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Mariya Kunichika, Morimasa Nakamura, Takashi Matsuoka, [Hidetoshi Somekawa](https://orcid.org/0000-0001-5007-5834)

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[Mechanical Properties of Powder Metallurgy Extruded Al Based Composites Using Sheath](https://mdr.nims.go.jp/datasets/37808a88-cb06-4944-b910-a743954d9a5e)

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Mechanical Properties of Powder Metallurgy Extruded Al Based Composites Using SheathMechanical Properties of Powder Metallurgy Extruded Al Based Composites UsingSheathMariya Kunichika1,2, Morimasa Nakamura1, Takashi Matsuoka1 and Hidetoshi Somekawa2,+1Department of Mechanical Engineering and Science, Doshisha University, Kyotanabe 610-0394, Japan2Research Center for Structural Materials, National Institute for Materials Science, Tsukuba 305-0047, JapanThe effects of extrusion and dispersed particles (SiC or SiO2) on the mechanical properties are examined on aluminum (Al) basedcomposites prepared from powder metallurgy. Extrusion is effective for i) grain refinement of the α-Al matrix and ii) producing high quality bulkspecimens on a large scale. This is because of a high applied stress during hot-extrusion contributes to the degradation of oxide films coveringthe powder particles, leading to the creation of new real surfaces. Microstructural observations show that powder-based extruded Al and itscomposites have fine-grained structures, i.e., an average grain size of less than 5µm in the α-Al matrix. Accordingly, associated to thesemicrostructures, they show higher strength (³30MPa) and hardness (³10Hv) than those of cast Al and its composite. In addition to beneficialmechanical properties, the extrusion process does not give a negative impression as for wear property, i.e., the wear rate. Plasticity-controlledvoid growth mechanism is focused to consider the impact of extrusion on bonding quality. The time required to shrink voids is estimated, andthis value is consistent with the actual processing duration. [doi:10.2320/matertrans.MT-M2025050](Received April 1, 2025; Accepted May 8, 2025; Published May 30, 2025)Keywords: aluminum, extrusion, mechanical property, voids, powder metallurgy1. IntroductionAlloying is the most classical and well-known method forimproving and controlling the mechanical properties ofmetallic materials. However, the number of applicablealloying elements is limited, because not all solutes can bedissolved into metallic materials associated with the dif-ferences in wettability between solute and solvent atoms. Inthe case of magnesium (Mg) and aluminum (Al) which areboth lightweight metals, there are 29 alloying elements witha maximum solubility of 0.1 at% for Mg and 16 alloyingelements for Al [1, 2]. In contrast, based on the powdermetallurgy (PM) route, a wide range of particles can be easilydispersed in the base metal matrix, (namely, metal matrixcomposites); thus, they are recognized as essential materialsfor structural applications. Metal matrix composites typicallyexhibit the combined properties of the base metal anddispersed particles, known as the compound law. The addedparticles also contribute to prevent dislocation slips at roomtemperature and grain growth at elevated temperatures. Asa result, these metal matrix composites have unique andsuperior properties under a wide range of conditions.Nevertheless, it is difficult to scale-up the processing forthe industrial manufactures and to obtain large-scaled metalmatrix composites. Sintering, hot press and hot isostatic pressmethods are commonly employed to produce these speci-mens, since the as-received (or raw) material is provided inthe powder form. In recent studies, new methods have beenreported to resolve these issues. Friction stir processing iseffective for uniformly dispersing the added particles with inthe matrix and for forming the specimens with higher strengththan the base metal [3–6]. Sandwich layer metal matrixcomposites are pointed out to be fabricated by explosivecompaction, potentially providing advantageous mechanicalproperties [7, 8]. Additive manufacture technique that can becombined with primary processing and final forming is alsoattracted significant attention [9–11]. In addition to the above-mentioned processes, extrusion that is one of the notablewrought-processes for metallic materials is also utilized toproduce metal matrix composites [12–16]. Sintered-speci-mens and hot pressed-specimens are generally used for theextrusion billet. On the other hands, in such cases, it takes alot of effort and time to prepare these billets, before extrusionprocess. In our current studies, the use of sheaths that is madeof dissimilar material as compared to the base powder metalis succeeded to produce bulk specimens under a wide rangeof conditions [17, 18]. Furthermore, this method offers asignificant reduction in time and effort, due to simply mixingof powders and then compounding into sheaths.Based on these knowledges, in this study, Al is selected asthe base powder metal, because this metal has a low densityand is relatively abundant and affordable. Mg alloy, which ismuch higher strength and hardness than those of pure Al, isused as the sheath to apply a high magnitude of stress duringextrusion. We examined the ability to produce bulk metalmatrix composite specimens, comprising SiC or SiO2dispersed Al matrix by hot-extrusion. We investigated themechanical properties of strength and tribology on the Al/SiC and Al/SiO2 composites, and compared with previouslyreported Al based composites. Finaly, with focus on voidgrowth mechanism, we considered the role of extrusion onbonding quality and the duration required to shrink the voids.This considered model will give a prediction of suitablecondition, i.e., holding time vs. extrusion temperature, and iseffective and important from an industrial viewpoint.2. Experimental ProceduresPM route was applied to produce Al based compositeswith dispersed SiC or SiO2 particles having their dispersedfraction, Vf, of 10%. Commercial Al powder with a purityof 99% (¯180 µm in size) and commercial SiC (or SiO2)powder (³2 to 3 µm in size) were used in this study. The Aland SiC (or SiO2) powders were mixed together with Al:SiC+Corresponding author, E-mail: SOMEKAWA.Hidetoshi@nims.go.jpMaterials Transactions, Vol. 66, No. 8 (2025) pp. 998 to 1005©2025 The Japan Institute of Metals and Materialshttps://doi.org/10.2320/matertrans.MT-M2025050(or Al:SiO2) volume fraction ratio of 9:1 using mortar andpestle. The mixtures were tap-packed by hand pressing intoa cylindrical sheath with an inner diameter of 20mm, innerlength of 55mm, outer diameter of 40mm and outer lengthof 70mm, made of commercial Mg alloy (AZ31). Note thatthe Mg alloy sheath is beneficial to apply high extrusion loadas compared to Al under high temperature. These billetscontaining the mixed Al and SiC (or SiO2) powders werekept in a furnace at the temperature of 523K for more than30mins, and then pressed at approximately 1,500 kN for10mins. They were subsequently extruded at the ram speedof 0.2mm/s with an extrusion ratio of 16:1, hereafter denotedas PM-extruded Al/SiC and PM-extruded Al/SiO2.To compare specimens with and without SiC (or SiO2),only the commercial Al powder (¯180 µm in size) was tap-packed into the cylindrical Mg alloy sheath. This billet wasextruded under the same conditions as mentioned above,denoted as PM-extruded Al. Apart from these PM extrudedspecimens, pure Al and Al/SiC composite were produced bycasting and they were used for comparison. The cast Al/SiCcomposite was diluted using Al/SiC with pure Al (99.9%).The dispersed volume fraction, Vf, of SiC was controlledto be 10%, which is the same as that of the PM extrudedAl/SiC. It is noted, to the best of our knowledge, that Al/SiCis the only commercial Al based composite that is fabricatedby casting process.Microstructural observations were carried out by electronbackscattered diffraction (EBSD) method with accompanyingfield-emission scanning electron microscopy (FE-SEM) atthe scanning step sizes of 2.5 µm or 125 nm. The observedarea was the TD-ED planes in the extruded specimens, whereTD and ED mean the transverse-direction and extrusion-direction. EBSD data were analyzed using EDAX/TSLsoftware ver. 7.0. Change in the oxide surface coveringpowder particles attributed to extrusion was examined bytransmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS) analysis. For the EBSDobservations, their specimens were prepared by polishing toa mirror-like surface finish. TEM specimens were preparedby focused ion beam using the lift-up method.Mechanical properties were examined by micro-Vickershardness and compression testing. The magnitude of theapplied load was 97N for a holding time of 15 sec in thehardness test. Each specimen was indented in at least 20positions. In the compression test, the initial strain rate was1 © 10¹3/s and the dimension for specimens was a height of6mm and a diameter of 3mm. The compression tests wereperformed more than three times to confirm the repeatability.In addition to these tests, wear tests were conducted toevaluate the wear rate under the ball-on-disk configuration.The sliding speed was set to 1mm/s, and counter ball wascomposed of high-carbon chromium bearing steel (SUJ2)with a diameter of 4.7mm. The wear rate, K, was calculatedusing the equation of K = V/P/L; P (= 0.49N) is theapplied load, L (= 1,000mm) is the sliding distance and Vis the loss volume. The value of V was measured as thedifference in volume before and after wear testing,determined by laser microscopy. Before wear testing, thespecimens were polished to a mirror-like surface finish. Inspecific specimens, the surface features after wear testingwere observed by SEM.3. ResultsCross-sectional features of PM extruded Al before andafter extrusion are provided in Fig. 1. Figure 1(a) is thecross-sectional image of the sheath in the just tapped state(i.e., before extrusion). Bright and dark regions indicate Alpowder and voids, respectively. This suggests that voids arepresent before extrusion with an average size of ³100 µm.The inset on the top left-side in Fig. 1(b) is the appearanceafter extrusion. The length of the produced bulk specimen ismore than 300mm. The contrast at the inner and outerregions are different, indicating the former consists of Alwith a diameter of approximately 4 to 5mm and the latter isMg associated with the sheath. The cross-sectional imageacquired after extrusion shows that there are some tracesowning to extrusion with parallel to the process direction,but the voids observed in Fig. 1(a) are found to be clearlyextinguished. Inverse pole figure images taken by EBSD areshown in Fig. 2. Figures 2(a) and 2(b) are the micro-structures of the cast pure Al and cast Al/SiC composite.The grain size of the α-Al matrix is coarse; greater than500 µm for cast Al and ³200 µm for cast Al/SiC,respectively. In Fig. 2(b), SiC particles represented by theblack points are dispersed in/around the matrix, which aremarked by arrows. Figures 2(c) to 2(e) are the micro-structures of the PM-extruded specimens. Grain structures inFig. 1 Cross-sectional images of powder metallurgy extruded Al for (a) before extrusion ( just tapped state) and (b) after extrusion. Wheretop of left-side in Fig. (b) is appearance of bulk specimen, and TD and ED mean the transverse-direction and extrusion-direction.Mechanical Properties of Powder Metallurgy Extruded Al Based Composites Using Sheath 999PM-extruded Al are elongated along the extrusion direction,associated with recovery and recrystallization during hotextrusion. Such a microstructural feature is well-observed inwrought-processed pure Al [19–21]. It is interesting to noticethat the grain size of the α-Al matrix is significantly reducedto ³5 µm in the direction perpendicular to extrusion axis.Similar to PM-extruded Al, the grain size of these compositesis ³2 to 3 µm; while, elongated grain structures are notobserved because the dispersed particles are sites fordislocation tangling and recrystallization.The results obtained from TEM observations of PM-extruded Al/SiC composite are shown in Fig. 3(a). Theseimages include the corresponding compositional mapsobtained by energy-dispersive X-ray spectroscopy (EDX).In Fig. 3(a) of top left-side, a bright field image taken by thescanning-TEM mode shows that the observed area containsseveral SiC particles and voids. EDX mapping shows thatoxide presents in void region, as expected. The interfacesbetween Al and SiC particle contain some oxide, but this isdifficult to identify in most interfaces. The XPS analysis forFig. 2 Inverse pole figure images for (a) cast Al, (b) cast Al/SiC, (c) powder metallurgy extruded Al, (d) powder metallurgy extrudedAl/SiC and (e) powder metallurgy extruded Al/SiO2. Where the black arrows in Figs. (b), (d), (e) indicate dispersed particles, and TDand ED mean the transverse-direction and extrusion-direction. (online color)Fig. 3 Change in oxide through extrusion process for (a) TEM observation containing bright field image taken by scanning TEM modeand EDX analysis using powder extruded Al/SiC, (b) XPS analysis for powder pure Al and powder metallurgy extruded Al.(online color)M. Kunichika, M. Nakamura, T. Matsuoka and H. Somekawa1000pure Al before extrusion (powder state in Al) and afterextrusion (PM-extruded Al) are provided in Fig. 3(b). In thisfigure, there is only a strong spectrum for oxide (i.e., Al2O3)before extrusion, whereas the extruded Al shows differentfeature; reduce in oxide spectrum and increase in the Alspectrum. There results appear to show that the extrusionprocess enhances the atomic scale interfacial bonds betweenthe powders, as a consequence of breaking oxide films.Nominal stress vs. strain curves in compression are shownin Fig. 4 for (a) cast Al and its composite and (b) PM-extruded Al and its composites. Notably, all compressiontests are stopped when the nominal strain reached to 0.4,owing to the measurable limitation of strain gauge. InFig. 4(b), the inset on the right-side shows the appearanceafter compression test, which reveals the change to a barrel-shape. Mechanical properties determined from compressionand hardness testing are summarized in Table 1. Theseproperties are found to be changed by processing. “PM-extruded” Al and its composites have higher yield strengthand hardness than those of “cast” Al and its composite. TheAl based composites are also found to exhibit superior yieldstrength and hardness to those of pure Al, regardless of theprocessing with or without extrusion. As comparison withPM-extruded specimens, the difference in yield strength (andhardness) between Al and its composite is 25³55MPa (and5³10Hv). In general, many factors, such as grain boundary,alloying element (solute), texture and particle dispersion,influence the strength and hardness of materials, which willbe considered in later section. However, in simple,considering that they exhibit similar grain sizes in the α-Almatrix, dispersed particles play an important role instrengthening, as a general trend among metal matrixcomposites.Surface features after wear testing in PM-extrudedspecimens are shown in Fig. 5. Figures 5(a) to 5(c) areSEM images, and Figs. 5(d) to 5(f ) are three-dimensionalprofiles taken by laser microscopy. Wear traces are clearlyconfirmed in all images, and pile-up occurs on both sidesof traces. The wear tracks appear to exhibit ductile flowbehavior, irrespective of dispersed particle or processing.These results indicate that this wear morphology is classifiedas typical two-dimensional abrasive wear [22]. Not only thewear testing condition (e.g., lubricant, temperature, magni-tude of applied load and sliding speed) but also themechanical properties of the specimens affect the wearmechanism. Several studies have reported the wear mechan-ism map, which is a function of external factors (i.e., the loadvs. speed) [23–28]. Comparing their maps with the presentconditions, abrasive wear is assumed to be the majormechanism, which is consistent with the surface feature asshown in Fig. 5. The wear property (i.e., the specific wearrate) for each specimen is summarized in Table 1 and isprovided in Fig. 6. It can be expected that the wear rates inthe PM-extruded specimens have relatively high values,because each interface readily becomes a site for delamina-tion. However, similar to the strength, PM-extruded Al andits composites exhibit beneficial wear properties.4. Discussion4.1 Effect of extrusion/particle dispersion on mechani-cal propertiesFigures 4 and 6 appear to show that extrusion and particledispersion are effective in increasing the strength (andhardness) and wear properties. As mentioned above, manyfactors affect these mechanical properties. Among them, theFig. 4 Nominal stress vs. strain curves in compression for (a) cast specimens and (b) powder metallurgy extruded specimens. Where rightside in Fig. (b) is appearance after compression testing. (online color)Table 1 List of properties obtained from hardness, compression and wear testing.where H is the hardness, ys is the yield strength in compression and W is the wear rate.Mechanical Properties of Powder Metallurgy Extruded Al Based Composites Using Sheath 1001most well-known mechanism is grain boundary strengthen-ing, σgb, which is expressed as follows [41, 42]:�gb ¼ �0 þ k� d�1=2 ð1Þwhere σ0 is the frictional stress, k is the Hall-Petch slope(= 60MPa·µm2 in pure Al [43]) and d is the grain size. InFig. 2, the grain sizes of the cast pure Al and PM-extrudedAl are greater than 500 µm and ³5µm, respectively. Bysubstituting these values for k and d into eq. (1), thecontribution of grain boundary strengthening is measuredto be approximately 25MPa (µ 25/3.3 = 7.6Hv). Thisestimated values of 25MPa and 7.6Hv are lower than theexperimental result (70MPa and 16Hv in Table 1). Crystalorientation is known to be the other factor that affectsstrength in wrought-processed metals [44]. In Fig. 2(c),grains are accumulated more along the (111) direction,which suggests that texture strengthening contributes to theenhanced strength in the PM-extruded Al. In addition to thesemechanisms, the elongated structure along the wrought-processed direction can bring about increasing strength [45].Turing to the results of Al composites, these compositeshave higher strength and hardness than those of pure Al (inTable 1 and Fig. 6). As mentioned above, PM-extruded Aland its composites have similar grained structure, e.g., grainsize. The order of them in terms of increasing strength isas follows; the PM-extruded Al < PM-extruded Al/SiO2 <PM-extruded Al/SiC. The strengthening due to particledispersion, σparticle-dis, is recognized as the Orowan strength-ening mechanism, which depends on the factors relating withdispersed particle morphology [46, 47]:�particle-dis ¼ A� G� "3=2 � b� fðVf � rÞ ð2Þwhere A is a constant, G is the shear modulus, ε is theabsolute in misfit strain and b is the Burgers vector. The termof f(Vf · r) is the function of Vf and r, which are the volumefraction and the radius of the dispersed particle, respectively.Fig. 5 Surface features after wear testing for (a), (d) powder metallurgy extruded Al, (b), (e) powder metallurgy extruded Al/SiC and (c),(f ) powder metallurgy extruded Al/SiO2. (online color)Fig. 6 Relationship between hardness and wear rate of pure Al [33, 35–39] and Al based composites [30–35, 37–40]. Where the values ofblank in footnote indicate the fraction of dispersed particles.M. Kunichika, M. Nakamura, T. Matsuoka and H. Somekawa1002Since shear modulus of SiC and SiO2 are ³130GPa [48] and33GPa [49], this physical factor is simply influential forstrength. In the term of misfit strain, this consideration isdisregarded here, because of the difficulty in measuring itsvalue in metal matrix composites. In contrast, Fig. 2 revealthat finer particles are dispersed in the PM-extruded Al/SiCas compared to that in the PM-extruded Al/SiO2, asapplicable in eq. (2). The dispersion of reinforced particle,which is a characteristic of high shear modulus and/orconsists of fine size, is beneficial for further improvementof the strength and hardness.Finaly, regarding wear property, the correlation betweenhardness and wear rate is referred to as the Archard law [29];a lower wear rate (wear volume) indicates a higher hardness.Figure 6 includes the previous results of pure Al and Albased composites [30–40]. The sliding speed and countermaterial significantly affect the wear rate. Hardness is alsodependent on the type of reinforced particles, as well as theirmorphology and microstructures of base metal; therefore,these values are somewhat scattered and difficult to comparedirectly without accounting for these variables. Nevertheless,the dispersion of particles is apparent to have a merit forenhanced hardness and wear properties.4.2 Estimation of total process duration based on voidgrowth modelSintering and hot isostatic pressing are the common usedmethods to fabricate the metal matrix composites from rawpowders. In the current study, extrusion was employed toshorten the processing time and to obtain the bulk specimenson a large scale with fewer defects. It hereafter is brieflydiscussed about the mechanism and role of extrusion, withfocusing on the void growth mechanism.Voids generally grow during plastic flow, particularly inthe tensile state. The void growth rate, which is a function ofthe temperature, strain rate and magnitude of applied stress, iscontrolled by two famous mechanisms, namely the diffusion-controlled and plasticity-controlled mechanisms [50–53].They are independent, and the mechanism with the fastergrowth rate is recognized as the dominant for a givencondition. The diffusion-controlled mechanism occurs wellat elevated temperatures and low strain rates, whereas theplasticity-controlled mechanism is favorable at high appliedstress. Considering the present extrusion condition, theapplied stress of ³1,500 kN corresponds to ³1,200MPa,which is much higher than the room-temperature yieldstrength (in Fig. 4 and Table 1). In such a case, the plasticity-controlled mechanism is enough to be dominant owing to thesmall contribution of diffusion. The void growth rate of thismechanism is expressed as follows [52];dr=dt ¼ _"� �=3� ðr� �=�Þ ð3Þwhere is _" the strain rate, η is the stress factor (= 3 [54]), γ isthe surface energy (= 1.2 J/m2 in Al [54]), r is the void radiusand σ is the degree of applied stress. The second term ineq. (3) can be ignored because of the high value for σ. Asa result, the void growth rate is roughly re-written as dr/dt µ _" © r. It is difficult to determine the actual strain rateassociated with the two processes (i.e., pressing andextrusion). However, the average strain rate obtained fromthe total process duration is used and is estimated to be10¹3/s, (where the holding time of 10mins, the extrusiontime of 5mins and the sheath height of 70mm). In the caseof general extrusion, it is interesting to notice that the strainrate in the present facility is reported to be 10¹2/s [55]. As forthe void radius of r, this value is assumed to be equivalentto half of the initial void size, ³50 µm (in Fig. 1(a)).Substituting these values of r and _" into eq. (3), the voidgrowth rate is calculated to be approximately 0.05 µm/s.Noted that the direction of applied stress to the billet inducesa compressive state during extrusion; that is to say, materialflow operates opposite direction. Hence, the growth rate isregarded as a shrinkage rate. For this situation, the voidshrinkage size (diameter) by extrusion is estimated to be³90 µm. Considering that the present used Mg alloy sheathmakes it too difficult to perform for wrought-process at roomtemperature, extrusion must be conducted at elevatedtemperature ranges (³523K) in the current case. Such ahigh temperature is assumed to support powder sintering.Although further studies on the growth/shrinkage mechan-ism are required, this calculated shrinkage size is similar tothe initial void size.Moreover, the application of high stress during extrusionis effective for producing defect-free bulk specimen. Whilethe oxide film on the surface (in the present case is powdersurface) is likely to prevent strong bonding, a new realsurface can be created under such severe applied stress levels.For instance, the explosive welding technique has beenused for difficult-to-join materials or joining with dissimilarmaterials [56, 57]. Both the high magnitude of applied stressand high strain rate lead to the removal of the oxide filmand to promote bonding quality [58, 59]. Friction weldingtechnique is also another example for the use of high appliedstress [60–62]. It is difficult to perform welding/joining inbulk metallic glass, owing to the ease of crystallizationthrough heating effect. A quite high stress, which is muchlarger than the yield strength in bulk metallic glass, is appliedfor a very short period. Hence, crystallization is not allowedto occur at the interface, and strength in the bonded specimendoes not decrease compared with the initial state. Returningto the current results, herein, Fig. 3 indicates that extrusioncauses a change in the oxide films covering the powdersparticles. A high magnitude of applied stress effectively leadsto break oxide films and to create new real surfaces; resultingin enhanced interfacial bonding.5. ConclusionsIn summary, bulk specimens with a long length couldbe produced from raw powders by extrusion. The resultsacquired from compression and hardness testing reveal thatPM-extruded Al based composites, i.e., Al/SiC and Al/SiO2,exhibit high strength and hardness while maintaining highcompressibility. These extruded Al based composites alsohave beneficial wear properties without delamination alongtheir particle interfaces. The application of high stress duringextrusion plays an important role in degrading the oxide filmson the particle and enhancing the bonding quality. Overall,this process is convenient and versatile, enabling the large-scale industrial production of various metal matrix compo-Mechanical Properties of Powder Metallurgy Extruded Al Based Composites Using Sheath 1003sites. For instance, from a recycling perspective, wastematerials (e.g., metal dust from machining or other industrialby products) can easily be reclaimed and upcycled intovaluable products.AcknowledgementsThe authors are grateful to Mr. M. Fukuda (DoshishaUniversity) and Dr. Y. Osawa (National Institute forMaterials Science) for their technical help. We are alsosincerely thankful for the Japan Fineceramics Co. Ltd.,supplied the cast Al/SiC alloy, commercially named as theSA301.REFERENCES[1] T.B. Massalski: Binary Alloy Phase Diagrams, 2nd ed., (ASMInternational, Materials Park, OH, 1990).[2] H. 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