Experimental investigation of the microstructural and wear behaviours of silicon carbide and boron nitride-reinforced AZ91D magnesium matrix hybrid composites

doi:10.21203/rs.3.rs-3910049/v1

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Experimental investigation of the microstructural and wear behaviours of silicon carbide and boron nitride-reinforced AZ91D magnesium matrix hybrid composites

https://doi.org/10.21203/rs.3.rs-3910049/v1

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This study aimed to fabricate hybrid metal matrix composites of AZ91D magnesium reinforced with varying various weight percentages of SiC and constant weight percentages of BN particles through the stir-squeeze casting method. The influence of the particle ratio on the microstructure and wear behaviour of the composites was studied. The dispersion patterns of particles within the matrix and the interactions between the alloy and the particles were thoroughly investigated using a variety of techniques, including optical microscopy, SEM, EPMA, and EDS.XRD analysis of the AZ91D/SiC/BN hybrid composite revealed a significant volume proportion of the strong Mg17Al12 phase. The synthesized magnesium hybrid composites (AZ91D/9%SiC/3%BN) experienced a volume loss reduction of up to 36.16% under a maximum load of 30 N and a maximum speed of 1 m/s when compared with the monolithic material AZ91D. The results of these analyses demonstrated that the resulting composites exhibited an even dispersion of particles, superior grain structure, and strong interfacial bonding between the AZ91 alloy and the reinforcing particles. The newly developed magnesium hybrid composites have better wear performance than monolithic AZ91D alloys. These findings highlight the enhanced wear resistance of the fabricated composites for antiwear applications.

Materials Engineering

Hybrid metal matrix composites

AZ91D magnesium

SiC and BN particles

Stir-squeeze casting method

Wear behaviour

In the realm of lightweight materials, both magnesium and aluminium hold prominent positions as acknowledged lightweight alloys. Magnesium, in particular, has captured significant attention within the aircraft sector due to its pivotal role in providing lightweight metals and alloys. This attention is well-studied considering the AZ91D magnesium alloy. Renowned for its low cost, exceptional mechanical properties, corrosion resistance, mobility, and excellent castability, the AZ91D alloy has found widespread application across diverse industrial sectors, firmly establishing itself as a highly utilized magnesium alloy [1–5]. In the pursuit of optimal alloy properties and fabrication methods, researchers have extensively explored various avenues. Nikhilesh Singh and Belokar conducted a comprehensive literature survey, leading them to advocate for the stir-casting technique as the preferred fabrication method. Their work also emphasized the significance of employing pin-on-disc tribometers for wear analysis on hybrid metal matrix composites (HMMCs) that incorporate both aluminium (Al) and magnesium (Mg) [6]. Sudip Banerjee et al. delved into the attributes of magnesium matrix nanocomposites by scrutinizing distinct fabrication methodologies, variations in reinforcement dimensions and weight percentages. Their insights illuminated the intricate interplay of process parameters, wear behaviour, wear mechanisms, and the coefficient of friction [7].

Sunu Surendran and Gnanavel Babu contributed to the field by fabricating ATC, ATB, and ATN composites based on the AZ91D alloy utilizing the stir-squeeze processing method. Their investigation encompassed a detailed tribological characterization of these materials across varying temperatures. Interestingly, their findings highlighted a substantial decrease in the wear rate of the fabricated composites at elevated temperatures. In stark contrast, the wear rate of the base AZ91 alloy sharply increased above 125°C [8]. Anandajothi and Vinod conducted an experiment involving the fabrication of AZ91D magnesium hybrid composites through powder metallurgy methodology. This study introduced diverse weight proportions of amorphous silica and hydroxyapatite particles and subsequently assessed the tribological properties through the use of a pin-on-disc apparatus [9]. The outcomes show that the wear resistance of the AZ91D/7.5% (SiO2-HA) hybrid composite was enhanced compared to that of alternative materials [9]. In the field of enhancing mechanical properties, Bassiouny Saleh et al. used the stir casting technique to reinforce AZ91/SiCp composites by manipulating the weight fraction of silicon carbide particles. This study meticulously explored the influence of SiC particle content on the microstructure, mechanical behavior, and wear performance of the alloy. These composites exhibited homogenous particle distributions, refined grains, and robust adhesion between the AZ91 alloy and the particles. Notably, the composites show improved mechanical properties and enhanced wear resistance, thus demonstrating their potential for diverse applications [10].

With a focused lens on metal matrix composites (MMCs), Nitin Srivastava and Mohd Anas delved into the effects of squeeze casting-related elements and processing factors. Their exploration extended to the realm of reinforcement effects, revealing how various mechanical, tribological, and wear qualities develop in this context. In particular, the automotive industry has leveraged squeeze casting as an alternative to conventional forging and casting techniques for the creation of critical components such as connecting rods and suspension arms [11–15]. These studies collectively underscore certain gaps in the existing research. The role of the crystal structure, size, orientation, and chemical composition of grains in influencing composite properties remains a compelling avenue for exploration [16]. The presence of crystal defects and the interplay of secondary phases also exert substantial impacts on the material properties. The complex interrelationship between the composition, manufacturing process, and resulting microstructure results in the formation of bedrock with material characteristics. Furthermore, the topography; structure; and physical, chemical, and mechanical attributes of surfaces emerge as pivotal factors governing wear processes.

In this evolving landscape, Akyüz's investigation into the percentage of aluminum (Al%) within AZ series magnesium alloys provides valuable insights into machinability, wear resistance, and hardness. The discovery of intermetallic phases and their role in improving alloy properties offers a pathway to enhancing wear resistance. Notably, the AZ91 alloy emerges as a frontrunner in terms of wear resistance and machinability among AZ series alloys. The study of intermetallic phases provides a nuanced understanding of machinability and its relation to alloy composition [17]. Yang et al. investigated the microstructural intricacies of AZ91D alloys through direct squeeze casting, revealing a sequence of microstructure sublayers. Notably, the morphology and distribution of the intermetallic compound β-Mg17Al12 within the alloy are significant factors [18]. Similarly, Mohammad Zarghami et al. explored the influence of SiC particle concentration on the microstructure, mechanical characteristics, and wear behavior of both cast and extruded AZ91-Mg2Si composites. These findings underscore the role of SiC particles in enhancing material hardness and wear properties and are accompanied by a nuanced understanding of wear mechanisms [19–24].

In light of the preceding discussions, a noticeable research gap emerges concerning the influence of weight fraction variations in primary hard particle reinforcement and secondary self-lubricating particle reinforcement on the refinement of the AZ91D alloy grain matrix. The integration of SiC as a primary reinforcement and BN as a secondary self-lubricating reinforcement within hybrid metal matrix composites, manufactured through the stir-squeeze casting technique, is proposed to contribute significantly to applications in the automotive and aerospace domains.

2.1 Material selection

The magnesium alloy AZ91D was used to make magnesium hybrid metal matrix composites through the stir-squeeze casting technique. This material was selected as the matrix due to its excellent quality, low cost, low density, and low weight, as well as because researchers usually choose it for use in aeronautical and automotive applications [25, 26]. The compositions of the AZ91D alloy are shown in Table 1.

Table 1

Components of AZ91D Magnesium Alloy
Concentration wt%
Al	Mn	Zn	Si	Fe	Cu	Ni	Mg
8.5	0.15	1	0.1	0.005	0.03	0.002	Bal

In this investigation, commercially available SiC (37 µm) and BN (10 µm) reinforcement particles were employed as reinforcement particles. The benefits of SiC and BN particles with alloys of magnesium include excellent chemical inertness, high heat stability, and good wettability [27, 28]. SiC and BN densities of 3.2 g/cm³ and 2.1 g/cm³, respectively. The BN particles are stable materials that chemically bond with the AZ91D alloy and contribute to the development of a stable and uniform microstructure. The weight percentage of boron nitride (BN) was kept constant at 3% for all the manufactured hybrid metal matrix composites. The hard reinforcement weight percentage is normally kept below 10% and practically never exceeds 12% in metal matrix composites such as magnesium [29, 30] due to brittleness; as a result, silicon carbide reinforcement is used for three distinct weight percentages of 3, 6 and 9%.

2.2 Stir-squeeze casting process

The stir-squeeze casting process has been employed mostly for creating magnesium hybrid composites due to its significant matrix reinforcement interface, near-net form, simplicity, flexibility, affordability, and use in manufacturing particle-reinforced hybrid composites. In this experiment, the pure magnesium alloy was melted in a furnace at a temperature of 685°C. To mitigate the potential flammability of magnesium, a stirring speed of 700 rpm was used for 20 minutes within the molten alloy. This process was carried out in an atmosphere comprising a mixture of the gases SF₆ and CO₂ at 40 liters/min to effectively prevent oxidation. The reinforcement of BN (3 wt. % as a constant) and the estimated mass fraction of SiC reinforcement particles (3, 6, and 9 wt. %) were preheated and added to the melt. When the metal reached a temperature of 850°C, it was stirred for 15 minutes at a speed of 500 rpm to ensure that the reinforcement was evenly distributed throughout the matrix melt. To reduce heterogeneity in the cast components and prevent melt surface adhesion to the steel die, a sulphur inner coating was added to the die before casting. Using the bottom pouring process, the melt was carefully transferred into the steel die via a heated conduit. A pressure of 150 MPa [31, 32] was maintained during casting at each pressing, and the pressure remained at this level until the solidification process ended. The hydraulic press, employed to punch the steel die after the introduction of the molten matrix, was permitted to naturally cool to ambient room temperature. The same methods were applied to prepare all the composites.

2.3 Measurement of properties

For improved microstructure examination, specimens were etched using HCl + HF + HNO₃. SEM analysis was used to analyze the microstructure. A pin-on-disc instrument was employed to study the wear performance of synthesized magnesium hybrid composites under dry sliding conditions according to the ASTM G99-04 standard [33]. The prepared specimen had a spherical end and was 6 mm in diameter by 30 mm in length. The steel material EN31, with a roughness of 0.3 µm, was employed as a rotating disc. The wear volume loss was estimated as per ASTM G77-83 [34].

3.1 Microstructural characterization

The etched and polished microstructures of the AZ91D/SiC/BN hybrid composites are shown in Fig. 4, and these results provide insightful insights. The AZ91D/3%SiC/3%BN composites primarily comprise extensive net-like lamellar Mg₁₇Al₁₂ phases along the grain boundaries, as depicted in Fig. 4a. However, a distinct transformation becomes evident in Fig. 4c, where the Mg₁₇Al₁₂ phase within the AZ91D/6%SiC/3%BN composite displays a finer and more homogeneous distribution than the AZ91D/3%SiC/3%BN composite. Remarkably, compared with the other composite variations, the AZ91D/9%SiC/3%BN composite, as shown in Fig. 4e, contains notably coarser and larger grains surrounded by the Mg₁₇Al₁₂ phase. The network of Mg₁₇Al₁₂ covers a greater percentage of the primary Mg cell borders in the case of AZ91D. As a result, both the increase in yield strength and ductility were reduced.

Figure 2 shows the SEM images of the prepared specimens The grain sizes decrease as the SiC content increases. The darkest phase, primary magnesium, is the dominant phase. A network of magnesium that has been heavily saturated with aluminum surrounds the primary magnesium and is the last to solidify (medium gray). This network contains Mg₁₇Al₁₂ intermetallic particles that appear in white. The microstructure of the hybrid composites (9 wt% SiC) exhibited coarse granules. However, as the SiC content increased, the second phase expanded, and the grain boundaries became coarser. However, the constitutional undercooling increases along with the SiC throughout the solidification process since the Zn and Alat the grain border are enriched, which boosts dendrite growth.

Figure 3 displays the XRD analysis of the magnesium matrix and fabricated hybrid composites. The samples are composed of the primary Mg phase and the secondary intermetallic phases. Furthermore, the secondary phase has a strong intensity in the hybrid composite, indicating that it accounts for a greater volume proportion of the composite. The Mg₁₇Al₁₂ phase precipitates in the matrix as a result of the ability of the reinforcements to accelerate the cooling rate of the Mg melt and increase its capacity to dissipate heat [11].

Few comparable reinforcing features were visible in the EPMA mapping images (Fig. 4). However, the corresponding peaks in the captured EDS spectra (Fig. 5) provide proof that reinforcing components exist. EDS research provides additional evidence that another oxygen-containing element exists in magnesium alloys, which raises the possibility that oxide growth may occur.

3.2 Tribological properties

3.2.1 Wear performance

To maintain a constant sliding time for all the prepared specimens, three different speeds and three different loads were used in the wear test. The rate of wear of the produced hybrid composites significantly increased across all the various sliding speeds and applied loads. This phenomenon can be ascribed to the tendency of the wear rate to increase as the load on the synthetic composites intensifies. This increase is related to the existence of stronger and more resilient reinforcements in the alloy matrix. Typically, there was a linear relationship between the sliding distance and material loss. (Fig. 6).

The wear performance of the synthesized hybrid composites substantially improved (Fig. 7), which can be attributed to a combination of factors. When the load is increased, the wear track on the synthetic composite surface tends to increase, consequently accelerating the wear rate. However, the inclusion of reinforcements in the matrix alloy leads to enhanced strength and stiffness, which restricts the movement of dislocations within the material. This phenomenon results in a lower rate of wear for the hybrid composites than for the base AZ91D alloy. Analyzing the wear rate for the applied normal load reveals interesting insights across different sliding velocities. For a sliding speed of 0.25 m/s, as shown in Fig. 7a, as the normal load increases, the wear rate generally follows an upward trend. This trend can be explained by the increased contact pressure between the mating surfaces, which leads to intensified material removal and subsequently increased wear rates.

At a higher sliding speed of 0.5 m/s, the wear rate continues to increase with increasing normal load, as shown in Fig. 7b. The increased kinetic energy and heat generated at higher sliding speeds contribute to higher wear rates, as more intensive frictional interactions occur between the sliding surfaces. Figure 7c shows that at a sliding speed of 1 m/s, the relationship between the wear rate and applied normal load becomes more nuanced. While there is a general trend of increasing wear rates with increasing load, the hybrid composites consistently exhibit lower wear rates than does the AZ91D alloy. This can be attributed to the reinforcing effect of SiC and BN particles, which contribute to improved wear resistance by enhancing the material's mechanical properties and reducing the propensity for material removal. Microstructural analyses of the AZ91D/SiC/BN hybrid composites revealed the presence of an α-Mg matrix and β-Mg₁₇Al₁₂ phases, as well as the uniform dispersion of SiC/BN particles. Furthermore, the formation of contact interfaces and diffusion bonding interfaces is evident between the precipitated β-Mg₁₇Al₁₂ phase, the reinforcing particles, and the magnesium matrix. These interactions significantly enhance the bonding strength between the reinforcing particles and the matrix. The incorporation of SiC/BN particles enhances the load transmission and refines the grain structure, resulting in an elevated microhardness in the composite compared to that of the AZ91 alloy. The effect of the lubricating layer generated by BN on the wear surface, which shifted from severe delamination wear to slight delamination and abrasive wear behavior, was responsible for the considerable improvement in the wear resistance of the composites. The intermetallic phase (Mg₁₇Al₁₂) formed in the AZ series of magnesium alloys as a result of the presence of Zn, and the wear resistance increased as the amount of Al% increased [17].

3.2.2 Volume loss of the prepared specimens

Abrasive wear induces surface distortion and degradation, manifesting as pronounced grooves along the sliding direction. Research has indicated a consistent correlation between wear loss and the dissipation of energy during contact, often resulting in an inverse relationship. Therefore, the found slope can be seen as the wear characteristic of a sliding condition. The material's characteristics govern the slope. The volume losses of the base matrix and its composites are shown in Fig. 8.

3.2.3 Coefficient of Friction

Figure 9 displays the variation in the friction coefficient for the synthesized hybrid composites with a 0.5 m/s velocity under three different loads. When sliding at a speed of 0.5 m/s and applying weights of 10, 20, and 30 N, the friction coefficients of the magnesium alloy AZ91D ranged from 0.10 to 0.18. The coefficients of friction for the hybrid composites 3, 6 and 9 weight percent SiC for the applied loads (10 N, 20 N, and 30 N) ranged from 0.12 to 0.28, 0.18 to 0.32, and 0.28 to 0.38, respectively, at a speed of 0.5 m/s. The debris in contact may also change its features during sliding movement due to mechanical hardness or chemical reactivity. The friction coefficient of the hybrid composites significantly increased. This is due to the strengthening effect of the reinforcements and matrix, which causes dislocations in the alloy, and increasing the hardness is the most important factor in enhancing the resistance to wear. Due to the abrasive nature of the SiC particles, the formation of Mg debris in the composites intensifies. At any given load, the peak COF values for magnesium and its composites fluctuate. The COF values obtained with the AZ91D/SiC composites are greater than those obtained with AZ91D, but this tendency changes when a higher volume fraction of SiC is added. This observation indicates that the volume proportion of the reinforcement significantly affects the fluctuations in the COF.

3.2.4 Worn Surface Morphology

The chemistry of the tribolayer sheds intriguing light on the changes after the worn surfaces were thoroughly examined. The scars that form on composite materials have characteristics that are almost identical to those found on AZ91D magnesium metal. The only significant difference is that SiC particles cause the abrasive wear to become more severe. However, the outcome of the reaction with the composites seems brighter than that with AZ91D, indicating that the chemistry of these films differs from that of AZ91D samples. All of the specimens had worn surfaces covered with grooves that ran in a direction similar to that of the wear, as did those with minor plastic deformations. These grooves are caused by abrasive wear, which occurs when the steel counter face between the pin and disc develops sharp asperities that remove material, causing wear. Localized plastic deformation and material smearing, both of which are signs of adhesive wear, were present together with the grooves (Fig. 10). The worn surfaces of the synthesized hybrid composite gradually grow rougher and change from apparent little scratches to deeper grooves as the load increases from 10 to 30 N. Additionally, it has been discovered that the existence of reinforcing particles and higher hardness leads to less adhesive wear and a smoother worn surface, which lowers the overall depth of deformation in reinforced hybrid composites.

This study accomplished the successful fabrication of AZ91D/SiC/BN hybrid composites utilizing the stir-squeeze casting process. Comprehensive microstructural analyses and wear behavior assessments were conducted considering various test parameter variations. The insights gained from this investigation led to the following conclusions regarding this study:

The improved mechanical properties are dependent on the even dispersion and wettability of the reinforcements with the magnesium metal matrix, both of which are ensured by the stir-squeeze cast technique.

A microstructural study confirmed the enhanced distribution of reinforcements within the composites and the reinforcement of grain boundaries in the alloys.

The SEM study showed that squeeze casting resulted in a finer cast structure with a more even dispersion of particulates. The addition of SiC and BN particles influences the grain size of AZ91D and enhances its structure and characteristics.

A strong Mg₁₇Al₁₂ phase in the AZ91D/SiC/BN hybrid composite was observed via XRD analysis, which showed that the Mg₁₇Al₁₂ phase made up a significant volume proportion of the composite.

The volume loss of the synthesized magnesium hybrid composites (AZ91D/9%SiC/3%BN) was suggestively reduced by up to 36.16% at a maximum load of 30 N and a maximum speed of 1 m/s compared with that of the monolithic material AZ91D.

Due to the particle microfractures in the composite, the foremost wear mechanism for all the composites was observed to be abrasion from the worn surface observation. The overall depth of the hybrid composites decreased due to wear, and the worn surface of the composites was smoother.

Competing Interests and Funding:

The authors declare that they have no conflict of interest and No funds, grants, or other support was received.

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The authors declare no competing interests.

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Experimental investigation of the microstructural and wear behaviours of silicon carbide and boron nitride-reinforced AZ91D magnesium matrix hybrid composites

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Abstract

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1 INTRODUCTION

2 MATERIALS AND METHODS

2.1 Material selection

2.2 Stir-squeeze casting process

2.3 Measurement of properties

3 RESULTS AND DISCUSSION

3.1 Microstructural characterization

3.2 Tribological properties

3.2.1 Wear performance

3.2.2 Volume loss of the prepared specimens

3.2.3 Coefficient of Friction

3.2.4 Worn Surface Morphology

4 CONCLUSIONS

Declarations

References

Additional Declarations

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