
Cite this article as: | Sheng Liu, Qing Yuan, Yutong Sima, Chenxi Liu, Fang Han, and Wenwei Qiao, Wear behavior of Zn–38Al–3.5Cu–1.2Mg/SiCp composite under different stabilization treatments, Int. J. Miner. Metall. Mater., 29(2022), No. 6, pp.1270-1279. https://dx.doi.org/10.1007/s12613-020-2217-7 |
Aluminum–zinc-based alloys have desirable abrasive resistance and other various mechanical properties; however, the abrasive resistance decreases drastically under high-speed and heavy-load friction condition. The literature shows that carborundum (SiC), which contains both silicon (Si) and soft graphite (Gr), is often added to Al–Zn alloys to enhance their abrasive resistance without affecting their strength and toughness [1–4]. Several studies on the impact of SiC particles on Al–Zn alloys have been undertaken in recent years [5–7]. The α(Al,Zn) phase, representing the leading abrasive resistance phase, occupies most of the Al–Zn alloy microstructure. The abrasive resistance of the η(Al,Zn) phase is relatively weaker than that of the α(Al,Zn) phase; nevertheless, its anti-friction effect is prominent. The α and η phases are saturated at room temperature, which results in the generation of precipitates in the microstructure. Under dry friction conditions, the solubility of α and η phases in the surface microstructure of the Al–Zn alloy increases with the increase in the friction temperature, thereby stimulating the transition from the abrasive-resistant α phase and the anti-friction η phase to the soft β phase. Eventually, the Al–Zn alloy microstructure becomes unstable, resulting in poor performance during friction [7].
Previous studies have shown that the grain dimension can be refined to improve the mechanical properties of the Al–Zn–Mg and Al–Zn–Cu alloys through solid solution and aging treatments, by which these grains turn into refined equiaxed grains [8–11]. The solid solution and aging treatments are collectively known as the stabilization treatment, and studies on the effect of this treatment are evolving. Some studies [12–14] have reported the impacts of alloying elements and stabilization treatment on the Al–Zn–Mg–Cu alloy microstructure. It has been observed that the stabilization treatment affects the precipitation behavior of the metal-based solid solutions, since the precipitated and enriched areas of the hard phase in the Al–Zn–Mg–Cu alloy become enlarged through this treatment, and the uniform distribution degree of reinforced particles in the composites improves. This results in the enhanced stability of the composite microstructure [15–19].
Under the condition of long-range, high-speed, and heavy-load friction environment, Al–Zn-based composites exhibit unstable abrasive resistance owing to the aging process and friction heating effect. Some authors have explored the impacts of this treatment on the microstructure evolution of the Al–Zn-based composites. However, relevant research on the microstructure evolution and wear property of Al–Zn-based composites reinforced with nano-SiC particles is lacking. In some studies, the inhibitory effect of the nano-SiC particles on the microstructure evolution is overlooked.
In this study, Zn–38Al–3.5Cu–1.2Mg composite reinforced with nano-SiCp was fabricated via stirring-assisted ultrasonic vibration. Different stabilization treatments with different solid solutions and aging temperatures were designed to optimize the composite microstructure and mechanical properties. The effects of the stabilization treatments on the abrasive resistance of the Zn–38Al–3.5Cu–1.2Mg/SiCp composite were explored. Finally, the role of nano-SiCp in the friction behavior of the studied composite was analyzed. The presented information will guide the fabrication of Al–Zn-based composites reinforced with nano-SiCp.
The schematic for the fabrication of the Zn–38Al–3.5Cu–1.2Mg/SiCp composite is presented in Fig. 1. The prepared Al ingot was placed in a graphite crucible and later placed in the SG2-3-10 resistance furnace, where it was heated until its melting point. The zinc ingot, Cu–30Zn alloy, and Mg particles were sequentially added to the melting Al fusant. The temperature of the graphite crucible was adjusted to the pre-set values after isothermal holding. The SiC nanoparticles (100 nm) were added through the high-pressure jetting process by introducing argon (Ar) gas. The powder flux, pressure, and time were set as 0.5–1 L/min, 0.2–0.5 MPa, and 3–8 min, respectively. Argon was used to avoid unnecessary oxidation. The stirring at 300 r/min and ultrasonic vibration at 850 W power were simultaneously applied under Ar environment for 5 min. The standing of the final composite melting, slagging-off, and casting process were performed after the first 2 min of the process. Finally, the Zn–38Al–3.5Cu–1.2Mg/SiCp was successfully obtained.
The as-cast Zn–38Al–3.5Cu–1.2Mg/SiCp composite was machined into a cylindrical specimen with 10 mm in diameter and 30 mm in height. The specimens were subjected to stabilization treatment at different solid solution temperatures (360, 380, 400, and 420°C) for 6 h and different aging temperatures (160, 170, 180, and 190°C) for 48 h. Specimens without stabilization treatment were used for comparison and are denoted as “none,” while specimens treated with different stabilization treatments are separately denoted as 360-160, 380-170, 400-180, and 420-190.
Room-temperature (about 20°C) compression tests were performed on a WE-100 hydraulic universal material testing machine. Before the compression process, the two contact surfaces of the specimens were polished using 1500-grade abrasive paper to remove the surface scratch and ensure the uniformity of the specimen sides. Graphite wafers of 0.1 mm thickness were placed on the specimen contact surfaces. The displacement loading speed of the squeeze head was set to 1 mm/min. Repeated tests were conducted to achieve average values. Cylindrical specimens of ϕ8 mm × 30 mm dimensions were machined to perform the dry-friction wear test on a frictional wear testing machine. The bearing steel GCr15 was used in manufacturing the abrasive disk. The degree of surface roughness (Ra) was calculated as 6.3. The frictional pressure, friction velocity, and time were determined as 1.2 MPa, 840 r/min (11.72 m/s), and 10 min, respectively. The frictional wear rate (mm3/m) was represented by the value of volume loss (mm3) per unit sliding distance (m), and the derivative of wear rate was considered to be the wear resistance coefficient. Here, the wear resistance coefficient does not refer to the coefficient of friction. Micro-hardness tests were conducted on an HV-1000 micro-hardness tester, with a loading force of 1.961 N.
Cylindrical specimens after the dry-friction wear test were split in half lengthwise. According to the microstructure characteristic along the lengthwise direction, three areas, namely as-cast area, wear sub-area, and wear area, were designated in sequence. More information on the observations of the wear sub-area and wear area is provided in a previous study [7]. Metallographic specimens were prepared to observe the as-cast microstructure, worn surface, and sub-surface morphology of specimens treated at different processing parameters. The related metallographic preparation methods have been previously detailed [20–26]. A PHILIPXL30TMP optical microscope and a field-emission scanning electron microscope coupled with an energy-dispersive spectrometer were used for analyses. Line analysis was performed to determine the composition distribution of the SiC particles, and different phases in the fabricated composites were identified via X-ray diffraction (XRD) with copper target.
The as-cast microstructures of specimens treated via different stabilization processes are displayed in Fig. 2. The grain dimension increased with the increase in the solid solution temperature and the aging temperature. According to the XRD analysis (Fig. 3), the main phase in the specimens treated via different stabilization processes remained unchanged. The microstructure consisted of the Al-rich α(Al,Zn) phase with a face-centered cubic structure, Zn-rich β(Al,Zn) phase with a face-centered cubic structure, Zn-rich η(Al,Zn) phase with a close-packed hexagonal structure, ε(Cu,Zn) phase with a close-packed hexagonal structure, and reinforcement-phase nano-SiCp. The XRD peaks of SiCp were accompanied by the α(Al,Zn) and η(Al,Zn) phases, indicating that the nano-SiCp was located around and in both phases. Owing to their small amount, some of the phases are not labeled in Fig. 3, and these phases resulted in some feeble peaks. Magnesium aluminate (MgAl2O4) with a spinel structure was not detected in the “none” specimen. With the increase in the stabilization temperature, the MgAl2O4 phase disappeared. A similar phenomenon was also observed in the Al4C3 phase. The appearance of Al4C3 suggests an interfacial reaction between the nano-SiCp and the metal matrix. The increased solubility of the α(Al,Zn) and η(Al,Zn) phase makes the C and Si occur as nano-SiCp, and consequently, the interfacial reaction becomes restrained with the increasing stabilization temperature.
With the increase in the stabilization temperature, the α(Al,Zn) phase first turned into a long irregular strip (Fig. 2(b)) and then transformed into diffused and small grains (Fig. 2(c)). However, as shown in Fig. 2(d), with a higher solid solution temperature of 400°C and aging temperature of 180°C, the (Al,Zn) phase exhibited apparent coarsening. Most of the α(Al,Zn) phase gets distributed into an irregular rectangle shape. Coarsening is quite obvious in the specimen treated by solid solution at 420°C and aging at 190°C (Fig. 2(e)); the α(Al,Zn) phase presented an irregular thick banding and reticular structure, which is different from the observations for the other specimens.
Fig. 4 presents the friction wear rates under different loading forces of the specimens treated via different stabilization processes and the related morphologies of friction surface under a loading force of 1.41 MPa. The data in Fig. 4(a) show that the friction wear rate increased with the increase in the loading force. This was because the coefficient of friction linearly increased with the loading force, making sliding friction difficult to occur, and the specimen surface can be easily scratched and peeled off under a larger normal stress; thus, the volume loss per unit time increased. In addition, the change rule of the friction wear rate in the specimens treated via different stabilization processes under different loading forces remained consistent. The friction wear rate in specimen 360-160 was lower than that in the “none” specimen, indicating the enhanced abrasive resistance after the 360°C solid solution treatment and 160°C aging process. The nano-SiCp is the hard phase that provides the fractional abrasive resistance. The stabilization process accelerates the nano-SiCp precipitation. Hence, the increased nano-SiCp can primarily explain the improved abrasive resistance in specimen 360-160. Moreover, nano-SiCp restrained the breaking of the soft phase, thereby contributing to the improved abrasive resistance behavior of the Zn–38Al–3.5Cu–1.2Mg alloy composites. Regarding the morphology of the friction surface, the surface morphology of the “none” specimen presented erratic scratches along the friction direction. The surface of specimen 360-160 was rougher than that of the “none” specimen, as the surface morphology consisted of smooth broad plow marks and an adhesive layer. Moreover, some pits also occurred in their surface morphology. With the further increase in the stabilization treatment temperature, the friction wear rate decreased to be 0.8 × 10−2 mm3/m in specimen 380-170. Regardless of the loading force, the friction wear rate of specimen 380-170 was the lowest among all specimens, which may be due to the reduced grain dimension and size of the wearable α(Al,Zn) phase (Fig. 2(c)). The intrinsic origin is the reinforced SiCp, which was distributed along the grain boundaries of the α(Al,Zn) phase and was wrapped by the grains, leading to a decrease in the grain dimension of the as-cast microstructures. The data also prove that a solid solution temperature of 380°C and an aging temperature of 170°C were optimum for the stabilization process. The flat friction surface of specimen 380-170 featured some fine abrasives accompanied by some relatively shallow plow marks. However, the number of these shallow plow marks was the lowest among all the specimens. Moreover, the improvement effect of the abrasive resistance increased with the loading force, as determined from the slope variation in the red rectangular frame of Fig. 4(a). With the increase in the stabilization temperature for specimen 400-180, the friction wear rate increased, which is associated with the microstructure evolution depicted in Fig. 2(d). Although the amount of nano-SiCp increased, the as-cast microstructure of specimen 400-180 coarsened due to the larger dimension of the α(Al,Zn) phase compared with that in specimen 380-170. The friction wear rate of specimen 420-190 was lower than that of specimen 400-180. Considering the increased nano-SiCp and the coarse α(Al,Zn) phase, the increased abrasive resistance may be related to the reticular-structured α(Al,Zn) phase. Furthermore, relatively shallow plow marks compared with those in specimen 400-180 were observed in the specimen 420-190 surface. Specimen 400-180 exhibited the worst abrasive resistance, as its number and depth of plow marks were the maximum, indicating a rugged and miry surface.
The displayed friction wear behavior (Fig. 4) is also related to the microstructure evolution in the sub-surface. Fig. 5 shows the friction morphologies of the sub-surface of the studied specimens under loading forces of 0.84, 1.12, and 1.41 MPa. With the increase in the stabilization temperature, the wearable α(Al,Zn) phase transformed from a small dendrite structure (in the “none” specimen) into long irregular strips (specimen 360-160) and then small grains (specimen 380-170). With further increase in the stabilization temperature, the apparent reticular-structured α(Al,Zn) phase became thicker (specimen 420-190). In addition to the evolution of the α(Al,Zn) phase, the number and distribution of other phases such as the β(Al,Zn) phase, η(Al,Zn) phase, and ε(Cu,Zn) phase also changed. Moreover, remarkable microstructure evolution occurred in the “none” specimen with the increase in the loading force from 0.84 to 1.41 MPa: the amount of the α(Al,Zn) phase decreased, while that of the soft β(Al,Zn) phase increased. However, in the other specimens treated through the stabilization process, almost no microstructure evolution was observed with the increase in the loading force. The microstructure evolution is linked with the interior temperature variation. As mentioned above, the stabilization process facilitates the precipitation of the nano-SiCp. The heat generated during the dry friction wear test in the frictional wear cross-sections quickly diffuses, followed by the coarsening of the microstructure in the alloy matrix. However, nano-SiCp is super hard and has impressive thermal diffusivity, which helps to effectively improve the heat loss of the wear surface and stabilize the wear-resistant phase of the composite matrix. Hence, the temperature rise in the specimens treated via stabilization is relatively gentler than that in the “none” specimen; as a result, almost no microstructure evolution occurred in the specimens treated via stabilization. These observations also prove that the stabilization process improved the abrasive resistance of the Zn–38Al–3.5Cu–1.2Mg/SiCp composite under high-speed and heavy-load conditions.
The range of temperature rise during the dry friction test was restricted to 260°C. Therefore, multiple micro-hardness tests at different friction temperatures were performed, as described earlier [4,7]. Fig. 6 depicts the micro-hardness change in the friction surface of all specimens. Specimens 380-170 and 400-180 exhibited the most outstanding and the worst micro-hardness, respectively. The micro-hardness of the stabilization specimens gradually increased with the increasing friction temperature, except for specimen 400-180. The increased micro-hardness at 255°C for specimen 380-170 also reflects the increased abrasive resistance of the Zn–38Al–3.5Cu–1.2Mg/SiCp composite under the high-speed and heavy-load conditions. The increased micro-hardness was a result of the increase in the amount of nano-SiCp, which can lead to effective heat transition and abrasive resistance. The microstructure evolution from the wearable α(Al,Zn) phase to the soft β(Al,Zn) phase was restrained. In the “none” specimen, the decreased micro-hardness was responsible for the unstable microstructure under the high friction temperature. The erratic micro-hardness in specimen 400-180 is related to its coarsening grain dimension.
Fig. 7 displays the corresponding compression fracture morphologies of the stabilization specimens. Specimen 360-160 presented a shear fracture mechanism involving a smooth fracture in a particular direction. Also, many apparent and dense dimples occurred in specimen 380-170, indicating a ductile fracture behavior. These dimples were fewer than those in specimen 400-180. The fracture in specimen 400-180 was uneven, and some secondary cracks occurred in the fracture of specimen 400-180. Specimen 420-190 exhibited a combination of ductile and cleavage fracture, in which the tearing peaks were quite noticeable. The observed morphology in the specimens agrees with their abrasive resistance. As a result, the optimal stabilization treatment is solution treatment at 380°C and aging at 170°C.
Fig. 8 compares the distributions of nano-SiCp in the specimen without stabilization and specimen 380-170, as determined through area scanning analysis. Many nano-SiCp clusters were detected in the specimen without stabilization, and the number of nano-SiCp clusters in specimen 380-170 was significantly lower. Fig. 7 demonstrates that the stabilization treatment facilitated the dispersed distribution of the nano-SiCp. The enhanced abrasive resistance caused by the stabilization treatment is also connected to the dispersed distribution of nano-SiCp. The related description of the importance of the dispersed distribution of nano-SiCp has been described in an earlier study [4,7].
Fig. 9 displays the corresponding distribution of nano-SiCp clusters in the specimen without stabilization and specimen 380-170, as obtained via line scanning analysis. The nano-SiCp cluster in the specimen without stabilization featured a larger size than that in specimen 380-170. Fig. 8 presents a similar result. The larger-sized nano-SiCp cluster was primarily the result of the incomplete dispersion of the nano-SiCp. This was because the nano-SiCp had poor miscibility in the metal melt. Although the high-pressure jetting process was conducted to prepare the as-cast composite, the possibility of the nano-SiCp agglomeration cannot be eliminated. From the line scanning results of these two specimens, the chemical compositions of the large-size nano-SiCp cluster closely overlapped with the main α(Al,Zn) and η(Al,Zn) phase. However, a clear demarcation existed in the small-size nano-SiCp cluster of specimen 380-170.
Fig. 10 displays the fracture morphology of frictional wear for the specimen without stabilization and specimen 380-170. Interconnected cracks occurred in the specimen without stabilization along with visibly long straight shape. Large-size cracks were generated at the end of the fine cracks. Only a few fuzzy cracks were observed in specimen 380-170. Moreover, the number of cracks in specimen 380-170 was significantly less than that in the specimen without stabilization.
The crack initiation and propagation are connected with the nano-SiCp. Fig. 11 describes the crack formation mechanism in the studied composite, indicating the two primary origins. The small-size SiCp clusters are highly susceptible to become the crack initiation origin because of the micro-hardness difference between the hard SiCp phase and the relatively soft β phase. Under the effect of external load, the stress in the composite will transmit from the soft β phase to the hard SiCp phase under the effect of the external load. The hard SiCp phase bears the primary stress. Nevertheless, the deformation coordination ability between the hard SiCp phase and the soft β phase is insufficient, which results in local stress concentration and consequently void generation and crack evolution [27]. The transfer enhancement effect of the load is good under the optimum combination of the Zn−Al metal matrix and the SiCp phase. The classical shear-lag theory satisfactorily explains the mechanism for the transfer enhancement effect [28]. However, due to the coexistence of the plastic deformation behavior and shear fracture behavior in the friction wear of the studied composite, the optimized shear-lag model [29−30] was used to clarify the effects of the transitive stress in the composite during the friction wear test:
σload=σm[Vp(s+4)4+Vm]+ϕ(s) | (1) |
where
In summary, the aforementioned data reveal that the stabilization treatment optimized the dispersion effect of the nano-SiCp and increased its amount in the composite. The existence of the nano-SiCp further restrained the microstructure evolution from the hard α(Al,Zn) phase to the soft β(Al,Zn) phase during the friction wear condition. Additionally, the stabilization treatment suppressed the crack initiation and propagation. Also, the increased amount of nano-SiCp refined the grain dimension and provided abrasive resistance. Eventually, the stabilization treatment enhanced the abrasive resistance of the Zn–38Al–3.5Cu–1.2Mg/SiCp composite. The stabilization treatment must be optimized to refine the grain dimension and size of the wearable α(Al,Zn) phase. In the investigated Zn–38Al–3.5Cu–1.2Mg/SiCp composite, the optimal stabilization treatment was solution treatment at 380°C for 6 h and aging at 170°C for 48 h, in which the friction wear rate was decreased to 0.8 × 10−2 mm3/m.
(1) The optimal stabilization treatment for the 38Al–3.5Cu–1.2Mg/SiCp composite was solution treatment at 380°C for 6 h and aging at 170°C for 48 h, which could decrease the friction wear rate to the minimum of 0.8 × 10−2 mm3/m.
(2) The stabilization treatment facilitated the formation of dispersive and homogeneous nano-SiCp, whereby the grain dimension was refined, and the abrasive resistance was improved.
(3) Owing to its impressive heat diffusivity, the nano-SiCp further restrained the microstructure evolution from the hard α(Al,Zn) phase to the soft β(Al,Zn) phase during the friction wear condition.
(4) The nano-SiCp with different sizes became the crack origin. The stabilization treatment suppressed the crack initiation and propagation in the friction wear process.
This work was financially supported by the National Natural Science Foundation of China (No. 52004193), the National Training Programs of Innovation and Entrepreneurship for Undergraduates (No. 202110488004), the Guidance Programs of Science and Technology Research for Hubei Provincial Department of Education (No. B2020008), the National Defence Pre-research Foundation of Wuhan Univesity of Science and Technology (No. GF202006), the Post-doctoral Innovative Research Post of Hubei Province, China, and the Post-doctoral Research Funding Program of Jiangsu Province, China.
The authors declare no conflict of interest.
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