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Article

Development of High-Performance SiCp/Al-Si Composites by Equal Channel Angular Pressing

by
Qiong Xu
1,2,
Aibin Ma
1,3,*,
Junjie Wang
1,
Jiapeng Sun
1,
Jinghua Jiang
1,
Yuhua Li
1,3 and
Chaoying Ni
2,*
1
College of Mechanics and Materials, Hohai University, Nanjing 211100, China
2
Department of Materials Science and Engineering, University of Delaware, Newark, DE 19716, USA
3
Suqian Institute of Hohai University, Suqian 223800, China
*
Authors to whom correspondence should be addressed.
Metals 2018, 8(10), 738; https://doi.org/10.3390/met8100738
Submission received: 15 August 2018 / Revised: 6 September 2018 / Accepted: 19 September 2018 / Published: 20 September 2018
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Abstract

:
Relatively low compactness and unsatisfactory uniformity of reinforced particles severely restrict the performance and widespread industry applications of the powder metallurgy (PM) metal matrix composites (MMCs). Here, we developed a combined processing route of PM and equal channel angular pressing (ECAP) to enhance the mechanical properties and wear resistance of the SiCp/Al-Si composite. The results indicate that ECAP significantly refined the matrix grains, eliminated pores and promoted the uniformity of the reinforcement particles. After 8p-ECAP, the SiCp/Al-Si composite consisted of ultrafine Al matrix grains (600 nm) modified by uniformly-dispersed Si and SiCp particles, and the composite relative density approached 100%. The hardness and wear resistance of the 8p-ECAP SiCp/Al-Si composite were markedly improved compared to the PM composite. More ECAP passes continued a trend of improvement for the wear resistance and hardness. Moreover, while abrasion and delamination dominated the wear of PM composites, less severe adhesive wear and fatigue mechanisms played more important roles in the wear of PM-ECAP composites. This study demonstrates a new approach to designing wear-resistant Al-MMCs and is readily applicable to other Al-MMCs.

1. Introduction

Aluminum metal matrix composites (Al-MMCs) are increasingly used in automobiles, high-speed trains, subways and airplanes due to their low density, high specific strength, low coefficient of thermal expansion and cost effectiveness [1,2,3,4,5,6]. Over the past few decades, several methods have been developed to prepare Al-MMCs, such as stir casting [7,8,9,10], powder metallurgy [11,12,13,14] and pressure infiltration [15,16]. However, flawless and uniform Al-MMCs are still difficult to achieve, which severely restricts their property advantage and industry applications [1,17].
Severe plastic deformation (SPD) has been successfully used to optimize the microstructure and thus to improve the mechanical and tribological properties of MMCs. The SPD process can effectively refine the matrix grains, eliminate pores and make uniform the secondary phases and particles so as to empower the MMCs with superior properties [18,19,20,21]. In Sabbaghianrad and Langdon’s work [19], significant grain refinement and superplasticity were achieved in an Al-7075 alloy reinforced with 10 vol.% Al2O3 particulates processed by high-pressure torsion (HPT). Reihanian et al. [21] prepared a nanostructured Al/SiC-graphite composite by accumulative roll bonding (ARB) and showed that a homogeneous ultra-fine grain structure and uniform distribution of particles could be obtained by eight ARB cycles. Haghighi et al. [18] revealed that the Al-5 vol.% nano-Al2O3 composite consolidated by equal channel angular pressing (ECAP) possessed higher mechanical properties and hardness. In addition, twist extrusion (TE), as a potent tool for obtaining advanced engineering materials, can be used to improve the mechanical and tribological properties of MMCs [22,23].
The tribological property is crucial to components sustaining wear. As important wear-resistant materials, Al-MMSs have been employed for vehicle discs. The optimized microstructure, especially the refined matrix grains, and improved mechanical properties of Al-MMCs by SPD lead to enhanced wear resistance. It was suggested that through the grain refinement, the wear-resistance of MMCs and some alloys can be improved to follow a linear relation with the d−0.5 (d is the average grain size), resembling the Hall–Petch effect [24,25,26,27]. However, there have been very limited reports in the literature dealing with the wear behavior of SPD-MMCs up to date, and among a few publications, there were conflicting results reported. Haghighi et al. [18,28] compared the Al-MMCs processed by ECAP or conventional extrusion and concluded that the ECAP samples possessed better wear resistance than the extruded counterparts. The improved wear resistance was attributed to pore elimination, homogeneity of the particle distribution and grain refinement by the ECAP. Similarly, enhanced wear resistance of Al-MMCs by ARB was reported by Darmiani [29]. However, decreased wear resistance was also reported by Jamaati et al. [26], who revealed that the wear resistance of ARB Al-MMCs decreased with the increasing number of ARB cycles. Karamıs et al. [30] indicated that no systematic relationship was observed between the wear loss and pass number of the reciprocating extrusion.
We developed a combined processing route of PM and ECAP to enhance the mechanical properties and wear resistance of the SiCp/Al-Si composite. The as-processed SiCp/Al-Si composite exhibited improved wear resistance and high hardness. Moreover, an effort was made to clarify the microstructure evolution and to understand the mechanism of the improvement of mechanical properties and wear resistance. This work demonstrates a new approach to designing wear-resistant Al-MMCs and other hard particulate reinforced light alloy composites.

2. Materials and Methods

2.1. Raw Materials

Commercial pure Al powders (Sinopharm Chemical Reagent Co., Ltd, Shanghai, China), Si particles (Xuzhou Lingyun Silicon Industry Co. Ltd., Jiangsu, China) and SiCp (Aladdin Industrial Corporation, Shanghai, China) were used in this experiment. The sizes of the raw powders were analyzed with scanning electron microscope (SEM), as shown in Figure 1. The average size of Al powders, Si powders (≥99.5 wt.%) and SiCp (≥99.0 wt.%) was about 100 μm, 5 μm and 0.5–0.7 μm, respectively. The chemical composition of Al powder is listed in Table 1.

2.2. Composite Fabrication and Processing

The SiCp/Al-Si composites were consolidated by PM and further processed by ECAP, as illustrated in Figure 2. Firstly, the Al powders with 10 wt.% Si and 8 wt.% SiCp were mixed with an SFM-2 planetary mixer for 100 h under 20 r/min. The premixed powders were compressed using a cold pressing die to form a prefabricated sample. The compaction pressure, which has a significant influence on the compactness and properties of the final composite [31], was chosen to be 305 MP, which gives rise to a large apparent density of 2.56–2.58 g cm−3. Then, the cold pressed specimens buried by graphite were sintered in a furnace at 873 K for 4 h. Finally, the PM samples were processed using a home-made rotary die for ECAP (RD-ECAP) with 90° channel intersection, the operation principle of which can be found in our earlier work [32,33,34,35,36]. The PM samples were pressed for 0, 4 and 8 ECAP passes (marked as PM-0p-ECAP, PM-4p-ECAP and PM-8p-ECAP) with a velocity of 0.5 mm/s at 703 K. Prior to ECAP, cubic PM samples (20 mm × 20 mm × 40 mm) were put into the ECAP die, and they were held at 703 K for 15 min before pressing. This RD-ECAP procedure was proven to be very effective to obtain ultrafine-grained microstructure in several materials [33,34,37,38,39]. Graphite was used as a lubricant to reduce the friction between the billet and the inner wall of the die. Preliminary examination did not reveal any cracks in the pressed billets.

2.3. Microstructure Characterization

The microstructure observations were performed by an optical microscope (OM, Olympus BX51M, Shinjuku, Tokyo, Japan), a focused ion beam and field emission scanning electron microscope (FIB/FE-SEM, Auriga 60, Zeiss, Oberkochen, Germany) and a field emission transmission electron microscope (TEM, JEM-2010F, JOEL, Akishima, Japan) operating at 200 kV. Samples for OM and SEM analysis were prepared via grinding with SiC abrasive papers and polishing with an Al2O3 suspension solution and diamond solutions of different abrasive sizes (6 μm, 3 μm, 1 μm and 0.3 μm). The TEM foil was mechanically polished to about 20 micrometers and further thinned via ion milling with a precision ion polishing system (PIPS, Model 691, Gatan, Pleasanton, CA, USA). To examine the microstructure of matrix/reinforcement interfaces, the Zeiss Auriga 60 FIB/FE-SEM was used for the preparation of the TEM foils (5 µm × 2 µm × <0.1 µm) from the feature of interest.
Sample density was measured by the Archimedes method using distilled water. The Vickers microhardness was measured with an applied load of 50 g for 15 s using an HXD-1000TC microhardness testing instrument (Shanghai Taiming Optical Instrument Co. LTD, Shanghai, China). The average value from ten test points was used.

2.4. Wear Test

A reciprocating wear test was carried out using a ball-on-disc dry sliding method. The abrasive spheres were made of AISI 52100 steel with HRC hardness of 64 and a diameter of 15 mm (Rockwell hardness is an index determined by plastic deformation depth measured with a diamond cone indenter under a load of 150 Kg). Before the test, the disc samples were ground with a 1500 # SiC abrasive paper and washed and rinsed in alcohol. The applied load was chosen to be 5 N, 10 N, 15 N, 20 N and 25 N respectively at a sliding speed of 10 mm/s for 20 min. After the test, the samples were cleaned and weighted. The mass loss was used to determine the wear rate based on the equation w = m/L, where w is the wear rate, m is the mass loss and L is the sliding distance, and the wear rate was averaged over at least 3 measurements. The wear surface was analyzed by SEM.

3. Results and Discussion

3.1. Microstructure

Figure 3a shows the optical micrograph of the PM SiCp/Al-Si composites with 10 wt.% Si and 8 wt.% SiCp. The grain boundaries of Al matrix were well defined. Typically, the Al matrix appeared heterogeneous, and the average grain size of Al was ~25 µm, measured by the linear intercept method. The distribution of Si particles was fairly uniform, and there was no segregation of Si particles observed. It is noticeable that there were Si particles imbedded within the Al matrix. In contrast, the SiCp dispersed around the Al grains, and there were some distinct particle agglomerations. The SiCp agglomeration was also observed in other SiCp/Al composites, consistent with the conventional notion that with decreasing size of the reinforcement particles, it becomes more difficult to homogeneously distribute these secondary phases in the metal matrix [40,41,42,43]. XRD analysis in Figure 4 indicates no detectible extra phases generated during the fabrication.
The optical images of the PM composites pressed by 4p-ECAP and 8p-ECAP indicate that the grains of the Al matrix were notably refined and the reinforced phases uniformly distributed as the ECAP passes increased. Notably, the PM-8p-ECAP sample exhibited a uniform microstructure, and its grain boundaries were not well defined, but rather poorly delineated, giving rise to fine and ultrafine grains.
Figure 5 shows the SEM image of the PM-8p-ECAP composite. The fine SiCp was largely dispersed uniformly in the Al matrix, but some segregated SiCp clusters were visible around the rather large (50–200 um) Al regions, as shown in Figure 5a. On the other hand, the fine Si particles were well separated by Al, one from the other, and some Si particles were broken into smaller pieces (Figure 5b). The strong flow of the ductile Al phase during ECAP offered the equally good opportunity for hard SiC and Si particles to be separated and surrounded by Al. Therefore, this observed difference in dispersion of SiC and Si particles resulted from the difference in the energies of the initial Si/Si and SiC/SiC grain boundaries and the forming interphase boundaries Si/Al and SiC/Al. The well-dispersed Si particles indicate that the Si/Al interface had relatively low energy and possessed a perfect structure, as characterized by subsequent TEM observation. This observation is also related to the complete and incomplete wetting of grain boundaries by the liquid or second solid phase [44,45].
Ultrafine grains of a few hundred nanometers were readily observed by TEM in the Al matrix of PM-8p-ECAP composite, as shown in Figure 6. The grain boundaries were relatively poorly defined with irregularly-shaped curves in contrast to the well-defined grain boundaries observed in pure Al [46,47], and the grain size reduction was significantly higher than those reported in previous studies. For example, Paydar et al. [48] used ECAP to consolidate Al particles and decreased the grain size from 45 μm to 11.5 μm in the parallel section. Zare et al. [49] achieved a fine grain size (about 1 μm) in the carbon nanotube-reinforced aluminum matrix composites synthesized via 8p-ECAP. Ramu and Bauri [50] reduced the grain size of Al-5 vol.% SiCp MMC to 8 μm by 2p-ECAP. These results suggest that ECAP of the PM SiCp/Al-Si composites can result in a better microstructure through the formation of ultrafine matrix grains. This positive effect is attributed partially to the inclusion of SiCp particles with adequate volume fraction, size and shape in addition to the sample fabrication and processing specifics. An improved dispersion of the reinforcements was also observed, including those of the original SiCp and newly-formed particles.
Figure 7 shows representative TEM images of a typical Si/Al interface and its surrounding environment in the PM-8p-ECAP composite. The interface between a Si particle and the Al matrix appeared delineated (Figure 7a), and the Si grain was surrounded by some ultrafine Al grains or grains with significant defects (Figure 7a,b). These fine Al grains were possibly formed due to severe deformation and probably also dynamic recrystallization activated by the strain and also fine Si precipitates through a particle-stimulated nucleation (PSN) mechanism [51]. Moreover, the relatively clean interface suggests that interfacial reaction between Al and Si was not favored thermodynamically in the processing condition. Figure 7c displays a high-resolution TEM image of the Al-Si interface. The lattice spacing of Si and Al was measured as 0.327 nm and 0.234 nm, respectively, corresponding to their (111) planes [52]. The curved interface between Si and Al (red dash line) suggests a physical bonding occurred without visible defects, voids or precipitates. Such an interfacial region may also benefit the mechanical properties of the composite [53,54,55].

3.2. Relative Density

The relative densities of the PM and PM-ECAP composites compared to their theoretical densities are shown in Figure 8. The relative density of PM composites was 0.9, indicating 10% porosity. Notably, the relative density of PM-ECAP composites was much higher than that of PM composites, and it monotonously increased with the increase of ECAP passes. Almost 100% densification was achieved for the PM-8p-ECAP composites after 8 ECAP passes. This demonstrates that the ECAP process can effectively reduce defects and improve the microstructure of the SiCp/Al-Si composites.

3.3. Hardness

Figure 9 shows the Vickers hardness measurements. A considerable enhancement in the microhardness occurred after ECAP, and it increased monotonously with the increase of ECAP passes. Compared with the PM composite, we ascribe the improved hardness of the PM-ECAP composite to the compound effects of the ultra-fine-grain Al matrix, the reduced defects and porosity, as well as the improved morphology and distribution of the reinforcement particles, which gives rise to enhanced dispersion strengthening. A similar fine-grain hardening was reported by Eizadjou et al. [56]. The reduced defects and porosity can improve the deformation resistance, and thus enhance the hardness. However, the dispersion strengthening was still the main strengthening mechanism compared with the Al metals.

3.4. Wear Behavior

The wear rate as a function of applied load and ECAP passes is shown in Figure 10. The wear rate of the PM-ECAP composites decreased with the increase of ECAP passes. The PM-8p-ECAP SiCp/Al-Si composite exhibited an optimal wear resistance with lower wear rates of 0.075 mg/m at 25 N and 0.033 mg/m at 5 N, respectively.
Figure 11 shows the typical SEM images of the wear surfaces of PM and PM-ECAP composites at an applied load of 15 N. Obvious ploughing and cracks were visible on the wear surface of the PM composite (Figure 11a). The main wear mechanisms appeared to be abrasion and delamination, resulting in surface deformation and damage in the form of deep grooves along the sliding direction. In contrast, the wear surfaces of the PM-4p-ECAP and PM-8p-ECAP samples were relatively smooth. For PM-8p-ECAP samples, no cracks, ploughing or pits were visible (Figure 11b,c). Minor adhesive wear and fatigue wear appeared to be the dominant mechanisms for the EACP composite samples. It appears that the improved morphology and distribution of reinforcement particles, grain refinement and associated hardness and density enhancement contributed synergistically to the wear resistance. Collectively, they shifted the wear of the PM-ECAP composites towards relatively benign mechanisms.

4. Conclusions

In this study, we developed a combined processing route of PM and ECAP to enhance the mechanical properties and wear resistance of the SiCp/Al-Si composite. Compared with single processing, PM combined with ECAP can achieve an optimized microstructure, effectively eliminate pores and significantly improve the wear resistance and other mechanical behaviors of the SiCp/Al-Si composites.
(a)
ECAP significantly refines the matrix grains and makes uniform the reinforced particle. After 8p-ECAP, the ultrafine Al matrix grains (~600 nm) were obtained, together with uniformly-dispersed nanoscale Si and SiCp.
(b)
The hardness and density of the SiCp/Al-Si composite were improved by ECAP, and both increased monotonously with increasing ECAP passes. The maximum hardness reached HV = 94, and almost 100% densification was obtained for the PM-8p-ECAP composites. The ECAP can effectively eliminate pores formed in the PM process.
(c)
The wear resistance of PM-ECAP SiCp/Al-Si composite was markedly improved compared to PM composite. The wear resistance increased linearly with the ECAP passes. The abrasion and delamination accounted for the wear for the PM composites, while fatigue wear, together with a light adhesive wear were the main wear mechanisms for the PM-ECAP composites.
This work provides a new approach and practical guidance on designing wear-resistant Al-MMCs, and the technique is readily applicable to other MMCs with similar reinforcements and/or matrices.

Author Contributions

A.M. and J.J. conceived of and designed the experiments. Q.X. and J.W. performed the experiments and analyzed the data. Y.L. contributed to the materials processing. Q.X. wrote the paper. J.S. and C.N. revised the paper. All authors have discussed the results and read and approved the final manuscript.

Acknowledgement

The study was supported by the Postgraduate Research & Practice Innovation Program of Jiangsu Province of China (Grant No. KYLX16_0701), the Fundamental Research Funds for the Central Universities (Grant No. HHU2016B45314 & 2018B48414), the Natural Science Foundation of Jiangsu Province (Grant No. BK20160867), the Key Research and Development Project of Jiangsu Province of China (Grant No. BE2017148) and the Public Science & Technology Service Platform Program of Suqian City of China (Grant No. M201614). Q.X. is grateful for the support from the China Scholarship Council and the W. M. Keck Center for Advanced Microscopy and Microanalysis at the University of Delaware.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. SEM of the raw powders: (a) Al, (b) Si, (c) SiCp.
Figure 1. SEM of the raw powders: (a) Al, (b) Si, (c) SiCp.
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Figure 2. Schematic of the material preparation.
Figure 2. Schematic of the material preparation.
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Figure 3. Optical images of the composites: (a) PM (referred to as zero pass (0p)-ECAP), (b) PM-4p-ECAP and (c) PM-8p-ECAP.
Figure 3. Optical images of the composites: (a) PM (referred to as zero pass (0p)-ECAP), (b) PM-4p-ECAP and (c) PM-8p-ECAP.
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Figure 4. XRD of the PM SiCp/Al-Si composite.
Figure 4. XRD of the PM SiCp/Al-Si composite.
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Figure 5. SEM images of the PM-8p-ECAP composite: (a) low and (b) high magnification.
Figure 5. SEM images of the PM-8p-ECAP composite: (a) low and (b) high magnification.
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Figure 6. TEM image of the PM-8p-ECAP composite.
Figure 6. TEM image of the PM-8p-ECAP composite.
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Figure 7. TEM micrographs of the Si/Al interface of the PM-8p-ECAP composite: (a) low magnification, (b) high magnification of Region A (yellow square in (a)) and (c) Region B (red square in (a)).
Figure 7. TEM micrographs of the Si/Al interface of the PM-8p-ECAP composite: (a) low magnification, (b) high magnification of Region A (yellow square in (a)) and (c) Region B (red square in (a)).
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Figure 8. Influence of the ECAP passes on the relative density of SiCp/Al-Si composites. The 0p-ECAP sample corresponds to the PM composite without ECAP processing.
Figure 8. Influence of the ECAP passes on the relative density of SiCp/Al-Si composites. The 0p-ECAP sample corresponds to the PM composite without ECAP processing.
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Figure 9. Influence of the ECAP passes on the microhardness of SiCp/Al-Si composites. The 0p-ECAP sample corresponds to the PM composite without ECAP processing.
Figure 9. Influence of the ECAP passes on the microhardness of SiCp/Al-Si composites. The 0p-ECAP sample corresponds to the PM composite without ECAP processing.
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Figure 10. The wear rate of the SiCp/Al-Si composite with different ECAP passes under the dry friction condition (sliding speed is 10 mm/s; loads are 5 N, 10 N, 15 N, 20 N and 25 N). The 0p-ECAP sample corresponds to PM composite.
Figure 10. The wear rate of the SiCp/Al-Si composite with different ECAP passes under the dry friction condition (sliding speed is 10 mm/s; loads are 5 N, 10 N, 15 N, 20 N and 25 N). The 0p-ECAP sample corresponds to PM composite.
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Figure 11. Surface morphology of the composite under the dry friction condition (sliding speed is 10 mm/s; load is 15 N): (a) PM, (b) PM-4p-ECAP and (c) PM-8p-ECAP.
Figure 11. Surface morphology of the composite under the dry friction condition (sliding speed is 10 mm/s; load is 15 N): (a) PM, (b) PM-4p-ECAP and (c) PM-8p-ECAP.
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Table
Table 1. Chemical composition of aluminum powder (weight fraction: wt.%).
Table 1. Chemical composition of aluminum powder (weight fraction: wt.%).
FeCuSiAl
≤0.2≤0.015≤0.2≥99.0

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MDPI and ACS Style

Xu, Q.; Ma, A.; Wang, J.; Sun, J.; Jiang, J.; Li, Y.; Ni, C. Development of High-Performance SiCp/Al-Si Composites by Equal Channel Angular Pressing. Metals 2018, 8, 738. https://doi.org/10.3390/met8100738

AMA Style

Xu Q, Ma A, Wang J, Sun J, Jiang J, Li Y, Ni C. Development of High-Performance SiCp/Al-Si Composites by Equal Channel Angular Pressing. Metals. 2018; 8(10):738. https://doi.org/10.3390/met8100738

Chicago/Turabian Style

Xu, Qiong, Aibin Ma, Junjie Wang, Jiapeng Sun, Jinghua Jiang, Yuhua Li, and Chaoying Ni. 2018. "Development of High-Performance SiCp/Al-Si Composites by Equal Channel Angular Pressing" Metals 8, no. 10: 738. https://doi.org/10.3390/met8100738

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