Open access peer-reviewed chapter

Influence of Loading Nanoclay on Properties of the Polymer-based Composite

Written By

Oluwatoyin Joseph Gbadeyan, Linda Zikhona Linganiso and Nirmala Deenadayalu

Submitted: 05 September 2022 Reviewed: 05 October 2022 Published: 30 November 2022

DOI: 10.5772/intechopen.108478

From the Edited Volume

Nanoclay - Recent Advances, New Perspectives and Applications

Edited by Walid Oueslati

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Abstract

The recent techniques for improving polymer-based composite properties using nanoclay infusion have been reviewed in this chapter. The recent progress in the printing of thermoplastic composite infused with different sizes of particles was reviewed. The processing of infusing clay into natural fiber and recent advancements in the printing of thermoplastic composite infused with nanoclays at different loading ratios also was discussed. Valid information on different apparatuses for determining mechanical properties, temperature dependence storage modulus, and tan α of the developed materials were provided. The loading effect of clay on the mechanical properties, temperature dependence storage modulus, and tan α of composite and nanocomposites was reviewed. Specific emphasis on printed nanocomposite application in gears and related engineering fields is considered. The innovative scope of infusing nanoclay for developing composite with improved mechanical properties, temperature dependence storage modulus, and tan α was discussed. Similarly, the application of clay-reinforced composite with the revolutionary scope of infusing nanoclay for different applications was suggested.

Keywords

  • clay
  • nanocomposite
  • composite
  • 3D printing
  • infusion techniques

1. Introduction

Polymers are the most flexible materials for several applications, including but not limited to automotive, construction, biomedical, packaging, aerospace, electronics, and packaging, to mention but a few. This material may be either synthetic binders or greener resin systems, which could be either thermosetting or thermoplastic polymer mainly used to provide shape stability and rigidity to composite materials [1]. These materials are widely used for several applications due to their inherent mechanical, thermal, electrical, optical, and tribological properties. It is well known that polymer matrix plays a vital role in reinforced polymer composites. The primary functions of the polymer matrix are to protect reinforcement, provide rigidity, and hold filler or reinforcement orientation in a specific configuration [2, 3]. Despite the acceptability of polymetric material for various applications, these materials have some constraints, reversing some of the above-mentioned properties. These limitations, such as low thermal conductivity and load-bearing capacity with a higher tendency to creep, poor thermal stability, better heat dissipation, and a very high coefficient of thermal expansion, provoke the clearance problem.

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2. Effect of incorporating filler materials on polymer-based composite materials

Several efforts have been explored toward solving the challenges mentioned above—loading several reinforcements or nanofiller into polymetric material to produce a polymer-based composite with improved properties [4, 5, 6, 7, 8, 9, 10, 11]. Dittanet and Pearson confirmed that incorporating filler is a viable way to improve the thermal, physical, and chemical of polymer-based composite or hybrid. Furthermore, adding filler/s has been adopted to reduce the cost of the expensive polymetric matrix for composite material development [4, 5, 6, 7, 8].

Several materials with required reinforcement have been manufactured into different sizes and used as fillers in polymer composites material with improved properties [9, 12, 13, 14, 15]. Fillers and reinforcement produced from SiO2, TiO2, and carbon-based materials have been widely explored [8, 12, 14, 16, 17, 18]. Among the material used for reinforcement or fillers, carbon-based materials and nanoclay are commonly used. Nanoclay is commonly used as filler or reinforcement in pulp and papers, paints, and polymer-based composite industries. Over many decades, montmorillonite (MMT) and kaolinite with a high concentration of CaCO3, commonly referred to as nanoclay, have been obtained from rock and synthesized using either gas pressure blasting or explosion method [19, 20, 21]. This filler is widely accepted and used for its reinforcement potential, availability, and low cost [11, 22, 23]. Furthermore, the development and application of nanoparticle-reinforced polymer-based composite have significantly increased over the decades. This increase in usage could be attributed to their availability, cost-effectiveness, easy processability, improved strength, stiffness, and lightweight [24, 25].

Yao and You [26] classified nanoclay-layered mineral silicate as montmorillonite, bentonite, and kaolinite in agreement with their chemical composition and morphology. They confirmed that montmorillonite is mostly used in industry and research. Mohan and Kanny confirmed the extended use of montmorillonite [14] as they confirmed that montmorillonite nanoparticle loading is a viable way of improving the composite mechanical, thermal, and tribological properties. However, the concentration and particle sizes of nanoclay have been explored, and it has been confirmed that these two factors substantially affect the inclusion of nanoclay in polymer composite properties.

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3. Influence of particle sizes and loading ratio of fillers on polymer composite materials

Authors have extensively investigated the effect of particle sizes and the addition ratio of fillers polymer composite properties [10, 15, 18, 27]. Their results proved that the loading of filler at different particle sizes and volumes often has different effects on composite, most times improving one property and harmfully affecting another in most cases [10, 15, 27]. These factors have been considered, and the positivity aspect has been capitalized, and work around the negative aspect through innovative moves and techniques. These factors led to much research to simplify the procedure for synthesizing and characterizing the fiber/filler-reinforced composite and authenticate the improvement in properties and the mechanism that governs the performance for repeatability.

Yue et al. [15] confirmed that the concentration effect of filler on polymer-based composite by establishing the amount of filler incorporated in the polymer composite strongly determines its thermal properties. Furthermore, Fröhlich et al. [9] and Donnet [23] provided information on the characterization and reinforcement loading effect on polymer-based composite, which provided an understanding of the kind of filler loaded in rubber. Nanoclay particle sizes, irrespective of chemical and morphological properties, proved to have dominated effect on polymer composite where clay is used as reinforcement [10, 28, 29]. Laouchedi et al. [28] investigated the effect of locally produced particle sizes and loading rate on epoxy composite material’s physical and mechanical properties. According to this study, the loading of more significant size particles damagingly influences composite properties. However, epoxy composite properties were improved after loading smaller particle sizes and loading of 2%wt. Similarly, several studies results are consistent with what Laouchedi et al. reported, proving that incorporating smaller particle sizes and loading of nanoclay are viable ways to produce composite material with improved properties. The discovery and loading of this filler with suitable loading concentrations and particle sizes have given birth to different composite materials adopted for different applications.

Aside from the dispersion of nanoclay in the matrix to enhance polymer composite, nanoclay has been used as an interfacial treatment agent for natural fiber. This filler treatment eventually resulted in improving natural fiber-reinforced composite. Furthermore, techniques like the infusion of nanoclay of nanoclay-layered mineral silicate on the printed layer to develop gear material have been explored [30, 31], and this chapter will provide information on how these techniques, clay particle sizes, and concentrations affect polymer composite properties.

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4. Infusion of nanoclay-layered mineral silicate into natural fiber for improved composite properties

Over the years, natural fibers have been chemically treated to remove wax, surface lignin, and another amorphous phase toward increasing properties [28, 32]. Researchers treat natural fiber to possess required properties that could be an alternative reinforcement to synthetic fiber. These treatment techniques have attracted several types of research resulting in the development of materials for different applications [33]. Mohan and Kanny [13] inched this process by infusing nanoclay into banana fiber through shear-induced force using sodium hydroxide chemical treatment techniques. The effect of the infused nanoparticle on the composite’s structural, mechanical, morphological, and thermal properties was investigated and compared with composite reinforced with sodium hydroxide chemically treated fibers [13]. The aim of infusing nanoclay with alkaline treatment was expected to enhance the interfacial adhesion of fiber to increase further the mechanical and thermal properties of banana fiber-reinforced composite. Similarly, this study achieved two aims: remove unwanted hemicellulose, lignin, and amorphous phases of banana fiber and incorporate nanoclay to increase its concentration of nanoparticle in-house cellulose phases. Achieving these aims shows that nanoclay could be incorporated to enhance natural fiber-reinforced biocomposite either by infusing nanoclay into in-house cellulose phases of fiber and infuse matrix or by dispersing it in matrix and infused into fiber mat or produce the composite using casting techniques.

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5. Materials and methods

Sodium hydroxide, clay, and banana fiber were the raw materials used for this study.

5.1 Chemical treatment and nanoclay infusion into the banana fiber

Nanoclay was infused into fibers’ in-house cellulose phases using shear-induced force treatment in two phases, which are alkaline (NaOH) and NaOH/clay treatment. Before chemical treatment, fiber was extracted from the banana plant, air-dried for a week, and chopped to a 5 cm uniform length. Similarly, removing unwanted phases before the chopped banana fiber achieved alkaline treatment was soaked, starred slowing in acetone for 30 min, and then oven-dried at 80°C for 120 min.

5.2 Fibers chemical treatment (NaOH)

Forty grams of dried chopped fiber, 40 grams of sodium hydroxide, and 600 ml of water were measured simultaneously for this process. Then, sodium hydroxide was added to distilled water and stirred at 500 rpm under a controlled temperature of 80°C for 15 min. Afterward, 40 grams of dried chopped fiber were added to the sodium hydroxide solution and stirred for another for 4 h at the same temperature (80°C). Later, the treated fibers were removed from the sodium hydroxide solution and softly washed using running water to remove retaining sodium hydroxide solution or unwanted phases in the fiber to ensure purity. The fiber was then dried at 80°C for 2 h and later used to develop banana fiber-reinforced composite and hybrid.

5.3 Sodium hydroxide/nanoclay treatment

Montmorillonite (MMT) nanoclay was a shear-induced force into banana fiber using the alkane treatment technique. Forty grams of sodium hydroxide were poured into 600 ml of water and stirred at 500 rpm at a conditional temperature of 80°C for 15 min. After which, 20 grams of Na+ montmorillonite were put into the sodium hydroxide solution and stirred together for 30 min to dissolve the clay particle in the solution. Chopped banana fiber (20 grams) was added to montmorillonite/sodium hydroxide solution and mixed for another 4 h at 750 rpm under the exact temperature of 80°C. The high stirring speed generates a high shear force generated, which enhance the dispersion of clay particle into fibers. Later, the treated fibers were removed from the montmorillonite/sodium hydroxide solution and softly washed using running water to remove retaining montmorillonite/sodium hydroxide solution or unwanted phases in the fiber to ensure purity. The fiber was then dried at 80°C for 2 h and later used to develop banana fiber-reinforced composite and hybrid.

5.4 Composite development

The treated and untreated fiber reinforced epoxy resin using conventional resin casting techniques. This process was employed to develop both untreated and treated banana fiber-reinforced composite. The fibers were chopped into different lengths between 30 and 50mm, and fiber with a specific length was incorporated as a reinforcement in the matrix (epoxy resin). This process was aimed to determine the required length and concentration of the fibers treated and untreated for these series and also to identify reinforcement suitability and influence of each fiber length on epoxy resin properties. The determination of critical length is a prerequisite to fiber concentrations in epoxy resin, meaning the fiber volume was committed only when the critical length was discovered.

The conventional resin casting techniques were conducted in two phases. The first phase was mixing fiber and resin, and the second entailed casting fiber/resin in a mold cavity. The first phase was achieved by measuring 100 grams of epoxy resin into a beaker and heating it to 80°C. Then, a specific concentration with fiber length was added and stirred for 1 hour with a magnetic stirrer at 500 rpm, still at a temperature of 80°C. This blend was removed from the stirrer, allowing it to cool down at ambient temperature for 30 min. A 10:30 mixing ratio of epoxy resin and catalyst, which had the 30%, was adopted. The catalyst mixing ratio of 30 was afterward added to the fiber-resin blend and stirred till homogeneousness was achieved. As mentioned, casting the fiber-resin blend in the mold cavity is the second. This process was achieved by pouring the fiber-resin catalyst into the top open-ended Perspex mold sheet gapped with a 3-mm rubber gasket on three sides. The composite cavity was quickly removed after curing by applying wax on the inner part of the mold before pouring fiber-resin catalyst. The casted banana fiber-reinforced epoxy resin composite was removed after 48 h, and its properties were investigated after 7 days of the initial casting—the effect of banana fiber distribution during casting on epoxy resin thermomechanical properties.

5.5 Testing

The thermal behaviors of the fiber and composite were investigated on a thermogravimetry (SDT Q600 model). The heating profile was obtained at a 10 °C/min heating rate under a dry nitrogen gas flow at 100 mL/min from 0°C to 600°C. Temperature dependence mechanical properties such as storage modulus and tan α were measured on a dynamic mechanical analyzer at a frequency of 10 Hz in a three-point bending mode. This investigation was carried out using the TA equipment (Q800) from room temperature to 100°C under atmospheric conditions. Resistance to pulling stress (tensile strength) and fiber and composite residual strength was investigated using an MTS-UTM machine with a 1 KN load cell. Short beam investigation was used to determine the shear properties of the untreated and treated fiber-reinforced epoxy composite series. This test was carried out in agreement with ASTM 2344-84 standard using a crosshead speed of 1 mm/min. The tensile test was carried out following ASTM D 3039 using an operating speed of 1 mm/min with a 1 KN load cell. The samples investigated were three cubical blocks of 1 cm by 1cm by 1cm cut from banana fiber (treated and untreated) reinforced composite. A fiber pull-out investigation was carried out on samples prepared with 10 cm fiber length entrenched in 3 mm depth in cured epoxy resin, which was subjected to a constant load of 1 kN until a failure occurred. Fiber pull-out strength was determined using the failure ratio on a load-displacement curve. Samples were stressed for both pull-out and tensile strength until the coefficient of variance (CV) was ≤16%.

5.5.1 Interfacial and tensile strength

The tensile strength of the untreated and treated banana fiber shown in Figure 1 depicts that the infusing of nanoclay and structural alterations due to chemical treatment has a strong positive effect on the tensile properties of the fiber. The tensile strength, stiffness, and elongation at break values shown in Figures 13 vary among untreated and treated fiber. The untreated fiber (UTBF) exhibited a tensile strength of 602 MPa and stiffness of 17 GPa with 4.3% elongation at break. An increase in tensile strength and stiffness after banana fiber was treated was with sodium hydroxide only (NTBF). The composite series exhibited tensile strength and stiffness of 713 MPa and 22 GPa. This performance depicts the effect of the chemical treating banana fiber using sodium hydroxide. A further increase in strength and stiffness was observed after the banana fiber was treated with a combination of sodium hydroxide and clay.

Figure 1.

Tensile strength of composite series.

Figure 2.

Tensile modulus of composite series.

Figure 3.

Elongation at the break for composite series.

Composite reinforced with banana fiber treated with sodium hydroxide, and clay (N&CTBF) exhibited a tensile modulus of 43 GPa, approximately threefold of untreated fiber stiffness, and tensile strength of 918 MPa, 51% higher than what is obtained with untreated fiber. Removing weak strength phases such as wax, lignin, hemicellulose, and other impurities from the fiber could be the primary reason for the observed tensile strength and stiffness.

Furthermore, the reinforcement effect of the infuse nanoclay is another reason for a significant improvement in tensile strength and stiffness. The increase in tensile stiffness and strength may be attributed to interfacial bonding between the matrix and the fiber due to the presence of nanoclay in the composite.

However, a linear reduction in elongation at break was seen. Composite with untreated fiber exhibited the highest elongation value of 4.3%, followed by composite reinforced with banana fiber treated with sodium hydroxide only, which is 3.5%, and composite filled with banana fiber treated with a combination of sodium hydroxide and clay exhibited the lowest elongation of 3.1%. This decrease in elongation value may be attributed to the absence of banana fiber’s waxy and amorphous phases, which were removed during chemical treatment.

5.5.2 Temperature-dependent mechanical properties

Figures 4 and 5 show the effect of the chemical treatment given to banana fiber on dynamic mechanical properties such as storage modulus and tan α. It was observed that the composite reinforced with untreated banana fiber exhibited high storage modulus of 6380 MPa at room temperature and declined with a corresponding increase in temperature. Fibers treated with sodium hydroxide solution and montmorillonite/sodium hydroxide filled composite exhibited 7553 and 8328 MPa at room temperature. This result depicts that giving fiber chemical treatment using a combination of montmorillonite and sodium hydroxide is a viable way to improve temperature-dependent storage modulus. The composite with banana fiber treated using montmorillonite/sodium hydroxide exhibited a temperature-dependent modulus at room temperature, 32% higher than the composite with untreated banana fiber.

Figure 4.

Temperature dependence storage module of composite series.

Figure 5.

Temperature dependence tan α of composite series.

The tan α curves shown in Figure 5 provided details on the composite series’ phase transformation, damping features, and interfacial strength. An increase in tan α value with a corresponding increase in temperature is till attaining a maximum point, followed by a decline in temperature. The temperature where tan α reaches a maximum value, referred to as the glass transition temperature of the polymer, was identified and recorded. At this glass transition temperature, the polymer changes from an amorphous to a rubbery state under increased temperature.

Composite with untreated fiber, treated with sodium hydroxide, and montmorillonite/sodium hydroxide exhibited glass transition at 69°C, 69°C, and 72°C, respectively. This output implied that composite filled with fiber treated with montmorillonite/sodium hydroxide, and this performance might be attributed to the presence of nanoclay in banana fiber. Nanoclay is known for its good thermal properties and ability to delay polymer deformation from a glassy region into a rubbery region [30, 31, 34]. Thus, infusion and dispersion of nanoclay into fiber may have reduced the polymer deformation leading to increased glass transition of composite with fiber treated with montmorillonite/sodium hydroxide. This result trend corresponds with what is experienced in the storage modulus.

These findings proved that the advanced way of infusing clay into natural fiber (banana fiber) could be used to produce composite materials with improved properties for different applications. Going by this technique, clay concentration for producing composite using conventional methods such as resin casting method and vacuum infusion may reduce to minimal, eventually affecting composite production cost positively. We employ infusing nanoclay on acrylonitrile butadiene styrene printer layers using a 3D printer. This technique was used to develop a gear material and determine printed material’s mechanical, thermal, and tribological properties. This idea was motivated by the challenging process of gear using conventional techniques, material selection, and production parameters [31]. The research aimed to reduce the time used for producing gear, selecting nanoclay to enhance the interfacial bonding acrylonitrile butadiene styrene printer layers toward developing more robust structures using relatively simple 3D printing processes.

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6. Experimental details

6.1 The 3D printing process of nanoclay-infused acrylonitrile butadiene styrene composite

A modified nanoclay and acrylonitrile butadiene styrene filament were explored for the development of gear material. The process was achieved using 3D printing and infusion techniques, which were accomplished in four steps. Drafting gear samples using a computer-aided program was the first step. A gear was designed and drawn on a Solid Edge 2019 software by creating a specific dimension of the gear for creating an ISO metric file as shown in Figure 6 and was saved as Standard Tessellation.

Figure 6.

Gear sample drafted on Solid Edge 2019.

This file was then exported to UP studio for finalizing the printing parameters. Afterward, acrylonitrile butadiene styrene filament was infilled into a 3D printer set at 99% with no support. Simultaneously, nanoclay was dissolved in acetone using a 10:1 mixing ratio to facilitate uniform dispersion of particles. Subsequently, a layer of acrylonitrile butadiene styrene was printed, then a premeasured acetone/nanoclay solution was applied to the first printed surface (Figure 7).

Figure 7.

Acetone/nanoclay solution-coated acrylonitrile butadiene styrene layer [31].

This process was repeated for six layers of printed nanoclay-infused acrylonitrile butadiene styrene-infused composite at equal spacing. All printed layers were coated uniformly to prevent vacuums in the 3D-printed composite. After the printing, the composite was removed and cured under ambient temperature. The effect of nanoclay infusing on the mechanical properties of 3D-printed acrylonitrile butadiene styrene was determined by varying loading from 0.5 to 5%. These investigations were conducted after 7 days.

6.2 Investigation procedures

3D-printed acrylonitrile butadiene styrene infused with nanoclay of different percentage loading resistance to impact, flexural, and tensile properties was investigated to determine the strength and stiffness of the printed nanocomposite. Tensile was carried out on a universal testing machine fitted with a 30 N load cell using ASTM 3039 test standard. Impact investigation was conducted according to ASTM D6110-10 using a Hounsfield Balance Impact Tester. For each investigation, five samples were investigated, and the average value was reported.

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7. Results and discussion

Mechanical properties such as tensile and impact properties of 3D-printed nanocomposite were shown in Figures 810. Figures 8 and 9 illustrate the tensile strength and modulus of neat acrylonitrile butadiene styrene and 3D-printed nanocomposite infused with different percentages of nanoclay. Although the tensile strength and stiffness vary with different loading percentages, the infusion of nanoclay increased both tensile strength and stiffness of neat acrylonitrile butadiene styrene, irrespective of loading weight percentages.

Figure 8.

Tensile strength of acrylonitrile butadiene styrene and nanoclay infused nanocomposite.

Figure 9.

Tensile stiffness of acrylonitrile butadiene styrene and nanoclay-infused nanocomposite.

Figure 10.

Impact strength of acrylonitrile butadiene styrene and nanoclay-infused nanocomposite.

However, superior tensile strength and modulus were achieved when 2%.wt nanoclay was infused. The addition of 2%.wt. improved tensile strength by 50% and increased acrylonitrile butadiene styrene tensile modulus by 90%. The apparent increase in tensile properties can be attributed to the presence of nanoclay serving as a reinforcing agent in the nanoclay-infused nanocomposite [35, 36, 37]. This performance depicts the strong positive effect on the pulling resistance of acrylonitrile butadiene styrene. Furthermore, the tensile strength and stiffness showed by acrylonitrile butadiene styrene solely depend on the amount of nanoclay infused as printed nanocomposite tensile properties increased with nanoclay loading. Infusion of nanoclay on every layer of printed acrylonitrile butadiene styrene may have increased interfacial bonding, increasing resistance to pulling stresses.

Besides, nanoclays are known for their stiffness, much stiffer than neat acrylonitrile butadiene styrene. This stiffness may be attributed to better resistance to stress yielding acrylonitrile butadiene styrene when subjected to pulling stress, resulting in nanocomposite stiffness improvement [35, 36, 37].

7.1 3D-printed nanocomposite resistance to impact stress

Figure 10 shows resistance to impact stress of printed acrylonitrile butadiene styrene and nanoclay-infused nanocomposite. Similar to the trend observed in Figures 8 and 9, the impact strength of printed nanocomposite varies with nanoclay loading. Infusing nanoclay enhances the impact property of printed acrylonitrile butadiene styrene. 3D-printed nanocomposite infused with 3 wt.% exhibited superior impact resistance with 20% higher than neat acrylonitrile butadiene styrene. However, trivial increased impact strength was observed with a corresponding increase of nanoclay loading from 2 wt.% (3.93) to 3 wt.% (3.96). This resistance to sock performance of 3D-printed nanoclay-infused nanocomposite may be attributed to the critical loading efficiency of nanoclay at lower concentrations. Besides, the interfacial bonding introduced by nanoclay infused on the acrylonitrile butadiene styrene printed layers may be attributed to the improvement in impact strength observed.

The infusion of nanoclay strengthens the bonding at the interface of each printed layer, improving the energy absorption capability and impact strength. A sharp drop in impact resistance at loading higher than 3 wt.% of nanoclay may be attributed to particle agglomeration, causing focal stress areas that exhibited poor resistance to impact stress.

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8. Conclusion

This chapter reviews the influence of recent clay infusion on mechanical and temperature dependence storage modulus and tan α of polymer-based composite and nanocomposite. Progress in techniques for developing clay-reinforced polymer-based composite and hybrid nanocomposite was examined. The infusing of clay into a naturally sourced banana fiber later used in the development of composite was discussed. Infusion of nanoclay into printed layers of acrylonitrile butadiene styrene was discussed. The effect of infused nanoclay on polymer-based composite properties was reported. It provides information on pieces of equipment used for developing polymer-based composite and nanocomposite and properties evaluation. This review confirmed that infusing clay into the banana fiber helps in tailoring and improving composite properties to achieve desired properties, predominantly mechanical and temperature dependence storage modulus and tan α. It also suggested the developed materials for the application of interior parts in automobile industries. Furthermore, the infusion of nanoclay on printed layers of acrylonitrile butadiene styrene significantly improves the mechanical properties of the printed nanocomposite. 3D-printed acrylonitrile butadiene styrene-infused nanoclay with improved mechanical properties suggested materials for a gear development application.

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Written By

Oluwatoyin Joseph Gbadeyan, Linda Zikhona Linganiso and Nirmala Deenadayalu

Submitted: 05 September 2022 Reviewed: 05 October 2022 Published: 30 November 2022