com
aircraft structures without composite materials. posite are the best alternatives to previous materials due to their flexi
Parveez et al. [133] and Lu et al. [134] reported that the Boeing 787 bility, remarkable mechanical properties, and low cost [138]. While
was the first commercial aircraft with the main structure 50 % composed selecting the material, Young’s modulus is the standard parameter for
of carbon-reinforced nanocomposite material. The details are high industries to measure the material strength and hardness, and it was
lighted in Fig. 15. The percentage of materials used are 50 % carbon found that Young’s modulus of CNTs is far better than steel and
composite, 20 % aluminum, 15 % titanium, 10 % steel and 5 % other aluminum.
materials. A 20 % weight reduction was achieved using composite ma Moreover, CNT composites are considerably resistant to weathering
terial. In comparison, the structure of Boeing 777 is composed of 50 % conditions, e.g., temperature variations, moisture, and pressure, making
aluminum and merely 12 % composite material. them suitable for experiments. Due to flexibility and structural integrity,
CNTs possess a bright future in aerospace applications, e.g., vehicle CNT composites are more favorable than traditional materials for the
weight reduction, enhanced self-healing properties, energy production, experimentation and molding of different structural designs for vehicles
improved controls with superior tolerance facilities and improved [139]. Fig. 16 summarizes the use of CNT composites in automobiles
thermal protection. Iqbal et al. [135] reported that CNT/EP nano reported by Cambridge Nanomaterials Technology Limited [140].
composites can play a substantial role in artificial intelligence and CNTs possess large bending constants due to their high strength and
telecommunication, especially for un-manned spaceships, and are straight structure. However, bending is essential to manufacture vehi
highly effective in weight reduction, aircraft wirings, ice protection, and cles of the desired shape. To make it possible, the points are marked at
fuel consumption. specific locations where bending is required, and structural faults are
However, aerospace materials are exposed to various stressors, introduced to obtain sharp bending. Such a facility is highly suitable for
including extreme temperatures, high altitudes, and varying pressure producing geometric and intricate automobiles [141].
conditions. Thus, long-term stability under environmental impact and Although these composites hold great potential in the aerospace and
extreme conditions is a crucial aspect and subject of exploration. Hence, automotive industries, they struggle with scalability and affordability on
studies are ongoing to evaluate competent CNT composites with high a large scale due to cost-effectiveness because recent production pro
thermal stability, erosion resistance, and resistance to radiation. Also, cedures are expensive and laborious. Thus, scaling of production
environmental impact, search for sustainable and recyclable composites methods, e.g., improvements in solution-based processing and roll-to-
and safety in extreme conditions are under consideration. roll manufacturing, can reduce costs and ease accessibility for world
wide applications. In comparison, affordability can be addressed
9.2. Automotive through various factors, including developing cost-effective production
processes, sourcing raw materials, and economies of scale. Moreover,
The automotive industry’s quest for low-weight, efficient vehicles recycling and sustainability aspects must be considered to ensure long-
with innovative designs and color schemes is headed to CNT/polymer term cost-effectiveness. The aerospace and automotive industries are
composites. It was determined that polymer composites reduce increasingly focusing on environmental sustainability, and CNT
Fig. 14. (a) The continuous conductive path of low resistance over the entire aircraft exterior. (b) Lightning strike effects. Adopted with permission from Ref. [132].
13
Fig. 15. Overall distribution of composite materials used in Boeing 787 aircraft. Adopted with permission from Ref. [132].
Fig. 16. Possible applications of CNT composites in automobiles. Adopted with permission from Ref. [140].
composites can contribute to this goal by reducing weight and designs for multi-functional electronic devices. Moreover, this minia
improving fuel efficiency. turization leads to device heating problems, which affects device effi
ciency and lifetime. So, there is a need for multi-functional materials to
9.3. Electronics reduce the device weight, cost, and size and establish attractive designs
with thermal heat dissipation at a time [142]. CNT polymer composites
Currently, the tendency towards smart electronic devices is over are ideal for flexible and wearable electronic applications due to the
whelming in the marketplace. Thus, the world’s research and engi substantial flexibility, mechanical strength, and thermal and electrical
neering community always looks for innovative, attractive, and smaller properties of CNTs [143,144]. The fabrication of CNTs composite
Fig. 17. Schematic of a typical module for thermoelectric generators (TEGs). Adopted with permission from Ref. [146].
14
networks plays a significant role in thermoelectric devices due to their thermal properties, CNTs and their polymer composites are promising
excellent thermal properties. These devices utilize waste heat to elec materials for energy storage devices. SWCNT composites are favorable
tricity using the Seebeck effect [145]. Fig. 17 depicts a representative for photovoltaic applications as it can absorb light with a wide range of
thermoelectric (TE) device that requires both n-type and p-type TE wavelengths, i.e., visible to infrared, and contain both (electrons and
materials. These materials are assembled using electrodes, bonding holes) charge carriers [167,168]. In batteries, CNT polymer composites
materials, and insulators to create thermoelectric generators (TEGs) are utilized as an active anode or cathode material due to higher elec
[146]. trical conductivity while, in solar cells decrease the need of noble metals
Wang et al. [147] developed Piezoelectric poly(vinylidene traditionally used as catalysts to enhance fuel cells’ performance [169,
fluoride-trifluoroethylene) P(VDF-TrFE) nanofibers and Poly 170].
dimethylsiloxane (PDMS)/MWCNT thin composite membrane-based Chen et al. [171] reported a CNT/PPy composite based on a flexible,
flexible nanogenerator for finger motion detector application, working high-performing super-capacitor. In preparation, primarily CNT flexible
under hybrid triboelectric and piezoelectric processes. While Processing, freestanding films were fabricated via a vacuum filtration approach, and
the electrospinning technique formed the triboelectric and piezoelectric then CNT/PPy electrodes were synthesized through the electrodeposi
functional layers, and nanogenerator triboelectric performance was tion process of PPy. It was observed that mechanical and electro
improved by increasing the initial capacitance of PDMS/MWCNT com chemical properties were significantly enhanced and a robust device
posite by doping of MWCNTs as a flexible frictional layer into PDMS with higher flexibility, longer lifetime, lightweight, and higher volu
films. The investigations showed that under 5 N pressure in open cir metric capacitance (4.9 F/cm3 at 0.05 A/cm3) was achieved. The per
cuits, the nanogenerator’s triboelectric and piezoelectric output peak formance analysis revealed that the device can light up 53 LEDs and a
voltages were 25 V and 2.5 V, respectively. Moreover, under 5 MΩ digital watch. Fracowiak et al. [172] developed supercapacitor elec
matched resistance, the triboelectric output power and power density trode materials using three different electrically conducting polymers
were 98.56 μ W and 1.98 mW/cm3, respectively, and with 30 MΩ (ECPs) namely polyaniline (PANI), polypyrrole (PPy) and poly-(3,
matched resistance, the piezoelectric output power and power density 4-ethylenedioxythiophene) (PEDOT) with MWCNTs. The prepared
were 9.747 μ W and 0.689 mW/cm3 respectively. composites were analyzed, and it was demonstrated that MWCNTs
Lin et al. [148] exhibited PP/MWCNT coated PET conductive com played a substantial role in polymers distribution through the compos
posite yarns with variable loadings (0 wt%, 0.5 wt%, 1 wt%, 2 wt%, 4 wt ites, higher conducting and mechanical properties, improved charge
%, and 8 wt%) of MWCNTs using melt extrusion technique. The pre transfer properties. It was stated that 20 wt.% CNTs loading in ECPs can
pared specimens were investigated for morphology, tensile properties, provide special electrodes i.e., with appropriate configurations, the
and electrical conductivity. A continuously connected structure was capacitance values can reach (100–330 F g− 1) with capacitor voltage
formed at 8 wt% MWCNTs, and electrical conductivity reached 0.8862 (0.6–1.8 V).
S/cm with the highest tensile strength, making it useful for wearable Muralidharan et al. [173] demonstrated ion-conducting epoxy elec
electronics applications, e.g., battery-heated armor and others. Kar et al. trolyte composites’ mechanical and energy storage properties reinforced
[149] proposed MWCNTs and silica-contained poly-vinylidene-fluoride with aligned CNTs grown on stainless steel mesh. It was observed that
(MWCNT@SiO2/PVDF) nanocomposite films with improved piezoelec energy storage composites also showed high mechanical strength (> 85
tric, dielectric, and ferromagnetic properties for cheap and flexible en MPa), elastic modulus (5 GPa) and energy density (> 3 mWh/kg).
ergy harvester nanogenerator. While investigating, the flexible Fig. 18(a) shows the structural concept of a supercapacitor and its
nanogenerator showed high output voltage (45 V), high current density fabrication in a vehicle framework. Fig. 18(b) represents the Optical and
(1.2 μA/cm2), and high power density (5400 W/m3), and power effi SEM images of CNT-steel mesh. Fig. 18(c) shows images of fiberglass and
ciency is so high that it can directly power 55 commercial LEDs. Kevlar, two different layering materials in the composite. Fig. 18(d)
Wang et al. [150] fabricated fluorinated CNTs/nano fibrillated cel refers to epoxy-IL (ion liquid) electrolyte photographs compared to in
luloses (FCNTs/NFCs) composites using vacuum-assisted filtration. dividual epoxy and IL components.
Composites were explored for thermal conductivity enhancement to Su et al. [174] formulated polytriphenylamine (PTPAn)/MWCNTs
resolve heat dissipation issues in electronic circuits. The investigations and PTPAn/super-p carbon composites to test and compare the effect of
showed that with 35 wt.% FCNT loading, the ultrahigh thermal con CNTs as cathode material in Li-ion batteries. The in-situ polymerization
ductivity of 14.1 W m− 1 K− 1 was achieved with an efficient mechanical, process and the mechanical mixing of super-p carbon followed the
flexible, and tough structure. preparation of the composite. Both composites were analyzed for per
Kozak et al. [151] developed in situ filled interconnected poly formance, and it was observed that PTPAn/MWCNT composite presents
urethane/CNT composites, polymer blend (polyurethane and linear poly higher discharge capacity, lower charge transfer resistance (Rct) and
(methylmethacrylate))/CNT composites and polymer blend/CNT/Ni cycle stability as compared to PTPAn/ super-p carbon composite.
composites with 1.5 wt.% and 3 wt.% filler loading and transformed Park et al. [175] proposed a sea urchin (SU) shaped CNT bimetallic
with Fe(3+)acetylacetonate or Cr(3+)acetylacetonate coordination composite such that MWCNTs were grown radially onto Ni and Al and
compounds to investigate the EMI shielding properties. The character later precisely dispersed in an active polymer layer. The specimen in
ization showed that chromium-modified composite showed better re vestigations confirmed that SU-CNTs doped solar cells showed better
sults, i.e., shielded efficiency at 25.8–37.5 GHz, which was about 25 dB performance as compared to pristine solar cell, the calculated current
in the isolated polymer. Several other references are reporting the mir density (7.5 to 9.5 mA/cm2), and power conversion efficiency (2.1 ±
acle of CNTs and polymer composites in electronics for EMI-shielding 0.1 % to 2.2 ± 0.2 %). Many studies have explored the role of CNTs
[152–155] heat dissipation, field emission, transistors [156], touch polymer composites in energy storage devices e.g., batteries [176–178],
screens, sensors [157–159], antennas, electric motor brushes, and solar cells [179–181], fuel cells [182,183], supercapacitors [184,185],
conductive coatings [160–166]. hydrogen storage and presented satisfactory results [186,187].
However, integrating CNT hybrid composites in solar panels and
9.4. Energy storage energy storage systems can greatly improve efficiency and present sus
tainable energy solutions for a greener future. However, cost-
The energy consumption rate is increasing rapidly, and unfortu effectiveness, production methods, and ecological impact must be
nately, the large-scale energy production sources are not environmen focused on making a significant influence. As high-quality CNTs are
tally friendly, causing terrible climate change. Thus, there is a need to expensive, integrating them into existing energy technologies can
store green energy to reduce the high energy demand and cost savings further increase the overall cost. Thus, innovative, cost-effective
for the future. Due to high surface area and optimized electrical and methods should be introduced by improving synthesis techniques and
15
Fig. 18. Application of CNT in supercapacitor (a) Strategic module of CNT reinforced structural supercapacitor in a vehicle framework. (b) SEM and optical pictures
of a CNT/steel mesh. (c) Images of fiberglass and Kevlar separators. (d) Representation of the epoxy-IL electrolyte (on the left) and individual components (on the
right). Adopted with permission from Ref. [173].
scaling up production. However, achieving production methods that properties significantly enhance the durability of blade structures.
yield consistent and reliable CNT quality of CNTs with zero ecological Fig. 19 shows the application of continuous CNT fibers in the future
impact is also challenging. To resolve these concerns, research should structure of ultra-mega wind turbine blades [189].
focus on recycling methods by removing harmful byproducts by Boncel et al. [190] stated that a large-scale wind turbine blade is
employing green chemistry principles for CNT composites and calcu typically a three-blade rotor rotating on a horizontal axis with two-face
lating their environmental affect via comprehensive life cycle studies. suction and pressure construction, joining faces via shear webs
combining upper and lower parts. While operating, the wind turbine
9.5. Wind turbine blade blade faces flap-wise load (due to wind pressure) and edgewise load (due
to gravity and torque), and thus flap-wise, the operation should be in
The energy demand is rapidly increasing, and efficient green energy compression-compression/tension-tension mode while edgewise in
sources are needed extensively to fulfill the demand. The wind turbine is compression-tension mode. Considering the variable load effects
among the best green energy sources with its sturdy blades rotating and through the blades, CNTs reinforced polymer composites are the best
producing electricity. However, severe weather conditions highly affect candidates for sandwich structures due to the feasibility of polymer
the structural behavior of blades, and structural damage reduces effi adhesion with the electrochemical and mechanical properties of CNTs.
ciency. In current designs, CNT thermoplastic polymer composites have Fig. 20 shows different wind turbine blade components and
replaced the traditional classical fibers to maximize the blade’s perfor load-carrying sections.
mance with high surface area, extraordinary strength and stiffness, Elhenawy et al. [191] proposed f-CNT/Ep composites via resin
weight reduction, and physicochemical, thermal, and electrical prop impregnation technique to design a small vertical axis wind turbine
erties. Moreover, CNT composites are impressive in sensor-making and blade. The investigation results were performed by finite element
are utilized to examine internal variations in wind turbine blades [188]. analysis (FEA) and the prepared composites were also investigated for
Due to their nanoscale dimensions and diameter ranging from 180 nm mechanical properties. Results showed that CNT/Ep composites signif
(Fig. 19b and c), CNTs possess an exceptionally high aspect ratio char icantly improved deflection and mechanical properties. Moreover, the
acterized by a substantial length-to-diameter ratio. These distinctive implementation and effectiveness of prepared CNT/Ep composites in the
Fig. 19. Application of CNTs in a wind turbine blade. (a,b,c,d) CNT types micro-macro scale overview and its implementation effect in wind turbine blade,
respectively. Adopted with permission from Ref. [189].
16
Fig. 20. Wind turbine blade simplified cross-section with an indication of working loads with their directionalities (left); major elements of a wind turbine blade,
based on linking of two aeroshells and shear webs (grey color indicates the primary load-carrying composites) (right). Adopted with permission from Ref. [190].
movement of wind turbine blades under variable loads were analyzed by CRediT authorship contribution statement
ANSYS code package, confirming that introducing CNTs into Ep com
posites highly influences the efficiency of the wind turbine blade. Zulfiqar Ali: Data curation, Writing – original draft. Saba Yaqoob:
The ice formation on wind turbine blades causes imbalances, reduces Investigation, Writing – original draft. Jinhong Yu: Conceptualization,
lifetime, and results in 20 % energy loss annually. Due to substantial Writing – original draft. Alberto D’Amore: Supervision, Writing – re
thermal properties, CNT composites greatly reduce the problem. Zheng view & editing.
et al. [192] established CNT-reinforced waterborne polyurethane (WPU)
composite films via roll-roll gap coating and hot-press method for highly Declaration of competing interest
flexible, durable, lightweight in situ deicing system. It was disclosed that
electrothermal composite film heaters can endure 100,000 times 240◦ The authors declare that they have no known competing financial
bending at 3.17 % resistance fluctuation, and in length direction, the interests or personal relationships that could have appeared to influence
repeated 2.0 % stretching without any influence on their temperature the work reported in this paper.
dispersal with impact strain of 10 %. Many references reported CNT
composites’ impact in advancing wind turbine blades [193–196]. Data availability
10. Conclusion and outlook No data was used for the research described in the article.
The addition of CNTs in polymers with multiple fillers has opened a

new corridor for structural applications. Based on existing studies, the
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Composites Part C: Open Access 13 (2024) 100434

Contents lists available at ScienceDirect

Composites Part C: Open Access

Critical review on the characterization, preparation, and enhanced

1. Introduction CNTs, being a one dimensional (1D) cylindrical, rolled up single-

Available online 6 January 2024

The laser ablation/evaporation process is like an electric arc

The addition of CNTs in polymers with multiple fillers has opened a

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