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Review

Nanoclay-Reinforced Nanocomposite Nanofibers—Fundamentals and State-of-the-Art Developments

by
Ayesha Kausar
1,2,3,*,
Ishaq Ahmad
1,2,3,
O. Aldaghri
4,
Khalid H. Ibnaouf
4 and
M. H. Eisa
4
1
NPU-NCP Joint International Research Center on Advanced Nanomaterials and Defects Engineering, National Centre for Physics, Islamabad 44000, Pakistan
2
UNESCO-UNISA Africa Chair in Nanosciences/Nanotechnology, iThemba LABS, Somerset West 7129, South Africa
3
NPU-NCP Joint International Research Center on Advanced Nanomaterials and Defects Engineering, Northwestern Polytechnical University, Xi’an 710072, China
4
Department of Physics, College of Science, Imam Mohammad Ibn Saud Islamic University (IMSIU), Riyadh 13318, Saudi Arabia
*
Author to whom correspondence should be addressed.
Minerals 2023, 13(6), 817; https://doi.org/10.3390/min13060817
Submission received: 1 May 2023 / Revised: 24 May 2023 / Accepted: 12 June 2023 / Published: 15 June 2023
(This article belongs to the Special Issue Feature Papers in Clays and Engineered Mineral Materials)
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Versions Notes

Abstract

:
Nanoclays are layered mineral silicates, i.e., layered silicate nanosheets. Nanoclays such as montmorillonite, bentonite, kaolinite, etc., have been used as reinforcements in the nanofibers. Numerous polymers have been used to fabricate the nanofibers, including poly(vinylidene fluoride), poly(vinyl alcohol), polycaprolactone, nylon, polyurethane, poly(ethylene oxide), and others. To develop better compatibility with polymers, nanoclays have been organo-modified prior to reinforcement in the nanofiber matrices. This state-of-the-art review highlights the fundamentals, design, fabrication, and characteristics of the polymer/nanoclay nanofibers. The nanoclay filled nanocomposite nanofibers have been fabricated using electrospinning and other fiber processing techniques. The electrospinning technique has been preferred to form the nanoclay-filled nanofibers, owing to the better control of processing parameters and resulting nanofiber properties. The electrospun polymer/nanoclay nanofibers usually have fine nanoparticle dispersions, microstructures, smooth textures, and narrow diameters. The physical properties of the designed nanofibers depend upon the processing technology used, solvent, solution/melt concentration, flow rate, spinning speed, voltage, and other process parameters. Hence, this review attempts to assess a literature-driven consequence of embedding nanoclays in the polymeric nanofibers in a broad context of the application of these fibrous materials. Conclusively, to design the polymer/nanoclay nanofibers, montmorillonite nanoclay has been observed as a nanofiller in most of the studies, and, similarly, the electrospinning technique was preferred as a fabrication technique. Almost all the physical properties of the nanofibers studied revealed dependences upon the choice of the polymer matrix for nanofiber formation as well as the nanoclay contents, modification, and dispersion state. Accordingly, the nylon/nanoclay nanofibers have been investigated for nanofiller dispersion, mechanical properties, and thermal profiles. The antibacterial properties were among the prominent features of the poly(vinyl alcohol)/nanoclay nanofibers. The poly(vinylidene fluoride)/nanoclay systems were explored for the microstructure, crystallinity, and piezoelectric properties. The polycaprolactone/nanoclay nanofibers having fine microstructure were capable of forming tissue engineering scaffolds. The drug delivery and sound absorption properties were noticeable for the polyurethane/nanoclay nanofiber systems. Moreover, the poly(lactic acid)/nanoclay nanofibers were found to have prominent biodegradability and low gas permeability features. The resulting polymer/nanoclay nanocomposite nanofiber systems found potential for the technical applications of sensors, packaging, tissue engineering, and wound healing. However, thorough research efforts have been found to be desirable to find the worth of polymer/nanoclay nanofibers in several concealed technological sectors of energy, electronics, aerospace, automotives, and biomedical fields.

Graphical Abstract

1. Introduction

The polymers and nanocomposites have been processed into nanofibers for technical purposes [1]. Nanoclay is a layered mineral silicate nanostructure, which is widely used for nanocompositing [2]. The chemical composition of nanoclays may be different, including the aluminum silicates, magnesium silicates, aluminum–magnesium silicates, and other mineral silicate nanoforms. The combination of polymers and nanoclays has been found to enhance the microscopic and physical features of the nanocomposites [3]. Enhancements in the nanocomposite properties have been credited to synergistic effects among polymers and nanofillers [4]. The polymer/nanoclay nanocomposites have also been developed in a nanofiber form through facile processing techniques [5]. Electrospinning has been used as an effective and facile method to form polymer- and nanocomposite-derived nanofibers [6,7,8]. Various tactics can be adopted for processing polymer/nanoclay nanocomposite nanofibers; however, electrospinning has been favored, owing to benefits such as a simple apparatus, the control of nanofiber diameter, texture, and morphology, and superior physical properties [9]. Rigid nanoclay nanoplatelets have been used to reinforce the polymer structures to hinder the free movements of adjacent polymeric chains [10]. Furthermore, the interfacial adhesion between the nanoplatelets and polymer chains was observed due to the load-bearing effect of nanoclays. The formation of novel polymer/nanoclay materials has been a progressing field in materials science for years [11,12].
This comprehensive review article states essentials and methodological aspects of polymer/nanoclay nanocomposite nanofibers. The amalgamation of polymeric matrices with nanoclays and fiber processing through appropriate techniques has led to high performance nanocomposite nanofibers. The properties and performance of the nanofibers depend upon the chemical compatibility between the matrix nanofiller, the interfacial interactions, and the homogeneous nanoclay dispersion. High efficiency nanocomposite nanofibers have been applied in technical fields ranging from electronics to the biomedical industry. To the best of our knowledge, this review is novel and pioneering to highpoint the field of nanoclay-derived nanofibers. Research has been reported on polymer/nanoclay nanofibers. Nevertheless, the literature is not in an assembled and updated form. Therefore, these polymer/nanoclay nanocomposite nanofibers will be certainly supportive for scientists in crucial future revolutions in nanoclay-based nanofiber manufacturing technologies.

2. Nanoclay

For polymeric nanocomposites, various inorganic or organic nanomaterials have been used as reinforcement [13]. Nanoclay is an exclusive inorganic nanofiller to form organic–inorganic hybrids with polymers [14]. Nanoclays are phyllosilicate minerals, having several different types such as montmorillonite, kaolinite, bentonite, etc. [15]. The two-dimensional nanoclay nanostructure consists of tetrahedral silica nanosheets layered with octahedral alumina nanosheets (Figure 1). The thickness of layered nanosheets may vary ~ 0.7–1 nm [16]. The layered nanosheet structure has been formed due to van der Waals interactions. The hydrophilic and inorganic nature of nanoclay layers render it difficult to interact and compatibilize with organic polymers [17]. Various organic molecules, ions, and surfactants have been used to enhance the organophillicity of nanoclays and to increase the spacing between layers [18]. The negatively charged nanosilicate nanosheets may have electrical conductivity values in the range of 25–100 mSm−1 [19]. As nanosilicate nanosheets are negatively charged, the interlayer spacing can easily accommodate cations such as K+, Na+, Mg2+, Ca2+, etc. [20]. Later, the organic cations in the nanoclay galleries can be replaced with the polymeric chains to form the compatibilized polymer/nanoclay hybrids. Nanoclays and organo-modified nanoclays have been reinforced in a range of polymers such as polyurethane, polyamide, polystyrene, epoxy, etc. [21].
The most commonly used nanoclays in the nanofibers include montmorillonite, Cloisite, bentonite, etc. In montmorillonite nanoclay, the most commonly used nanoclay for nanofibers, the tetrahedral/octahedral/tetrahedral layers have parallel orientations with negative charges [23]. The negative charges can be neutralized with the positive ions at the interlayer spaces. These nanoclays possess high adsorption capacities. The montmorillonite is a smectite nanoclay and the aluminum ions can be easily substituted by the magnesium ions in the octahedral sites. Owing to the formation of stable colloidal dispersion, swelling properties, and thermal and chemical stability, the montmorillonite nanoclay has been widely used with the polymers. Cloisite is also a natural phyllosilicate mineral. Its structure and properties are similar to those of montmorillonite nanoclays [24]. It has fine flame-retardant properties; thus, it can be used as a halogen-free flame retardant. Bentonite is an aluminum phyllosilicate nanoclay. Bentonite is a swelling clay, having absorbent properties [25]. Pristine nanoclays cannot be dispersed in the organic polymers due to their inorganic nature and inherent hydrophilic character. Moreover, face-to-face stacking of the nanoplatelets render these incompatible with the hydrophobic polymers. To use these nanoclays, treatment with organic compounds is essential to enhance the dispersion and compatibility with polymers [26]. After the modification of nanoclay platelets with organic ions between the galleries, these nanofillers can be effectively used with polymers to form the mixed phases. During the formation of polymer/nanoclay nanofibers, three types of interactions can be developed between the polymer and nanoclay: (i) the formation of micro-composites has been observed if nanoclay platelets are not dispersed and develop agglomerates [27]; (ii) the development of the intercalated nanocomposite through the intercalation of the polymer chains between the well-spaced nanoclay galleries (used after organic modification) [28]; and (iii) the exfoliated nanocomposites may be detected when polymer chains can be dispersed in the fully delaminated randomly oriented nanoclay platelets [29]. Among these interactions, the intercalated polymer/nanoclay nanocomposites have been found to develop well compatible interfaces [30]. The well dispersed nanoclays in polymers have been found to enhance the mechanical, electrical thermal, non-flammability, barrier, and several other physical properties of the nanocomposites [31,32,33,34]. The industrial applications of polymer/nanoclay nanocomposites have been experiential in industries such as aerospace, automotive, civil engineering, membranes, coatings, drug delivery, and so on [35,36,37].

3. Polymer and Nanocomposite Nanofiber

Polymer nanofibers have diameters of few nanometers and lengths of several millimeters [38]. The resulting nanostructures own enhanced physical characteristics and methodological applications [39]. The choice of nanofiber manufacturing practices defines the nanofibers’ diameters, textures, and physical features. The nanofiber texture can be smooth or wrinkled, and it can be solid or ribbon-like. Core shell nanofibers have also been produced and studied [40]. The solid polymer nanofibers with smooth textures have been favored for engineering applications. Hollow nanofibers have been found to be desirable for certain applications such as drug or gene delivery [41]. Synthetic as well as natural polymers have been employed to design the nanofibers. Synthetic polymers such as thermoplastic polymers and conjugated polymers have been broadly utilized to fabricate the nanofibers [42]. The nanofibers with high surface areas, fine flexibilities, electrical conductivities, toughness properties, and strengths have been applied for industrial applications such as electronics, energy, coatings, membranes, drug delivery, and tissue engineering [43]. The polymer nanofibers can be fabricated using the spinning processes, template method, template-free procedure, melt technique, and solution drawing technique [44]. The diameter of as-spun nanofibers usually varies from nanometers to few micrometers [45].
Similar to polymers, polymeric nanocomposite nanofibers have been formed using polymers and inorganic nanoparticles as well as organic nanoparticles [46]. Among inorganic nanoparticles, silica, titania, zinc oxide, nanoclay, and other inorganic nanoparticles have been used as nanofillers in polymeric nanofibers [47]. Poly(vinyl alcohol) has been filled with silica, titania, silver, etc. [48,49,50]. The template technique has been applied to form nanofibers of a polyaniline/titania nanocomposite [51]. The spinning method has been used to fabricate polyaniline/zinc oxide and nylon 6,6/zinc oxide nanocomposite nanofibers [52,53]. Among carbon nanoparticles, carbon nanotubes, graphene, carbon fibers, and other organic nanofillers have been used [54,55]. Carbon-nanotube-filled polyamide [56], polystyrene [57], and polyaniline-filled [58] nanofibers have been processed through the spinning process, template method, phase separation, freeze-drying, solution technique, and melt process.
Since the 20th century, nanofiber formation processes have been focused on [59]. After that, various methods and the commercial practicalities of nanofibers have been researched. In the template method, mold is employed to attain the desired polymer nanofibers or nanocomposite nanofibers [60]. The porous template is usually used to produce nanofibers by exerting pressure on one side and extruding the fibrous material. The phase separation technique involves physical parting, owing to solvent incompatibility, leading to solid nanofibers [61,62]. However, this technique cannot form long fibers. In this regard, spinning processes have been used to form nanofibers with several micrometer lengths. Moreover, this technique can easily control the nanofiber diameter and uniform surface. Among spinning techniques, electrospinning has been widely used to form aligned nanofibers with uniform morphologies. In electrospinning, fiber production utilizes electric force to form charged strands from polymer melts/solutions. The charged strand is then stretched and elongated to generate nanofibers, which are collected on the collector. The schematic of the electrospinning set-up and the lab scale system used are shown in Figure 2 [63]. It consists of a syringe with a needle, spinneret, voltage source, collector, etc. Electrospinning parameters affect the nanofibers’ textures, diameters, and morphologies.
Major electrospinning parameters affecting the nanofiber aspects include:
  • The distance between the spinneret and the collector influences fiber diameter and morphology [64]. The optimum distance is important to avoid bead formation and to form solid round fibers.
  • The feed rate affects polymer solution delivery speed [65]. Solution feed rate defines the nanofiber diameter and morphology.
  • The voltage between the needle and collector (metal) is significant to form thin polymer jets and minimize the surface tension [66]. A very low electric field cannot cause jet elongation to form uniform nanofibers.
  • The pressure of pumping a polymer solution or melt from a spinneret also affects the nanofiber diameter and morphology [67].
Table 1 briefly lists the comparison of different fabrication methods, parameters, and features. Briefly speaking, the processing method opted for, the processing parameters, the polymer type, and the nanofiller type and content used affect the nanofibers’ diameters, consistencies, and properties. Controlling and monitoring all the factors may lead to uniform nanofibers [68].

4. Polymer/Nanoclay Nanocomposite Nanofiber

4.1. Poly(Vinylidene Fluoride)/Nanoclay Nanofiber

Polymer nanocomposites have been manufactured into nanofibers having high surface areas, optimum porosities, and uniform alignments [97,98]. Poly(vinylidene fluoride) is a thermoplastic polymer with fine mechanical strength, biocompatibility, UV resistance, nuclear radiation confrontation, chemical stability, and low dielectric constant [99,100]. Poly(vinylidene fluoride) has been applied in a range of technical applications such as sensors, actuators, and energy devices [99]. Similar to other polymers, nanoclay nanofiller has been used to reinforce the poly(vinylidene fluoride) matrix [101,102]. Yu et al. [103] reported on poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers. The poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers were electrospun in the presence of N,N-dimethylformamide/acetone solvents. The nanofibers had diameters of 50–800 nm with homogeneous surfaces and uniformities. Due to ion-dipole interactions, STN has the capability to bond with poly(vinylidene fluoride). Figure 3 shows the interactions between the electrospun poly(vinylidene fluoride) and the nanoclay in the nanofiber. During the electrospinning, the nanoclay generated β phases due to the aligned CH2 dipole on one side in the presence of an electric field [104]. STN was found to be more effective in crystallizing the α and β phases.
Yang et al. [105] developed fine poly(vinylidene fluoride)/organomodified montmorillonite nanocomposite nanofibers with fine piezoelectric properties. The inclusion of organomodified montmorillonite generated polar crystalline β and γ phases in the nanocomposite nanofibers (Figure 4). The ion–dipole interactions between the polymer and the organomodified nanoclay generated stabilized trans conformers on the nanoplatelets. Consequently, static and dynamic samples have been prepared. The polar β crystalline phase caused fine piezoelectric and toughness properties. The mechanical properties of poly(vinylidene fluoride) and poly(vinylidene fluoride)/organomodified montmorillonite nanocomposite nanofibers were studied using stress–strain plots (Figure 5). In static samples, enhancing nanoclay contents up to 2 wt.% enhanced the polar phase contents from 5.5%–62% and the elongation at break by 244%. In the dynamic samples, the addition of 2 wt.% nanoclay enhanced the polar phase content from 13%–79.5% and the elongation at break by 165%–227%. The dynamic samples revealed better crystalline phase generation and mechanical properties of the poly(vinylidene fluoride)/organomodified montmorillonite nanocomposites.
Liu et al. [106] reported poly(vinylidene fluoride)/organically modified montmorillonite nanocomposite nanofibers through electrospinning. Due to the synergistic effect between poly(vinylidene fluoride) and nanoclay in the electrospun nanofibers, polar crystalline β and γ phases exist. The inclusion of organically modified montmorillonite nanoclay in nanofibers prevented the entanglement effect and produced fine uniform nanomaterials. Tiwari et al. [107] also designed electrospun poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers. As compared to the neat polymer nanofibers, poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers have 300% toughness properties. The addition of nanoclay stabilized 90% of the piezoelectric active phase, i.e., it was appropriate for device application. The hybrid device had the capability to transform mechanical energy to electric power. The poly(vinylidene fluoride)/nanoclay nanocomposite nanofiber-based device had power generation up to 100 ms for 50 ms tenure. The device had a power density of 68 μW cm−2 and an output voltage of 70 V. Hence, the inclusion of organomodified nanoclay developed crystalline phases in the poly(vinylidene fluoride) matrix and piezoelectric properties, which have been found to be applicable for electronic and energy devices.

4.2. Poly(Vinyl Alcohol)/Nanoclay Nanofiber

Poly(vinyl alcohol) is a synthetic, biodegradable, biocompatible, non-toxic, and mechanically stable polymer [108]. Poly(vinyl alcohol) nanofibers have been produced [109]. Poly(vinyl alcohol) nanofibers have been loaded with drugs or active agents for drug delivery and tissue engineering applications [110]. Tian et al. [111] produced neat poly(vinyl alcohol) nanofibers that were hydrophilic. However, upon the inclusion of glutaraldehyde as a crosslinking agent, the water resistance and mechanical properties were considerably enhanced. Park et al. [112] produced poly(vinyl alcohol)-, chitosan oligosaccharide-, and montmorillonite-based nanocomposite nanofibers by electrospinning. The morphological, mechanical, and thermal properties of the nanofibers were enhanced with the inclusion of nanofillers. Elhami et al. [113] fabricated poly(vinyl alcohol)/nanoclay nanocomposite nanofibers by electrospinning. The electrospun nanofibers had diameters of ~300 nm. The nanofiber morphologies, miscibilities, and interactions have been studied. Elhami et al. [114] prepared poly(vinyl alcohol)/montmorillonite nanocomposite nanofibers through the electrospinning process. The barrier effect of the nanocomposite nanofibers has been studied. Sharma et al. [115] fabricated poly(vinyl alcohol)/nanoclay nanocomposite nanofibers. In this regard, poly(vinyl alcohol)/Cloisite 30B and poly(vinyl alcohol)/Cu-montmorillonite nanocomposite nanofibers have been formed. During electrospinning, nanoclays were exfoliated. The mechanism of nanoclay exfoliation in the electrospinning process is given in Figure 6. The poly(vinyl alcohol)/nanoclay nanofibers have average diameters of 107–140 nm. Figure 7 reveals the field emission scanning electron microscopic images of the poly(vinyl alcohol)/nanoclay nanocomposite. The nanoclay nanoparticles were found to be consistently dispersed in the nanofibrous web. Moreover, the poly(vinyl alcohol)/Cloisite 30B and poly(vinyl alcohol)/Cu-montmorillonite nanocomposite nanofibers had antibacterial properties towards the Gram-positive bacterial strain Staphylococcus aureus and the Gram-negative bacterial strain Escherichia coli [116,117,118]. In the antimicrobial tests, the poly(vinyl alcohol)/Cu-montmorillonite formed a larger zone of inhibition than the poly(vinyl alcohol)/Cloisite 30B, inhibiting the bacterial actions. This effect was observed due to the diffusion rate and inherent antibacterial properties of copper ions present in the montmorillonite nanoclay galleries. Thus, the nanoclay-based nanofibers have been found to be useful for microbial protection applications.

4.3. Nylon/Nanoclay Nanofiber

Nylon, or polyamide, is a synthetic polymer with amide units in its backbone [119]. Nylon 6 has been used to develop nanofibers by electrospinning [120]. Uniform and aligned nanofibers of nylon 6 have been produced using a 20 wt.% solution, an applied voltage of 15 kV, and a spinning distance of 8 cm. Li et al. [121] prepared nylon 6 nanofibers reinforced with montmorillonite and Cloisite-30B nanoclays. Consistent and cylindrical nylon 6/nanoclay nanocomposite nanofibers with diameters of 70–140 nm were formed. The melt-extruded nylon 6/nanoclay nanocomposite was used to form the nanofibers. The mechanical properties, especially the Young’s modulus of the nanofibers, were found to enhance with the nanoclay loading. Saeed et al. [122] produced electrospun nylon 6 and nylon 6/nanoclay nanocomposite nanofibers. The nanofibers were uniform and smooth with diameters of ~350 nm. According to differential scanning calorimetric analysis, the α- and γ-crystalline phases revealed endotherms in the range of 214–220 °C. Wu et al. [123] processed electrospun nylon 6/montmorillonite nanocomposite nanofibers. The nanofibers were formed both from solution and melt. Transmission electron microscopy (TEM) exhibited fine nanoclay dispersion and exfoliation in the nanofiber matrix. The inclusion of montmorillonite nanoclay enhanced the non-flammability and char yield of the nanocomposite nanofibers. Agarwal et al. [124] formed electrospun nylon 6/montmorillonite nanocomposite nanofibers and analyzed their morphological and mechanical features. The TEM micrographs of the nylon 6/montmorillonite nanocomposite nanofibers are given in Figure 8. The nylon 6-derived nanofibers had homogeneous surfaces, and no nanoclay aggregates were observed in the polymer matrix. The results revealed the effectiveness of the fiber processing technique and the fine dispersion of the nanofiller in the polymer matrix. The mechanical properties of the nylon 6/montmorillonite nanocomposite nanofibers have been investigated. The inclusion of 5 wt.% nanoclay enhanced the tensile properties of the nanofibers. Neat nylon 6 had a tensile stress and an elongation at break of 3.9 ± 0.8 MPa and 3.73 ± 0.6%, respectively. The inclusion of montmorillonite nanoclay significantly enhanced the tensile strength and the elongation at break to 5.3 ± 0.5 MPa and 5.71 ± 0.2%, respectively. The effect was observed due to the optimum concentration of nanoclay nanofiller added, nanoparticle dispersion, as well as the alignment and reinforcement effects in the polymer matrix. However, beyond that concentration, mechanical properties were declined due to the nanoclay aggregation effect [125].

4.4. Polycaprolactone/Nanoclay Nanofiber

Polycaprolactone is a biodegradable polyester [126]. This biomaterial has better rheological and viscoelastic properties than other aliphatic polyesters. Polycaprolactone has been used in drug-delivery, bioimplant, and biomedical devices [127,128]. Irandoost et al. [129] designed polycaprolactone/nanoclay nanofibers formed by electrospinning. The structures, morphologies, and adsorption capacities of the nanofibers were investigated. The nanoclay inclusion enhanced the adsorption processes of the nanocomposite nanofibers. Devina Merin et al. [130] also examined morphologies, thermal stabilities, and sorption properties of electrospun polycaprolactone/nanoclay nanofibers. The porosities, pore sizes, and diameters influenced the final nanofiber properties. Zhou et al. [131] formed electrospun polycaprolactone/nanoclay nanocomposite nanofibers. The inclusion of nanoclay enhanced the homogeneity of the nanofibers for tissue engineering scaffolds. Moreover, the microstructures and nanofiber diameters, densities, and alignments in the scaffolds affect the tissue engineering capability. Ahmadi et al. [132] fabricated electrospun polycaprolactone/gelatin and layered double-hydroxide-based nanofibers. Figure 9 shows the electrospinning process to form the nanocomposite nanofibers. The polycaprolactone/gelatin/layered double hydroxide nanocomposite nanofibers have been applied in nerve tissue engineering. The nanocomposite nanofibers-based scaffolds have been studied for physicochemical and biological features. The inclusion of nanoclays in polycaprolactone-based scaffolds enhanced the cell attachment and proliferation features. The nanofibers have been found to be efficient contenders for nerve tissue engineering. Future research on polycaprolactone/nanoclay nanocomposite nanofibers may lead to efficient biocompatible tissue engineering scaffolds.

4.5. Polyurethane/Nanoclay Nanofiber

Polyurethane nanofibers have been developed using electrospinning [133,134,135]. The electrospun nanofibers of polyurethane have been produced using an N,N-dimethylformamide solvent. The polyurethane nanofibers may have diameters in the range of 50–700 nm. The polyurethane nanofibers’ morphologies and properties were found dependent on the polyurethane type, solution concentration, feed rate, applied voltage, etc. Nanoparticle-filled polyurethane nanocomposite nanofibers have also been developed [136]. Saha et al. [137] formed electrospun polyurethane/nanoclay nanocomposite nanofibers. The montmorillonite nanoclay has been filled in polyurethane nanofibers. The nanofibrous material was used for the drug delivery of chlorhexidine acetate, i.e., an antiseptic drug. The polyurethane/montmorillonite nanoclay nanofibers revealed controlled drug loading and drug release behaviors. Bahrambeygi et al. [138] also produced polyurethane/montmorillonite nanoclay nanocomposite nanofibers. The nanofibers were tested for sound absorption properties. The sound absorption material revealed better performance with increasing numbers of nanofiber layers. However, limited literature reports are available on polyurethane/nanoclay nanofiber designs, and future efforts may lead to more advanced application zones of innovative nanofibers [139].

4.6. Poly(Lactic Acid)/Nanoclay Nanofiber

The poly(lactic acid) and nanoclays form an important class of polymer/nanoclay nanocomposites [140]. Poly(lactic acid) is an important aliphatic polyester [141]. Poly(lactic acid) has low cost, fine processability, formability, stiffness, and oil resistance properties [142]. It has wide ranging applications in automobiles, packaging, textiles, and other commercial uses [143,144]. An important application of poly(lactic acid) has been observed in the formation of the nanofibers [145,146,147]. Nevertheless, the uses of poly(lactic acid) and derived materials have been limited due to brittleness, low thermal stability, high gas permeability, etc. Several methods have been assumed to overpower these disadvantages [148,149]. One method is the inclusion of nanoclay nanofillers to attain high-performance poly(lactic acid) nanocomposites [150]. Even low montmorillonite contents have been found to improve the physical features of the nanocomposites. Especially, the mechanical properties of poly(lactic acid)/nanoclay nanocomposites enhanced with nanofiller loading [151]. Nanoparticles were found to behave as nucleating agents, thus increasing the crystallinity properties and tensile strengths of the nanocomposites. Lewitus and co-workers [152] caused a 30% upsurge in the tensile modulus of the matrix. Ray and researchers [153] studied the enhancements in the mechanical and biodegradability features and reduced the gas permeability of the nanocomposites. Mayekar et al. [154] prepared the nanocomposites of poly(lactic acid) with organo-modified montmorillonite and unmodified montmorillonite. The effect of the nanoclay addition was observed on the crystallinity and biodegradation properties of the materials. The hydrolysis tests were carried out on the poly(lactic acid)/montmorillonite nanocomposites for 30 days to understand the biodegradation of the materials. Biodegradation was found to be dependent upon the competitive balance in the diffusion and absorption of water in the nanocomposite system.

5. Significance of Polymer/Nanoclay Nanocomposite Nanofiber

5.1. Sensors

Due to nanoscale size and unique dimensions, nanoclays have manifold applications in varied industrial zones [155,156]. Due to ion exchange capacities, polymer/nanoclay nanocomposites and polymer nanoclay nanofibers may easily incorporate biomolecules, electroactive ions, enzymes, and fluorescence probes and thus have been used as sensors [157,158]. Poly(vinylidene fluoride) with induced β-phases revealed fine electrical or mechanical features [159]. The β-phase in poly(vinylidene fluoride) is usually induced by the poling processes, which may be formed by the addition of nanoparticles. The polar crystalline phase in poly(vinylidene fluoride) can be initiated by the inclusion of nanoclays, leading to piezoelectricity [160,161,162]. The electrospinning process has also been known to induce piezoelectricity in polymer nanofibers due to electric field poling [163]. In addition, nanoclay nanofiller may enhance the electrospinning poling of poly(vinylidene fluoride). The piezoelectric properties of poly(vinylidene fluoride) and poly(vinylidene fluoride)/nanoclay nanofibers have been applied for sensor applications. Xin et al. [164] reported a sensor based on poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers. Near-distance-wheeling electrospinning was applied to form the nanofibers. In this method, a high electric field as well as high mechanical stretching were applied on the nanofibers. Figure 10 shows the experimental setup for the full-fiber sensor. It contains the poly(vinylidene fluoride) fiber adhesively bonded to the cantilever elastic plastic beam. The voltage output was noted on an oscilloscope. The inset displays a photograph of the obtained fiber sensor. During this process, the nickel–copper-plated polyester fabric was used to collect the fibers. The conductive fabric and adhesive transparent breathable tape were adhered to the outer surface to assemble a sandwich structure. Thus, the finally formed sensor was full fiber and breathable. Moreover, the FT-IR and XRD analyses of these nanofibers demonstrated the formation of β crystals in the nanofibers. The fine piezoelectric properties of the poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers were attained, which were suitable for full-fiber sensor formation. The full-fiber sensor was usable for intelligent clothes due to good reproducibility and response speed for recording the respiration rate and pulse of a human being. However, comprehensive future research efforts are needed on textiles with nanodevice sensing systems for advancement in this field.

5.2. Packaging

For packaging applications, fine barrier properties have been found indispensable [165,166]. The nanoclay nanocomposite-derived packaging has high barrier features towards oxygen and moisture [167]. Particularly, polymer/nanoclay nanocomposite nanofibers may form uniform coatings for packaging applications. As compared to traditional packaging, food-grade polymers and nanoclay-based nanomaterials have been advantageously used for the food packaging industry [168]. Such packaging materials have been used to extend the shelf life of food products. Electrospinning has been used to form the nanofibers using polymer/nanoclay nanocomposite nanofibers [169]. The electrospun polymer/montmorillonite nanocomposite nanofiber membranes revealed superior morphological, mechanical, and thermal features, in addition to barrier properties. The nylon 6/nanoclay nanocomposite nanofibers enhanced the barrier properties for packaging applications [170]. Agarwal et al. [124] reported nylon 6/montmorillonite nanocomposite nanofiber-based coatings on polypropylene packaging. In the case of neat polypropylene packaging, fungal growth was observed on bread after five days (Figure 11). Microbial counts of 2.9 × 104 CFU/g (after five days) and 7.25 × 104 CFU/g (after seven days) were observed for bread. However, food in polypropylene packaging coated with nylon 6/montmorillonite nanocomposite revealed no fungal growth. The nylon 6/montmorillonite nanocomposite nanofiber-coated packaging had a much lower bacterial count of 92 CFU/g (after five days) and 230 CFU/g (after seven days). However, fewer studies have been observed regarding nanoclay-derived nanofiber coatings on polymer packaging, and future research is desirable.

5.3. Tissue Engineering and Wound Healing

Tissue engineering has been identified as an emerging technology for the regenerative medicine field [171,172]. Engineered tissue scaffolds have been used as replacement of the tissue matrix [173]. The nanofiber-based scaffolds offer physical architectures for new tissue generation. Usually, nanofibrous mats for tissue engineering have been produced using the electrospinning method. The appropriately designed nanofibers using biopolymers and nanoclays revealed fine cell proliferations and attachments [174]. The electrospun nanofibrous scaffolds had fine biological and mechanical properties depending upon the polymer used and processing parameters [175]. Nouri et al. [176] developed poly(ɛ-caprolactone)/nanoclay nanocomposite nanofibers by electrospinning. The inclusion of nanoclay endorsed the formation of uniform nanofiber creations with lesser diameters than neat poly(ɛ-caprolactone) nanofibers. The nanocomposite nanofibers revealed fine degradability, wettability, and mechanical stability for tissue engineering. Moreover, the bioactivity and cell adhesion of poly(ɛ-caprolactone)/nanoclay nanocomposites towards fibroblasts cells were tested. Koosha et al. [177] produced chitosan/poly(vinyl alcohol)/montmorillonite nanocomposite nanofibers using the electrospinning technique. The bead-free uniform nanofibers were tested for cytotoxicity by an MTT assay on the A-431 cell line. The nanofibers revealed fine cell attachments and viability properties. Ghasemi et al. [178] prepared chitosan-intercalated poly(vinyl alcohol)/montmorillonite nanocomposite nanofibers for the tissue engineering of human dental pulp stem cells. The nanofibers had homogeneous morphologies, mechanical stabilities, viabilities, and non-toxicity properties. The poly(vinyl alcohol)/montmorillonite nanocomposite nanofibers were used as artificial nerve graft culture for the regrowth of damaged neural tissues. Hakimi et al. [179] prepared hydrogel of chitosan/polyethylene oxide/nanoclay–alginate nanofibers. The nanomaterial scaffold had the capability to form a bone-like apatite. The compatibility of the nanomaterial scaffolds was tested using the osteoblastic cell line. The crystalline phase of the bone-like apatite was studied using XRD. Moreover, hemolysis and MTT assays were investigated for scaffolds and were found to be compatible with human cells.
In addition, biodegradable and biocompatible natural polymers such as poly(vinyl alcohol) have been used for tissue scaffolds and wound healing [180,181,182]. Heydary et al. [183] produced electrospun poly(vinyl alcohol)/nanoclay nanocomposite nanofibers having nontoxicity, biodegradability, mechanical stability, and antibacterial properties for wound healing applications. The poly(vinyl alcohol)/nanoclay nanocomposite with Iranian Gum Tragacanth was used for wound healing applications. The nanomaterial had fine resistance properties towards bacterial attacks. Novel nanofibrous materials need to be designed for wound healing to expand the application of these materials and to see their true potential.

6. Future Prospects

The application areas studied, thus far, for polymer/nanoclay nanocomposite nanofibers include sensors, packaging, tissue engineering, and wound healing. Although, thorough research efforts have not been observed in these fields, and future research seems to be desirable. The lack of research for polymer/nanoclay nanocomposite nanofibers has been observed for important application areas such as membrane technology. The development of polymer/nanoclay nanocomposite nanofibrous membranes may further broaden their scope for biomedical applications. In energy storage applications, the interactions between polymers and nanoclays may lead to supercapacitor electrodes to support electrons and charge transportation properties. Other concealed application areas of polymer/nanoclay nanocomposite nanofibers include aerospace and automobiles. The coatings and textiles areas also need to be focused on for polymer/nanoclay nanofibers. At this juncture, challenges regarding nanoclay dispersion, modification, and ultra-high conductivity, mechanical, and heat stability properties need to be overcome.

7. Conclusions

In this article, the fabrication and features of polymer/nanoclay nanocomposite nanofibers have been studied. The nanofibers can be processed by different techniques (solution, template, phase separation, freeze-drying, etc.). However, electrospinning was preferred, owing to its facile design, parameters, and the final nanomaterial properties. The electrospinning method has been found to enhance the structural, morphological, electrical, thermal, mechanical, and other physical properties of the nanofibers. The polymer solution as well as the melt has been used to form the nanoclay-filled nanofibers. The electrospun polymer/nanoclay nanofibers have fine nanoparticle dispersions and smooth and non-beaded surfaces. Consequently, the choice of fabrication technique, nanoclay type, nanofiller contents, polymer type, solvent, concentration, spinning speed, flow rate, applied voltage, and other parameters affect the uniformity, texture, morphology, diameter, and uses of the polymer/nanoclay nanocomposite nanofibers. The resulting nanoclay-based nanofibers revealed fine microstructures, crystalline phase formations, enhanced mechanical (stress, elongation at break, toughness, Young’s modulus) and thermal profiles, piezoelectric features, and antibacterial and electrical properties. The high-performance polymer/nanoclay nanocomposite nanofibers exposed potential sensors, packaging, tissue engineering, and wound healing. Future progressions in the field of polymer/nanoclay nanocomposite nanofibers and associated application zones rely on the usage of innovative designs and manufacturing practices.

Author Contributions

Conceptualization, A.K.; data curation, A.K.; writing of original draft preparation, A.K.; Review and editing, A.K., I.A., O.A., K.H.I. and M.H.E. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Structure of montmorillonite nanoclay [22]. Reproduced with permission from Springer.
Figure 1. Structure of montmorillonite nanoclay [22]. Reproduced with permission from Springer.
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Figure 2. (A) The schematic of electrospinning set-up; and (B) setup and collectors for electrospinning in the laboratory [63]. Reproduced with permission from Future Medicine LTD.
Figure 2. (A) The schematic of electrospinning set-up; and (B) setup and collectors for electrospinning in the laboratory [63]. Reproduced with permission from Future Medicine LTD.
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Figure 3. Schematic of interactions between electrospun poly(vinylidene fluoride) and nanoclay-based nanocomposite nanofiber: partially positive C–H bond attracted to negatively charged silicate layer in STN and SWN due to static electric force [103]. Reproduced with permission from Elsevier.
Figure 3. Schematic of interactions between electrospun poly(vinylidene fluoride) and nanoclay-based nanocomposite nanofiber: partially positive C–H bond attracted to negatively charged silicate layer in STN and SWN due to static electric force [103]. Reproduced with permission from Elsevier.
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Figure 4. Proposed mechanism of cooperative effect of (a) shear addition of organomodified montmorillonite to polymer; and (b,c) facile formation of polar crystalline β and γ phases in poly(vinylidene fluoride)/organomodified montmorillonite nanocomposite nanofibers [105]. Reproduced with permission from Elsevier.
Figure 4. Proposed mechanism of cooperative effect of (a) shear addition of organomodified montmorillonite to polymer; and (b,c) facile formation of polar crystalline β and γ phases in poly(vinylidene fluoride)/organomodified montmorillonite nanocomposite nanofibers [105]. Reproduced with permission from Elsevier.
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Figure 5. Strain–stress curves of static (S) and dynamic (D) poly(vinylidene fluoride) (PVDF) and poly(vinylidene fluoride)/organomodified montmorillonite (OMMT) nanocomposite nanofibers. Symbol list inside the plot frame are going from left to right [105]. Reproduced with permission from Elsevier.
Figure 5. Strain–stress curves of static (S) and dynamic (D) poly(vinylidene fluoride) (PVDF) and poly(vinylidene fluoride)/organomodified montmorillonite (OMMT) nanocomposite nanofibers. Symbol list inside the plot frame are going from left to right [105]. Reproduced with permission from Elsevier.
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Figure 6. Schematic of exfoliation of poly(vinyl alcohol)/nanoclay nanocomposite nanofiber [115]. Reproduced with permission from Taylor and Francis.
Figure 6. Schematic of exfoliation of poly(vinyl alcohol)/nanoclay nanocomposite nanofiber [115]. Reproduced with permission from Taylor and Francis.
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Figure 7. Field emission scanning electron microscopy image of nanofibrous mats: (A) poly(vinyl alcohol)/0.75 wt.% Cloisite 30B; and (B) poly(vinyl alcohol)/0.75 wt.% Cu-montmorillonite [115]. Reproduced with permission from Taylor and Francis.
Figure 7. Field emission scanning electron microscopy image of nanofibrous mats: (A) poly(vinyl alcohol)/0.75 wt.% Cloisite 30B; and (B) poly(vinyl alcohol)/0.75 wt.% Cu-montmorillonite [115]. Reproduced with permission from Taylor and Francis.
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Figure 8. Transmission electron microscopy image of (A) nylon 6/montmorillonite nanocomposite nanofibers; (B) clay platelets pointed by arrows [124]. Reproduced with permission from Elsevier.
Figure 8. Transmission electron microscopy image of (A) nylon 6/montmorillonite nanocomposite nanofibers; (B) clay platelets pointed by arrows [124]. Reproduced with permission from Elsevier.
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Figure 9. Formation of electrospun polycaprolactone (PCL), gelatin, and layered double hydroxide (LDH) based nanofibers [132]. Reproduced with permission from ACS.
Figure 9. Formation of electrospun polycaprolactone (PCL), gelatin, and layered double hydroxide (LDH) based nanofibers [132]. Reproduced with permission from ACS.
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Figure 10. Sensor application of poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers [164]. PVDF = poly(vinylidene fluoride); NWS = near distance-wheeling electrospinning. Reproduced with permission from Elsevier.
Figure 10. Sensor application of poly(vinylidene fluoride)/nanoclay nanocomposite nanofibers [164]. PVDF = poly(vinylidene fluoride); NWS = near distance-wheeling electrospinning. Reproduced with permission from Elsevier.
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Figure 11. Effect of nylon 6/nanoclay nanocomposite nanofiber coating on polypropylene packaging used on bread [124]. Reproduced with permission from Elsevier.
Figure 11. Effect of nylon 6/nanoclay nanocomposite nanofiber coating on polypropylene packaging used on bread [124]. Reproduced with permission from Elsevier.
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Table
Table 1. Techniques, process parameters, and properties of polymer and polymer nanocomposite nanofibers.
Table 1. Techniques, process parameters, and properties of polymer and polymer nanocomposite nanofibers.
MethodsNanofiber DiameterEffecting ParametersProduction/Injection Rate Voltage IndustrializationFormation of Aligned NanofibersPolymer/Composite Fiber FormedRef.
Electrospinning40 nm–2 μmViscosity;
voltage; distance; solution feed rate		5 μL/min10–40 kVYesYesPolystyrene; polyamide; polyaniline;
poly(lactic acid);
poly(lactic acid)/polyaniline; poly(lactic acid)/poly(vinylpyrrolidone);
polystyrene/graphene; polystyrene/carbon nanotube 		[51,52,53,56,57,58,69,70,71,72,73,74]
Solution blowing40 nm–several
μm		Voltage; viscosity; nozzle geometry; solution feed Rate20 μL/minNoYesYesPolystyrene/carbon nanotube; polyamide/carbon nanotube;
polyaniline/carbon nanotube;
polyaniline/carbon nanotube nanofiber; polyaniline/titania; nylon 6,6/zinc oxide;
poly(vinyl fluoride)/bentonite/
poly(vinyl alcohol);
polyaniline/polyimide		[75,76,77,78,79,80]
Template synthesis40 nm–200 nmTemplate shape; template pore size-~30 VNoYesPoly (lactic acid); poly(vinyl alcohol);
poly(lactic acid)/titanium dioxide; poly(vinyl alcohol)/zinc oxide; poly (1-naphthylamine);
cellulose nanofiber; polypyrrole nanofibers;
poly(ϵ-caprolactone) nanowires; poly (3-Hexylselenophene)		[81,82,83,84,85,86,87,88]
Phase inversion/freeze drying50 nm–1 μmPolymer concentration;
solvent properties;
freezing rate;		-NoNoYesPolyaniline; polypyrrole;
polypyrrole/silica;
poly (ε-caprolactone); poly(vinyl alcohol)/maghemite; cellulose nanofibrils; chitosan; polytetrafluoroethylene		[89,90,91,92,93,94,95,96]
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Kausar, A.; Ahmad, I.; Aldaghri, O.; Ibnaouf, K.H.; Eisa, M.H. Nanoclay-Reinforced Nanocomposite Nanofibers—Fundamentals and State-of-the-Art Developments. Minerals 2023, 13, 817. https://doi.org/10.3390/min13060817

AMA Style

Kausar A, Ahmad I, Aldaghri O, Ibnaouf KH, Eisa MH. Nanoclay-Reinforced Nanocomposite Nanofibers—Fundamentals and State-of-the-Art Developments. Minerals. 2023; 13(6):817. https://doi.org/10.3390/min13060817

Chicago/Turabian Style

Kausar, Ayesha, Ishaq Ahmad, O. Aldaghri, Khalid H. Ibnaouf, and M. H. Eisa. 2023. "Nanoclay-Reinforced Nanocomposite Nanofibers—Fundamentals and State-of-the-Art Developments" Minerals 13, no. 6: 817. https://doi.org/10.3390/min13060817

APA Style

Kausar, A., Ahmad, I., Aldaghri, O., Ibnaouf, K. H., & Eisa, M. H. (2023). Nanoclay-Reinforced Nanocomposite Nanofibers—Fundamentals and State-of-the-Art Developments. Minerals, 13(6), 817. https://doi.org/10.3390/min13060817

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