The eect of processing on the mechanical properties and interfacial
strength of aluminium/TiC MMCs
A.R. Kennedy*, S.M. Wyatt Department of Materials Engineering and Materials Design, University of Nottingham, Nottingham NG7 2RD, UK Received 28 May 1999; received in revised form 1 August 1999; accepted 9 August 1999 Abstract The microstructure and mechanical properties of aluminium/TiC MMCs made by powder processing (PM), by a ux-casting process, and by melting PM material, have been compared. Particle clustering is more prevalent in cast than in PM composites, but the grain-rening nature of TiC particles signicantly reduces the degree of clustering commonly observed in cast MMCs. Melting PM material enables oxide lms to `trawl' the particles into large clusters. The stiness and ductility are similar for cast and the PM composites but melting the PM material results in signicant reductions in strength and ductility. In all cases, composite ductility is enhanced by extrusion through the removal of porosity and the break-up of particle clusters. Modulus measurements as a function of plastic strain indicate that rates of damage accumulation are lowest, and hence interfacial bonding is strongest, in cast compo- sites as a result of the attainment of intimate contact and strong chemical bonding between the two phases. #2000 Elsevier Science Ltd. All rights reserved. Keywords: A. Metal-matrix composites (MMCs); B. Mechanical properties; B. Interfacial strength; B. Microstructure; Processing 1. Introduction The nature of the technique used to fabricate particle- reinforced metal-matrix composites (MMCs) has been shown to have a signicant eect on the product's mechanical properties and hence the applications for which it is suitable [14]. Composite products manu- factured by power metallurgy (PM) are mainly targeted for use as structural components. Cast composites, on the other hand, are mainly considered as replacements for conventional materials in non-critical, wear resistant applications. The breakthrough of MMCs into large volume markets, such as the automotive and aerospace industries, is reliant upon achieving the mechanical properties of PM materials at cast composite prices. Composite mechanical property enhancement is not only a function of the volume fraction, size, shape and spatial distribution of the reinforcement, but is also dependent upon how well the externally applied load is transferred to the reinforcing phase. Stronger adhesion at the particle/matrix interface improves load transfer, increasing the yield strength and stiness increases and delays the onset of particle/matrix de-cohesion [3,57]. The integrity of the reinforcement/matrix interface can be quantied by measuring the decrease in modulus with increasing plastic strain. This decrease is then taken as a direct measure of the extent of progressive damage to the reinforcement [8,9]. Damage takes the form of either reinforcement cracking or de-cohesion at the particle/matrix interface. At low strains, and for particles less than 20 mm in diameter, particle cracking seldom occurs [5,6,8,9]. Thus for similar composites containing ne reinforcements, dierent rates of damage accumulation can be linked to dierent eases with which the particle/matrix interface de-coheres. The mechanical properties of cast composites tend to be poorer than those produced by PM [7,1015]. The main problem associated with developing cast MMCs with mechanical properties similar to their PM equiva- lents, is not so much an issue of poor interfacial bond- ing, but the formation of clusters of reinforcement during solidication processing [1419]. Fewstudies have enabled the eect of primary processing route on the mechanical properties and microstructure of 0266-3538/00/$ - see front matter # 2000 Elsevier Science Ltd. All rights reserved. PI I : S0266- 3538( 99) 00125- 6 Composites Science and Technology 60 (2000) 307314 * Corresponding author. Tel.: +1-44-115-951-3744; fax: +1-44-115- 95-1-3764. E-mail address: andrew.kennedy@nottingham.ac.uk (A.R. Kennedy). similar composites to be determined. Most studies have investigated aluminium/SiC systems but the particle sizes and spatial distributions often dier between com- posites. Reaction between SiC particles and most mol- ten aluminium alloys means that the chemical compositions of PM and cast composite matrices also dier. A ux-assisted casting method has been developed [2022] which enables transition metal compounds such as TiC to be incorporated into molten aluminium. The role of the ux is to remove oxides from the melt and reinforcement surfaces thus enabling intimate contact and encouraging wetting [23]. Particle clustering in the Al/TiC system is signicantly reduced and is attributed to good wetting of the particles by the liquid metal and the nucleation of solid aluminium on the reinforcing particle surfaces [22,24]. The as-cast Al/TiC composite particle distributions more closely resemble those observed in powder-route processed composites, enabling more meaningful comparisons between their mechanical and physical properties. 2. Experimental Commercial-purity (99.7 wt%) aluminium composites containing 10 vol% of 10 mm diameter TiC particles were prepared by three dierent manufacturing meth- ods. Composites were manufactured using a ux-assis- ted casting method (henceforth referred to as cast composite), the details of which can be found elsewhere [2022]. Composites were also manufactured from powders, by simple mixing of the two components fol- lowed by hot isostatic pressing (PM) and by melting and casting the aforementioned powder-route material (melted PM). It was hoped that by melting and casting PM material, interfacial bonding might be improved. Melts were poured in a cast iron mould to produce cylindrical specimens 36 mm in diameter and 100 mm long. Composite billets were extruded to 10 mm dia- meter bar at 400
C, through shear faced dies, at a
reduction ratio of 13:1 and a speed of 1 mm s 1 . Den- sities of the base material and the composites were measured before and after extrusion using Archimedes' principle [24]. Specimens were polished and viewed in an optical microscope in order to observe the distribution of particles in the matrix. Matrix grain structures were revealed by anodising in Barker's reagent for 1 min at 24 V and viewing under polarised light conditions. Mechanical testing was performed on both composite and unreinforced, ingot and powder-derived materials, in the as-manufactured and as-extruded conditions. The tensile and extrusion axes were parallel. The modulus was measured and averaged over three loading cycles using a twin strain gauge method [24]. The 0.1% proof stress, which was interpreted to be a consistently measurable yield point, ultimate tensile stress and ductility were also measured. The results in each case represent an average of a minimum of six test samples. The change in modulus with increasing plastic strain was measured using a clip gauge arrangement. The initial modulus was measured over three loading cycles, and then averaged, before plastically straining the spe- cimen by a set amount and re-measuring the modulus in the same way. This testing operation was then repeated until necking was observed. Results for three similar tests were averaged. 3. Results 3.1. Microstructure and particle distribution Fig. 1 compares particle distributions in cast and PM composites and it can be seen that although there are particle-free zones in both materials, there are few highly clustered regions. There is, however, slightly less clustering in the PM composite and in the cast material areas of porosity can be observed. It should be noted that large, blocky Al 3 Ti particles, indicative of reaction between the matrix and the reinforcement, were not Fig. 1. Optical micrographs showing the particle distribution in (a) liquid and (b) PM processed CP Al10 vol% TiC composites. 308 A.R. Kennedy, S.M. Wyatt / Composites Science and Technology 60 (2000) 307314 observed in any of the microstructures. Fig. 2 shows the grain structures for the cast and PM composites and Table 1 presents the grain sizes for as-manufactured composites and base materials, measured using a line intercept method. The cast aluminium matrix is exten- sively grain rened by the TiC particles and a signicant proportion of the reinforcing particles are situated within the metal grains. The grain size of the PM com- posite is smaller still and is similar to the size of the aluminium powder, between 20 and 50 mm. The rein- forcing particles delineate the PM composite matrix grains but the extent of clustering is small. As a result of melting and casting PM material, very large clusters and signicant particle-free regions are formed. The TiC particles still act as nucleation sites for solid aluminium and a rened microstructure is obtained. The grain size is, however, over 30% larger than that in the cast composite, indicating that a lower percentage of the particles stimulate grain renement. The particle distribution and microstructure can be seen in Fig. 3, with clusters of particles visible both within and around the metal grains. Fig. 4 shows that extrusion improves the homogeneity of the cast material and little dierence between the spatial distribution of particles in the cast and PM extruded products can be observed. Extrusion also breaks down most of the large agglomerates in the mel- ted PM composite, as illustrated in Fig. 5(a), but there are still more clusters present than in either of the other two extruded composites. For all composites, the grain structure of the extruded product is ne and elongated, a typical example of which is shown in Fig. 5(b), and there are fewer signs of porosity when compared with as-manufactured material. Fig. 2. Optical micrographs showing the grain structure in (a) liquid and (b) PM processed CP Al10 vol% TiC composites. Table 1 Grain sizes (in mm) for materials in the as-manufactured condition Al cast Al PM Al 10TiC cast Al 10TiC PM Al 10TiC melted PM 36542 354 7710 326 10217 Fig. 3. Optical micrographs showing (a) the particle distribution and (b) the grain structure in melted PM processed CP Al10 vol% TiC composites. A.R. Kennedy, S.M. Wyatt / Composites Science and Technology 60 (2000) 307314 309 3.2. Mechanical properties Mechanical property data are shown in Table 2. Composite stiness values in the as-manufactured con- dition are similar, ranging from 86 to 88 GPa. This corresponds to a 1.8 GPa approx. increase in modulus per vol% of particles added. There is, however, a clear dierence in the yield (0.1% proof) stress for composites produced by dierent routes. The proof stress and ulti- mate tensile stress values are highest in the powder- route material. Melting and casting the PM composite results in a signicant reduction in strength and ducti- lity. The ductilities for the cast and PM composites are high and not signicantly below those for their unrein- forced equivalents. Table 3 presents grain sizes, measured on sections perpendicular to the tensile axis, and calculates the cor- responding increases in composite yield stress expected as a result of the reduction in grain size. This estimation is based on the HallPetch equation, with a k value of 0.15 [6] and assumes that the friction stress does not vary between materials compared. By subtracting the strengthening contribution associated with grain-size reduction from the actual increase, a rough indication of the contribution from other strengthening mechan- isms can be obtained. In the unreinforced material, the dierence in yield strength between the PM and cast aluminium is attrib- uted to both a grain-size reduction and a strengthening contribution (8.5 MPa) from ne oxide on the powder surfaces. Since in the melted PM composite the con- tribution from ne oxide is expected to be lost, through its association with particle clusters, it was compared with the cast composite. Although this analysis has several simplications, it suggests that the contribution to the yield stress from the reinforcement in the cast composite, 13.5 MPa, is greater than in the PMcomposite, 10.5 MPa, which is in turn greater than that in the melted PM com- posite, 8 MPa. Extrusion increases the proof stress, ultimate tensile stress and ductility for all the materials studied and slightly increases the stiness along the extrusion direc- tion. After extrusion, the mechanical properties of extruded cast and PM composites are similar and the ductility of the melted PM material recovers to a value approaching that of the original PM material. Extrusion also produces increases in the product density, as shown Fig. 4. Optical micrographs showing the particle distribution in (a) liquid and (b) PM processed CP Al10 vol% TiC composites after extrusion. Fig. 5. Optical micrographs showing (a) the particle distribution and (b) the grain structure in melted PM processed CP Al10 vol% TiC composites after extrusion. 310 A.R. Kennedy, S.M. Wyatt / Composites Science and Technology 60 (2000) 307314 in Table 2. Similar values for extruded composite den- sities indicate little variation in particle volume fraction. 3.3. Modulus change as a function of strain Figs. 6 and 7 show the modulus ratio, the modulus at a given strain divided by the modulus at zero strain, as a function of strain. Scatter values for the modulus ratio are not shown but are typically 2%. In all cases the modulus ratio, and hence the modulus, decreases with increasing plastic strain. Both Figs. 6 and 7 indicate that cast composites exhibit the least amount of damage at any given strain. Above strains of about 1% for as-manufactured and about 2% for as-extruded composites, the decrease in the modulus ratio, or increase in damage, is approxi- mately linear. Table 4 presents values for the gradients of the linear parts of these plots. It is clear from both the table and the plots that the rates of decrease in the modulus ratio are similar for PM and melted PM com- posites, in both the as-manufactured and as-extruded conditions, and that the damage accumulation rate is signicantly lower for composites made by casting. Extrusion, in all instances, decreases the damage-accu- mulation rate. Fig. 8 presents the modulus ratio as a function of true stress for as-extruded materials. By extrapolating the linear parts of these plots to zero damage, approximate damage initiation stresses of 120, 110 and 100 MPa are obtained for cast, PM and melted PM composites respectively, re-arming that the cast composite is most resistant to damage. Whilst the dierences in initiation stress may be small, dierences in the modulus ratio are signicant. For example, at 10% plastic strain a mod- ulus ratio dierence of 0.1 is observed between the PM and the cast-extruded composites, corresponding to a 9 GPa dierence in stiness. 4. Discussion 4.1. Microstructure and particle distribution Although not quantied, it is clear that there is less clustering in PM than cast composites. Since for the PM composite, the matrix and reinforcement powder parti- cle sizes are comparable, as long as mixing is thorough, the generation of severe clusters will be avoided. Simple mixing and isostatic compaction does not, however, enable the particles to be enveloped within the matrix grains. Grain renement of aluminium by TiC is expected through close face-centred cubic-crystal-structure matching [25,26]. The grain rening nature of TiC par- ticles may reduce the degree of clustering commonly observed in cast MMCs because solid metal nucleating and growing from the TiC particle surfaces can result in many of the particles being located within the matrix grains. Table 3 Comparison of predicted and actual yield stress variations caused by reductions in the grain size Grain Size (mm) Predicted y increase (MPa) Actual y increase (MPa) Dierence (actualpredicted) (MPa) Al cast 36542 Al 10TiC cast 7710 9.5 23 13.5 Al PM a 354 17.5 26 8.5 Al 10TiC PM b 326 1.2 12 10.8 Al 10TiC melted PM a 10217 7.0 15 8.0 a Compared to Al cast. b Compared to Al PM. Table 2 Mechanical properties for materials in the as-manufactured and as-extruded conditions Material Modulus (GPa) 0.1% PS (MPa) UTS (MPa) Elongation (%) Density (kgm 3 ) Al cast 690.5 343 663 332 2.707 Al cast+ext 700.5 412 893 403 2.713 Al 10TiC cast 871.0 573 1094 242 2.915 Al 10TiC cast+ext 900.5 692 1235 302 2.929 Al PM 700.5 603 755 325 2.701 Al PM+ext 710.5 672 924 392 2.710 Al 10TiC PM 880.5 723 1204 253 2.920 Al 10TiC PM+ext 890.5 792 1294 322 2.927 Al 10TiC melted PM 861.5 494 886 83 2.912 Al 10TiC melted PM+ext 881.0 674 1177 223 2.932 A.R. Kennedy, S.M. Wyatt / Composites Science and Technology 60 (2000) 307314 311 Melting PM material has a marked eect on particle clustering. It is likely that ne oxide lms present on the aluminium powder particle surfaces are released and mobile after melting and cause `trawling' of the particles into clusters. It is expected that TiC particle surfaces are not as clean as those introduced via the ux-assisted casting method, and hence not wet so well by molten aluminium, and hence have an increased tendency to agglomerate. It should be noted that particle-melt interactions in the melted PM system are not so dier- ent that grain renement becomes impossible, although the increased level of clustering seemingly results in a larger grain size than that for the cast composite. Reac- tion between TiC and aluminium has been reported [27] but it is believed that in this instance the short proces- sing times minimise particle/matrix reaction. Extrusion did not produce severe banding of the reinforcement. Instead, shear processes during extrusion reduce porosity, facilitate the break-up of both small and very large particle clusters and reduce the size of particle-free regions. These observations are in keeping with those of other researchers [5,10,14,28]. 4.2. Mechanical properties In this study, the matrix composition, reinforcement volume fraction, shape and size, and in the case of extruded composites, distribution, are near identical. Thus, dierences in work hardening rate and damage accumulation rate are more easily attributed to varying strengths of bonding at the particle/matrix interface. Dierences in values for the initial modulus were small suggesting that at low strains, corresponding to stresses below the yield point, the load transfer behaviour is similar. Above stresses greater than about 100 MPa, the interfacial bonding behaviour diers with manufactur- ing method. Signicantly lower rates of damage accu- mulation for composites made by ux-casting indicate that they exhibit the strongest interfacial bonding. Reinforcements in the cast composite produce greater strengthening than those in PM and melted PM com- posites indicating reduced load transfer and interfacial bond strength in the same sequence. This conclusion is consistent with that for damage accumulation rate measurement. Whilst it is clear that hot isostatic pressing produces a bond suciently strong for load transfer at low applied stresses, it is apparent that interfacial bonding is stron- ger in cast composites. Improved interfacial bonding is attributed to the production of clean interfaces, through the use of a ux, which enables good wetting by molten aluminium. As a result of the metallic nature of the bonding in transition metal carbides such as TiC [29], it is thought that simply bringing clean TiC and alumi- nium surfaces together is sucient to enable good bonding. Clean, coherent interfaces with strong chemi- cal bonding have been observed in in-situ processed Al/ Fig. 6. Decrease in modulus ratio as a function of plastic strain, for composites in the as-manufactured condition. Fig. 7. Decrease in modulus ratio as a function of plastic strain, for composites in the as-extruded condition. Table 4 Damage accumulation rates as a function of strain for composites produced by dierent methods As-manufactured As-extruded Al 10TiC cast 1.6 0.7 Al 10TiC PM 2.5 1.7 Al 10TiC melted PM 2.4 1.8 Fig. 8. Decrease in modulus ratio as a function of true stress, for composites in the as-extruded condition. 312 A.R. Kennedy, S.M. Wyatt / Composites Science and Technology 60 (2000) 307314 TiC composites [26] and it is expected that similar interfaces to these are produced as a result of ux-casting. The TiC particles in the PM composite are likely to be in contact with an alumina layer on the aluminium powder surfaces, which cannot be removed or by-passed during hot isostatic pressing. It is this layer which pre- vents intimate Al/TiC contact and inhibits strong bonding. Simply melting PM composites is not sucient to remove the oxide lm, achieve intimate contact and produce a strong bond. The presence of oxide lms is also likely to result in microporosity at the non-wetted particle/matrix interfaces. Small increases in the modulus after extrusion are expected to be a result of alignment of reinforcement with their major axes in the direction of extrusion, causing an eective increase in the aspect ratio of the reinforcing phase [5,28]. Reduction in porosity, as evi- denced by density measurements, is also likely to increase the modulus. Since the clustering, and the number of sites for premature void formation, decrease after extrusion [5,8,14], we expect damage initiation to be deferred to higher macroscopic strains. The observed shift in the onset of damage initiation was, however, only small. Shearing at the particle/matrix interface during extrusion could be responsible for decreasing the damage rate by generating clean aluminium and TiC surfaces, much like those produced during friction welding, and thus increasing the likelihood of forming strong chemical bonds. Microporosity at the particle/ matrix interface may also be closed. The dierence between the damage rates in cast and PM composites was not signicantly reduced after extrusion. It is prob- able that the extrusion ratio and speed were insucient to produce sucient shearing to improve greatly the interfacial bond strength. 5. Conclusions Fewer particle clusters and particle-free regions are present in PM Al/TiC composites than in cast ones. Melting PM material enables oxide lms to become mobile and seemingly results in `trawling' of the particles into large clusters. Mechanical properties are similar for cast and PM composites, but melting PM material results in severe particle clustering and signicant losses in both strength and ductility. In all cases, composite ductility is enhanced by extrusion through the removal of porosity and the break-up of particle clusters. Flux-cast Al/TiC composites exhibit the lowest rates of interfacial damage with progressive plastic straining and require higher stresses to initiate damage. This is inter- preted as being caused by bonding between the reinforce- ment and the matrix being strongest in these composites. Enhanced interfacial bonding in cast Al/TiC compo- sites is in turn attributed to the use of a ux, which cleans the particle and matrix surfaces, enabling intimate contact and the formation of strong chemical bonds. 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