Metal Matrix Composite Fabricated from Electrospun PAN, EGNS/PAN Nanofibers and AL 5049 Alloy by Using Friction Stir Processing

doi:10.21203/rs.3.rs-2630230/v1

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Metal Matrix Composite Fabricated from Electrospun PAN, EGNS/PAN Nanofibers and AL 5049 Alloy by Using Friction Stir Processing

https://doi.org/10.21203/rs.3.rs-2630230/v1

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published 03 Jun, 2023

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This work is an attempt to fabricate aluminum (AA 5049) matrix composites (AMCs) reinforced with electrospun polyacrylonitrile (PAN) nanofibers and consisting of exfoliated graphite nanosheets (EGNS/PAN) by utilizing friction stir processing (FSP) to improve the mechanical characteristics of AA 5049. PAN and EGNS/PAN nanofibers were fabricated using the electrospinning technique. The average diameter of the electrospun PAN nanofibers is 195 ± 57 nm, and after EGNS incorporation is 180 ± 68nm. The incorporation of nanofiber reinforcement can enhance the mechanical characteristics of AA5049. The mechanical characteristics of AA5049 can be enhanced by the procedure of incorporating nanofibers, making them an ideal choice for applications in the automotive and aerospace industries. PAN and EGNS/PAN nanofiber reinforcement enhanced the hardness to 89 and 98 Hv, respectively. Also, the ultimate tensile strength was raised to 291 MPa and 344 MPa, respectively.

Electrospinning

graphite

aluminum

reinforcement

mechanical properties

Aluminum and magnesium were chosen as the metal matrices, and carbon and ceramic nanofibers were utilized as the reinforcement fibers. These fibers were created utilizing the electrospinning method, and the metal-matrix composites were condensed by heat induction sintering. However, the percentage of reinforcement needs to be optimized to improve the mechanical properties (such strength, hardness, and young's modulus) of the composites [1].

A promising method called electrospinning enables the creation of micro or nanofibers with the potential to form membranes with linked porosity, superior mechanical characteristics, and a large surface area. The technology of electrospinning has numerous applications, including in the fields of medicine [2], energy transportation [3, 4], optoelectronic devices [5, 6], and water treatment [7–10, 11]. Micro- and nanoscale electrospinning can be used to create electrospun fibres with the potential to incorporate cutting-edge materials to enhance their mechanical or physicochemical properties [12–14]. Because of their large surface area and interconnected porosity structure, nanofibers make better substrates for depositing material removal nanomaterials [15]. Continuous and non-woven fibers with micro and nanoscale dimensions can be created using the electrospinning technique [16, 17]. Electrospun fibers have a number of characteristics, including high surface, extremely porous, interconnected porosity, and the ability to use a variety of polymers [17, 18]. The electrospun fibers were therefore excellent for potential applications in a wide range of fields, including the conveyance or storage of energy [11, 19], membrane [20, 21], adsorption processes [22], and air filtration [23, 24], Among the topics covered are medication delivery [25, 26], plat grafting [27], optoelectronic devices [28, 29], electrochemical sensors [30], and others. The interface of the polymer solution with the electric field constitutes the electrospinning process. Uncompensated charges collect on the polymeric surface as a result of the voltage being applied. The forces created an alignment of the polymer chains as it went through the needle shear. Once they outweigh the forces of surface tension and viscosity, the repellent charges on the polymer's surface begin to increase. When the repellent charges on the polymer's surface start to increase, they eventually outweigh the forces of surface tension and viscosity. This event creates a jet and a conical shape over the solution that is known as Taylor's cone. The jet that exits Taylor's cone starts out linear and accelerates to the collector. The solvent then evaporates while the jet is travelling, maintaining the polymer's intermolecular stability. Finally, the fibres are collected, forming a non-woven mesh across the collector surface [31, 32, and 11].

Aluminum matrix composites (AMCs) manufacture has recently grown in importance for applications in industries including aerospace and automotive. This is because they have a number of promising benefits over traditional alloys, including remarkable formability, enhanced wear resistance, higher specific stiffness, good fatigue characteristics, and outstanding strength to weight ratio at low or high temperatures [33].

When the goal is to change the physical properties throughout the entirety of the matrix, manufacturing processes including stir casting, squeeze casting, powder metallurgy, diffusion bonding, etc. are frequently used. On the other hand, there are a number of surface modification processes, including the laser melt technique, centrifugal casting, and plasma spraying, which are used to modify only the surface of a material while leaving the interior unaltered. When using such methods, the bulk of the material loses a tiny amount of other attributes like toughness while surface properties like hardness and wear resistance only slightly improve [34]. While all of these methods have been successfully used to create surface MMCs, a significant worry is that they need material phase changes (from solid to liquid or from liquid to vapour) throughout the procedure. As a result of the interfacial interactions between the material and the reinforcement caused by the phase change, the interfacial bonding strength is reduced and harmful phases are formed [35].

A possible solid-state processing method for creating surface MMCs and customizing the surface's microstructure through extreme plastic deformation is friction stir processing (FSP) [36–38]. When compared to alternative methods, FSP is quicker, uses less energy, and ensures that the secondary phase is distributed uniformly due to a strong thermomechanical effect, [39] which improves the mechanical characteristics [40]. In FSP, the material is manipulated at temperatures below its melting point and is only mechanically deformed in a plastic way. To create the composite, the reinforcing particles are mechanically combined with the plasticized metal. The fine dispersion of the reinforcement particles without segregation at the grain boundaries is the result of the base material not melting [41]. There are numerous processing variables that affect the FSP process, including the pin geometry, the pin's travel and rotating speeds, tilt angle, and the number of FSP cycles [42–45].

The most typical use of FSP is to change the mechanical characteristics and microstructure of metallic components with thin surface layers regulated [46–49]. Homogeneity and densification of the FSP zone [50] and the elimination of manufacturing process flaws [6] have both been shown to be effective methods for achieving significant microstructure refinement. Mehdi et al. [51] effective fabrication of an aluminium matrix composite (AMC) with nanoparticles of SiC and investigation of the microstructure and mechanical characteristics of the multi-pass FSP/SiC of AA6082-T6. In selecting the characteristics of the composite, the properties of the reinforcements are crucial [52]. The targeted application and the compatibility of the particles with the substrate matrix are the two main factors that influence the reinforcing choice. Outstanding neutron absorption, combined with heat and wear resistance, are all features of boron carbide (B4C). The B4C reinforced composites are employed as the primary neutron shield material in reactors because of its great neutron absorbing capacity. Mg-CNT composites have exceptional mechanical properties, but Mg-Al2O3 composites have better wear resistance [53]. The hardness of the created composite was enhanced to 92% of the base metal in the carbon nanotubes/Mg alloy surface composite created using FSP [54]. In comparison to the substrate material, the surface composite created by reinforcing an aluminium substrate with Al2O3 particles showed improved hardness [55]. It was noted that the addition of silicon carbide particles significantly increased the hardness and flexural strength of the SiC reinforced aluminium surface composite [56]. Al7075/B4C surface composite was claimed to have a 62% higher hardness than matrix [57]. According to research, the Al7075/Al2O3 surface composite's hardness nearly doubles while its impact toughness rises by 29% [55]. In one investigation, aluminium oxide nanoparticles were added to the tool and holes were drilled in Al 1200 aluminium plate using friction stirring to create the nanocomposite layer. It was discovered that the nanocomposite layer enhanced the hole's hardness, compressive strength, and fatigue resistance [58].

Friction stir processing (FSP), which creates Al/SiC composites on the surface of Al 1050 sheets, was studied by El-Mahallawy et al. [59]. Additionally, it was found that FSPed composites showed a significant improvement in microstructure changes, with equiaxed and refined grain structures obtained as opposed to the base metal's elongated and coarse grains, likely as a result of the severe plastic deformation and continuous dynamic recrystallization caused by FSP. The microstructure, hardness, and wear characteristics of the friction stir-processed AA6061/tungsten carbide nanocomposite were studied by A.A. Megahed et al. [60] the results also showed that the processed composite's microhardness value was found to be 144 VHN, which is 39.81% greater than the value for the base metal. Additionally, all samples lost less weight than the base metal. According to Zoalfakar,SH et al. [61], they investigated the impact of friction stir processing parameters on the creation of AA6061/tungsten carbide nanocomposite and the findings show that using the right FSP settings produces an AA6061/WC nanocomposite devoid of defects and voids by uniformly dispersing the WC particles throughout the matrix. Additionally, during FSP, heat is generated and intense plastic deformation results in the breaking of coarse and WC particles, the removal of porous pores, and the dynamic recrystallization of an ultrafine grain-sized structure.

This study's objective is to prepare, characterize, and evaluate a metal matrix composite made from this intriguing material, electrospun PAN and EGNS/PAN nanofibers, via the FSP approach. The investigation of the interfaces and ensuing mechanical properties of the metal matrix composites produced by FSP, specifically the two PAN/AA5049 composites produced from electrospun PAN nanofibers and exfoliated graphite nanosheets.

2.1 Materials

Polyacrylonitrile (PAN) with a molecular weight of 150,000 g/mol,catalogue no. (1813150), N, N- dimethylformamide (DMF purity 99.8%) was purchased from Aldrich catalogue no. (227056) and graphite flakes (GF, particle size 75 mesh, 99.9% min purity, catalogue number is 332461), were purchased from Sigma-Aldrich. Nitric acid and sulfuric acid were provided by Elnasr Pharmaceutical Chemicals Co., Egypt.

2.2 Electrospinning of EGNS/PAN/DMF

Our previous research [62] described the exfoliated graphite nanosheets (EGNS) fabrication process and procedures. First, sulfuric and nitric acid mixtures were mixed with graphite particles (ratio 4:1 by volume). The Graphite Intercalation compound was made by stirring the mixture constantly for 24 hours at room temperature (GIC). The GIC was then cleaned with distilled water and dried to remove any moisture at 100°C to produce expanded graphite, the dry particles were heated and thermally shocked for 30 seconds at 1050°C. Finally, a 600 ml alcohol solution was poured over one gramme of expanded graphite (alcohol and distilled water with a ratio of 65:35). Before employing the dispersion in the electrospinning procedure, the dispersion was filtered and dried after 16 rounds of sonication to obtain the EGNS.

PAN/DMF polymer solution was prepared a ratio of 10 wt. % under continuous stirring at room temperature for 3 hours to produce a homogeneous solution. EGNS were dispersed in DMF using ultrasonication for 16 hours. The PAN/DMF polymer solution contained 10 weight percent of the EGNS weight concentration. The PAN was subsequently added to the EGNS/DMF suspension to produce a homogeneous and uniformly dispersed EGNS/PAN/DMF polymer solution. After that, the mixture was stirred for 10 hours at 60°C. The polymer solution was placed into a 10 mL glass syringe that was connected to a stainless-steel needle (inner diameter of 0.9 mm). A high voltage power supply was utilized to create a 25 kV electric field between the needle and a grounded, horizontally centered metal collector. The electrospun PAN and EGNS/PAN fibers were collected on a metal collector that was wrapped in aluminum foil. The collector was modified for all tests and placed 20 cm vertically from the needle tip for nanofiber deposition. Figure 1a show the electrospinning technique.

2.3Friction stir processing (FSP)

Aluminum (AA5049) sheet, whose chemical composition is shown in Table 1, was used to create surface composites. The base metal (BM) AA5049 sheets were wire-cut with dimensions of 100×50×6 mm. Applying wire electrical discharge machining, a rectangular groove with a depth and width of 3 mm and 1 mm, respectively, was created. The electrospun PAN nanofibers (or EGNS/PAN nanofibers) weighing 8 g were inserted into the wire-cut grooves. To prevent the escapement of any fabrics from the groove during processing, the groove entrance is initially sealed off using a tool with a shoulder without a pin. A computer numerical control vertical milling center with an FSP tool was used to produce the surface composite. The FSP tool had screwed pin profile, shoulder diameter of 18 mm, a pin diameter of 6 mm, and a height of 5.7 mm. Hardened H13 steel was used to manufacture the FSP tool. Based on the optimum values acquired from the prior study, the FSP process window was chosen [63]. The FSP tool rotation speed and traverse speed were both held constant at 1000 rpm and 40 mm/min, respectively. Figure 1b illustrate the FSP procedure.

Table 1

Chemical composition of aluminum AA5049.
Element	Si	Fe	Cu	Mn	Mg	Cr	Ti	Al
Content (%)	0.17	0.35	0.08	0.8	1.9	0.12	0.05	balance

3.1 Scanning electron microscopy (SEM)

Scanning electron microscopy Model Quanta 250FEG (Field Emission Gun) with EDX Unit (Energy Dispersive X-ray Analyses) at the Tabbin Institute for Metallurgical Studies (TIMS), Egypt was used to analyze the morphology of electrospun PAN,EGNS/ PAN nanofiber and the distribution of the nanofiber reinforcement after FSP. Microstructural samples were extracted from the AA5049 plates in the processed zone. Before displaying the surface metallographic, the surfaces of all samples were ground and polished to a mirror-like finish. Following mechanical polishing, the samples were etched with Keller's reagent (190 mL distilled water, 5 mL nitric acid, 3 mL hydrochloric acid, and 2 mL hydrofluoric acid). Also, the morphology of EGNS/PAN nanofiber was studied using a high-resolution transmission electron microscope (HRTEM) (JEOL model JEM 2100) at the Petroleum Research Institute in Egypt.

3.3 Mechanical characterization

A Vickers' microhardness tester was used to measure the microhardness at various points in the stir zone, with a 100-g load and 10-second dwell times. According to ASTM E8M-04 standards [64], the tensile sample is manufactured by wire cut EDM with dimensions of 2.5 mm thick, 4 mm wide, 58 mm long, and a gauge length of 26 mm, as depicted in the figure (2). Uniaxial tensile tests are conducted with a crosshead speed of 1 mm/min at room temperature.

4.1. Morphology of electrospun EGNS/PAN nanofiber composite

Figures 3a-b exhibit the morphology and diameter distribution of electrospun PAN nanofiber and EGNS/PAN composite nanofiber. As depicted in the figures, all of the fiber mats are uniformly distributed and randomly orientated. The electrospun PAN nanofibers have an average diameter of 195 ± 57 nm and a homogeneous, beadles morphology as shown in Fig. 3 (a). The morphology of EGNS/PAN electrospun nanofibers changed significantly after EGNS was incorporated. In a related nanocomposite, the diameter of electrospun nanofibers can be reduced by adding conductive nanofiller to the polymer matrix [65–66]. Figure 3b shows EGNS/PAN nanofibers with decreased diameter after EGNS addition(180 ± 68nm). The reduction in fiber diameter reveals that the electrical conductivity of EGNS can predominate in the decreasing of fiber diameter. Since graphene nanosheets have a large surface area, they exhibit powerful interactions with polymer matrices [67–68]. The micrograph of EGNS/PAN composite nanofibers obtained by transmission electron microscopy (TEM) containing 10 weight percent EGNS is shown in Fig. 4. The EGNS layer on the PAN nanofiber surface is visible in the TEM image.

By using Raman spectroscopy, the presence of EGNS in the produced EGNS/PAN has been further established. The D-band line (1350 cm^− 1) and the G-band line (1650 cm^− 1) are two significant peaks in the Raman spectra of PAN/GO displayed in Fig. 5. The existence of these two bands strongly suggested that all composite nanofiber membranes have disordered and graphitic layers. The G bands on the EGNS/PAN nanofiber were noticeably higher than the D bands. The EGNS/PAN nanofiber with the I_D/I_G ratio of 0.95 suggested the presence of disordered graphite since the intensity ratio of the D band and G band is frequently utilized as an indicator for the degree of disorder[69–70].

4.2 Microstructural characteristics

Optical micrographs of the FSP AA5049 substrate, PAN nanofiber, and EGNS/PAN nanofiber reinforced AA5049 taken at the stir zone are shown in Figs. 6a-c. A recrystallized fine-grained microstructure is produced within the stir zone as a result of the intense plastic deformation and frictional heating that occur during FSW and FSP. The term for this occurrence is dynamic recrystallization (DRX) [71–72]. At the base of the stir zone, a concentric arc-shaped banded structure of PAN and EGNS/PAN nanofiber can be observed (Figs. 6b-c). This is an inherent feature of FSP and is termed as onion ring structure. An onion-ring structure is produced by the interaction of material flow between the warmer zone at the top and the colder zone at the bottom [73]. The rings of the tool tip during the FSP show that the distribution of Electrospun PAN Nano Fiber 195 ± 57nm has been spread neatly inside the AA 5049 matrix (Fig. 6b). The presence of nanofibers caused onion rings to occasionally be rich and unreinforced. Regions with and without nanofibers are represented by the dark and light rings, respectively. Figure 6c shows that when particle-rich and particle-free regions were compared, the former had finer grains than the latter. The grain structure refinement of the produced nanocomposite was accelerated by including EGNS/PAN nanofiber (180 ± 68nm) inside the SZ. Figures 7 and 8 from the EDS analysis indicate the distribution of the different constituents in the PAN nanofiber and EGNS/PAN nanofiber reinforced AA 5049 surface composite. The EDS mapping analysis is applied to investigate the distribution of the reinforcements and the detrimental impacts of agglomeration and nanoclusters on the reinforcing nanofibers. In all samples, the reinforcing nanofibers were uniformly distributed in the SZ, and no significant clustering was observed.

4.3 Mechanical Results

4.3.1 Micro hardness behavior of MMNCs

Vickers micro-hardness curves for the AA5049 pure and SZ specimens as performed, with and without reinforcing nanofibers, are shown in Fig. 9. The average micro-hardness in the pure AA5049 and SZ is shown in Fig. 10. The pure AA 5049 has an average micro-hardness of 70 HV. The surface composite's SZ had increased hardness; the main factors contributing to this improvement were the uniform distribution and refining action of the nanofiber reinforcements. In the case of friction stir processed AA5049, the growth of fine grains and dislocations increased the initial hardness to 81 Hv. The hardness was increased to 89 and 98 Hv, respectively, by the reinforcement of PAN and EGNS/PAN nanofibers. The EGNS/PAN nanofiber has a harder reinforcement than pure AA5049, which results in a stronger reinforcement that strengthens the AA5049 matrix many fold [74]. The homogeneous distribution of electrospun EGNS/PAN nanofiber in the aluminum matrix enhances the strengthening since it serves as a barrier for the movement of dislocations. The variation in the thermal contraction coefficient of the matrix and the reinforcing phase is what causes the fine dispersion of the reinforcement nanofibers in addition to the quench hardening impact [75]. Therefore, the hardness of the electrospun nanofibers is transferred to the composite, further enhancing its hardness.

Figure 10 Average micro-hardness values of pure AA5049 and the SZ for the investigated aluminum composites

4.3.2 Tensile properties

The stress-strain curves and tensile characteristics of the examined composites are shown in Fig. 11. Figure 12 indicates the mechanical properties of the investigated aluminum composites. The yield strength, ultimate strength, Young's modulus, and elongation to break of the pure AA5049 alloys were found to be 125 MPa, 216 MPa, 70 GPa, and 12%, respectively. During FSP, the processing region's microstructure was improved, which improved its mechanical and plastic properties and raised the elongation to break to 24%. More grain boundaries and finer grains produce a better resistance to dislocation motion [76]. The ultimate tensile strength of the AA55049 increased to 291 and 344 MPa after being reinforced with PAN and EGNS/PAN nanofibers, with corresponding decreases in elongation (18 and 14.2%). This demonstrated the significant influence of nanofiber on alloy composites. For all composites, the yield strength and the elastic modulus were both improved. The electrospun nanofibers functioned as barriers for dislocation motions in the SZ, improving the mechanical characteristics of the produced composites. Improved mechanical characteristics were achieved as a result of the EGNS/PAN nanofiber's large specific surface area having good interfacial adhesion with the AA5049 matrix. Also, due to EGNS nanofillers' atomic thickness, excellent mechanical strength, and chemical inertness.

Figure 12 Mechanical properties of the investigated aluminum composites

PAN and EGNS/PAN nanofiber fabrics were produced using the electrospinning process, while MMCs were created using FSP with both the fabrics and the aluminium (AA5049) substrate. The following statements serve as conclusions:

The electrospun PAN diameter was found to be in the range of 195±57 nm, but the electrospun EGNS/PAN nano fibril composite was reduced to 180±68 nm by the presence of EGNS.
Microstructure analysis of composite samples revealed that both PAN and EGNS/PAN reinforcement were distributed uniformly inside the AA5049 metal matrix.
The superior mechanical qualities of PAN and EGNS/PAN nanofibers, when introduced into the metal matrix, enhance the metal's strength, microhardness, and mechanical properties.
Microhardness was reported to be 89 and 98 Hv, respectively, for PAN and EGNS/PAN reinforcement, with a significant rise in microhardness along the SZ.
The tensile properties of the composites were apparently improved by 35% and 60%, respectively, by the incorporation of PAN and EGNS/PAN nanofibers.
The rising need for high-performance and lightweight materials in the aerospace and automotive industries as well as for military applications like defensive armor, the creation of metal matrix composites with PAN nanofibers and EGNS additives employing FSP has been gaining interest.

Acknowledgments:

No funding sources that supported the research presented.

Author contributions:

All authors have read and agreed to the research presented.

Conflict of interest:

The authors declare that there is no conflict of interest.

Data and code availability: Not applicable

Supplementary Information: Not applicable

Ethical approval: Not applicable

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published 03 Jun, 2023

Read the published version in The International Journal of Advanced Manufacturing Technology →

Editorial decision: Major Revisions Needed
22 Apr, 2023
Reviewers agreed at journal
01 Mar, 2023
Editor assigned by journal
27 Feb, 2023
First submitted to journal
26 Feb, 2023

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Metal Matrix Composite Fabricated from Electrospun PAN, EGNS/PAN Nanofibers and AL 5049 Alloy by Using Friction Stir Processing

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental Procedure

2.1 Materials

2.2 Electrospinning of EGNS/PAN/DMF

3. Characterization

3.1 Scanning electron microscopy (SEM)

3.3 Mechanical characterization

4 Results And Discussion

4.1. Morphology of electrospun EGNS/PAN nanofiber composite

4.2 Microstructural characteristics

4.3 Mechanical Results

4.3.1 Micro hardness behavior of MMNCs

4.3.2 Tensile properties

Conclusion

Declarations

References

Status:

Journal Publication

Version 1