Ablation of Hybrid Metal Matrix Composites
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Ablation of Hybrid Metal Matrix Composites
Paper 11-057.pdf, Page 1 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA Ablation of Hybrid Metal Matrix Composites D. Weiss Eck Industries, Manitowoc, WI J. Grassi Alotech LLC Ltd., Brooklyn, OH B. Schultz, P. Rohatgi University of Wisconsin-Milwaukee, Milwaukee, WI Copyright 2011 American Foundry Society ABSTRACT Ablation is a process in which an alloy is solidified using a core package that the liquid alloy resides or is “suspended” within, while a liquid or gas and combinations thereof remove the core while simultaneously facilitating a rapid heat removal to cause solidification of the alloy. This method has been successfully used for monolithic alloys to get higher solidification rates to improve mechanical properties. This paper describes the early development of ablation casting for MMC’s and the mechanical properties of an Al-SiC-C hybrid composite alloy. The microstructures and mechanical properties of ablation cast Al-10SiC-4Ni graphite have been characterized and compared with conventionally sand cast composites. The effects of ablation casting on dendrite size and particle distribution have been characterized along with its effect on tensile strength. graphite in the Al-SiC alloy made it much more machinable and wear resistant due to the presence of the graphite. Moreover, in addition to improved strength and wear behavior the Al-SiC-C (graphite) castings have a lower density than Al-SiC castings due to the presence of graphite. In the ablation process3, 4 the core package is made using a proprietary binder and, shortly after the alloy is poured, an ablation media is directed to the core surface. The ablation media dissociates the binder and “erodes” the silica sand cores enabling the ablation media solvent to come in direct contact with the liquid alloy thereby removing the latent heat of solidification with high cooling rates. Figure 1 illustrates the process in the casting of an aluminum A356 steering knuckle.4. Key Words: Ablation Casting, Hybrid Metal Matrix Composite, Aluminum, Silicon Carbide, Graphite INTRODUCTION Al-SiC alloys have been used as brake rotors in several automobiles including the Lotus Elise, the Chrysler Prowler, the General Motors EV-1, and several other cars made in Japan and Europe. The Al-SiC composite brake rotors have also been investigated for use in railway applications.1 However, the manufacture of Al-SiC brake rotors for high volume applications using conventional silica sand casting may present problems due to the settling of the silicon carbide particles. The particles are heavier than molten aluminum, and there are difficulties in machining due to high hardness of the silicon carbide particles. In view of this, Rohatgi et al.2 have developed hybrid composites incorporating both silicon carbide and graphite particles in the matrix of aluminum alloys. The simultaneous presence of heavier SiC particles and lighter graphite particles resulted in a buoyancy neutral composite melt where the SiC and graphite particles tend to remain in suspension during casting. This is due to the mutual hinderance they place on their respective movement through the melt. In addition, the presence of (a) (b) Fig. 1 a) Beginning of ablation casting process, where ablation solvent erodes the surface of the core package b) Solidified stearing knuckle with sand cores removed by the ablation solvent.4 Paper 11-057.pdf, Page 2 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA The ablation solvent progressively moves from one end of the casting to the other resulting in rapid unidirectional solidification. Heavy sections, where solidification is slower, typically show higher rates of cooling when ablated. These characteristics of ablation are expected to lead to a much more refined microstructure, especially in the case of the interdendritic eutectic3, and a uniform distribution of reinforcement particles. The degree to which the ablation casting process is able to reduce the dendrite cell size and to increase solidification rate in relation to other casting processes is presented schematically in Figure 2. A comparison of relative properties of monolithic A356 alloy resulting from the various casting methods is given in Table 1. the trade as 10S4G, and consists of 10 vol% SiC and 4 vol% Ni coated graphite in AA359 alloy2. EXPERIMENTAL METHODS A plate shaped pattern was constructed suitable for both conventional sand casting and ablation. The dimensions of the cast plate were 20.32 cm (8 in) wide by 40.64 cm (16 in) long. The section thickness on the left side of the plate casting shown in Figure 3 is 6.35 cm (2.5 in) and the right side is 3.81 cm (1.5 in). The total casting weight was 11.6 kg (25.6 lbs) The model, showing placement and scale of the risers and runners is shown in Figure 3. The gating for the conventional casting was fully modeled using MAGMA software so that the effects of turbulence could be minimized. The results of modeling indicated that the gating and riser system were adequate to prevent shrinkage defects in the casting, as shown in Figure 3, and, therefore, the same riser and gating system was used for both conventional and the ablation processes. It is possible that the increased cooling rates and thermal gradients realized through the ablation process may lead to changes in the gating/risering requirements, and this may be explored in future work. Fig. 2 Ablation cooling rates and dendrite cell size compared to other conventional casting methods. Table 1 Comparison of Mechanical Properties of A356 Alloy Aluminum Cast by Various Methods 3 Property Sand Squeeze cast 312 (45) Ablation 228 (33) Perm. Mold 262 (38) UTS MPa (ksi) Y.S. MPa (ksi) %El 179 (26) 207 (30) 243 (35) 261 (38) 3.5 4 11.0 12.5 325 (47) During the solidification of a discontinuously reinforced metal matrix composite, the solidifying alloy will interact with the particulate reinforcement to either push the particles into the last freezing, interdendritic regions, or to engulf them in the solidified dendrites. This tendency is a natural hindrance to the goal of achieving a uniform dispersion of reinforcements in cast MMCs. In order to improve the dispersion of micron size particles in the MMC, the solidification rate must be high enough either to promote engulfment of the particles or to refine the dendritic microstructure or both. Ablation has the potential to increase the solidification rate and to, therefore, improve the dispersion of the particulate reinforcement in the finished casting. In this work, hybrid Al-SiC-graphite composites were conventionally cast and then produced by ablation to study the effect of this process on the matrix microstructure and dispersion of the reinforcement in the composite as well as the resulting mechanical properties. The composite used is known in Fig. 3. Results of casting simulation, showing the location of shrinkage in the casting with the current gating and riser system. The initial work involved the molding and pouring of the composite in conventional sand molds. Mechanical properties were developed for these pieces followed by pouring and mechanical property determination of the ablated components. After mixing the alloy for 30 minutes, the melt was hand poured into the static molds using steel ladle(s) at the same rate and at a pouring temperature of 732 C (1350 F). Figure 4 shows the assembled mold for the conventionally cast plate. The height of the pouring cup was increased to compensate for the increased viscosity of the composite melt. Cast iron chills were used at select locations to ensure a sound casting and polyurethane no bake binder was used in preparation of the mold. Paper 11-057.pdf, Page 3 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA (a) (b) Fig. 4. a) Conventional sand cast mold ready for pouring. b) Pouring of the first casting. Ablation was carried out using identical molds in appearance but using the Alotech/DeVenne inorganic binder formulated for ablation. The overall dimensions of the mold between the conventional cast and ablation component were the same; however, the cope portion of the mold for the ablation process was modified as follows: 1) Approximately 6 in. of sand was removed directly above the casting to increase the rate of ablation at this location, 2) A channel was cut at the edge of the cope to allow water to drain from the mold cavity. Use of the soluble binder allowed for ablation of the mold via solvent jets. The solvent jets were turned on sequentially from the thinnest sections to the thickest sections of the casting (or from the right side to the left side of the piece shown in Figure 3). The temperature of the solvent ablating the mold was maintained at ambient conditions. Figure 5 shows the final cast product produced by conventional casting. Note the evidence of high melt turbulence shown near the ingate of the casting. Fig. 5. Conventionally cast product The conventionally cast and ablated castings were solutionized at 538 C (1000 F) for 12 hours followed by hot water quenching at 60C (140F) and then aged at 155 C (310 F) for 5 hours. Samples sectioned from the thin walled section of the castings were sent to Rio Tinto Alcan and to the University of Wisconsin-Milwaukee for evaluation. At least eight samples from each casting were tensile tested according to ASTM Standard B557. Sections from the conventional casting and ablated component were cold mounted in epoxy resin and metallographically polished. Optical characterization was carried out using an optical microscope coupled with an image analysis system. The volume percentage of phases was determined using an image analysis routine to determine the area percentage of phases relative to the field area based on the size, shape and gray threshold of the respective phases over at least 10 fields. It should be noted that the phases are assumed equiaxed in this analysis, which may not be the case for all phases present. The polished specimens, as well as of the fracture surfaces examined via scanning electron microscope with Energy dispersive X-ray spectroscopy (EDS) capability. RESULTS The microstructure of the conventionally cast and ablation product (hereafter referred to as “conventional” and “ablated” respectively) hybrid 10S4G MMC were characterized as containing a dispersion of ~84 µm (0.003 in) graphite platelets, and ~15 µm (0.0006 in) SiC particles. The particles were found only at the boundaries of dendrites within interdendritic/intercellular regions. In addition, present in the cast microstructure were silicon and nickel intermetallics that were identified by SEM/EDS. In addition to these general features, the samples from both conventional casting and ablation casting techniques had porosity defects. The microstructure of the composite was significantly affected by the increased solidification rate achieved by the ablation. Figure 6 shows the microstructure of the conventional casting and ablated component. It is clear from the figures that the graphite and SiC particles (labeled in Figure 6a) in the ablated sample have a higher volume fraction and are more evenly dispersed than those found in the conventional casting. The volume percent of the graphite in the conventional sample and ablated sample was ~ 4 v% and ~ 7 v% respectively. Likewise, the volume percent of SiC found in the conventional sample and ablated sample was 11 v% and 25 v% respectively. It should be noted that the graphite particles are in the form of flakes and thus the total volume percent of graphite will be lower than reported. The dendrite arm spacing (DAS) was reduced via the ablation process. In the case of the ablated sample, the DAS/cell size was 50.3 µm (0.00198 in), compared to the DAS of the conventionally cast specimen of 62.5 µm (0.00246 in). Assuming that the dendrite arm spacing is proportional to the square root of the solidification time, the ablation casting process resulted in a 35% decrease in solidification time compared to the conventional sand casting process in the location where microscopy was performed. Paper 11-057.pdf, Page 4 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA SiC particles SiC particles α-Aluminum dendrite Reinforcement poor region (a) Graphite (a) Intermetallics Porosity (b) (b) Fig. 6. a) Conventionally cast composite. SiC is found in large clusters among in the interdendritic regions. Large graphite flakes are also visible b) Ablation composite sample. The SiC and graphite particles are more evenly distributed in the microstructure (with a higher volume fraction than found in the conventionally cast sample). Both the conventionally cast and ablation specimens exhibited a significant amount of porosity due to shrinkage and entrapment of gas. Figure 7 a-c show microstructures containing porosity in the conventional and ablated samples. Close examination, of the gas pores shows that they are lined with SiC particles. The increased viscosity of the metal matrix composite melt often prevents entrapped gas bubbles from leaving the liquid melt, and thus the particles can stabilize the bubble within the suspension. Also evident from Figure 7(a) is a large, reinforcement poor region where few, if any, reinforcement particles are present due to the movement of particles during low solidification rates. The presence of such regions can reduce the overall strength of the composite material. Such reinforcement poor regions were not observed in the ablated samples. (c) Fig. 7. a) Microstructure of the conventionally cast composite showing shrinkage type pores in lower left hand side of the micrograph, b) microstructure of the ablation specimen showing round gas pores, c) Gas bubble in the modified sample that has been stabilized by SiC particles. Chemical analysis of the surface by means of EDS showed bright intermetallics among the SiC particles as can be seen in Figure 8. Dot mapping of the surface shown reveals the presence of Ni in the blocky intermetallic, and not at the interface between the large graphite particle centered in the view. This is as a result of the dissolution of Ni from the surface of the graphite particles into the alloy melt and its reaction with molten aluminum to form intermetallics. Also, present were needle like eutectic Si. It was observed that the intermetallics in the ablated specimen were finer in size than those found in the conventionally cast specimen. Paper 11-057.pdf, Page 5 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA Table 2. Comparison between the Properties of the Ablated Component and Conventional Casting. SiC particles Intermetallics (a) C (b) Al (c) Si Ni (d) (e) Fig. 8 a) SEM micrograph of conventionally cast sample and EDS dot mapping showing presence of b) graphite, c) Al, d) Si and e) Ni. Tensile testing was performed on samples taken from the thin section of the cast plate, and Table 2 presents the ultimate tensile strength and percentage elongation for the conventional casting and ablated component. The tensile strength of the conventionally cast specimen was 217 MPa (31.5 ksi), and the tensile strength of the ablated specimen was on average 249 MPa (36.1 ksi). The average percentage elongation of the conventional and ablated specimens was .38 and .33% respectively. Conventional casting Tensile # 30.6 1 30.7 2 30.3 3 31.2 4 31.2 5 34.1 6 32.5 7 33.2 8 30 9 31.2 10 Mean 31.5 St Dev. 1.34 %E 0.35 0.35 0.25 0.4 0.45 0.45 0.4 0.4 0.35 0.4 0.38% 0.06 Ablation component Tensile # 38.4 1 41 2 31.6 3 37 4 35.7 5 36 6 33.2 7 35.6 8 Mean 36.1 %E 0.35 0.4 0.3 0.25 0.4 0.3 0.3 0.3 0.33% St. Dev. 2.91 0.05 The fracture surfaces are shown in Figure 10. The surfaces were very similar in character, with evidence of brittle fracture at intermetallics, and particulate reinforcement exposed and protruding from the surface. Shrinkage pores were found in the fracture surface of the conventionally cast specimen, and likewise, gas pores were found in the surface of the ablated specimen that likely contributed to failure. Paper 11-057.pdf, Page 6 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA ablation component compared to the thin section of the conventional casting could be from the casting process, if metal is ladled from the top, middle, or bottom of the melt charge. The increased percentage of reinforcement in the thin section of the ablation component may have partly contributed to the higher strength of the ablated samples. Future work will need to be undertaken in ablation to examine the effect of solidification in varying thicknesses, cooling rates, particle dispersion, and mixing/holding time of the melt on the distribution of particles in the solidification microstructure. (a) (b) Fig. 9 a) Shrinkage porosity (dendrite) in fracture surface of the conventionally cast sample, b) gas pore found in the fracture surface of the ablated cast sample. Note: interior wall of the gas pore has features corresponding to the SiC particles that stabilized it in the casting. DISCUSSION Examination of the microstructure of both the conventional casting and the ablated component revealed the presence of SiC and graphite particles at cell or dendrite boundaries. This is evidence that both the particulate reinforcements including silicon carbide and graphite were pushed by growing αAluminum dendrites into the solute rich last freezing zones. The increased volume percentage of reinforcement in the ablated sample was likely due to the increased solidification rate, and decreased floatation or settling of the reinforcement. As the microstructure is more cellular in the ablated specimen, reinforcement particles were trapped in a tight network of cell boundaries thus increasing the local concentrations of reinforcement, and reducing the average interparticle spacing. In addition to this, it is known that although the combination of SiC and graphite particles in the liquid aluminum results in a near neutrally buoyant suspension, there is some settling and flotation that occurs over time when melting a large batch. If the melt is insufficiently mixed, the reinforcements can migrate resulting in areas that are rich in either SiC or graphite. This can result in rather large differences in the volume percentage of reinforcement in the solidified microstructure2. It is possible that the increase in reinforcement volume percent in the thin section of the In addition to improving the distribution of particles in the casting, ablation has appeared to refine the dendritic cell size. This is in contrast to published earlier reports in a monolithic A356 alloy, 3,4 where the microstructural refinement was process limited only in the eutectic silicon formation. The particulate reinforcement within the liquid melt during solidification may act to restrict the dendrite cell size while they are pushed by the solidifying α-Aluminum. With the increased cooling rates caused by the impingement of solvent on the solidifying surface, the particles are entrapped more rapidly without time to migrate substantially, resulting in increased branching of the dendrites and a finer cell size over all. It should be noted that finer intermetallics due to the solidification of interdendritic solute rich liquid were also found in the ablated sample. Nickel intermetallics, not commonly found in the unreinforced alloy, were formed due to the dissolution of the nickel coating on the graphite into the matrix. The samples showed relatively high levels of porosity, even in the case of the ablation component. In the case of the ablation component, gas porosity was observed which is likely due to poor gating design and filling system that was not designed or optimized for ablation, but rather, the conventional casting, which aided feeding for the cast product. The pouring technique and the mold geometry should be modified significantly for ablation in the future work since the time delay to remove the mold was rather significant in duration. Despite this porosity, the strength of the ablated sample was higher than that of the conventionally cast sample, and further improvement in the mechanical properties may be realized by improving the pouring technique to reduce turbulence in the melt. CONCLUSION 1. 2. Ablation of composites has shown to increase the yield strength of hybrid Al-SiC-graphite composite by 20% over conventional heavily chilled sand casting. Further improvements are possible, through higher cooling rates and a reduction in porosity. The percent elongations of ablated components were similar to conventional castings despite the higher strength of ablated castings. The microstructure of ablated samples exhibit four distinct phases: SiC particles, graphite platelets, αaluminum dendrites, and Si eutectic second phase. In addition, some porosity was also present. Paper 11-057.pdf, Page 7 of 7 AFS Proceedings 2011 © American Foundry Society, Schaumburg, IL USA 3. 4. 5. 6. The average particle size of the SiC was 15 microns. The graphite platelet size was 84 microns. The SiC and graphite particles were present in the interdendritic regions along with eutectic silicon. The dispersion of reinforcements is more uniform in the ablated sample than in the conventionally cast sample. The DAS/cell size of the ablated specimen was 50.3 µm (0.00198 in), compared to the DAS of the conventionally cast specimen of 62.5 µm (0.00246 in). In addition to the refinement of the α-Aluminum phase, the eutectic silicon and nickel intermetallics also were refined by the ablation process. The fracture surface of each sample exhibits predominantly brittle characteristics, with evidence of graphite flakes, shrinkage pores and gas pores at the surface, which may have contributed to the initiation of failure. ACKNOWLEDGMENTS The work presented in this publication was funded through the SBIR program: W56HZV-08-0067. Work at UW-Milwaukee is funded through the US-Army Tank and Automotive Command (TACOM): W56HZV-08-C0716. REFERENCES 1. 2. 3. 4. http://mmc-assess.tuwien.ac.at/mmc/Article296.html Rohatgi, P.K., “Casting Characteristics of Hybrid (Al/SiC/Gr) Composites,” AFS Transactions, vol. 19, pp.191-197 (1998). Grassi, J., U.S. Patent No. US 2008/0041499A1 (Feb. 21, 2008). Grassi, J., “Ablation Casting,” Aluminum Alloys: Fabrication, Characterization and Applications, TMS, (2008).