Investigation on the Mechanical Properties of Powder Metallurgy-Manufactured AA7178/ZrSiO<sub>4</sub> Nanocomposites

Srinivasan, R.; Karunakaran, S.; Hariprabhu, M.; Arunbharathi, R.; Suresh, S.; Nanthakumar, S.; Ahammad, S. K. H.; Mayakannan, S.; Jayakumar, Mani

doi:https://doi.org/10.1155/2023/3085478

Advances in Materials Science and Engineering

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Abstract Introduction Methods and Materials Results Conclusions Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

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Materials Behaviors and Characterization of Composite Materials for Automotive Application

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Research Article | Open Access

Volume 2023 | Article ID 3085478 | https://doi.org/10.1155/2023/3085478

Investigation on the Mechanical Properties of Powder Metallurgy-Manufactured AA7178/ZrSiO₄ Nanocomposites

R. Srinivasan,¹S. Karunakaran,²M. Hariprabhu,³R. Arunbharathi,⁴S. Suresh,⁵S. Nanthakumar,⁶S. K. H. Ahammad,⁷S. Mayakannan,⁸and Mani Jayakumar⁹

Academic Editor: V. Vijayan

Received13 Jan 2023

Revised07 Apr 2023

Accepted04 May 2023

Published22 May 2023

Abstract

The versatility of metal matrix composites (MMCs) makes them a promising material for various industrial applications. The current study used a ball milling to mechanically AA7178 powder and strengthened with zirconium silicate (ZrSiO₄) nanoparticles. In addition, the AA7178 matrix was ball-milled to distribute the ZrSiO₄ nanoparticles throughout the material. The AA7178 reinforced with ZrSiO₄ nanoparticles was compacted and consolidated using two distinct powder metallurgy (PM) sequences: double pressing, double sintering, and hot pressing. In tests measuring microhardness, compression strength, and elongational break, the new nanocomposites surpassed the AA7178. The adequate interfacial bonding and even distribution of ZrSiO₄ nanoparticles throughout the AA7178 matrix were essential to the strengthening mechanism. With the use of hot pressing, the mechanical characteristics of the nanocomposites were enhanced. As reinforcement concentration increased beyond 2.5% by weight, mechanical properties drastically degraded due to ZrSiO₄ nanoparticles clumping and unequal distribution. Improved mechanical parts attain through the uniform distribution of ZrSiO₄ nanoparticles in the AA7178 and the maintenance of their mechanical properties.

1. Introduction

Due to naturally enhanced mechanical capabilities and exceptional weight, ZrSiO₄ nanoparticles have been the focus of research and development in the scientific and industrial communities over the past decade [1]. Applications in transportation and security, where the combination of lighter materials with improved mechanical qualities is desirable, show great promise for the use of ZrSiO₄ nanoparticles as reinforcing material for the fabrication of MMC [2]. Close connections developed between the matrix and the scattered ZrSiO₄ nanoparticles, which helped to fine-tune the grain and boost the mechanical characteristics of the materials. The mechanisms of grain refining, load transfer, and Orowan looping provide the basis of the reinforcement contributions [3, 4]. ZrSiO₄ nanoparticles are often researched as reinforcing materials due to their higher efficiency and simplicity of manufacture. However, ZrSiO₄ nanoparticles offer better mechanical characteristics (from 60 to 160 GPa) and high elastic modulus (1.9 TPa) [5].

The latest review by the authors [6] indicates that several studies discuss using powder methods to reinforce aluminum or aluminum alloys. However, effective nanoaluminum alloy composites with state-of-the-art properties continue to be hampered by various obstacles brought on by the features of ZrSiO₄ nanoparticles [7]. The most urgent issues to be addressed include clustering, minimal wettability of ZrSiO₄ nanoparticles with aluminum, and the development of numerous distinct phases at 450°C, such as aluminum carbide (Al₄C₃) or aluminum oxides [8–10]. Aluminum-ZrSiO₄ nanoparticles interfacial bond strength, ZrSiO₄ aspect ratio, and nano ZrSiO₄ quality all play a vital role in the mechanical characteristics of ZrSiO₄-reinforced aluminum alloys [11–13].

Many different chemical pretreatments have been applied to the ZrSiO₄ nanoparticles, and conditions have been used in the ZrSiO₄ nanoparticle powder combination (like nanoparticles or graphite) to enhance the original shape and surface qualities of metal powders [14, 15]. Ball milling is frequently used, but because of the lengthy milling process substantial damage to ZrSiO₄ nanoparticles, the Nano ZrSiO₄/Al composite’s mechanical characteristics are typically subpar [16, 17]. Composite aluminum alloy reinforced with ZrSiO₄ nanoparticles can be made using a wide variety of powder consolidation techniques, such as cold pressing, hot pressing, hot extrusion, and spark plasma sintering (SPS) [18].

The research reports the fabrication of AA7075-based hybrid composites using TiO₂ and fly ash as reinforcements via stir casting and hot forging. The mechanical behavior of the composites was studied through compression tests, showing increased compressive strength with higher weight fractions of TiO₂. The coefficient of thermal expansion decreased with the addition of TiO₂ and fly ash, while a slight decrease in thermal conductivity was observed compared to AA7075 [19].

The study reports on the development of A357 alloy composite reinforced with dual size SiC particles by stir casting. Different weight fractions of dual size SiC particles were investigated for their influence on mechanical properties and wear resistance of A357 composites. The composites showed improvement in hardness, yield, and tensile strength compared to A357 alloy, with 4 wt. % of fine and 2 wt. % of large SiC particles displaying the highest tensile strength and 4 wt. % of large and 2 wt. % of fine SiC particles exhibiting high hardness and wear resistance [20].

Aluminum alloy composites with graphene nanoplates were produced by ball milling and stir casting. The addition of graphene nanoplates reduced grain size and increased the strength of the composites. T6 heat treatment improved the strength of the composites, but at higher graphene content, agglomerates on grain boundaries facilitated crack growth [21].

Aluminum hybrid composites were produced using powder metallurgy with varying weight fractions of graphene and fixed CNT content. Wear tests were conducted with varying applied load, and worn surface analysis was done using SEM. Increasing graphene content increased bulk hardness and reduced wear rate due to the formation of a lubricating layer [22]. Aluminum hybrid composites were developed using powder metallurgy technique with Si₃N₄ and CNT as reinforcements. Scanning electron microscope studies showed uniform dispersion of both reinforcements. Microhardness increased with CNT content, electrical conductivity decreased, and coefficient of friction decreased due to the lubricating nature of CNTs [22, 23].

This research successfully produced AA7178 reinforced with ZrSiO₄ nanoparticles using milling, mechanical alloying, and two distinct compaction and sintering processes. The proposed manufacturing processes use commercial technologies that could enable mass production of high-value AA7178/ZrSiO₄ nanocomposites for use in demanding lightweight constructions, including armored assault vehicles. The goal was to minimize structural failure of the ZrSiO₄ nanoparticles while achieving a homogeneous dispersion of the nanoparticles in the metal matrix using powder technology approaches that could eventually lead to commercial mass production. Al7075 nanocomposites with varying B4C contents were produced using powder metallurgy technique. Microstructure, grain size, and wear behavior were analyzed. Dry sliding wear test was conducted using Taguchi L9 approach, and the most influential parameter on wear volume was found to be the B4C nanoparticle content.

2. Methods and Materials

The AA7178 created through mechanical alloying, and its nominal composition is 2% copper, 2.7% magnesium, 6.8% zinc, and aluminum balance. The Sigma/Aldrich firm obtained all the materials mentioned previously. The AA7178 mix matrix was created in a high-energy, vertically agitated ball mill for three hours at 500 revolutions per minute to avoid oxidation during production. Powder agglomeration was avoided by adding a small amount of ethanol to the mixture. Stearic acid was added to the mix at a 1 wt. % to ensure uniformity throughout the manufacturing process [24, 25]. The researcher used a 10 : 1 ball-to-powder ratio in our mechanical alloying technique involving stainless-steel balls.

Ball milling was also employed to create the nanocomposite material. The previously milled AA7178 powder was combined with various amounts of ZrSiO₄ nanoparticles (1.5, 2.5, 3.5, 4.5, 5.5, and 6.5 wt. %) in a planetary ball mill with the same milling conditions. To avoid damaging the ZrSiO₄ nanoparticles, the milling speed was reduced to 250 rpm, and the milling time was extended to 60 minutes.

“A stainless-steel cylinder mold with an internal radius of 9 mm was used to perform uniaxial compression on milled powder combinations of AA7178 and ZrSiO₄ nanoparticles. Graphene oxide was used as an additive to reduce the effects of friction. Hot-pressing (HP) and double pressing and sintering techniques (DPST) were used for compaction. The powder used to create the AA7178 for this investigation is shown in Figure 1(a).”

After being heated and compacted under 250 MPa of pressure for 10 minutes at a specific temperature of 400°C, the milled composite powder mixes were presintered in a low vacuum furnace for 60 minutes at 520°C. Green compacts were lightly sprayed with a graphite spray to reduce resistance to the mold before being pressed for a second time. After 10 minutes at 400°C and 550 MPa, the second hot compaction was completed. After preheating to 590°C, the green compacts were sintered for 120 minutes in a low vacuum.

For the HP process, hot pressing was done for 60 minutes at 400 MPa under 550°C on mixtures of milled composite powders. The green compacts were heated to 590°C for 120 minutes in a low vacuum environment. Milled AA7178 were hot-pressed, and sintered AA7178 were both processed for this study.

Both sintered composite samples and milled composite powders have their crystal structures evaluated using X-ray diffraction (XRD). During this sintering process, a TA Instruments DSC 25 differential scanning calorimeter was used to determine the phase transition from RT to 600°C at 15°C/min. Microstructural characterization and phase distribution in sintered composite samples were assessed using SEM [26, 27].

Sintered composite samples were subjected to mechanical testing on a Vickers microhardness analyzer with a 100 g load and a dwell time of 20 seconds [28]. At least five readings were averaged to arrive at the final microhardness value using a strain rate of 0.01 s⁻¹, which is common for materials with lower modulus. The researcher performed quasistatic compression tests, with each sample tested three times to achieve repeatable and dependable results. The compressive stress-strain characteristics were determined by averaging the data from the three tests. The dimensions of the samples used for ASTM E9 solid compressive testing were calculated. Small samples are commonly used for compressive testing since compliant metals, which are often used as thin plates to transmit vertical load to the surfaces, are typically employed [29]. In the compression test, each sample was 20 mm long and 16 mm in diameter (L/D = 1.25). Scanning electron microscopy (SEM) was employed to analyze the fractured surfaces of specimen pieces taken from the crushed materials [30, 31].

3. Results and Discussions

3.1. Sintered Composite and Milled Composite Structural Property

The flake-shaped morphology of the AA7178 powder created after the ball-milling process is considered favorable for incorporating ZrSiO₄ nanoparticles into the matrix [32, 33]. Ball-milled AA7178/ZrSiO₄ nanoparticles powder mixtures are shown in SEM. There were no ZrSiO₄ nanoparticle aggregates to be seen, indicating that they had been evenly distributed and integrated into the AA7178 powders. Although most of the ZrSiO₄ nanoparticles look fragmented and smaller than the original ones, their estimated length is still sufficient, demonstrating that ball milling did not cause damage.

Figure 2 shows the X-Ray Diffraction pattern for the milled AA7178, and the milled AA7178-ZrSiO₄ nanocomposites. The ZrSiO₄ nanoparticles peak at 2θ = 34°, identical to the graphite C height, is readily observed [34–36]. The peak’s exceptional sharpness indicates that the two-dimensional Graphene layer providing the tubular pattern of the zirconia has nearly perfect crystallinity. A further indicator of the ZrSiO₄ nanoparticles’ excellent purity is that the C curve was not filtered toward the highest values of 2θ (greater than 34°). At 2θ = 46°, also known as the graphite peak, and at 2θ = 78°, also known as the graphite peak, are peaks of noticeably lesser intensity [37, 38]. These peaks are not crisp. Hence the crystallinity of the different ZrSiO₄ nanoparticles can differ. The enlargement of this peak may indicate that other graphitized carbon types are present [39–41].

Both milled AA7178 samples show aluminum diffraction peaks. There are also a few peaks that are associated with copper and magnesium. Magnesium peaks vanish after 2 hours of ZrSiO₄ nanoparticles milling on the AA7178, leaving only copper peaks to be seen. Both the intensity and the width of these peaks are waning. This outcome implies that mechanical alloying was used successfully to produce AA7178. Once the ZrSiO₄ nanoparticles are fine-tuned, the remaining C peaks vanish, suggesting that few of the C content has been liquefied into the aluminum to generate a solid state. For the AA7178-2.5 wt. % after milling, a differential scanning calorimeter was performed. This assumption was tested by a process involving 100% ZrSiO₄ nanoparticles.

In Figure 3, the DSC curve is displayed. This low-temperature first peak is associated with the evaporation and subsequent release of humidity from ethanol. A small exothermic peak between 410 and 440°C was observed for the AA7178-ZrSiO₄ nanoparticles powder mixture. Al₄C₃ formation may be related to this peak. During sintering, the metastable Al-C solid solution breaks down, forming Al₄C₃ [42].

In contrast, the XRD patterns of milled AA7178-ZrSiO₄ nanoparticles did not show any broadening of the aluminum peaks compared to milled AA7178. This shows that aluminum’s structure has not absorbed significant carbon material. The aluminum’s lattice parameter and crystallite size remained constant throughout all examined situations, indicating that the metal contains negligible amounts of carbon [43, 44]. Milled and sintered AA7178-ZrSiO₄ nanoparticle samples exhibited XRD structures devoid of pronounced Al₄C₃ peaks. This confirms that the ZrSiO₄ nanoparticles utilized in this analysis are steady when interacting with aluminum and do not break into aluminum carbide [45]. The XRD results show that the ZrSiO₄ nanoparticles are the most excellent possible quality and contain no silicon oxide or imperfections in the carbon [46].

Specimens of milled and sintered AA7178-ZrSiO₄ nanoparticles, manufactured using the HP process, with (a) 4.5% and (b) 2.5% ZrSiO₄ nanoparticles compositions, are shown as XRD patterns in Figure 4. Sintered AA7178 in its purest form is displayed in Figure 4(c). While sintering eliminated the oxide peak, the intermetallic phase Al₂O was still present in all sintered specimens (AA7178 and the composite), regardless of the ZrSiO₄ nanoparticles amount. The microstructure progression of intermetallic stages in AA7178 is significantly influenced by zirconia, as evidenced by the considerable changes in the intensity of these peaks with increasing ZrSiO₄ nanoparticles content.

Each composite material XRD pattern lacked the characteristic ZrSiO₄ nanoparticles C peak (Figures 4(a) and 4(b)). Due to low concentration of ZrSiO₄ nanoparticles on the surface of the specimen under analysis and the small scattering distance among carbon and metal atoms.

Microstructures of the AA7178-2.5% ZrSiO₄ nanoparticles composite produced by the two compaction techniques are shown in Figure 5. Both approaches consolidate the metal particles well. All methods can identify the intermetallic Al₂O phase, which can be easily identified by the lines and is found in both the grain borders and the interior regions of the grains. HP techniques appear to favor the formation of Al₂O intermetallic phases in the nanocomposite’s microstructure. The DPSD compaction method preserves the flake shape of the initial AA7178 powders. HP causes grain strengthening.

Furthermore, the nanocomposite made using HP techniques exhibits subgrains. For instance, a few subgrains are indicated by red-dashed lines. This result provided support for the hypothesis that the hot-pressing technique led to grain strengthening via two distinct methodologies: (i) demolition of the flake morphologies of the ball-milling utilized, resulting in particle size drop of the first grains generated by the AA7178 and (ii) formation of the particle within these grains. This dynamic recovery and recrystallization cause high levels of plastic strain and heat, which are stamps of HP.

In contrast, the first grains for AA7178 powders are only revealed using the DPDS technique. Given the high oxygen content, these regions seem to belong to Al₂O. These oxides developed in the open air at the hot compaction phase of both production processes. The metallographic processing of this sample likely caused any porosity in this oxide by fracturing such brittle stages, leading to the formation of pores [47]. The argon atmosphere employed in the DPDS process causes varied shapes of the oxides. When HP is given to Al-ZrSiO₄ nanoparticles composites in a neutral atmosphere, the amorphous Al₂O₃ transforms into coarse, lump-shaped crystalline Al₂O₃ at matrix grain boundaries. The AA7178 grains must contain the oxide due to the high oxygen content. Additionally, due to the reaction of ZrSiO₄ nanoparticles with aluminum to generate brittle aluminum carbides, the oxide is present in the AA7178 grains [48].

3.2. Mechanical Properties

Figure 6(a) depicts the stress-strain relationship under compression for DPDS-created AA7178 nanocomposites with various ZrSiO₄ nanoparticles. Adding ZrSiO₄ nanoparticles, even at a low concentration of 2.5% by weight, enhances the nanocomposite’s mechanical characteristics. Figures 6(a) and 6(b) indicate that for the 4.5% ZrSiO₄ nanoparticles with AA7178 nanocomposite, the results improve with increasing ZrSiO₄ nanoparticles content. Below the percentage mentioned above, mechanical properties begin to deteriorate noticeably. The observed findings explain the weak interface bonding among the AA7178 and the ZrSiO₄ nanoparticles, caused by the silicon oxide clustering and unequal distribution in the AA7178 matrix.

(a)

(b)

(c)

ZrSiO₄ nanoparticles have been shown to play an essential role in the compression behavior and modulus of AA7178 nanocomposites. When the concentration of ZrSiO₄ nanoparticles in AA7178 is increased, it causes a significant increase in the yield stress, indicating that the nanoparticles strengthen the composite. This is because the nanoparticles create barriers to dislocation motion, which causes an increase in the yield stress. In addition, the ZrSiO₄ nanoparticles also contribute to the increased modulus of the composite. This is because the nanoparticles are stiffer than the aluminum matrix, and their incorporation into the composite results in a stiffer overall structure. The increased modulus also means that the composite is more resistant to deformation.

However, as the concentration of ZrSiO₄ nanoparticles is further increased to 2.5%, the compression behavior of the composite starts to deteriorate. This is because the nanoparticles become clustered, resulting in the formation of large clusters that can cause cracks in the composite. The cracks act as stress concentrators and reduce the strength of the composite, leading to a decrease in the yield stress and modulus. Therefore, the concentration of nanoparticles should be carefully controlled to achieve the optimal balance between strength and toughness.

Figure 6(b) displays stress and strain curvature and representative images of tested samples for AA7178 and numerous AA7178-ZrSiO₄ nanocomposites made under varying conditions. For comparison, the researcher also provides flawless AA7178 (Figure 6(b)). The AA7178-2.5% ZrSiO₄ nanoparticles composite produced by the DPDS or HP techniques has ultimate strength and considerably higher yield than pure AA7178. Fracture elongation was also greatly improved from 0.13 for AA7178 to 0.19 for the double pressing double sintering technique and 0.21 for the hot-pressing approach. The improved flexibility of the AA7178 matrix can be accredited to the uniform dispersal of ZrSiO₄ nanoparticles throughout the matrix [49].

Young’s modulus and other mechanical parameters of the nanocomposite are improved more by the HP compaction method than by the DPDS approach. The matrix material has been refined, leading to a denser composite. Compared to the HP method, which yielded composites with a density of 2.65 g/cm³ (equal to 98%), the DPDS method yielded composites with a thickness of 2.6 g/cm³ (equivalent to 93.5% of the theoretical value). When comparing AA7178-2.5 wt. % ZrSiO₄ nanoparticles produced by DPDS and HP, the strength-ductility effectiveness (compressive strength × elongation) was calculated to be 5.25 GPa for DPDS and 8.17 GPa for HP, showing that the balance among highest strength and elasticity was effectively attained in the case of HP.

The AA7178 matrix and ZrSiO₄ nanoparticles may strengthen the resultant nanocomposites through various mechanisms, including grain boundary reinforcement, grain strengthening, stress transfer from AA7178 to ZrSiO₄ nanoparticles, and Orowan looping. ZrSiO₄ nanoparticles alone reveal essential reinforcing when the aluminum grains are more significant than the strengthening, and the ZrSiO4 nanoparticles are predominantly positioned on the grain restrictions, as is the case here.

Utilizing the increased mechanical properties of the nanotubes requires a successful load transfer from the AA7178 matrix to the ZrSiO₄ nanoparticles. Mechanical parameters correlate highly with ZrSiO₄-AA7178 interfacial bonding, ZrSiO₄ nanoparticles structural integrity, and uniform nanotube dispersion in the metal matrix. Reinforcement of the composites may also result from a favorable mechanism, the contact of dislocations with the nanotubes. A fractographic study of compressed samples was carried out to verify the load transmission.

The mechanical compressive testing findings demonstrate that the composites made with AA7178-2.5 wt. % ZrSiO₄ nanoparticles are more complex than pure AA7178. This is supported by the composite materials’ microhardness ratings (Table 1). The AA7178-4.5 wt. % ZrSiO₄ nanoparticles nanocomposite is much less mechanically robust, as evidenced by microhardness measurements. The samples passed microhardness testing with flying colors, demonstrating efficient load transmission because of the lack of cracking.

Figure 7 shows the SEM images of the cracked surfaces of AA7178-ZrSiO₄ nanocomposites with 2.5 wt. % and 4.5 wt. % ZrSiO₄ nanoparticles content, respectively. Load transmission efficiency at the ZrSiO₄/matrix contact was demonstrated by ZrSiO₄ nanoparticle pull-outs (arrows) on the AA7178 fracture surface. The pull-outs evident during tensile testing provide insight into the load transferring at the ZrSiO₄ nanoparticles/matrix interaction and the disposition of ZrSiO₄ nanoparticles during the fracturing behavior of the sample. Some places were subjected to shear and tension, even if the overall application of stress was just compressive. Extensive pull-outs indicate a strong connection between the matrix and the ZrSiO₄ nanoparticles, enhancing strengthening effects. These exceptionally long pull-outs prove that the silicon oxide was not significantly reduced in length during milling. It is important to note that the distribution of pull-out ZrSiO₄ nanoparticles in the broken surfaces of the samples under study was correlated with their existence.

Cracks in an AA7178-4.5 wt. % ZrSiO₄ nanoparticles nanocomposite reveal clusters of ZrSiO₄ nanoparticles and inhomogeneous distribution in the matrix (Figure 7(b)). Poor mechanical qualities result from aggregate formation, which weakens the interfacial bond among the ZrSiO₄ nanoparticles and AA7178 composites. According to the results of other researchers [50, 51], the percentage of ZrSiO₄ nanoparticles employed in the reinforcement can be used to estimate the maximum content of the integrated reinforcement, with a lower portion resulting in more distribution of ZrSiO₄ nanoparticles in the matrix.

4. Conclusions

An AA7178 composite reinforcing with ZrSiO₄ nanoparticles was successfully created employing a mechanical alloy process and milling process, succeeded by two compacting and sintering processes. The produced nanocomposites’ mechanical characteristics and corresponding microstructural morphologies were investigated and correlated. Insights like these can be gleaned from the data:(1)Both compaction methods led to the development of a composite material with improved mechanical properties when compared to pure AA7178 alloy. However, the high-pressure (HP) method resulted in a composite with denser microstructure and smaller grain size, which led to even better mechanical properties. Despite experiencing significant splintering, the structural integration of the ZrSiO₄ nanoparticles remained intact. It is likely that the fracturing facilitated the efficient transmission of loads from the aluminum matrix to the ZrSiO₄ nanoparticles.(2)The study demonstrated a direct correlation between the mechanical strength of the composite and the amount of ZrSiO₄ nanoparticles added to the matrix, up to a certain point. However, adding more than 2.5 wt. % ZrSiO₄ nanoparticles caused a significant reduction in the mechanical properties of the composite due to the clustering of the nanoparticles.(3)The AA7178-2.5wt. % ZrSiO₄ nanocomposite, when produced using the DPDS method, exhibited a compressive strength of 372 MPa, while the same nanocomposite manufactured through the HP approach displayed a higher strength of 445 MPa. However, both methods resulted in the development of nanocomposites with sufficient strength-ductility efficiency, as evidenced by their elongation values of 19% and 21%, respectively.

Data Availability

The data supporting the current study are available from the corresponding author upon request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

The authors would like to sincerely thank those techniques that have contributed to this research.

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Copyright © 2023 R. Srinivasan et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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