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Abstract

As one of most fascinating form of carbonaceous nanoentities, presently, carbon nano-onions and derived nanomaterials attained intense scientific curiosities. Accordingly, this review bids readers with an updated account on recent progresses in the arenas of thermoplastic polymers/carbon nano-onions hybrids. Carbon nano-onions and modified forms have been reinforced in a variety of thermoplastics to form advanced polyethylene/carbon nano-onions, poly (methyl methacrylate)/carbonaceous nano-onions, polyacrylonitrile/carbonaceous nano-onions, polyamide/carbonaceous nano-onions, polystyrene/carbonaceous nano-onions, and other multifunctional nanocomposites. Similarly, with biodegradable thermoplastics, poly (vinyl alcohol)/carbon nano-onions, poly (lactic acid)/carbonaceous nano-onions, chitosan/carbonaceous nano-onions, etc., have been designed. The ensuing nanocomposites had noticeable microstructural features, electrical conductivity, mechanical robustness, thermal stability, ecological/sustainability, and other valuable physical properties. Depending upon explicit technical features, carbon nano-onions based nanomaterials revealed applications in a number of industrial sectors. Currently, thermoplastic polymers/carbon nano-onions nanomaterials seemed to be promising for electromagnetic interference shielding, sustainable water purification, biomedical (drug delivery, bioimplants), and scientific interests continuously growing in these areas. Along with the design varieties, synthetic routes, compatibility aspects, etc., of carbon nano-onions filled nanocomposites, the underlying challenges towards their practical utilization were also concisely detailed out.

Keywords

Carbon nano-onions thermoplastic biodegradable electromagnetic interference shielding water remediation drug delivery

Introduction

Thermoplastics have been considered as the most significant category of polymers for nanocomposite fabrication, especially with carbonaceous nanoparticles (fullerene, nanodiamond, graphene, etc.).¹ For this purpose, innumerable polymers have been devised, including non biodegradable thermoplastic polymers as well as biodegradable thermoplastic polymers (or bioplastics).^2,3 Carbon nano-onions are unique zero dimensional carbonaceous nanoentities resembling multi layered fullerene molecules, i.e., hollow, spherical, and sp² hybridized.⁴ Like other carbonaceous nanoparticles,⁵ inclusion of carbon nano-onions in thermoplastic matrices seems to notably enhanced the structural, morphological, physical, and technological aspects of these materials.^6–8 In this concern, carbon nano-onions surface functionalities, dispersion, and interaction towards thermoplastic polymers seem to enhance the desired features of thermoplastic polymers/carbon nano-onions hybrids.^9–11 Moreover, manufacturing of these hybrids via efficient technique may enhance their probability towards variety of scientific arenas, such as energy, electronics, space engineering, medical sectors, and so on.^12,13

Notably, recent research seemed to be trending towards the utilization of green or bio based carbon nano-onion hybrids in advanced technological fields including devices, engineering, biomedical, and environment/sustainability concerns.¹⁴ Accordingly, carbonaceous nanoparticles (such as carbon nano onion) filled three dimensional hydrogels of biocompatible and ecological polymers (like chitosan, polycaprolactone, poly (lactic acid), ultra-high-molecular-weight polyethylene, gelatin) have been discovered promising for biomedical and ecological applications.^15,16 Moreover, these multifunctional nanomaterials revealed worth for bridging the gap between ecological/sustainability needs and medical uses.¹⁷ For tissue engineering scaffolds and drug delivery applications, Mamidi et. al.^18–20 proposed several efficient biocompatible and biodegradable nanocomposites of gelatin/carbon nano onions, zein protein/carbon nano onions, and other systems. Furthermore, literature reports up till now state the potential of biocompatible polymer/carbon nanoparticle hybrids for the elimination of toxins (like mercury, phosphates) and drug remains from aquatic systems.^21,22

This review focuses on state of the art advancements of thermoplastic polymers/carbon nano-onions hybrids. First, it momentarily summarizes some vital fundamentals of thermoplastic polymeric matrices and carbon nano-onions nanoparticles. This is followed by the major sections on carbon nano-onions reinforced thermoplastic polymeric and biodegradable polymeric nanocomposites, so, offering an update to the readers on recent advancements in this field. Finally, this manuscript gives a suitable account elucidating technical applications of thermoplastic or biodegradable thermoplastic polymers/carbon nano-onions nanocomposites, as per literature to date. Moreover, it addresses drawbacks for possible implication of carbon nano-onions reinforced hybrids. To the best of the knowledge, this novel article (for the first time in literature so far) documented distinct structural/microstructural/physical attributes, dispersion/compatibility facets, technological possibilities, and bottlenecks for designing high tech carbon nano-onions based thermoplastic nanocomposites.

Thermoplastic and biodegradable thermoplastic polymers

The term ‘thermoplastic’ is basically derived from the word ‘plastic’ and denotes to any macromolecular material which can be reversibly soften upon heating and hardened on cooling.²³ Accordingly, thermoplastics can be easily molded or remolded into different shapes/forms.²⁴ Under the category of thermoplastics, incalculable polymers have been documented to date.²⁵ Table 1 displays physical properties of some common thermoplastic polymers.²⁶ Generally, thermoplastic polymers have been recognized for facile processing, molding/remolding, low density, thermal, and mechanical aspects.^27–29 High tech stipulations of thermoplastic polymers may involve aerospace/automobile industry, engineering and civil sectors, textile and medical fields, and so on.³⁰ Subsequently, numerous carbon, organic, or inorganic additives or nanoadditives have been used to enhance the physical properties and applied characteristics of thermoplastic polymers.³¹ Figure 1 illustrates macromolecular crosslinking and molding features of thermoplastic polymers.³²

Table 1.

Physical features of few important thermoplastic polymers.²⁶ Reproduced with permission from Elsevier.

Properties	Polypropylene	Low density polyethylene	High density polyethylene	Polycarbonate	Polybutylene terephthalate	Poly (amide imide)s
Density, ρ (g/cm³)	0.89-0.92	0.91-0.93	1.0-1.000	1.19-1.24	1.3-1.4	1.38-1.45
Glass transition temperature, T_g (°C)	−23 - -10	∼ -125	−133 - -100	141-150	69-110	244-290
Strength, σ_max(MPa)	26-42	4.0-10	15-38	53-72	52-56	90-192
Modulus, E (GPa)	1.0-1.8	0.06-0.38	0.4-1.5	2.3-3.0	∼2.37	2.8-4.4

Figure 1.

Molecular and formability behavior of thermoplastic polymers.³² Reproduced with permission from ACS.

Biodegradable thermoplastic polymers belong to the category of thermoplastics which can be decomposed by natural means, such as microbials, moisture, or other environmental effects.^33,34 Figure 2 A demonstrates life cycle and end of life disposal of biodegradable thermoplastics and related self reinforced polymer composites. Moreover, Figure 2 B & C show chemical structures and applications of essential biodegradable thermoplastic polymerscomposites, respectively.³⁵

Figure 2.

(A) A view of lifecycle of biodegradable plastics including several options for end-of-life disposal; (B) chemical structures of few important biodegradable plastics; (C) potential applications for biodegradable thermoplastic polymers and composites.³⁵ SRPC = self reinforced polymer composites. Reproduced with permission from Springer (Open access).

Carbon nano-onions

Carbon nano-onions were primarily recognized as polygonized carbon rings, by Ijima (1980), i.e., before the discovery of carbon nanotubes.³⁶ Afterwards, concentric graphite shells were identified in carbon nano-onions nanostructures by Ugarte et al. (1990s).³⁷ In simple words, carbon nano-onions are multi walled fullerenes, which are made up of few overlapping hollow fullerene molecules.³⁸ Initially, carbon nano-onions were synthesized using arc discharge practice using carbon electrodes in water.³⁹ Lin et al.⁴⁰ investigated the microstructural specifications of carbonaceous nano-onions in electron irradiation environment. Figure 3 A (a-c) show high resolution transmission electron microscopy micrographs of pristine carbon nano-onions, and nano-onion nanostructure under electron irradiation of 5.68 × 10²⁴ e/cm² and 8.52 × 10²⁴ e/cm², respectively. As per results, pristine carbon nano-onions had diameter of ∼7 nm, with ∼10 graphitic shells. On the other hand, electron beam irradiation not only improved the perfection of spherical carbon nano-onions structure with distinct shells, but also increased the number of graphitic shells in the nanostructure (i.e., up to 12). Figure 3 B shows plots for number of graphitic layer distribution and interplanar spacing of carbon nano-onions versus in situ in situ transmission electron microscopy irradiation. Accordingly, electron beam irradiation caused formation of undistorted graphitic shells and planes in the carbon nano-onions nanostructure. Moreover, irradiation led to increase in interplanar spacing from 0.32 nm to 0.335 nm, showing the formation of perfect nano-onion nanostructure.

Figure 3.

(A) High resolution transmission electron microscopy micrographs: (a) pristine carbon nano-onions (CNOs), (b) structural evolutions of CNOs at electron irradiation of 5.68 × 10²⁴ e/cm²; (c) 8.52 × 10²⁴ e/cm²; (B) distributions of number of graphitic layers and interplanar spacing of CNO under in situ transmission electron microscopy irradiation.⁴⁰ Reproduced with permission from Elsevier.

Studies on structural and physical characters of carbon nano-onions depicted high aspect ratio and notable electronic, optical, optoelectronic, electrical, mechanical, thermal, biological, and other technical features.^41,42 For these remarkable carbon nanoentities, a number of fabrication techniques have been reported in the literature so far, such as ion implementation, microwave plasma, arc discharge, chemical vapour deposition, pyrolysis, annealing, and several others.^41,43 Nevertheless, all these synthesis approaches own relative advantages and disadvantages in terms of carbon nano-onions sizes, process feasibility, product yield/purity, cost, etc.⁴⁴ Table 2 compares various synthesis methods for carbon nano onions in terms of process conditions, yield, scalability, environmental impact, etc.

Table 2.

A comparative analysis of synthesis techniques for carbon nano-onions.

Technique	Substrate	Method conditions	Yield	Cost/scalability	Environmental impact	Ref.
Microwave plasma technique	Carbon residues, bioresiduesetc	Microwave-based C₂H₂ plasma reactor	Vey high	Low/economical	Environmentally safe/green method	^45,46
Chemical vapor deposition	Deposition of methane or carbon layer over metal catalyst	Metal catalyst (cobalt, nickel, etc.)	Large quantities	High	Environmentally hazardous due to metal catalysts	^47–49
Ion implantation	Carbon ion into copper or silver substrate	600°C–1000°C (cu)	Low	High	Moderate	^46,47,50
Arc-discharge	Amorphous carbon soot	Arc discharge between two graphite electrodes in water	High	Reasonable	Environmentally reliable	^47,51,52
		30 A
		16 V
Pyrolysis	Polyethylene, polystyrene, plastic waste, etc	Oxygen flame	Low	Modest	Environmentally hazardous	^47,53–56
Thermal annealing	Nanodiamonds	800°C–2100°C	High	High	Environmentally moderate	^47,57

Despite the research on synthesis of carbon nano-onions so far, a single economical, ecological, and efficient technique for scalable production of high quality carbon nano-onions has not been discovered yet.⁵⁸ Looking at the applied arenas of carbon nano-onions, these nanoentities seemed to be functional for myriad of energy/electronics devices, aerospace engineering, biomedical, and other multidisciplinary fields.⁵⁹ In future, further experimental as well as theoretical studies must be performed to examine the structural, physical, as well as applied aspects of carbon nano-onions.⁶⁰

Thermoplastic polymers/carbon nano-onions nanocomposites

Polyethylene or polythene is undoubtedly the most commonly known thermoplastic, which is produced tonnes per year.⁶¹ Polyethylene can be seen in different forms, like low density polyethylene, high density polyethylene, or ultra high molecular weight polyethylene.⁶² Numerous types of carbonaceous nanocomposites of polyethylene have been reported, including polyethylene/fullerene,⁶³ polyethylene/nanodiamonds,⁶⁴ polyethylene/carbon nanotubes,⁶⁵ polyethylene/graphene or graphene oxide,⁶⁶ etc. Similarly, carbon nano-onions filled polyethylene hybrids were also reported.⁶⁷ Mamidi et. al.⁶⁸ generated polyethylene/modified carbonaceous nano-onions nanocomposites via solution method and hydraulic pressing route (Figure 4 A).

Figure 4.

(A) Covalent functionalization of pristine carbon nano-onions (CNOs) using 4-mercaptophenol; (B) stress strain plots of unfilled UHMWPE, and UHMWPE/f-CNOs nanocomposites; (C) roughness plots of UHMWPE and UHMWPE/f-CNOs nanocomposites; (D) thermogravimetric graph of pristine UHMWPE, and UHMWPE/f-CNOs nanocomposites.⁶⁸ Reproduced with permission from Elsevier. UHMWPE = ultra-high molecular weight polyethylene; CNOs-MPMA = mercaptophenyl methacrylate functional carbon nano-onions; f-CNOs or CNOs-PMPMA = polymercaptophenyl polymethacrylate functional carbon nano-onions; CNOs-MP = carbon nano-onions-4-mercaptophenol; UHMWPE/f-CNOs = ultra-high molecular weight polyethylene/functionalized carbon nano-onions; DMAP = 4-dimethylamiynopyridine; EDC = 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide; NHS = N-hydroxysuccinimide; AlBN = 2,2′-azobis (2-methylpropionitrile); THF = tetrahydrofuran.

For this, carbon nano-onions were modified using mercaptophenol. Inclusion of 0.1 % modified carbon nano-onions to ultra high molecular weight polyethylene notably increased the tensile strength to 83 MPa, compared with the neat matrix (∼28 MPa) (Figure 4 B). Similarly, roughness of ultra high molecular weight polyethylene matrix with 0.1 % modified carbon nano-onions (0.31 mm) was found higher than the neat matrix (0.12 mm) (Figure 4 C). Such results pointed to strong interfacial bonding and load transfer properties related to polyethylene and modified nano-onions based hybrids. As per thermogravimetric analysis, thermal decomposition temperature of polyethylene matrix was enhanced, in the range of 439 °C–513°C, with rising nanofiller contents (Figure 4 D). It seems that thermal stability was due to matrix nanofiller interactions and barrier effects caused by dispersed carbon nano-onions nanoparticles in the polyethylene matrix.

Poly (methyl methacrylate), belongs to the grouping of acrylic thermoplastic, and is a transparent polymer.⁶⁹ This polymer has been widely explored with different types of carbon nanoentities to form poly (methyl methacrylate)/graphene,⁷⁰ poly (methyl methacrylate)/fullerene,⁷¹ poly (methyl methacrylate)/nanodiamonds,⁷² poly (methyl methacrylate)/carbon nanotubes,⁷³ and like so. Nanocomposite systems of poly (methyl methacrylate)/carbon nano-onions nanocomposites have also been documented.⁷⁴ Among initial efforts, Macutkevic et. al.⁷⁵ reported on poly (methyl mehtacrylate)/carbon nano-onions nanocomposites using a simple solution route. Figure 5 displays dielectric permittivity versus frequencies plots of poly (methyl methacrylate)/carbon nano-onions hybrids, at changing temperatures. Owing to changes in the polarization states of the nanocomposites caused by carbon nano-onions and related temperature changes, dielectric permittivity properties were affected.

Figure 5.

(Left) real part and (Right) imaginary part of dielectric permittivity versus frequencies of poly (methyl methacrylate)/carbon nano-onions (1 wt%) nanocomposite measured at varying temperatures.⁷⁵ Reproduced with permission from Elsevier.

Accordingly, Table 3 shows changes in thermal parameters with adding carbon nano-onions contents in poly (methyl methacrylate) based hybrids. It can be observed that carbon nano-onions inclusion caused significant enhancements of thermal parameters (obtained from dielectric studies) of poly (methyl methacrylate)/carbon nano-onions hybrids.

Table 3.

Thermal parameters of poly (methyl methacrylate)/carbon nano-onions nanocomposites using dielectric analysis (129 Hz).⁷⁵ Reproduced with permission from Elsevier.

Sample	Carbon nano-onions (wt.%)	T_α (K)	T_β (K)	Yield (%)
Pure poly (methyl methacrylate)	0	325.0	360.0	428
Poly (methyl methacrylate)/carbon nano-onions nanocomposites	0.5	323.8	403.9	463
	1	328.4	388.5	517
	2	328.8	398.7	457

Polyacrylonitrile is an important semicrystalline thermoplastic engineering polymer.⁷⁶ Carbonaceous nanoparticles, such as carbon nanotubes, graphene, fullerene, nanodiamonds, etc., have been reinforced in polyacrylonitrile matrix to form high performance nanomaterials.^77–79 Carbon nano-onions filled polyacrylonitrile nanocomposites have been reported in the literature up till now.^80,81 Zhang et al.⁸² fabricated polyacrylonitrile/carbon nano-onions hybrid nanofibers by using in situ polymerization and electrospinning methods (Figure 6). Adding carbon nano-onions instigated crystalline domains in the polyacrylonitrile matrix, subsequently leading to compatible nanostructure and superior physical features. Accordingly, carbon nano-onions inclusions in polyacrylonitrile led to >53% augmentation in tensile strength of the polyacrylonitrile nanofibers.

Figure 6.

Manufacturing of polyacrylonitrile/carbon nano-onions nanocomposites and derived nanofibers.⁸² PAN = polyacrylonitrile; OLC = onion like carbon; PAN/OLC = polyacrylonitrile/onion like carbon nanocomposite; CNFs = carbon nanofibers. Reproduced with permission from ACS.

Besides trivial research endeavors were noticed so far on polyamide/carbon nano-onions nanocomposites.⁸³ Polyamides can be named as a group of most common thermoplastic polymer.⁸⁴ Herein, Gopalsamy et. al.⁸⁵ formed nylon 6 (an aliphatic polyamide) grafted carbon nano-onions nanocomposites. For this purpose, carbon nano-onions were first modified with ruthenium dioxide and diazonium compounds and then grafted to nylon 6 to form hybrids. Another very common commodity thermoplastic is polystyrene, which is transparent, hard, and brittle.⁸⁶ Polystyrene has been explored with a number of carbon nanoparticles.⁸⁷ Some research articles can be noted on polystyrene/carbon nano-onions hybrids.⁸⁸ For example, Babar et.al.⁸⁹ produced polystyrene/carbon nano-onions nanomaterials for sensor designs. Consequently, polystyrene/carbon nano-onions depicted high sensitivity for detecting sulfur containing amino acids (methionine and cysteine). In this way, limited but noteworthy research was noticed for high tech carbon nano-onions containing thermoplastic hybrids. Nevertheless, comprehensive future efforts on thermoplastic/carbon nano-onions nanocomposites seem necessary to unveil real world technical potential of these high tech systems.

Biodegradable thermoplastic polymers/carbon nano-onions hybrids

As per today’s environment and sustainability demands, biodegradable thermoplastics have been considered, rather than commodity thermoplastics, for technical utilizations.⁹⁰ Similarly, carbon nano-onions have been reinforced in biodegradable thermoplastics to form advanced nanomaterials.⁹¹

Poly (lactic acid) (or polylactide) is a biodegradable thermoplastic polyesters.⁹² To enhance the physical and technical features, variety of carbonaceous nanofillers reinforced poly (lactic acid) based nanocomposites have been, e.g., poly (lactic acid)/fullerene,⁹³ poly (lactic acid)/nanodiamonds,⁹⁴ poly (lactic acid)/carbon nanotubes,⁹⁵ poly (lactic acid)/graphene,⁹⁶ and others. Nevertheless, restricted literature seen to date on poly (lactic acid)/carbon nano-onions nanocomposites.⁹⁷ Notably, Chowdhury et. al.⁹⁸ applied in situ spray layer by layer technique for poly (lactic acid)/carbon nano-onions nanocomposites. These hybrids were used as piezoresistive strain sensors and had a gauge factor of ∼6, so, can be suggested for commercial level applications. Razzaq and researchers⁴⁵ adopted solution technique to form poly (lactic acid)/carbon nano-onions nanocomposites. Mechanical and thermal features of poly (lactic acid)/carbon nano-onions systems have been analyzed. Consequently, including 0.5 wt% carbon nano-onions enhanced the tensile strength, modulus, and impact strength of neat matrix by 30%, 56%, and 37%, correspondingly (Table 4). These results seemed to be because of reinforcing effects of carbon nano-onions, matrix-nanofiller associations, and load transfer properties of hybrids. In accordance with differential scanning calorimetry and thermogravimetric analysis, carbon nano-onions loadings significantly upgraded glass transition temperature, 5% weight loss temperature, and maximum weight loss temperature by 10%, 5%, and 4%, respectively, relative to pristine poly (lactic acid) (Table 5). It appears that carbon nano-onions reinforcements to poly (lactic acid) matrix led to optimal anchoring to macromolecular chains, therefore increasing the thermal stability of poly (lactic acid)/carbon nano-onions nanocomposites.

Table 4.

Mechanical characteristics of unfilled poly (lactic acid) and poly (lactic acid)/carbon nano-onions nanocomposites.⁴⁵ Reproduced with permission from Elsevier.

Material	Strength (MPa)	Modulus (GPa)	Impact strength (J/m)
0% carbon nano-onions	67.0	2.50	20.0
0.5% carbon nano-onions	96.3	5.70	38.0

Table 5.

Thermal properties of unfilled poly (lactic acid) and poly (lactic acid)/carbon nano-onions nanocomposites (T_g = glass transition temperature; T_5% = 5% weight loss temperature; T_max = maximum weight loss temperature).⁴⁵ Reproduced with permission from Elsevier.

Material	T_g (°C)	T_5% (°C)	T_max (°C)
0% carbon nano-onions	57.1	319	358
0.1% carbon nano-onions	64.0	328	368
0.5% carbon nano-onions	63.4	333	370

Poly (vinyl alcohol) is a commonly known water soluble thermoplastic polymer.⁹⁹ Nanocarbon hybrids of poly (vinyl alcohol) have been reported as poly (vinyl alcohol)/nanodiamonds,¹⁰⁰ poly (vinyl alcohol)/fullerene,¹⁰¹ poly (vinyl alcohol)/carbon nanotubes,¹⁰² poly (vinyl alcohol)/graphene or graphene oxide,¹⁰³ etc. With carbon nano-onions, few nanocomposites have been reported for poly (vinyl alcohol) and poly (vinyl alcohol) blends systems.^104,105 Consequently, Serban et al.¹⁰⁶ followed drop casting method for the formation of poly (vinyl alcohol)/carbon nano-onions nanocomposites based humidity sensor. Figure 7 A displays swelling tendency and percolation networking of poly (vinyl alcohol) based hybrid sensor, when in contact with water.

Figure 7.

(A) Swelling tendencies and conducting network formation in poly (vinyl alcohol)/carbon nano-onions hybrid based sensors; (B) relative humidity and resistance variation versus time for poly (vinyl alcohol)/carbon nano-onions nanocomposites derivative sensor: (a) 1:1 (w/w), and (b) 2:1 (w/w).¹⁰⁶ PVA = poly (vinyl alcohol); CNOs = carbon nano-onions. Reproduced with permission from MDPI.

Figure 7 B shows relative humidity and resistance trends versus time for poly (vinyl alcohol)/carbon nano-onions hybrid sensor having varying nanofiller loading levels. Adding carbon nano-onions amounts enhanced the relative humidity (5–95 %) and resistance fluctuations for poly (vinyl alcohol)/carbon nano-onions nanocomposite samples, proving their fine sensing properties.

Chitosan is a thermoplastic polysaccharide having advantageous properties of biodegradability, biocompatibility, and sustainability.¹⁰⁷ As effective nano-additives, nanocarbon nanoparticles have been composited with chitosan to form chitosan/fullerene,¹⁰⁸ chitosan/nanodiamonds,¹⁰⁹ chitosan/carbon nanotubes,¹¹⁰ chitosan/graphene,¹¹¹ etc. However, scarce scientific reports seen up till now for chitosan/carbon nano-onions nanocomposites.^112–114 Noticeably, Castro et. al.¹¹⁵ developed chitosan/carbon nano-onions nanocomposite nanofibers by electrospinning approach. These nanofibers had diameter of ∼100-150 nm and varying crystallinity index from 0.85 to 12.5%. The biocompatible chitosan/carbon nano-onions nanocomposite nanofibers can be suggested for biomedical applications, such as tissue engineering and biomedical devices. Additionally, Grande Tovar et al.¹¹⁶ industrialized chitosan grafted carbon nano-onions nanocomposites via solution refluxing and centrifugation methods. A route for the conversion of neat carbonaceous nano-onions to oxidized carbonaceous nano-onions, acyl chloride carbon nano-onions, and nanocomposites is shown in Figure 8 A. The thermogravimetric analysis plots for pristine chitosan, oxidized carbon nano-onions, and chitosan grafted carbon nano-onions nanocomposites are illustrated in Figure 8 B (a-c). In the case of unfilled chitosan, degradation of N-acetyl and amine side chain functionalities caused a weight loss < 400°C. In chitosan/carbon nano-onions nanocomposites, a two-stage decomposition behavior was perceived at 170 °C–260 °C and 600 °C–700 °C, owing to decomposition of hydroxyl/carboxylic functionalities on carbonaceous nano-onions and chitosan-carbonaceous nano-onions linkages, respectively.

Figure 8.

(A) A formation route to chitosan grafted carbon nano-onions (CS-g-CNO) nanocomposite; (B) thermogravimetric analysis of (a) CS-g-CNO; (b) oxidized carbon nano-onions (ox-CNO); (C) pristine chitosan (CS).¹¹⁶ p-CNO = purified carbon nano-onions; Cl-CNO = acyl chloride functional carbon nano-onions. Reproduced with permission from MDPI.

Technological influence of carbonaceous nano-onions nanoadditives towards thermoplastic or biodegradable thermoplastic nanomaterials

Since discovery, applied aspects pertinent to carbonaceous nano-onions were scrutinized for various technologically significant materials and industries.¹¹⁷ Furthermore, pristine carbon nano-onions, their nanocomposites have been designed for essential commercial level utilizations.¹¹⁸ Like several other nanocarbons (nanodiamond, fullerene, carbon nanotube, graphene, etc.), carbon nano-onions have been used to form polymeric nanocomposites, e.g., thermoplastic polymers/carbon nano-onions hybrids.¹¹⁹ Consequently, myriad of thermoplastic polymers/carbon nano-onions systems have been designed using facile methods and studies for physical features (Table 6).¹²⁰

Table 6.

Specifications of thermoplastic polymers/carbon nano-onions nanocomposites.

Thermoplastic/biodegradable thermoplastic polymer	Nanofiller	Manufacturing	Functional characteristics/applications	Ref
Ultra high molecular weight polyethylene	Mercaptophenol modified carbon nano-onions	Solution method; hydraulic pressing route	Tensile strength and roughness increase from ∼28 MPa to 0.12 mm (neat matrix) to 83 MPa and 0.31 mm (0.1% nanocomposite), respectively; thermal decomposition temperature increased around 439°C–513°C	⁶⁸
Poly (methyl methacrylate)	Carbon nano-onions	Solution route	Dielectric permittivity due to changes in the polarization states; increase in thermal parameters (obtained from dielectric studies)	⁷⁵
Polyacrylonitrile	Carbon nano-onions	In situ polymerization; electrospinning methods	>53% increase in tensile strength with carbon nano-onions	⁸²
Nylon 6 (an aliphatic polyamide)	Carbon nano-onions modified with ruthenium dioxide and diazonium compounds	Solution method	Covalent grafting	⁸⁵
Polystyrene	Carbon nano-onions	Solution method	Sensing properties; sulfur containing amino acids (methionine and cysteine)	⁸⁹
Poly (lactic acid)	Carbon nano-onions	In situ spray layer by layer technique	Piezoresistive strain sensors; gauge factor ∼6,	⁹⁸
Poly (lactic acid)	Carbon nano-onions	Solution approach	Increases in tensile strength, modulus, and impact strength by 30%, 56%, and 37%, correspondingly (0.5 wt% loading); increase in glass transition temperature, 5% weight loss temperature, and maximum weight loss temperature by 10 %, 5 %, and 4%, respectively, relative to neat matrix	⁴⁵
Poly (vinyl alcohol)	Carbon nano-onions	Drop casting method	Humidity sensor; enhancements in relative humidity (5-95%); resistance fluctuations	¹⁰⁶
Chitosan	Carbon nano-onions	Electrospinning approach	Nanofibers diameter ∼100-150 nm; crystallinity index 0.85-12.5%;	¹¹⁵
			Biocompatibility
			Biomedical uses
Chitosan	Carbon nano-onions; oxidized carbonaceous nano-onions; acyl chloride carbon nano-onions	Solution technique; refluxing/centrifugation methods	Nanocomposite had two-stage decomposition at 170°C–260°C and 600–700°C; unfilled chitosan had weight loss < 400°C	¹¹⁶

An important application of carbon nano-onions based thermoplastic nanocomposites have been noticed for electromagnetic absorption.¹²¹ In this concern, Grimaldi et al.¹²² reported electrical conductivity properties of poly (methyl methacrylate)/carbon nano-onions hybrids, even with low nanofiller loadings. Remarkedly high electrical conductivity and dielectric permittivity features were observed at atmospheric pressure of 2 GPa, owing to superior electron percolation. Kuzhir et. al.¹²³ designed poly (methyl methacrylate)/carbon nano-onions nanocomposites using solution method. These nanomaterials depicted electromagnetic attenuation in the frequency region of 26-38 GHz, due to fine nanocarbon dispersion and percolation properties. Pan et al.¹²⁴ adopted layer by layer electrostatic assembly and electroless plating methods (accompanying freeze drying) for the formation of β-chitin/carbon nano-onions/Ni-P hybrid films and aerogels (Figure 9 A). The β-chitin/carbon nano-onions/Ni-P nanocomposite film was used to light a light emitting diode bulb, owing to low resistivity (Figure 9 B (a)). Figure 9 B (b) shows the increase in electrical conductivity of β-chitin/carbon nano-onions/Ni-P nanocomposite film from 10 to 125 S m⁻¹, with nanofiller loading of 1-3 wt%. Owing to the formation of incessant conducting network of carbon nano-onions (with rising loading levels) in the matrix, total shielding effectiveness, shielding effectiveness of absorbance, and shielding effectiveness of reflectance were found to consistently enhanced (Figure 9 B (c)). Accordingly, electromagnetic interference shielding effectiveness of about 66.7 dB was observed for these of β-chitin and carbon nano-onions based hybrids. Although, literature efforts seemed to be limiting on electromagnetic interference shielding thermoplastic nanocomposites of carbon nano-onions.

Figure 9.

(A) Schematic for synthesis of CONA and CONF; (B) (a) digital image showing lighting of CONF based LED (light emitting diode) lamp; (b) electrical conductivity; and (c) comparison of average SE_T, SE_A, and SE_R.¹²⁴ CA = β-chitin aerogel; COA = β-chitin/CNO aerogel; CONA = β-chitin/carbon nano-onions/Ni-P aerogel; CF = β-chitin film; COF = wet β-Chitin/CNO film; CONF = β-chitin/carbon nano-onions/Ni-P film; SE_T = total shielding effectiveness; SE_A = shielding effectiveness of absorbance; SE_R = shielding effectiveness of reflectance. Reproduced with permission from Springer.

Another notable application of thermoplastic polymers/carbon nano-onions nanocomposites can be listed for sustainable water remediation membranes.^125–127 Prior to carbon nano-onions derived hybrids, carbonaceous nanoparticles such as carbon nanotube, fullerene, nanodiamonds, graphene, etc., based nanomaterials have been exploited for water purification membranes.^128,129 Kumari et. al.¹³⁰ evaluated the performance of carbon nano-onions for separating methyl orange dye from water by using second order kinetics and Langmuir isotherm model. These nanocarbons showed 100% dye removal efficiency within 0.5 h. In a similar attempt, the same group¹³¹ investigated the diesel/petrol uptake capacity (∼37-58 mg mg⁻¹) of carbon nano-onions through Langmuir’s isotherm model and pseudo second order kinetics methods. Later, Kumari and co-workers¹³² developed sulfonated poly (ether sulfone)/carbon nano-onions nanocomposite membranes via flame pyrolysis and solution approaches. This system depicted water uptake of >9.3%. Zhang et. al.¹³³ applied nonsolvent induced phase separation method for the formation of sulfonated carbon nano onions and related ultrafiltration membranes of poly (ether sulfone)/sulfonated carbon nano-onions nanocomposites (Figure 10 A).

Figure 10.

(A) Non-solvent induced phase separation technique for the formation of poly (ether sulfone)/sulfonated carbon nano-onions hybrid membrane; (B) cross flow filtration mechanism for separation of bovine serum albumin (BSA) from water via poly (ether sulfone)/sulfonated carbon nano-onions hybrid membrane.¹³³ CNO = carbon nano-onion; BPO = benzoyl peroxide; PCNO = purified carbon nano-onion; SCNO = sulfonated carbon nano-onion. Reproduced with permission from Elsevier.

The cross flow filtration system and performance mechanism of poly (ether sulfone)/sulfonated carbon nano-onions nanocomposite membrane are illustrated in Figure 10 B. The poly (ether sulfone)/sulfonated carbon nano-onions nanocomposite membrane with 1 wt% nanofiller revealed pure water flux and recovery ratio of ∼164 kg m⁻² h⁻¹ and >93 %, respectively.

In biomedical sector, worth of carbon nano-onions derived nanomaterials has been inspected for drug delivery, bioimplants, and tissue scaffolding applications.⁵⁴ Modified carbon nano-onions have been applied for stimuli responsive drug loading/release applications.^16,134,135 For example, Mamidi et. al.¹³⁶ used layer by layer self assembly approach for the formation of anilinated-poly (ether ether ketone) and poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions derivative hybrids (Figure 11 A). According to scanning electron microscopy micrograph, the 5 wt% functional carbon nano-onions loaded nanocomposite had ordered and layered nanostructure owing to the effectiveness of layer by layer technique. Figure 11 B shows stress-strain plots of pristine anilinated-poly (ether ether ketone) and anilinated-poly (ether ether ketone)/poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions nanocomposites. A per results, adding 5 wt% nanofiller caused increments of ∼356% and 336% for stress and modulus, respectively, of the nanocomposite, compared with the unfilled matrix due to matrix-nanofiller interactions and stress transfer characters. Figure 11 C shows stimuli sensitive drug release (doxorubicin) performance of anilinated-poly (ether ether ketone)/poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions nanocomposites (1.5-5 wt% loading levels). At a specific pH (4.5), adding nanocarbon caused considerable enhancement in drug release of these nanocomposites. Subsequently, a maximum of >99 % drug release was observed for 5 wt% loaded anilinated-poly (ether ether ketone)/poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions nanocomposite. This performance can be credited to supramolecular aromatic stacking interactions between functional nano-onions and drug molecules.

Figure 11.

(A) Fabrication of poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions (PAPMA-CNOs = f-CNOs) and anilinated-poly (ether ether ketone) (AN-PEEK) based AN-PEEK/f-CNOs (anilinated-poly (ether ether ketone)/functional carbon nano-onions) nanocomposite films using layer by layer self assembly technique; where inset: scanning electron microscopy image of 5 wt% f-CNOs loaded nanocomposite film; (B) tensile plots of neat An-PEEK and 1.5-10 wt% loaded AN-PEEK/f-CNOs nanocomposite samples; (C) stimuli responsive drug release from neat An-PEEK and 1.5-5 wt% loaded AN-PEEK/f-CNOs nanocomposite samples, at pH = 4.5.¹³⁶ Reproduced with permission from MDPI.

Mamidi et al.¹³⁷ formed gelatin and poly (4-hydroxyphenyl methacrylate) modified carbonaceous nano-onions derivative hybrid aerogels by a sonochemical technique. Compared with pristine gelatin having maximum decomposition temperature of ˂ 300°C, gelatin/poly (4-hydroxyphenyl methacrylate) modified carbon nano-onions nanocomposites had higher value of >420°C. Consequently, the nanomaterials were analyzed for drug release and tissue scaffolding applications. The gelatin/poly (4-hydroxyphenyl methacrylate) modified carbon nano-onions nanocomposites were examined for 5-fluorouracil drug release behavior at pH = 5. These hybrids had van der Waals and π-π towards drug molecules for controlled drug release overtime. Furthermore, gelatin/poly (4-hydroxyphenyl methacrylate-carbon nano-onions nanocomposites showed cytotoxicity and optimum cell growth for tissue engineering purposes. For application in bio implants, limited reports available to date concerning biodegradable thermoplastic/carbon nano-onions nanocomposites.¹³⁸ As explained above, Castro et al.¹¹⁵ designed chitosan grafted carbon nano-onions nanocomposite nanofibers via facile solution, centrifugation, and electrospinning procedures. The chitosan/carbon nano-onions nanofibers depicted fine biocompatibility with collagen and applied for subdermal bioimplantations. Briefly, biocompatibility and superior physical characters of thermoplastic polymers/carbonaceous nano-onions for biomedical applications can be credited to synergetic matrix-nanofiller effects and interfacial miscibility.

Challenges and summation

Notwithstanding the above explained successful design and applied specs of thermoplastic polymers/carbon nano-onions hybrids (Figure 12 and Table 7), it is important to look into the field challenges hindering the multitude methodological disposition of these nanomaterials. In the field of electromagnetic interference shielding, modified forms of carbon nano-onions need to be engrossed to develop better matrix-nanofiller and percolation interlinks to support facilitated electrical conductivity and to overcome the challenges of restricted dielectric and permittivity features. Accordingly, Figure 13 A presents a general mechanism for the formation of percolation zone due to carbon nanoparticle addition and interconnected network formation in the matrix.¹³⁹ For this purpose, dispersion and solubility properties of carbon nano-onions must be improved toward macromolecular phases, by adopting appropriate modification strategies.

Figure 12.

Thermoplastic carbon nano-onions nanocomposites: Design—to—applications.

Table 7.

Applied significance of thermoplastic carbon nano-onions nanocomposites.

Thermoplastic/biodegradable thermoplastic polymer	Nanofiller	Manufacturing	Functional characteristics/applications	Ref
Poly (methyl methacrylate)	Carbon nano-onions	Solution technique	Electrical conductivity; dielectric permittivity at 2 GPa atmospheric pressure	¹²²
Poly (methyl methacrylate)	Carbon nano-onions	Solution process	Percolation properties; nanocarbon dispersion; electromagnetic attenuation in frequency region ∼26-38 GHz	¹²³
β-chitin	Carbon nano-onions/Ni-P	Layer by layer electrostatic assembly; electroless plating methods	Electrical conductivity	¹²⁴
			10-125 S m⁻¹; lightning of LED bulb, due to low resistivity;
			Electromagnetic interference shielding effectiveness
			∼66.7 dB
-	Carbon nano-onions	Second order kinetics; Langmuir isotherm model studies	Methyl orange dye separation	¹³⁰
-	Carbon nano-onions	Second order kinetics; Langmuir isotherm model studies	100% dye removal efficiency (0.5 h)	¹³⁰
-	Carbon nano-onions	Second order kinetics; Langmuir isotherm model studies	Diesel/petrol uptake capacity ∼37-58 mg mg⁻¹	¹³¹
Poly (ether sulfone)	Carbon nano-onions	Flame pyrolysis; solution approach	Membranes had water uptake >9.3%; pure water flux and recovery ratio of ∼164 kg m⁻² h⁻¹ and >93%, respectively (1 wt% nanofiller)	¹³²
Poly (ether sulfone)	Sulfonated carbon nano onions	Phase separation method	Ultrafiltration membranes; cross flow filtration system	¹³³
Anilinated-poly (ether ether ketone)	Poly (N-(4-aminophenyl) methacrylamide))-carbon nano-onions	Layer by layer self assembly approach	Stress and modulus increments by ∼ 356% and 336%,	¹³⁶
			respectively (5 wt% loading);
			Doxorubicin drug release
			>99% at pH 4.5, (5 wt% loading)
Gelatin	Poly (4-hydroxyphenyl methacrylate) modified carbon nano-onions	Sonochemical technique	Higher maximum decomposition temperature of >420°C, than neat matrix (< 300°C); fluorouracil drug release behavior at pH = 5;	¹³⁷
Gelatin		Sonochemical technique	Controlled drug release overtime	¹³⁷
Chitosan	Carbon nano-onions	Solution process; centrifugation; electrospinning procedures	Covalent grafting; biocompatibility with collagen;	¹¹⁵
Chitosan	Carbon nano-onions		Subdermal bioimplants	¹¹⁵

Figure 13.

(A) Mechanism of percolation threshold in polymeric nanocomposites with increasing nanofiller loading levels.¹³⁹ Reproduced with permission from MDPI; (B) load transfer mechanism of nanoparticle filled polymeric nanocomposite depending upon interface formation and matrix-nanofiller interlinking in the nanostructure.¹⁴⁰ Reproduced with permission from ACS.

In addition, matrix-nanofiller interfacial interactions seem to be beneficial to enhance the load transfer and mechanical properties of high performance carbon nano-onions based nanocomposites. In these polymer nanocomposites, a general load transfer mechanism involves the formation of an effective interface with interfacial interactions and matrix-nanoparticle networks (Figure 13 B).¹⁴⁰ Consequently, the interfacially connected nanocomposite has capability to absorb the load energy and transfer stress through interphase, therefore enhancing the overall macroscopic and mechanical properties.

In addition, scalable and sustainable production strategies must be researched for progressive radiation shielding carbon nano-onions filled biodegradable nanocomposites. In order to offer more future insights into sustainable water treatment, challenges such as membrane fouling need to be overcome via new functional carbon nano-onions based designs with better matrix-nanofiller miscibility and interfacial agreement. In this way, superior permeation flux, rejection, membrane life, and low operating costs can be attained to promote long term operations and high performance sustainable thermoplastic polymers/carbon nano-onions hybrid membranes. For drug delivery applications, main encountering factors seemed to involve well controlled drug encapsulation and release efficiencies, biocompatibility, and least toxicity or cytotoxicity effects. Here again, extensive research efforts towards the formation of new optimally functional nanocomposites appears indispensable for future high tech drug transfusion systems. Similarly, progressive endeavors by field researchers can also resolve the probable challenges for thermoplastic polymers/carbon nano-onions based bioimplants. Especially, future functional carbon nano-onions derived nanocomposites must have competence to overcome infectious complications and poor long term strength/stiffness and biological miscibility issues. Hence, by carefully monitoring all these challenging factors and development of innovative carbon nano-onions based materials and technologies, industrial footprint of these systems can be expanded in the upcoming decades.

Despite the research progression to date, synthesis of carbon nano-onion nanocomposites seemed to be limited to the lab. scale. Consequently, several challenges have been observed impeding the ecological fabrication and scalability of these hybrids. In particular, choice of precursor material, choice of synthesis technique, process conditions/parameters, price of precursor and process adopted, yield, purity, and similar aspects. Out of all these, production cost of carbon nano-onion and nanocomposites appeared as a major factor hindering their large scale production.^45,141 In this regard, economic and environmental concerns for the synthesis carbon nano-onions include the use of expensive hydrocarbons, metal catalysts, harmful solvents/chemicals, and energy demands.¹⁴² According to the scientific papers, the estimated cost for carbon nano-onions (>1000/Kg) has been reported higher than that of the carbon nanotubes (>100-150/Kg) and graphene nanostructures (80-100/Kg).¹⁴³ In addition, Table 8 is presented to better analyze the advantages and limitations of carbon nano-onions (relative to other nanocarbons) for commercial scale deployments. Thus, use of low cost green precursors, catalysts, and solvents (if required) and careful choice of synthesis route can significantly reduce the economical or environmental/sustainability concerns for large scale production of carbon nano-onions. In this way, manufacturing of carbon nano-onions and related nanomaterials can be scaled up to meet today’s growing market demands for high tech industries.

Table 8.

Comparison of essential properties, dispersion, and cost analysis of carbon nano-onions with allied nanocarbons.

Nanocarbons	Surface area (m² g⁻¹)	Electrical/thermal conductivity	Mechanical properties	Dispersion properties	Cost/scalability	Ref.
Carbon nano-onions	>400-800	2-4 Scm⁻¹/25 W/mK	Tensile strength (>1 GPa), tensile modulus (∼100 GPa); mechanical properties mostly studied as reinforcing agent for polymer or inorganic matrices	Uniform and superior than other nanocarbons (especially in functional forms)	>1000/Kg/lab scale modules	^143–145
Carbon nanotube	370–1600 (multi walled to single walled, respectively)	5000 Scm⁻¹/3000 W/mK	Fracture strength (>40 GPa), tensile strength (>100 GPa), tensile modulus (>1000 GPa).	Mostly moderate dispersion, entanglement issues	>100-150/Kg; mostly lab scale modules; few industries employ highly purified form	^143,146
Graphene nanostructures	>2600	10⁶ Scm⁻¹/3000 W/mK	Fracture strength (>120 GPa), tensile strength (>130 GPa), tensile modulus (>1 TPa)	Meager in nonfunctional form, than other nanocarbons	∼80-100/Kg; lab scale modules;	^143,146,147
Graphene nanostructures	>2600	10⁶ Scm⁻¹/3000 W/mK		Meager in nonfunctional form, than other nanocarbons	Scaled up for few industries	^143,146,147

To evaluate the sustainability and safe uses of carbon nano-onions, scientific efforts to date have been observed for life cycle assessments (or LCAs) of these nanomaterials.¹⁴⁸ For an all-inclusive estimation of LCAs for synthesizing environmentally safe and sustainable carbon nano-onions, future studies must focus: (i) careful collection of LCA data, (ii) development and practice of an appropriate characterization model, (iii) analysis of ecological impacts of carbon nano-onions during entire life cycle, (iv) identifying potential environmental risks or toxicity of carbon nano-onions, (v) analyzing uncertainty and sensitivity of carbon nano-onion synthesis and degradation processes, and (vi) understanding the mechanisms involved in entire LCAs of carbon nano-onions, from green synthesis to the end-of-life stages. Following these lines, thorough future analysis regarding LCAs of carbon nano-onions can open innovative ways for next generation green and industrial level nanomaterials.

Briefly, this dynamic review article throws light on the fundamentals of thermoplastics, biodegradable thermoplastics, and carbon nano-onions, along with the designs and technological worth of carbon nano-onions reinforced thermoplastic and biodegradable thermoplastic nanocomposites. For this purpose, significant structural and physical aspects of different categories of thermoplastic polymers/carbon nano-onions and biodegradable thermoplastic polymers/carbon nano-onions hybrids have been systematically discussed in preceding sections of this article. Besides, functional applications of carbon nano-onions filled commodity thermoplastic/biodegradable thermoplastic hybrids were stated for radiation shielding, membranes, and biomedical areas. It can be noted that despite much scientific interest in wide ranging varieties of thermoplastic polymers/carbon nano-onions nanocomposites, deployment of these nanomaterials in further advanced applied areas (energy, electronics, defense, civil, etc.) and real field challenges hindering the scalability and commercialization of these hybrids have yet not been explored. Thus, it can be concluded that focused future research on thermoplastic polymers/carbon nano-onions nanocomposites could in principle add new attractive methodical avenues for worldwide modern scientific communities.

Footnotes

Declaration of conflicting interests

The author declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author received no financial support for the research, authorship, and/or publication of this article.

ORCID iD

Ayesha Kausar

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The promise of carbon nano-onions for thermoplastic and biodegradable thermoplastic nanocomposites—status quo and future vision

Abstract

Keywords

Introduction

Thermoplastic and biodegradable thermoplastic polymers

Carbon nano-onions

Thermoplastic polymers/carbon nano-onions nanocomposites

Biodegradable thermoplastic polymers/carbon nano-onions hybrids

Technological influence of carbonaceous nano-onions nanoadditives towards thermoplastic or biodegradable thermoplastic nanomaterials

Challenges and summation

Footnotes

Declaration of conflicting interests

Funding

ORCID iD

References