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Journal of Materials Processing Technology 168 (2005) 262269

Process optimisation for a squeeze cast magnesium alloy metal matrix composite
M.S. Yong a, , A.J. Clegg b
b a Singapore Institute of Manufacturing Technology, 71 Nanyang Drive, Singapore 638075, Singapore Wolfson School of Mechanical and Manufacturing Engineering, Loughborough University, Loughborough, Leicestershire LE11 3TU, UK

Received 5 January 2004; received in revised form 5 January 2004; accepted 27 January 2005

Abstract The paper reports the inuence of process variables on a zirconium-free (RZ5DF) magnesium alloy metal matrix composite (MMC) containing 14 vol.% Safl bres. The squeeze casting process was used to produce the composites and the process variables evaluated were applied pressure, from 0.1 MPa to 120 MPa, and preform temperature from 250 C to 750 C. The principal ndings from this research were that a minimum applied pressure of 60 MPa is necessary to eliminate porosity and that applied pressures greater than 100 MPa cause bre clustering and breakage. The optimum applied pressure was established to be 80 MPa. It was also established that to ensure successful preform inltration a preform temperature of 600 C or above was necessary. For the optimum combination of a preform preheat temperature of 600 C and an applied pressure of 80 MPa, an UTS of 259 MPa was obtained for the composite. This represented an increase of 30% compared to the UTS for the squeeze cast base alloy. 2005 Elsevier B.V. All rights reserved.
Keywords: Magnesium alloys; Squeeze casting; Metal matrix composites; Mechanical properties

1. Introduction Metal matrix composite (MMC) components can be manufactured by several methods. The metal casting route is especially attractive in terms of its ability to produce complex near net shapes. However, castings produced by conventional casting processes may contain gas and/or shrinkage porosity. The tendency for porosity formation will be exacerbated when bres are introduced because they tend to restrict the ow of molten metal and cause even greater gas entrapment within the casting. It is pointless to use bres to reinforce a casting if defects are present, since the addition of bres will not compensate for poor metallurgical integrity. In order to full the potential of bre reinforcement and produce pore free castings the squeeze casting process can be selected. The unique feature of this process is that metal is pressurised throughout solidication. This prevents the formation of gas and shrinkage porosity and produces a metallurgically sound casting.

Corresponding author. E-mail address: msyong@simtech.a-star.edu.sg (M.S. Yong).

Selection of this process is also based on its suitability for mass production, ease of fabrication and its consistency in producing high quality composite parts. With the development of MMCs, magnesium alloys can better meet the various demands of diverse applications. The addition of reinforcement to magnesium alloy produces superior mechanical properties [13] and good thermal stability [4,5]. Of the various composite types, the discontinuous and randomly oriented bre-reinforced composites provide the best value to strength ratio. Despite the potential advantage of using magnesium MMC for lightweight and high strength applications, little is known about the inuence of squeeze inltration parameters. Key parameters, such as applied pressure and preform temperature must be optimised, especially for the squeeze inltration of a magnesiumzinc MMC. These process parameters were researched and the results are presented in this paper. However, it was rst necessary to select appropriate bres and binders since their selection is fundamental to the success of the MMC. The main criterion determining the selection of bre type is compatibility with the matrix. Two

0924-0136/$ see front matter 2005 Elsevier B.V. All rights reserved. doi:10.1016/j.jmatprotec.2005.01.012

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bre types that are known to be compatible with magnesium are Safl and carbon [6]. Silica and alumina-based binders are widely used in preform production, mainly due to their high temperature properties [7]. However, there are concerns about chemical reactions between magnesium alloys and silica [8]. To ensure full inltration of liquid metal into the bre preform, researchers [911] have emphasised the importance of preheating the preforms. However, there has been little research to determine optimum preform temperature for magnesium alloys and that reported has focused on AZ91 (magnesiumaluminium) alloy. The wetting capability of these alloys is different, for instance the wetting and the interfacial reaction between Al2 O3 reinforcement and cerium, lanthanum (both rare earth elements) or magnesium is far better in comparison to aluminium. Most work on applied pressure has focused on aluminium alloys and their composites. However, Ha [12] and Chadwick [13] investigated the inuence of applied pressure on the short freezing range MgAl family of alloys. The effect on solidication will inevitably be different for long freezing range alloys, such as the MgZn family alloys that are the focus of this research. The difference in solidication morphology will be signicant when inltrating the melt into a porous bre preform. Long freezing range alloys retain a liquid phase over a longer period during inltration and this may promote better inltration, reduce voids and consequently improve the soundness of the composite.

alloy is in the fully molten state). These experiments were conducted at three applied pressures: 60 MPa, 80 MPa and 100 MPa. The mechanical properties were evaluated using tensile and hardness tests. These tests were complemented by optical microscopy and, for the tensile fracture surfaces, SEM. 2.1. Test casting The test casting was a rectangular plate of 126 mm in length, 75 mm in width and 16 mm in depth. 2.2. Melt processing The alloy was melted in an electric resistance furnace using a steel crucible, the uxless method and an argon gas cover. The die was coated with boron nitride suspended in water to protect it from excessive wear. 2.3. Tensile testing Tensile tests were conducted on a 50 kN Mayes testing machine using position control. Modied test specimens were machined according to BS18 (1987) and magnesium Elektron Ltd RB4 specications [16]. 2.4. Hardness testing Hardness was measured to determine and study the inuence of reinforcement on the magnesium and the isotropy of bre distribution. The locations of hardness measurements are shown in Fig. 1. Hardness measurements were conducted using the Rockwell B scale for both the alloys and composites. The preference for the Rockwell rather than Vickers hardness measurement was due to the larger indentation needed to ensure a more consistent measurement on the composite. The area of the Vickers hardness indentation is so small that, in some cases, the measurement could be taken from the hard bre causing large variations in hardness values.

2. Experimental methodology A zirconium-free magnesium4.2% zinc1%-rare earths alloy, designated RZ5DF, was used for this research. Several bre preform materials, proportions and binder systems, were evaluated to determine their compatibility with the magnesium alloys and the mechanical properties that they delivered to the composite [14]. This preliminary research established that a compopsite based on a silica-bonded, 14 vol.% Safl bre preform delivered the best characteristics in terms of ease of production and maximum value to strength ratio. The effect of applied pressure, between 0.1 MPa and 120 MPa, on the RZ5DF-14 vol.% Safl bre composite was rst evaluated. The maximum permissible applied pressure was limited by both the capability of the squeeze casting press and die design. The metal pouring temperature was maintained at 750 C, the die temperature at 250 C, the duration of applied pressure at 25 s, and delay before application of pressure at 4 s. These conditions replicated those employed for the base alloy that was reported previously [15]. Following this, the inuence of preform temperature was evaluated for a restricted range of applied pressures. Four preform temperatures were selected: 250 C (similar to the die temperature), 400 C (intermediate temperature), 600 C (at which temperature the RZ5DF alloy is a mixture of liquid and solid), and 750 C (at which temperature the RZ5DF

Fig. 1. Locations of hardness measurements (each dot represents the position of a hardness measurement) taken in both Longitudinal and Transverse directions.

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2.5. Metallography An optical microscope and stereoscan 360 electrom microscope (SEM) were used to examine the microstructure of the MMC specimens. Metallographic samples were prepared using standard techniques and were etched using an acetic picral solution. The electron microscope was equipped with a back-scatter detector and was used to characterise fracture surfaces from the tensile test specimens. 2.6. Cell size The cell size was established using the intersection method. Five areas were selected at random and 21 measurements of cell size were taken for each area. The average value for the 105 readings was determined.

Fig. 3. The average material hardness along the longitudinal and transverse direction of the squeeze inltrated RZ5DF alloy with 14 vol.% fraction Safl bres, cast with constant pouring temperature of 750 C and die temperature of 250 C.

3. Results and observations The results are reported in the sequence in which the experiments were conducted. In the rst series of experiments, the effect of applied pressure was evaluated. In the second series, the combined inuences of applied pressure and preform preheat temperature were evaluated. 3.1. Series 1 experiments: the inuence of applied pressure 3.1.1. Tensile properties The effect of applied pressure on UTS and ductility of squeeze cast, RZ5DF-14 vol.%, Safl bre composites is shown in Fig. 2. It can be seen that the highest UTS value was obtained with an applied pressure of 80 MPa. It would appear from the gure that a pressure in excess of 40 MPa is essential to develop a signicant improvement in UTS but that levels above 80 MPa have a detrimental effect. 3.1.2. Hardness The hardness values along the longitudinal and transverse directions of the composite castings produced at different

applied pressures are shown graphically in Fig. 3. Whilst the dominating inuence on hardness is provided by the presence of the Safl bres, the results show that the hardness at the two lowest levels of applied pressure (0.1 MPa and 20 MPa) is distinctly lower than that associated with applied pressure levels of 40 MPa and above. 3.1.3. Metallography Metallography was conducted to examine the inuence of applied pressure on the cast structure. Selected optical microstructures are presented in Fig. 4. The metallographic examination identied the presence of microporosity in those samples produced with applied pressures below 60 MPa. The microporosity, as expected, occurred mainly at cell boundaries and was most easily conrmed by adjusting the depth of eld. It also identied the tendency for bre clustering and fracture at applied pressures greater than 80 MPa. The presence of fractured bres is demonstrated more clearly in the SEM micrographs shown in Fig. 5. These micrographs show fractured bres in the plane transverse to that of load application during the tensile test. 3.2. Series 2 experiments: the inuence of preform temperature The preliminary experiments showed that the optimum applied pressure was 80 MPa. However, to ensure robustness in the experimentation, the effects of preform preheat temperature were evaluated for the optimum applied pressure and pressures of 60 MPa and 100 MPa. 3.2.1. Tensile tests The effects of preform temperature and applied pressure on UTS are summarised in Fig. 6. The results show that a preform preheat temperature of 750 C produced the most consistent UTS values across the range of applied pressures

Fig. 2. The effects of squeeze inltration applied pressure on the tensile properties of the RZ5DF matrix with 14 vol.% fraction Safl bres.

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Fig. 4. Optical microstructure of squeeze inltrated RZ5DF-14 vol.% fraction Safl bres produced under (i) atmospheric pressure, 0.1 MPa, applied pressure of (ii) 20 MPa, (iii) 40 MPa, (iv) 60 MPa, (v) 80 MPa, (vi) 100 MPa and (vii) 120 MPa.

and that the maximum UTS of 259 MPa was obtained with a preform temperature of 600 C and an applied pressure of 80 MPa. These results conrm the status of 80 MPa as the optimum value of applied pressure.

3.2.2. Hardness The results of the hardness tests are shown in Fig. 7. The greatest variation in hardness was demonstrated by the test casting produced with the lowest value of applied pressure

Fig. 5. SEM micrograph of the fracture face of a squeeze inltrated RZ5DF-14 vol.% fraction Safl bres produced under applied pressure of (i) 100 MPa and (ii) 120 MPa.

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3.2.3. Metallography Metallographic examination of the composite structures showed that more densely packed bres occurred at the preform surface at the lowest preform temperature. This effect is illustrated in Fig. 8. The sequence of microstructures show that preform deformation and bre clustering were less evident at higher preform temperatures. The SEM micrographs of tensile fracture surfaces, Fig. 9, conrm the clustering of bres and provide evidence of bre to bre contact, for the preheat temperature of 400 C. This effect was not evident for the preheat temperature of 600 C.
Fig. 6. The plot of UTS for RZ5DF-14 vol.% Safl MMC produced from various combinations of applied pressure and preform temperature.

4. Discussion (60 MPa) and preform temperature of 400 C. The range of variation was 8 HRB compared to 6 HRB observed for the other combinations of preform temperature and applied pressure. To achieve the successful inltration of a bre preform the liquid metal must penetrate the preform completely. Potential barriers to this are presented by: the density of the preform, which can be represented by the preform permeability [14];

Fig. 7. The average material hardness along the longitudinal and transverse direction of the squeeze inltrated RZ5DF alloy with 14 vol.% fraction Safl bres produced under different combinations of preform temperatures and applied pressures.

Fig. 8. A micrograph taken at the preform inltration region of a squeeze inltrated specimen produced with a preform temperature of (i) 750 C, (ii) 600 C, (iii) 400 C and (iv) 250 C.

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an insufcient pressure head, necessary to displace the air and overcome resistances to metal ow; and/or a low preform temperature that promotes premature solidication of the solid before complete inltration. Increasing either the applied pressure or the preform preheat temperature, independently or in combination, may improve inltration. However, there may be adverse consequences. Too high a level of applied pressure may physically damage the preform through compression. This leads to compacted preforms that resist inltration together with bre clustering and bre breakage that reduce the bres effectiveness for strengthening the matrix. Although researchers [11,17,18] have resorted to high preform temperatures to achieve inltration, this too can have adverse effects. For example, an increased heat content in the system may retard solidication. This in turn extends the time during which there is the opportunity for adverse interfacial reactions to occur between the alloy and bres. Furthermore, an extended period of solidication can promote the formation of larger cell sizes that in turn impair the mechanical properties. The inuence of applied pressure is quite clearly demonstrated in Fig. 2. The gure can be divided into three distinct regions: <60 MPa, 6190 MPa, >91 MPa. The rst of these regions is associated with the presence of porosity and voids in the castings and this porosity is associated with low UTS values. As the applied pressure is increased the porosity is eliminated and the composite develops its optimum UTS of 259 MPa at an applied pressure of 80 MPa. Thereafter, an increase in applied pressure produces bre clustering and breakage leading to more initiation points for fracture and so the UTS declines. The tensile evidence is supported by evidence from hardness tests and metallography. The presence of porosity, revealed in Fig. 4, adversely affects the hardness of the castings. Quite simply, low levels of applied pressure are not sufcient to either suppress porosity formation or completely inltrate the bre preform. It is interesting to note that the optimum applied pressure level of 80 MPa for the composite is 20 MPa higher than that necessary to develop the highest level of strength in the bre-free base alloy [15]. Metallographic examination revealed that preform deformation and bre clustering was less evident and bres were less densely packed at the surfaces of the preforms preheated to 600 C or 750 C (see Fig. 8) when compared with 400 C and 250 C.

It was found that the highest preform temperature (750 C) produced the most consistent UTS values over the range of applied pressures considered. This preform temperature is above the liquidus temperature of the alloy. It would, therefore, be expected that inltration of the preform would not be impeded by the early onset of solidication of the alloy on the bre preforms. The preform temperature of 600 C produced a higher variation in UTS than was observed for the 750 C preform preheat temperature. However, the highest value of UTS of all the experiments was produced with this preheat temperature in combination with an applied pressure of 80 MPa. A preform temperature of 750 C supported a wider range of applied pressure because, even at the lowest level of 60 MPa, there was a minimal resistance to inltration. It was also noted that there was less variation in bre distribution. An even distribution of bres was also evident in the specimens produced at a preheat temperature of 600 C, see Fig. 9. This temperature is 33 C below the alloys liquidus temperature. Although inltration was not a problem, it can be postulated that solidication would occur quite quickly under these conditions. This postulation is supported by microstructural evidence and cell size measurements, see Fig. 8, that show a smaller cell size, associated with better UTS, in the samples produced with a preform temperature of 600 C. With preheat temperatures of 400 C and, especially, 250 C the UTS values are generally poor and there is clear evidence of ineffective inltration. The microstructural evidence clearly shows that preform deformation, bre clustering and bre breakage is evident to varying degrees. However, such effects were not uniform and produced inconsistent effects. For example, for the combination of 400 C and 60 MPa applied pressure, microstructural evaluation, see Fig. 10, revealed a high concentration of bres in the centre of the inltrated preform. This effect was caused by two factors. Firstly, the low preform preheat temperature promoted rapid solidication of the alloy prior to the application of pressure at both the preform surface and at locations near to the die wall. Secondly, the low applied pressure resulted in irregular and curtailed inltration. In consequence, the applied pressure compacts rather than inltrates the preform. This produces inltrated regions that have a higher concentration of bres and

Fig. 9. SEM micrograph of the fracture face of a squeeze inltrated RZ5DF-14 vol.% Safl MMC produced with (i) 400 C and (ii) 600 C preform temperature.

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Fig. 10. Microstructure showing different parts of the squeeze inltrated RZ5DF-14 vol.% fraction Safl specimen produced with a preform temperature of 400 C and applied pressure of 60 MPa. The sequence is (i) top, (ii) centre and (iii) bottom portion of the fabricated composite.

this can produce higher values of UTS, see Fig. 10. However, the effect is inconsistent and therefore undesirable. Hardness measurements also conrmed the inconsistency. For example, the specimen produced with 60 MPa and 400 C preheat demonstrated the greatest variation in hardness, see Fig. 7, and this was attributable to the central clustering of bres. Examination of the fracture surface of the specimen produced with a preform temperature of 400 C and an applied pressure of 80 MPa clearly shows the bres in contact with one another, see Fig. 9. 4.1. The inuence of zinc Alloying magnesium with 4.2% of the lower melting point metal zinc produces a binary alloy that has a long freezing range. Experimentation [16] determined the values of the liquidus and solidus of the RZ5DF alloy to be 633 C and 474 C, respectively, a freezing range of 159 C. Although long freezing range alloys are the most prone to shrinkage porosity, this problem is overcome by squeeze casting. The long freezing range may in fact be benecial in the production of a composite since the extended period during which a liquid phase is present may promote inltration. The presence of zinc may also be signicant for the preform preheat temperature. The results show that the optimum UTS of 259 MPa was obtained with a preform temperature of 600 C, a temperature just 33 C below the alloys liquidus temperature. Cell size measurements revealed that specimens produced at this preheat temperature had a smaller average cell size, typically 30 m, see Fig. 8. For specimens produced with preheat temperatures of 750 C, 400 C and 250 C the average cell size was >50 m. This variation can be explained by consideration of the nucleation and growth sequence in the various specimens. The high preform preheat temperature retards the rate of solidication because time is necessary for the heat of the preform to be transferred through the alloy to the die. Nucleating cells have time to grow. Conversely, at low preheat temperatures of 400 C and 250 C, the alloy solidies

quickly in contact with the relatively cold bres. The rst solid formed is rich in the primary phase and the remaining liquid becomes richer in the low melting point eutectic. Although primary phase still forms by nucleation and growth in the inter-bre regions, the number of cells formed is reduced and their size is larger.

5. Conclusions 1. The optimum applied pressure for the squeeze casting of RZ5DF-14 vol.% Safl bre composites was determined to be 80 MPa. At applied pressures below 60 MPa, microporosity was not suppressed. Conversely, a high applied pressure of 100 MPa or above causes bre clustering and breakage and a concomitant reduction in UTS. 2. The optimum preform preheat temperature was established to be 600 C. At this temperature consistent bre inltration was achieved and the optimum cell size of 30 m was obtained in the matrix. 3. The optimum combination of applied pressure and preform preheat temperature was determined to be 80 MPa and 600 C, respectively. For this combination, a UTS value of 259 MPa was obtained. The composite delivered a 30% increase in UTS compared with that developed in the squeeze cast base alloy.

Acknowledgements Dr. Yong gratefully acknowledges the receipt of an Overseas Research Students Award and a Loughborough University Research Studentship.

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