Mechanical Characterization of B4C-Gr Reinforced Al–Zn–Mg Alloy Hybrid Nanocomposites

Abstract

The current study is an attempt made to synthesize nano B4C/Graphite reinforced Aluminum–Zinc–Magnesium alloy composites by altering the weight %age of B4C (2%, 4%, and 6%). SEM was used to examine the morphology and mechanical behaviour was done in accordance with ASTM standards (ASTM E8, E9, E23, and D790). The microstructure displays a nearly uniform dispersion of reinforcement particles in the matrix alloy, with no residual pore visible. From the XRD analysis it is identified that interfacial phases between the base material and ceramic strengthening particulates are identified as Al₃BC, AlB₁₂, Mg₂Si, SiAl₂ and it strive as strengthening mechanism of synthetic composites. The interfacial phases identified as Al₃BC, AlB₁₂, Mg₂Si, and SiAl₂, and serve as a strengthening mechanism for synthetic composites, according to XRD. When compared to the base material, intermixtures had higher hardness (28.07%), ultimate tensile strength (69.31%), compressive strength (18.58%). The flexural strength is improved (29.32%) due to higher dislocation density in the matrix and wider variations in the elastic modulus. The impact strength improved significantly (72%) due to a reduction in porosity and grain refinement.

1. Introduction

Low-density materials have played a prominent role in functional applications, particularly in the automotive and marine industries, throughout the last decade. Metal matrix composites captivate those applications due to their improved strength-to-weight ratio and lower cost.¹⁾ Aluminium and its alloys, in the midst of diverse metals, perform infinite engineering applications due to their low density and enormous endurance. They did, nevertheless, limit the use of such materials for functional applications because of their inferior hardness and wear resistance.²⁾ This can be overcome by adding sufficient ceramic strengthening particles to parent materials to improve their properties. Computing discrete strengthening particles on such alloys has been used in separate investigations.³⁾ Cast metal matrix composites frequently use micron-sized ceramic reinforcing particles. Moreover, utilizing such particles has the disadvantage of having increased toughness and poorer ductility. Furthermore, during machining qualities, tool wear issues are related to it. Nanocomposites⁴⁾ have been used to minimize this weakness. At least a few proportions of ductility and improved wear resistance are achieved in nanocomposites, making them more favourable for the aforesaid applications. Besides, it increased tensile strength, hardness, and fracture toughness at both low and high temperatures.⁵⁾ It did, however, have particle aggregation as a result of the larger surface to volume ratio, which generates widespread adverse qualities. This can be solved with the use of appropriate process parameters and a flexible processing strategy.

The incorporation of two or more micro-ceramic particles with base materials has lately increased, and they are classified as hybrid composites, according to the literature. Adding unique ceramic particles to the basic material improves mechanical characteristics, corrosion resistance, and wear resistance. Additionally, the introduction of ceramic particles does not warrant the enhancement of hybrid composites. Particle size, homogeneous distribution of strengthening particles with base material, weight fraction, and manufacturing procedures are all factors to consider.⁶⁾ Hardening particles (borides, carbides, and nitrides) and solid lubricants are frequently used in base materials. Solid lubricants, such as graphite, MoS₂, CNT, and Graphene, are frequently employed as secondary reinforcement in conjunction with primary hard ceramic strengthening particles. These secondary reinforcements are widely used in the manufacture of metal matrix composites to increase qualities such as fatigue life, corrosion resistance, wear resistance, and tribological properties.^7,8) Due to the emergence of a tribo-layer in the sliding contact region, the weight %age of solid lubricants in the base matrix cannot be increased to its maximum, and it displays a drop in hardness and wear rate. The effect of nano graphite (50 nm) ceramic particulates enhanced Aluminium Zinc alloy composites were fabricated using the stir casting method. The density of synthetic composites was shown to decrease as the porosity % was increased.⁹⁾ The liquid casting process was used to develop a comparative analysis of boron carbide and graphite reinforced aluminium alloy composites. It has been discovered that strengthening particles made of AA7075 have better qualities than those made of Al6061.¹⁰⁾ The stir casting method was used to generate boron carbide and graphite reinforced aluminium hybrid composites. The mechanical properties of aluminium hybrid composites were found to be significantly improved when compared to the basic material.¹¹⁾

Using the liquid metallurgy method, aluminium hybrid composites with variable strengthening particulates of dissimilar weight proportions were developed. It was found that the physical properties of the fabricated composite (B4C/Gr) were significantly improved compared to SiC/Gr strengthened aluminium composites.¹²⁾ However, from the literature review it was found that graphite as a solid lubricant makes it difficult to detect the physical features of hybrid composites, which can be done by using nano-sized particulates.⁹⁾ It is known that just a few studies have been conducted on the use of boron carbide and graphite at the nanoscale level, and their mechanical properties have not been defined. In order to address investigation differences, an attempt was made to synthesize boron carbide with different weight proportions (2, 4, and 6%) and unvarying graphite (2 wt%) using the squeeze casting process, and its physical properties were assessed for vehicle implications.³⁵⁾ However a couple of investigatory had disputation that by using graphite as solid lubricants it finds complex to identifying the physical properties of hybrid composites and this can be accomplished by exerting nano-sized graphite strengthening particulates and in addition, the wettability between such hybrid reinforcement in the aluminium matrix has not yet carried out.⁹⁾ In consideration of investigative dissimilarities an effort has been made to synthesize boron carbide of varying its weight proportions (2%, 4% and 6%) and unvarying graphite (2 wt%) using squeeze casting method and its physical properties has been characterized for automobile implications Refs. 33) and 34). In this study, we attempt to characterize the hardness, tensile, compressive, flexural, impact strength, and corrosion resistance.

2. Materials and Methods

2.1 Assortment of base material and strengthening particulates

The foundation material for producing aluminium alloy hybrid composites using the squeeze casting method is an Aluminium–Zinc–Magnesium alloy (AA7075). Table 1 highlights their chemical combinations. These alloys are now used in transportation applications where weight reduction is a key component. Moreover, when compared to other aluminium alloys, it has greater physical qualities. The incorporation of reinforcing ceramic particles in the parent materials is assumed to be unable to increase the density of manufactured composites due to weight reduction features that are unbalanced for functional application. As a result, the present research used commercially available nano-ceramic strengthening particulates of B₄C (2.25 g/cm³) and Graphite (2.16 g/cm³) with particle sizes of 60 nm and 80 nm (Sigma Aldrich). To homogenize the mixture, B₄C’s primary hard ceramic strengthening particle is used. B₄C has higher physical qualities such as hardness, flexural strength, elastic modulus, wear resistance, lower density, chemical, and thermal stability.¹³⁾ In addition, in this study, the secondary reinforcement Graphite is postulated. It has a lamellar crystal structure and a low coefficient of friction (0.1 to 0.2), which improves antifriction characteristics and corrosion resistance in produced composites.¹⁴⁾

Table 1 Chemical combinations of Aluminium–Zinc–Magnesium alloy.

2.2 Squeeze casting

The squeeze casting method was used to cast aluminium alloy hybrid composites in this investigation is shown in Fig. 1. During the solidification stage of this process, the molten slurry is subjected to increased pressure. As a result decrease in solidification temperature and intensification of cooling, revealing nucleation momentum. This prevents air from passing between the mould and the molten composites, resulting in improved heat diffusion and grain refinement on the hybrid composites. In addition, it has a lower deformity in the produced composites.¹⁵⁾

Fig. 1

(a) Experimental Setup of stir casting, (b) Test Specimen.

The alloy (Aluminum–Zinc–Magnesium) was placed in a resistive heating furnace and melted for 10 minutes at 700°C. To guarantee that the alloy was thoroughly melted, the stirring speed was kept at 400 rpm. Nano boron carbide (nB₄C) reinforcement particles in various weight proportions (2%, 4%, 6%) and nano graphite (nGr) 2% reinforcement particles are warmed at 250°C to eliminate moisture and inflate the wettability between the matrix and reinforcement particulates.¹⁶⁾ The melting temperature was raised to 750°C, and the ceramic reinforcing particles were introduced into the melt via an external sprue. The molten slurry’s stirring speed is increased to 500 rpm to avoid particle aggregation. Owing to the dissolution of the chemical reaction between the matrix and reinforcement particles, it creates a vortex that prevents the accumulation of those strengthening nanoparticles in a specific place. This has an impact on the uniform distribution of reinforcement preserved in the molten slurry. Moreover, the temperature of the molten metal was raised to 800°C, lowering the viscosity of the composite slurry and causing the ceramic reinforcement particles to float throughout the liquid during stirring. In addition, the stirring speed and time were increased to 600 rpm and 15 minutes, respectively. It was discovered that increasing the amount of micro boron carbide (8 wt%) causes the ceramic particulates to agglomerate, even with good processing methods, therefore it was decided to limit such ceramic particulates to 6 wt%. According to research, the addition of secondary micro graphite reinforcement reduces tensile characteristics while increasing the fraction of such particles in the aluminium matrix. Because these ceramic particles are smooth and brittle, weak bonding between the parent material alloys is observed.¹⁷⁾ This has been limited in the current work by keeping graphite at a low concentration of 2 wt%. Because the die was heated to eliminate any trapped gas before pouring the molten slurry into the die cavity, the effect of matrix porosity was minimised. The molten slurry was poured into the die cavity and left to cool at room temperature.

ASTM standards (ASTM E8, E9, E23, and D790) were used to create performance metrics for aluminium alloy hybrid composites. The microstructure of Aluminum hybrid composites was studied using an optical microscope. SEM analysis was used to analyse the morphology of the reinforcing particle dispersion in the matrix alloy. Tensile, compressive, flexural, and impact resistance of aluminium alloy hybrid composites are studied. The corrosion resistance was tested using a salt spray chamber in accordance with ASTM B117.¹⁸⁾

3. Results and Discussions

3.1 Microstructure

The microstructure of nano boron carbide-graphite reinforced aluminium hybrid composites were studied using an optical microscope in this study. Figure 2–4 depicts as-cast and etched composites with various weight proportions. As an etchant, Keller’s reagent is utilized. The micrograph depicts the dispersion of nano boron carbide and graphite-strengthening particles. In the matrix, these particles are uniformly dispersed and spaced. The entrapment of strengthening particles at the grain boundaries has thickened the grain boundaries. The density dispersion is lesser when the ceramic particles are added in smaller amounts. The precipitated particles of the alloy’s eutectic constituents can also be seen near the grain boundaries. Inside the grains of primary aluminium solid solution, several eutectic particles were also discovered.¹⁹⁾

Fig. 2

(a) Microstructure of 2 wt% of nB4C + 2 wt% graphite strengthened Aluminum–Zinc–Magnesium alloy composite as cast, (b) Etchant application.

Fig. 3

(a) Microstructure of 4 wt% of nB4C + 2 wt% Gr strengthened Aluminum–Zinc–Magnesium alloy composite as cast, (b) Etchant application.

Fig. 4

(a) Microstructure of 6 wt% of nB4C + 2 wt% Gr strengthened Aluminum–Zinc–Magnesium alloy composite as cast, (b) Etchant application.

The strengthening particles are piled up in certain locations due to an increase in the fraction of ceramic particulates even though the process parameter is increased, according to the scanning electron microscope (SEM) of Aluminium hybrid composites (Fig. 5). It’s also been noticed that the boron carbide particles have a needle-like structure and can’t be dissolved due to their high-temperature properties. During the solidification process, the secondary strengthening particles (Graphite) of solid lubricant connect firmly with the phase of aluminium, forming an aluminium dendritic pattern that significantly improves Al-grains. The presence of secondary ceramic particles acts as a nucleus, causing this grain to crystallise. As a result, these secondary particles obstruct the expansion of Al-grains, escalating the grain boundaries of hybrid composites by overlapping the areas of the Al–Zn–Mg-phase alloy, reducing dislocation motion and reducing the grain size. The mechanical properties of manufactured aluminium hybrid composites are mostly determined by the strengthening technique. The peaks factor for aluminium–zinc–magnesium alloys are 38.2°, 44.5°, 66.3°, 78.2°, followed by ceramic strengthening particulates B₄C 31.78°, 35.54°, 48.37°, 64.95°, 73.14°, 76.88°, and Graphite 15.04°, 20.47°, 28.47°, 35.57° at 2 with indices of (111), (200), (220), (222), (012), (021), (104), (110), (128), (211), (100), (110), (112), (205) (Fig. 6).

Fig. 5

(a) SEM images of 6 wt% of nB4C + 2 wt% n-graphite strengthened Aluminum–Zinc–Magnesium alloy composite, (b) Emphasizes on Boron carbide.

Fig. 6

XRD images of 6 wt% of nB₄C + 2 wt% nGr strengthened Aluminum–Zinc–Magnesium alloy composites.

It has been observed that the inclusion of boron carbide interacts with aluminium and it forms interfacial phases such as Al₃BC, AlB₁₂, Mg₂Si, and SiAl₂ and it strives as strengthening mechanism of synthetic composites.²⁰⁾

3.2 Hardness

The hardness of Aluminum–Zinc–Magnesium alloy hybrid composites is measured by considering an average of 5 indentations using the Vickers microhardness test of Wilson MICI with a load range of 1 Kg with diamond pyramid as indenter for a dwell period of 10 s, as per ASTM E381 standards.²¹⁾ The hardness of the Aluminium alloy hybrid composites was considerably increased compared to the parent material due to an increase in hard ceramic strengthening particulates, Orawan strengthening mechanism, interfacial bonding between the base material and strengthening particulates, and inadequacy of porosity as shown in Fig. 7. During solidification, the presence of B4C in the matrix material provides an auxiliary substratum for the intermixtures. As a result of the increased nuclear rate, a reduction in grain size is attached, resulting in a larger resistance and a reduction in dislocation motion during indentation. As a result, the hardness of hybrid intermixtures is greatly increased. Additionally, as shown in many literatures,^22–26) the addition of secondary strengthening ceramic particles of graphite reduces the hardness of composites. This is due to the fact that when the fraction of graphite increases, it tends to float, causing discontinuities in the liquid melt due to its low density, resulting in insufficient adhesion between the base material and ceramic strengthening particles. Effective processing parameters, on the other hand, were able to overcome it in our study. It is concluded that the created intermixture’s hardness values cannot be reduced when the secondary reinforcement remains constant and the primary strengthening particles in the matrix alloy increase.

Fig. 7

Hardness of hybridized Aluminum–Zinc–Magnesium alloy nanocomposites.

3.3 Tensile and compressive properties

The tensile qualities of Aluminum hybrid composites were tested at room temperature using an ASTM E8 universal testing equipment with a maximum load of 10 tonnes and a crosshead rate of 0.5 mm/min. In comparison to the parent Aluminum–Zinc–Magnesium alloy illustrated in Fig. 8(a) and Fig. 8(b), the hybridized mixture’s ultimate tensile strength increased to a maximum of 69.31% and the percentage elongation dropped to 1.68% as shown. According to previous findings,²⁷⁾ this is due to an increasing proportion of nano ceramic strengthening particulates (B₄C) in the base matrix, strong interfacing between the combinations, grain refinement, dislocation density, and a virtual load transfer mechanism between the matrix alloy and nano-ceramic particulates.

Fig. 8

(a) Ultimate Tensile strength of Aluminium hybrid composites with varying weight proportion, (b) % of elongation of Aluminium hybrid intermixture of varying weight proportion.

Furthermore, the uniform distribution of hard nano-ceramic strengthening particles in the base matrix acts as a load carrier mechanism, causing the base alloy to have a higher strength, which stimulates superior reluctance for produced nanohybrid mixes. Furthermore, the presence of nano-hard graphite particles acts as a barrier, preventing crack propagation under immediate loading conditions. In addition, the squeeze-casting processing method was used in this research. This prevents the affected gases from escaping during processing, resulting in a decrease in porosity and a considerable increase in the tensile characteristics of the hybridized intermixture.²⁴⁾ However, when compared to base Aluminium alloy, the % of elongation was reduced substantially. Due to the brittle nature of ceramic strengthening particles. When such particles are added to the matrix alloy, the ductile characteristics of produced composites are reduced, and necking is reduced. Along with this, the inclusion of nano graphite particles in the composites inhibited the flow behaviour of the Aluminum–Zinc–Magnesium alloy matrix, which resulted in a reduction in the elongation of the produced composites.

The compressive strength of hybridized aluminium nanocomposites was tested according to ASTM E9 standards as shown in Fig. 9. According to previous findings,²⁸⁾ the compressive strength of Aluminum–Zinc–Magnesium alloy material rose dramatically resulting in the introduction of tougher ceramic reinforcing particles. During solidification, ceramic strengthening particles are driven into the primary regions of -Al grains, where they act as a nucleus, preventing dislocation motion in the Al phase through the dispersion strengthening mechanism.²⁹⁾ Furthermore, the presence of Mg₂Si, silicon, in the eutectic interdendritic intermetallic’s solid solution of Aluminum–Zinc–Magnesium alloys works as a reinforcing mechanism, increasing the compressive strength of the generated nanohybrid composites.

Fig. 9

Compressive strength of nano aluminium hybrid composites.

3.4 Flexural and impact strength

The impact energy of Aluminum–Zinc–Magnesium alloy and various proportions of nano ceramic strengthening particulates of produced aluminium hybrid composites are assessed according to ASTM E 290 and ASTM E23-07a standards in this work as shown in Fig. 10(a), the addition of elastic modulus and toughness of hybrid intermixtures that block disruption enhances grain refinement resulted in an increase in flexural strength of 87.40% when compared to Aluminum–Zinc–Magnesium alloy. According to literature, increasing the quantity of graphite in the molten slurry causes air bubbles to form in the ceramic particles and causes poor wettability, which significantly reduces the physical properties.³⁰⁾

Fig. 10

(a) Flexural strength of Aluminium hybrid composites, (b) Impact strength of Aluminium hybrid composites.

This is suppressed in the present study by adding stable secondary ceramic particles in the matrix alloy, preventing air bubble formation, nanoparticle accumulation, and floating in the molten slurry through an effective processing approach. It has been noticed that the uniform distribution of ceramic strengthening particles restricts the plastic flow of intermixtures. The flexural behaviour of hybrid composites is significantly improved as a result of this.

As shown in Fig. 10(b), the impact strength of synthesized composites improved to a maximum of 72% when compared to the base alloy material, owing to the reduction in porosity achieved through the squeeze casting process, uniform distribution of ceramic strengthening particulates in the matrix alloy, increases in yield strength of composites improving ductility, and the presence of Mg₂Si interface in the composites. It should also be emphasized that the addition of such hard ceramic reinforcing particles to create hybrid composites inhibited fracture propagation at grain boundaries due to transgranular facets. These particles operate as a stress concentration factor, resulting in an equilibrated crack that absorbs a lot of energy under load. In addition, the presence of secondary reinforced particles prevents void nucleation, limiting the creation of cracks in the composite.

3.5 Corrosion resistant

ASTM B117 (Conducted salt spray test exposure at 33°C) with a salt concentration of 5% Sodium Chloride (NaCL) for 24 Hours was used in this investigation to assess the corrosion resistance of synthesized aluminium alloy hybrid composites, and its processing parameters were derived from the literature.³¹⁾ It is well known that the presence of micro ceramic strengthening particles breaks the continuities of the base material and induces the formation of a protective surface oxide film, making the intermixture corrosive. In contrast, when hard ceramic strengthening particles are incorporated in Aluminum–Zinc–Magnesium alloys, the corrosion rate drops dramatically, as illustrated in Fig. 11. This is because these ceramic-strengthening particles are evenly distributed throughout the base materials and operate as a protective surface layer in saltwater settings.

Fig. 11

Corrosion-resistant of Aluminum–Zinc–Magnesium alloy hybridized composites.

In NaCl solution, AA7075 normally exhibit corrosion resistance, however, the improvement to corrosion resistance was further improved in the current investigation. Furthermore, as indicated in eq. (1),³²⁾ the layer may form and it reduces the oxidation rate of the synthesized hybridized composites. However, it is resulting in wear loss at high temperatures and raising the corrosion rate of produced composites in a saltwater environment. It’s also shown that the inclusion of strengthening particles like Al₃BC, AlB₁₂, Mg₂Si, and SiAl₂ works as an impediment to the development of composites, slowing the rate of oxidation of intermixtures.   

\begin{equation} \text{B$_{4}$C} + \text{8H$_{2}$O} \Rightarrow \text{2B$_{2}$O$_{3}$} + \text{CO$_{2}$} + \text{8H$_{2}{}\uparrow$} \end{equation} (1)

The presence of Al₃BC works as a metastable phase that surrounds the strengthening particles as disintegrated precipitates, forming a protective thick coating on the intermixture’s surface. The inclusion of secondary reinforcing graphite, on the other hand, reacts with aluminium and forms aluminium carbides. These particles form along grain boundaries and hinder interdendritic corrosion of intermixtures, slowing down the oxidation of parent materials significantly.

4. Conclusion

The microstructure mechanical properties of nano boron carbide (2%wt, 4%wt, 6%wt) and graphite (2%wt) enhanced Al–Mg–Zn alloy hybrid composites using squeeze casting process have been evaluated for vehicle and marine applications in this study.

1. (1)    The nano ceramic reinforcing particles are uniformly dispersed in the base material with no evidence of residual porosity, and their agglomeration is detected when the weight proportion of ceramic particulates is increased (at 8 wt%).
2. (2)    According to SEM examination, Boron carbide particles have a needle-like structure that cannot be dissolved due to its high thermal properties, and secondary reinforcing graphite precipitates along the grain boundaries (at Al 92% + B₄C 6% + Gr 2%) of hybridized composites.
3. (3)    Between the intermixture, interfacial phases, such as Al₃BC, AlB₁₂, Mg₂Si, and SiAl₂ are detected, and they operate as strengthening particles that improves the properties of created composites.
4. (4)    When compared to the parent Aluminum–Zinc–Magnesium alloy, the hardness and ultimate tensile strength of the hybridized combination B₄C – Graphite Reinforced Aluminum–Zinc–Magnesium increased to a maximum of 28.07%, 69.31%, and the percentage elongation dropped to 1.68%.
5. (5)    When compared to a base material, the compressive, flexural, and impact strengths of nanohybrid composites increase by 18.58%, 29.32%, and 72%, respectively, due to the dispersion strengthening mechanism of hard particles of B₄C (at Al 92% + B₄C 6% + Gr 2%).
6. (6)    The corrosion resistance of hybridized intermixture consistently improved 45.54% compared to monolithic Aluminum–Zinc–Magnesium alloy owing to reduction of interdendritic corrosion along the grain boundaries.
7. (7)    Present work is limited to the constant Gr %. So there is wide scope to increase its percentage to enhance the properties for various applications in automobile and allied sectors.
8. (8)    Since the produced composite has a low density and high strength, the engine and suspension systems for automobiles are expected to use it.

Acknowledgements

The authors are thankful to Madras Institute of Technology, Anna University, Chennai for providing the facilities to conduct the experiments.

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