Development of a magnesium/amorphous nano-SiO2 composite using accumulative extrusion method

doi:10.21203/rs.3.rs-4053307/v1

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Development of a magnesium/amorphous nano-SiO2 composite using accumulative extrusion method

https://doi.org/10.21203/rs.3.rs-4053307/v1

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published 13 Jun, 2024

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In this study, a Mg-X%SiO₂ (X = 1, 2) nanocomposite was developed using amorphous silica nanoparticles via the accumulative extrusion method. The reinforcement phase was added to the matrix between extrusion passes. The study evaluated the mechanical properties of the composite samples via compression and hardness tests, while the microstructure and texture were analyzed using an optical microscope and X-ray diffraction analysis. To remove the deformation history and examine the effect of the reinforcement phase on mechanical properties, the samples were annealed in an argon atmosphere. In addition, monolithic magnesium samples were fabricated through the same process to serve as a basis for comparison. This study revealed that adding 1 wt.% amorphous silica nanoparticles to the magnesium matrix improved the overall mechanical properties. However, the nanocomposites displayed varying properties in different directions. Along the extrusion direction, the yield strength and ductility increased up to 57% and 5%, respectively, while the ultimate compressive strength decreased by about 8%. Along the normal direction, the yield strength and ductility increased up to 37% and 45%, respectively, while the ultimate compressive strength decreased by about 9%. The Mg/2%SiO₂ nanocomposite sample showed superior Brinell hardness. The number of extrusion passes had a significant impact on the distribution of nanoparticles within the matrix. The optical microscope micrographs revealed that the reinforcement phase was uniformly distributed throughout the matrix, and no agglomeration of nanoparticles was observed. The X-ray diffraction results demonstrated that the texture of nanocomposite samples weakened after adding nanoparticles, resulting in improved ductility.

Magnesium matrix nanocomposite

amorphous silica nanoparticles

accumulative extrusion.

Magnesium is an industrial metal renowned for its remarkable lightweight properties, with a density of 1.738 g/cm³. Its lightweight and durable properties have made it a material of interest for various industries [1]. However, its industrial application has been limited by certain drawbacks, including low ductility at room temperature, low corrosion resistance, and low strength at temperatures above 175°C [2]. To address these limitations, researchers are working on developing magnesium matrix nanocomposites. These nanocomposites have unique properties such as a high strength-to-weight ratio, making them an ideal choice for use in the automobile and aircraft industries [3, 4].

Adding a second phase of particles is a well-established technique to improve the strength of metals and alloys. In the case of magnesium composites, ceramic reinforcements can significantly enhance their mechanical properties [5]. Achieving a more uniform distribution of smaller-sized reinforcement particles is known to improve the strength and toughness of composites. Previous studies have also demonstrated that incorporating nano-sized reinforcement particles can increase the ductility of metal matrix composites [6]. To fabricate composites with superior mechanical properties, it is crucial to use micro- and nano-sized reinforcement particles. In recent years, several studies have focused on enhancing the mechanical properties of magnesium by incorporating nano-sized reinforcement particles [7, 8]. Therefore, to improve the ductility of magnesium matrix composites, the use of nano-metric reinforcement is recommended. Crystalline ceramic nanoparticles such as TiB₂, SiC, and Al₂O₃ have shown to reinforce the magnesium matrix and enhance its strength. However, it should be noted that the use of these reinforcements can decrease the ductility of the matrix, which could be attributed to the weakened interface between the matrix and reinforcement [9].

Nie et al. [10] conducted a study to synthesize AZ91/SiC nanocomposites using the semi-solid state process under ultrasonic vibration followed by extrusion at 350°C. Their study examined the effect of hot extrusion on the microstructure and mechanical properties of their nanocomposites. As a result, they observed extensive dynamic recrystallization and a more uniform distribution of SiC nanoparticles. This uniform distribution of nanoparticles and grain refinement led to significant improvements in the ultimate tensile strength, yield strength, and elongation of their nanocomposite. Hassan et al. [11] produced Mg/Al2O3 nanocomposites that exhibited a 90% increase in yield strength and up to 45% improvement in ductility compared to pure magnesium. Their research attributed this improvement to the uniform distribution of nanoparticles and grain refinement. Lv et al. [12] employed accumulative roll bonding (ARB) to manufacture Mg/SiC nanocomposites. Their study revealed a homogeneous distribution of nanoparticles and a significant reduction in the matrix grain size in the microstructure of the nanocomposites. Sankaranarayanan et al. [13] developed Mg/ZnO nanocomposites through liquid-state processing, followed by hot extrusion. They reported that the presence of nanoparticles resulted in increased yield strength and ductility, indicating that the uniform distribution of nanoparticles played a crucial role in the enhancement of their nanocomposites' mechanical properties.

Using crystalline ceramic particles as reinforcements in magnesium matrices is common, but it comes with certain limitations, particularly in low ductility. To address this, Issa et al. [14] conducted a study on the relationship between the properties and structure of amorphous and crystalline silica nanoparticles reinforced magnesium matrix nanocomposites by using an accumulative extrusion (AE) process. The researchers added 0.25, 0.5, and 1 wt.% of amorphous and crystalline silica nanoparticles to the matrix and examined the nanocomposites' mechanical behavior through hardness and uniaxial compression tests. The results showed that the compressive yield strength increased by 28.5% after extrusion. In contrast, the ultimate compressive strength remained unchanged, and ductility increased by 20% in the Mg/0.5% SiO2 nanocomposite compared to the monolithic sample. Furthermore, the hardness of the nanocomposite reinforced with amorphous silica nanoparticles was higher than those reinforced with crystalline silica. The researchers concluded that both amorphous and crystalline silica nanoparticles were uniformly distributed after the AE process due to the accumulative extrusion process's capacity to prepare appropriate solid-state nanocomposites.

Karimi et al.[15] successfully synthesized a nanocomposite consisting of Sn-0.7wt.%Cu/Xwt.%SiO2 using the angular accumulative extrusion process, which is a method of severe plastic deformation. By adding silica nanoparticles via angular accumulative extrusion, the properties of the nanocomposite have been enhanced compared to the monolithic sample. The characterization results indicated that the tensile properties of the as-extruded nanocomposite samples containing 0.5 and 1 wt.% nanoparticles have increased by up to 22% and 12%, respectively.

The mechanical properties and final cost of a composite material heavily depend on the manufacturing process used in its production. The high reactivity of magnesium powder during powder metallurgy can result in spontaneous ignition when exposed to oxygen. Casting, on the other hand, can lead to shrinkage porosities that can degrade the mechanical properties of the final product. Additionally, ARB, or Accumulative Roll Bonding, is susceptible to material failure due to cracks in the material. To overcome these challenges, the low-temperature deformation process called Accumulative Extrusion (AE) can be used to prepare metal strips without surface cracks, making it a highly beneficial method for solid-state metal matrix composite preparation [14]. Therefore, this study aims to employ AE as a solid-state approach to synthesizing magnesium matrix nanocomposites reinforced with amorphous SiO2 nanoparticles, thus overcoming the challenges associated with other processing routes.

2.1. Materials

The present study employed commercial pure magnesium and silica nanoparticles. Table 1 presents the chemical composition of the magnesium ingot. Cuboids measuring 25×25×65 mm were used in the extrusion process.

Table 1

Chemical composition of the commercial pure magnesium ingot
Mg	Al	Be	Cu	Mn	Zn
99.8	0.0020>	0.003	0.0418	0.115	0.0195

To produce amorphous silica nanoparticles, a silicone polymer (HTV) was subjected to pyrolysis at 700°C for one hour, as per the procedure suggested by Senemar et al. [16]. The X-ray diffraction (XRD) pattern of the synthesized nano-silica is displayed in Fig. 1-a, which shows that the product structure is amorphous, with a broad peak around 22 degrees. The size of the silica nanoparticles, as observed through transmission electron microscopy in Fig. 1-b, is below 100 nm.

2.2. Manufacturing of the samples

Two composite samples (designated as Mg-X% SiO₂, where X is either 1 or 2) were extruded. The extrusion process consisted of 14 passes with a ratio of 5:1 at a temperature of 300°C. For the first 13 passes, no lubricant was used, but for the final (14th) pass, a lubricant was applied using graphite and grease. After each pass, the resulting extrusion product (a strip) was cut into five equal-length pieces and cleaned using sandpaper. The five strips were then stacked with nanoparticles added in between. To compare the mechanical properties of the nanocomposite samples with those of pure magnesium, a pure magnesium sample without SiO₂ nanoparticles was also extruded using the same process. Figure 2a defines the normal direction (ND) and transverse direction (TD) with respect to the extrusion direction (ED) on the strip.

2.3. Investigation of the samples

Metallography was performed after each extrusion pass to acquire the microscopic images of the products. Samples were etched for 20 seconds with an etchant solution comprising 15 ml of acetic acid, 5 ml of nitric acid, 20 ml of distilled water, and 60 ml of ethanol as the etchant. The samples were investigated using an optical microscope. X-ray diffractometry was conducted using a θ-2θ diffractometer at a scan speed of 3°min^-1.

To provide a comparison of the mechanical properties of the composite with the monolithic samples, an analysis of the hardness and compressive strength at ambient temperature was undertaken. In order to conduct this analysis, uniaxial compression tests were carried out in both ED and ND directions, according to the ASTM E9 standard. Samples with a height (H) to diameter (D) ratio of 1.1 (Fig. 2b) were cut by a wire cut machine. The tests were performed on an STM-50 uniaxial tension-compression machine at a strain rate of 6×10^− 4 s^-1. The Brinell hardness test was also conducted according to the ASTM E10 standard. For each sample, hardness was measured by at least 10 points, and the average hardness was reported.

3.1. Microstructure

The optical micrographs of pure magnesium samples after extrusion and annealing are presented in Fig. 3. It is evident that the grain size is reduced after extrusion (Fig. <link rid="fig3">3</link>-a and 3-b) compared to that after annealing (Fig. <link rid="fig3">3</link>-c and 3-d). This phenomenon is due to recrystallization and grain growth during annealing.

The optical micrographs of the Mg-1% SiO2 composite samples at two different magnifications are depicted in Fig. 4. The figure highlights the comparison between the grain size observed after extrusion and the grain size observed after annealing. It is noteworthy that the inclusion of 1% of nanoparticles in the composite material appears to have a noticeable impact on the annealing process as it limits the growth of grains during the process. A comparison between Fig. 3 and Fig. 4 confirms that adding nanoparticles to the composite material significantly impacts the material's grain size.

Figures 5a-f depict the optical microscope images of pure magnesium and Mg-1% SiO2 composite after the extrusion process. The images suggest that the composite sample has a smaller average grain size when compared to the pure magnesium sample. The primary reason for this is the pinning of grain boundaries by nanoparticles, which inhibits the growth of grains.

Twinning is a mechanism of deformation in the hexagonal crystallographic lattice of magnesium. Figure 6 displays deformation twins that occur after the extrusion process. In this mechanism, a region of the atomic lattice is deformed so that it forms a mirror image relative to a twinning plane [17, 18]. These twins appear inside the grains and are visible as two parallel lines.

3.2. Texture of the extruded composite

The X-ray diffraction patterns for pure magnesium and composite samples after accumulative extrusion and annealing are presented in Fig. 7. The diffraction patterns observed at 2θ = 32°, 34° and 36° in the extruded magnesium and Mg-2% SiO2 samples correspond to the prismatic planes (10–10), basal planes (0002), and pyramidal planes (11 − 10), respectively, according to [13]. A comparison of pure magnesium X-ray diffraction patterns (Fig. 7a) shows that the basal planes in the extrusion direction have a higher peak intensity than those in the normal direction. It was observed that the pure magnesium is deformed in the direction in which the basal planes intersect, leading to the formation of a strong texture [10]. On annealing the pure magnesium samples, recrystallization occurs, which replaces deformed grains with recrystallized grains, resulting in a weakening of the texture created by the extrusion process and a decrease in the intensity of basal planes in the extrusion direction [14, 19]. It is worth noting that the pyramidal planes' peak intensity in the ND diagram of pure magnesium is higher than that of the prismatic and basal planes. Moreover, when recrystallization occurs, the intensity of the basal planes in the ND diagram decreases, indicating the texture's weakening [14].

The results from Fig. 7b indicate that the pyramidal planes have the highest peak intensity in the ND of the composite samples. The presence of nanoparticles in the composite leads to a decrease in the intensity of the basal planes [20, 21]. The maximum peak intensity of the composite in the ED direction belongs to the basal planes, and with the presence of nanoparticles, the peak intensity of the basal planes decreases. As a result, magnesium crystals exhibit a preferred orientation, which subsequently reduces the compressive stress asymmetry [9]. In general, it reduces the nucleation and development of twins, which leads to a decrease in the ultimate strength [9]. The inclusion of nanoparticles leads to a reduction in the peak intensity of the basal planes in the ED direction, causing a weakening of the basal texture in the composite relative to pure magnesium [13]. Figures 7c and 7d show that the peak intensity of the basal planes decreases for the annealed Mg-2%SiO2 composite samples, indicating that recrystallization weakens the texture of the composites. Furthermore, the intensity of the basal plane peaks in the annealed Mg-1 wt.% SiO₂ composite samples is significantly greater than that in the annealed pure magnesium. This can be attributed to the uniform distribution of 1wt.% nanoparticles in the grain boundaries, effectively preventing grain growth during annealing. These findings demonstrate that the texture of the composites is preserved even after the annealing process.

3.3. Compression test

Figure 8 illustrates the compression stress-strain curves of pure magnesium samples after undergoing extrusion and annealing processes along the ND and ED of the samples. The curves show that the elastic response of magnesium is different along these directions, indicating its anisotropic behavior in elastic deformation. According to Tromans [22], the elastic modulus in the base planes differs from that in the prismatic and pyramidal planes for a hexagonal close-packed crystal structure. For magnesium, the elastic modulus in the base planes is 50.8 GPa, while it is 45.5 GPa in the prismatic and pyramidal planes [22]. Since the intensity of the basal planes in the ED is less than that in the prismatic planes, the elastic modulus in the ED is smaller than that in the ND. The two different behaviors of pure magnesium in these loading directions are worth noting. When the stress-strain curve is applied along the ED direction, the nucleation of the tensile twin is activated. The deformation of twins leads to a preferred crystal orientation, and the basal planes align in a perpendicular direction to the loading direction. After further loading, the deformation of a strong basal texture (parallel to the loading direction) begins at a strain of about 0.08. This strain magnitude corresponds to the maximum shear stress produced by the tensile twins. Thus, it is predicted that most grains in these samples will form a basal texture due to the tensile twins at a strain of approximately 0.08 [20, 23].

As can be seen from Fig. 8a, the loading direction parallel to the c-axis of the crystalline structure (ND) results in prevention of the slip in the basal planes. At high temperatures, pyramidal and prismatic systems can be activated, leading to the nucleation and growth of contraction twins [13, 24]. Due to the critical shear stress, the possibility of activation of the contraction twins is higher than that of the tensile ones, resulting in significant work-hardening at the beginning of the ND stress-strain curve. This work-hardening includes three regions, as reported elsewhere [23, 25]: elastic deformation, plastic deformation with activation of contraction twins, and fracture.

The stress-strain curves for pure magnesium after annealing are displayed in Fig. 8b. The X-ray diffraction patterns of pure magnesium in Fig. 7a indicate that the basal planes in the ED and ND directions have a higher peak intensity compared to other planes, signifying the texture generated in the samples' extrusion process. In contrast, the X-ray diffraction patterns of pure magnesium after the annealing process (Fig. 7a) demonstrate that the peak intensity of the basal planes has decreased in the ED and ND directions due to the texture weakening caused by the annealing process. Furthermore, Fig. 8b indicates that the samples' yield strength has decreased due to the annealing process. The stress-strain curves in Fig. 8b show that the grains increased in size during the annealing process of the samples. This caused tension twins to form when the sample was compressed. As a result, the ultimate strength of the annealed sample increased compared to the non-annealed sample [17, 23].

In Fig. 8 the curve of the ND similar to many ductile metals. However, the curve of the ED is quite different and can be divided into four regions [24, 26, 27]:

1- elastic deformation

2- plastic deformation by dislocations slip in the basal planes and tensile twin mechanisms.

3- plastic deformation with nucleation, growth and multiplication of tensile twins, interaction of dislocations with tensile twins and increase of hardening rate.

4- instability and fracture

When a load is applied along the ED direction, deformation in magnesium is initiated by the slip of dislocations on the basal planes. Based on Table 2, the critical resolved shear stress required for activating these systems is approximately 1 MPa. Therefore, deformation commences with the movement of dislocations. Subsequently, as the applied load increases, the shear stress increases, and the tensile twin mechanism comes into action. With the nucleation and growth of the tensile twins, the grains become finer, leading to an increase in the material strength according to the Hall-Petch law [17, 28].

Table 2

Room temperature critical resolved shear stress for the main deformation modes measured in single crystals of pure magnesium [28]
Deformation mode	Critical shear stress (MPa)
Basal < 𝑎 > slip	0.5-1
Prismatic < 𝑎 > slip	40–50
Pyramidal < 𝑐 + 𝑎 > slip	40–80
Tension twinning	2.4
Contraction twinning	115

Figure 9a displays a comparison of stress-strain curves between pure magnesium and nanocomposites along ND. Upon adding amorphous nanoparticles to the magnesium matrix, an enhancement in the yield strength and ductility is observed. This is attributed to the interaction between nanoparticles and dislocations, thus contributing to an increase in the strength of the nanocomposite. Additionally, the critical shear stress required to activate prismatic slip systems increases, which further strengthens the nanocomposite. In contrast, pure magnesium has a lower rate of work-hardening due to the absence of a reinforcing phase. Consequently, the improvement in the ductility of the nanocomposite can be attributed to the activation of the non-basal slip systems [13]. It is important to note that under compressive load, the dominant plastic deformation mechanism is twinning [28]. However, the addition of nanoparticles, while increasing strength, also limits the formation of twins. By adding 1wt.% of amorphous silica nanoparticles, an increase in both the yield strength and ductility is observed, while the ultimate strength decreases. Therefore, nanoparticles by being placed in the grain boundary, lead to an increase in yield strength and increase ductility while limit basal slip systems and activation of non-basal systems [29, 30].

Figure 9b shows comparison between stress-strain curves of the nanocomposites and pure magnesium samples along ED. The graph reveals that the addition of 1wt.% of amorphous nanoparticles to the magnesium matrix results in an increase in yield strength and strength within the strain range of 0.02–0.13, while the ultimate compressive strength decreases. The uniform dispersion of the nanoparticles in the microstructure during the extrusion process reduces the grain size [14]. According to Hall-Petch relationship, the yield strength increases as the grain size decreases [17, 31]. In addition, the presence of nanoparticles weakens the texture, leading to a decrease in the work-hardening rate and ultimate strength in the composite compared to the monolithic sample [13].

Figures 9c and d display how annealing affects the stress-strain response of pure magnesium and nanocomposite samples. The annealing process reduces the difference in the elastic modulus in different directions. This is due the fact that the annealing process weakens the texture [14, 24]. The Figure also indicates that the ultimate strength of the nanocomposite specimen increases after annealing. This increase may be due to the prevention of grain growth by the nanoparticles in the nanocomposites during the annealing process. As a result, the speed of the twin nucleation decreases, and the presence of nanoparticles limits the dislocation movement. [14, 32]. Both mechanisms increase the ultimate strength [33, 34]. Tables 3 and 4 list the mechanical properties of the nanocomposites and pure magnesium after extrusion and annealing, respectively. The tables show that nanocomposite specimen's yield strength, ductility, and ultimate strength have increased after the AE process and annealing.

Table 3

Mechanical properties of Mg-SiO₂ nanocomposite and pure magnesium after the AE process
Sample	Yield strength (MPa)	Ultimate compression strength (MPa)	Elongation (%)
Pure Mg (ED)	49 ± 3	260 ± 3	-
Pure Mg (ND)	25 ± 3	235 ± 4	-
Mg-1%SiO₂ (ED)	96 ± 2	240 ± 3	5
Mg-1%SiO₂ (ND)	48 ± 3	215 ± 2	45
Mg-2%SiO₂ (ED)	80 ± 3	230 ± 3	11
Mg-2%SiO₂ (ND)	46 ± 2	220 ± 3	38

Table 4

Mechanical properties of annealed Mg-SiO₂ nanocomposite and pure magnesium samples
Sample	Yield strength (MPa)	Ultimate compression strength (MPa)	Elongation (%)
Pure Mg (ED)	27 ± 3	250 ± 3	-
Pure Mg (ND)	23 ± 3	248 ± 4	-
Mg-1%SiO₂ (ED)	47 ± 2	270 ± 3	5
Mg-1%SiO₂ (ND)	42 ± 3	270 ± 2	40
Mg-2%SiO₂ (ED)	40 ± 3	230 ± 3	4
Mg-2%SiO₂ (ND)	39 ± 2	255 ± 3	25

3.4. Hardness

Numerous techniques have been proposed to enhance the mechanical properties of magnesium matrix composites. By analyzing the size and shape of the grains and the properties of the composite samples, it is possible to evaluate the effectiveness of the manufacturing process [9, 14, 35]. To assess the impact of the accumulative extrusion process on the hardness of the extruded materials, Brinell hardness was measured in the ND and TD planes for pure magnesium and nanocomposites samples. Figure 10 compares the hardness of the pure magnesium and nanocomposite samples after the extrusion and annealing processes. The hardness of the as-extruded pure magnesium increased from 35.1 Brinell to 40.6 Brinell in the Mg-2wt.%SiO₂ nanocomposite, representing a 15.7% rise in hardness. This significant increase in hardness could be attributed to the presence of uniformly distributed nanoparticles in the magnesium matrix. During the AE process, the driving force of dynamic recrystallization increases, leading to more grain refinement. Therefore, AE is a highly effective solid-state process for dispersing nanoparticles in the matrix. Furthermore, the hardness of pure magnesium increased from 28.1 Brinell after annealing to 37.5 Brinell in the Mg-2wt.%SiO₂ composite sample, indicating a 33.5% hike in hardness. This suggests that individual nanoparticles inhibited grain growth during recrystallization, leading to improved hardness.

This study employed the accumulative extrusion process to produce nanocomposites of Mg-1 wt.% SiO₂ and Mg-2wt.% SiO₂. This process entailed the dispersion of nanoparticles among the layers through multiple extrusion passes. The composites underwent several tests to determine their mechanical properties, and their microstructure was also examined. The results obtained from the mechanical and microstructural investigations were compared to draw the following conclusions:

1. After performing 14 extrusion passes, it was observed that there was no agglomerate of reinforcing particles in the microstructure of Mg-1wt.% SiO₂ composite.

2- By adding nanoparticles during the first six extrusion passes to Mg-1wt. % SiO₂, and eight subsequent passes to distribute the particles, the particle distribution within the matrix was improved.

3- The addition of 1wt.% amorphous silica nanoparticles to the magnesium matrix resulted in a 57% increase in yield strength, a 5% increase in ductility and an 8% decrease in ultimate strength along the ED. However, along ND, there was a 37% increase in yield strength, a 45% increase in ductility and a 9% decrease in ultimate strength.

4- After extrusion and annealing, the maximum increase in Brinell hardness was observed in the Mg-2wt.% SiO₂ sample with a 15% increase after extrusion and 33.5% increase after annealing.

Acknowledgments: Not Applicable

Conflicts of interest or competing interests: The authors declare they have no known competing financial interests.

Funding: The authors declare that no funds, grants, or other support were received during the preparation of this manuscript.

Data and code availability: Not Applicable

Supplementary information: Not Applicable

Ethical approval: Not Applicable

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Development of a magnesium/amorphous nano-SiO2 composite using accumulative extrusion method

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Abstract

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1. Introduction

2. Materials and methods

2.1. Materials

2.2. Manufacturing of the samples

2.3. Investigation of the samples

3. Results and discussion

3.1. Microstructure

3.2. Texture of the extruded composite

3.3. Compression test

3.4. Hardness

4. Conclusions

Declarations

References

Additional Declarations

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