Wear 268 (2010) 976983

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Wear
journal homepage: www.elsevier.com/locate/wear

Effects of sliding velocity and normal load on the tribological behavior of a nanocrystalline Al based composite
Yanqiang Liu, Zhong Han, Hongtao Cong
Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016, PR China

a r t i c l e

i n f o

a b s t r a c t
Nanocrystalline Al based composite containing 39 vol.% AlN nanoparticles with enhanced mechanical properties was subjected to friction and wear characterization under various conditions. It is interesting to found that an oxygen-rich tribolayer was formed at all sliding speeds and normal loads, which seems to control the tribological behavior of the composite to a large extent. Friction coefcient of the composite increases with the increase in sliding velocity, while the wear rate decreases in a hyperbolic trend. The improved wear resistance at higher velocity was attributed to increased tribolayer coverage on the worn surface, and the enhanced tribo-oxidation. Increase in the applied load leads to steady reduction of the friction coefcient, and slight variation of the wear rate in load range of 525 N. In this range, tribolayer is the most import feature on worn surface, and wear occurs mainly by delaminating within the tribolayer. Whereas, when the load increases up to 35 N, both the friction coefcient and wear rate steeply increase up to high values, indicating a severe wear. At this load, tribolayer only covers small part area of worn scar, and delamination happens within the composite underneath the tribolayer. 2009 Elsevier B.V. All rights reserved.

Article history: Received 7 April 2009 Received in revised form 7 December 2009 Accepted 14 December 2009 Available online 23 December 2009 Keywords: Nanocrystalline composite Aluminum Sliding wear Normal load Sliding velocity

1. Introduction In the past decades, particle-reinforced aluminum matrix composites (AMCs) have been one of the most important subjects owning to their superior specic strength, specic stiffness, elevated service temperature and high wear resistance [1,2]. In particular, tribological properties of AMCs have attracted much attention because of their applications as braking disc, piston and cylinder of engine in vehicles [1]. For most of the AMCs, incorporation of ceramic particles can remarkably reduces the wear rate, by bearing most of the load applied on the composite parts [1,3]. Recently, vigorous advance has been achieved in the science and techniques of nanocrystalline (NC) materials, which exhibit extremely high strength and hardness in compared to their coarse-grained polycrystalline counterparts [4]. By combining the tailorability of AMCs and superior mechanical properties of NC materials, composites with NC matrix can be designed in a wide range. For instance, several Al, Cu and Fe based NC composites have been fabricated, with remarkably enhanced hardness and strength compared with single-phase NC materials [5,6]. Therefore, NC composites could have better wear resistance than their NC matrix. Actually, good wear resistance should be very important for bulk NC materials employed as structured components. Friction and wear properties of NC materials have been

Corresponding author. Tel.: +86 24 2397 1863; fax: +86 24 2389 1320. E-mail address: htcong@imr.ac.cn (H. Cong). 0043-1648/$ see front matter 2009 Elsevier B.V. All rights reserved. doi:10.1016/j.wear.2009.12.027

investigated on several common metals [712]. However, up to now, these properties of bulk NC composite have been seldom focused. NC Al matrix composites reinforced with aluminum nitride (AlN) nanoparticles were fabricated by a combined method of arc-discharge plasma deposition and hot pressing consolidation [6]. These nanocomposites have enhanced hardness due to the combination of grain-renement strengthening and particle strengthening in compared to non-reinforced NC Al. As a result, wear resistance of these composites was superior in compared to non-reinforced NC Al. In that study, surface oxidation was proved to be partially responsible for the improved wear resistance [13]. Friction and wear tests of NC Al and its alloy were also performed by Farhat et al. [7] and Takagi et al. [8], but no oxygen-rich surface layer was found. Also, oxidation and tribolayer was thought to be important for wear behavior of NC Cu, ultrane-grained Ti and Cu [12,1416]. But hardly any experimental work was performed to determine how and to what extent the tribological properties of NC materials are inuenced by the tribo-oxidation. In the present paper, dry sliding friction and wear tests were conducted on a 39 vol.% AlN/Al nanocomposite at various normal load and sliding velocity. Based on detailed observations of wear-induced changes in the microstructure and composition, the evolution of wear process with the applied condition was investigated. It was expected that this investigation was helpful to understand the tribological behaviors and mechanisms of Al based composites with ultrane microstructure.

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2. Experimental Nanocrystalline Al matrix composite reinforced with 39 vol.% AlN nanoparticles was prepared by hot-pressing consolidation of AlN/Al nanocomposite powders. The nanocomposite powders were produced by arc-discharge plasma evaporation and deposition of pure Al (99.85) at a mixing gas of nitrogen/hydrogen. After collection, the powders were consolidated by hot pressing at 773 K at a vacuum of about 2 104 Pa, with an applied pressure of 1000 MPa. Detailed description of the materials preparation can be referred in Ref. [6]. The as hot-pressed composite specimens are discs with dimensions of 10 mm in diameter and 23 mm in height. Relative density of all the specimens is higher than 98%. Micro-hardness of the composite is Hv 348. Scanning electron microscopy (SEM, Nova Nano SEM-430) equipped with energy dispersive spectrum (EDS) and transmission electron microscopy (TEM, JEOL-2010) operated at 200 kV was used for microstructure observation. Fig. 1 shows a typical SEM micrograph (a) and TEM bright-eld micrograph (b) and inserted selective area electron diffraction pattern (SAED) of as-prepared 39 vol.% AlN/Al NC composite. The two phases exhibit equiaxial nanograins, with AlN particles (marked by the arrows) uniformly dispersed within NC Al matrix. Mean grain size of Al and AlN, mea-

sured by using TEM dark-eld images, is 65 44 and 68 35 nm, respectively. The surface of specimens underwent a nal machine-polish using 0.5 m paste before wear tests. The surface roughness was measured to below 0.6 m (measured using a surface prolometer, Model 2205, Harbin Measuring & Cutting Tool Group Co. Ltd., China). Dry sliding wear tests of the composite were performed on an Optimol SRVIII oscillating friction and wear tester using ball-ondisc contact conguration, at room temperature (298 K), in air with the relative humidity of 4050%. WC-Co balls with Vickers hardness of Hv 1750 and diameter of 10 mm were used as the frictional counterpart. Surface roughness Ra of the ball is about 0.01 m. The parameters used are listed as follows, oscillating stroke of 1 mm, oscillating frequency of 540 Hz (equivalent sliding velocity is 0.010.08 m/s), applied normal load of 535 N, and the total sliding time of 30 min. The worn surface was ultrasonically cleaned in acetone solution to remove the residual wear debris attached on the worn surface. The friction coefcient varying with the sliding duration was continuously recorded by a computer connected with the wear tester. The wear volume was directly measured using a 3D optical surface prolometer (Micro XAM-3D), by observing worn scar of the specimens formed by wear with the WC/Co ball. Wear rate was calculated by dividing the wear volume by sliding distance (30 min (0.010.8) m/s). The worn morphology and microstructure were observed by using SEM and EDS. Moreover, cross-sectional specimens perpendicular to the worn surface and along the sliding direction were cut, ground and polished for SEM observation of the subsurface microstructure. 3. Results and discussion 3.1. Effect of sliding velocity Fig. 2 shows the friction coefcient curves of 39 vol.% AlN/Al nanocomposite at sliding velocities of 0.010.08 m/s, at a normal

Fig. 1. Typical SEM micrograph (a) and TEM bright-eld micrograph (b), associated with the SAED patterns of as-prepared 39 vol.% AlN/Al nanocomposite.

Fig. 2. Friction coefcient variation with the sliding duration at sliding velocities of 0.010.04 m/s (a), and 0.060.08 m/s (b) under a load of 10 N.

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Fig. 3. Wear rate of 39 vol.% AlN/Al nanocomposite as a function of sliding velocity under the load of 10 N.

load of 10 N. The friction coefcient at sliding velocities from 0.01 to 0.04 m/s undergoes acute uctuation at the initial stage (varying from 200 to 800 s with the velocity), and then approaches relatively smooth stage. Fluctuating time of the friction coefcient seems to be shorter at higher sliding velocity, suggesting that steady-state wear is easier to approach at higher velocity. In this velocity range, the steady-state friction coefcient (SFC) increases with an increase in sliding velocity. Whereas, the friction coefcient at 0.06 and 0.08 m/s steadily climb up with the sliding duration at the starting 1200 s, followed by an abrupt drop. After then, the friction coefcient starts to increase again. Smooth friction coefcient curves were not achieved at high sliding velocities. The graph in Fig. 3 shows the wear rate of 39 vol.% AlN/Al varying with sliding velocity at the normal load of 10 N. It can be seen that the wear rate reduces with sliding velocity in a hyperbolic-like curve, e.g., it drops down by 75% when the sliding velocity varies from 0.01 to 0.02 m/s, and the reducing amplitude decreases with further increase of sliding velocity. The wear rate at 0.08 m/s is one order of magnitude lower than that at 0.01 m/s. Worth to note that the wear rate at 0.06 m/s is slightly higher than that at 0.04 m/s. The exceptional variation in either the wear rate or friction coefcient at 0.06 m/s may indicate a change in wear mechanism of this composite. In order to understand the underlying wear mechanism of 39 vol.% AlN/Al nanocomposite upon the variation of velocity, SEM observations of the worn surface and subsurface were conducted, as shown in Figs. 46. Fig. 4a is a typical full view image of the wear scar formed at velocity of 0.04 m/s. It is interesting to nd that the worn surface is almost completely covered by layer (darkcontrast area) which is much smoother than the area without layer. The low-magnication SEM morphology of the worn surface at different sliding velocity is similar, but the layer coverage in Fig. 4a is distinctly larger than that formed at 0.01 m/s (seeing Fig. 10a in Section 3.2.1 in the following text). The magnied image of the layer in Fig. 4b shows numerous cracks on it, mainly being perpendicular to the sliding direction. EDS pattern shown in Fig. 4c indicates the layer is rich in oxygen. Herein, this wear-induced layer was called tribological layer or tribolayer as named by many other researchers. Atomic fraction of oxygen on the tribolayer is higher than 60%. Fig. 5a and b shows two high-magnied SEM images of the tribolayer formed at velocities of 0.01 and 0.08 m/s, respectively. The surface of tribolayer formed at low velocity is smooth, while that formed at high velocity is rougher and presents evident micro-cutting and -ploughing. That is, the tribolayer formed at high velocity undergoes enhanced plastic deformation under wear.

Fig. 4. (a) SEM image showing the typical full-view morphology of wear scar formed at 0.04 m/s and the load of 10 N, (b) a magnied worn morphology, (c) EDS pattern collected on the surface of tribolayer in (b).

Wear-induced changes in the subsurface microstructure and composition during sliding process are illustrated by the crosssectional SEM images in Fig. 6ad. The most apparent structural feature in the subsurface is the tribolayer with thickness of 512 m at the most top layer of the specimens. The composite underneath the layer is almost uninuenced by wear. Unlike the mechanically mixing layer formed in the reported SiC/Al composites or AlSi alloys [1719], the tribolayer in AlN/Al nanocomposite is denser and has better bonding with the composite. In addition, microcracks can be found within the tribolayer formed at all conditions (see Fig. 6c). In particular, from the line-scanning EDS pattern crossing the interface of tribolayer/composite as shown in Fig. 6b, we can found that the intensities of element O and Al undergo continuous variation in opposite trends through the tribolayer along the scanning position. This fact indicates a continual oxidation process involved in the formation of tribolayer. In contrast to the case at low sliding velocity, the intensities of Al and O undergo abrupt drop and rise, respectively, at the tribolayer/composite interface at high velocity, as shown in Fig. 6d. It seems that oxidation is more sufcient at higher sliding velocity. The thickness of tribolayer formed at different sliding velocities was statistically measured under SEM, as presented in Fig. 7. It seems that the tribolayer thickness increases in the velocity range of 0.010.04 m/s, whereas it starts to reduce with further elevating the sliding velocity. It is inferred that this distinct transition at high velocities is correlative with the transition of friction coefcient curve shown in Fig. 2b. Oxidation has not been thought as an important mechanism for wear of Al alloys and composites [20]. However, oxidation plays

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Fig. 5. High-magnied SEM images of the surface morphologies of tribolayer formed at 0.01 m/s (a) and 0.08 m/s (b), respectively, at normal load of 10 N.

an important role in wear of NC metals, since high-volume fraction grain boundaries in NC metals can act as either nucleation sites or fast diffusive paths [21,22]. Oxidation wear was proposed for ultrane-grained Ti [14] and Cu [16] and NC Cu [12]. According to the authors study [13], the wear resistance of NC AlN/Al composite is markedly improved in contrast with non-reinforced NC Al, owing to both the enhanced hardness and the protection given by O-rich tribolayer. The tribolayer was thought to be formed by oxidation of surface materials. It was thought that fracture of AlNAl interface and interconnection of these fractures can generate dispersed microcracks under the compressing and shearing stress [13,20]. The microcracks are thought as the favorite shortcircuit diffusion paths for oxygen in the ambient. O-rich tribolayer can prevent the direct contact between the composite and frictional pair, and hence results in steady state wear. Both delamination and micro-ploughing of tribolayer were responsible for wear loss of the composite [13]. Thus, the friction and wear properties of this composite at various sliding velocity could be interpreted in terms of the evolution of tribolayer. Generally, higher sliding velocity results in generation of much more frictional heat, accordingly higher temperature elevation on the contact asperities. Thus, with the accelerated oxidation process, tribolayer is much easier to form. As a result, the tribolayer coverage on worn surface is larger and oxygen content is higher at higher sliding velocity. So the wear rate is much lower at higher sliding velocity. Similar velocity dependence of wear rate of ultranegrained Ti was presented by La et al. [14], which was interpreted by the argument of enhanced tribo-oxidation at higher sliding speed. Similarly, Shaei et al. [23] reported reduced wear rate at higher sliding speed for NC Ni worn in atmosphere of argon, but attributed it to the strain-rate sensitivity of NC Ni. Zhang et al. [12] attributed the small variation of wear rate of NC Cu with sliding speed at low speed range to the generation of semi-continuous O-rich mixing layer on worn surface, however, oxides hardly can be found at sliding speed exceeding 0.08 m/s. So it is thought that oxidation probably is easier to take place in NC Al based materials worn at atmosphere. Besides the reduced wear rate, La also reported a peak value for the friction coefcient varying with sliding speed. Whereas, Zhang et al. reported similar velocity dependence of the friction coefcient and wear rate of Cu containing nano-scaled twins. In contrast to above results, friction coefcient of the present NC composite increases with sliding velocity at low velocity range. The increased stable-state frictional coefcient with sliding velocity may come from the elevated ash temperature at higher sliding

velocity [24]. On the other hand, NC metals are often thought to be strain-rate sensitive as the deformation mechanism is dominated by the activities of grain boundaries [4,25,26]. Lu et al. [25] and Mishra et al. [26] have proposed that NC metals exhibit enhanced tensile fracture stain at high strain rate and low temperature. So it is expected that the enhanced surface plasticity (see Fig. 5b) at high strain rate could also be the reason for the increase in stable-state friction coefcient. It is well accepted that real tribo-contacts always only happen between some asperities on the surface subjected to friction, which means the applied load is mostly carried over by those asperities [24]. According to Kalin [24], the real contact temperature can be extremely higher than that calculated using some theoretical models when the asperities are very small. For the case of AlN/Al, softening and even transient melting of asperities of Al is possible at high sliding velocity. As the thermal conductivity of AlN/Al composite distinctly reduced with rise of the temperature [27], accumulating heat at asperities could be very high. Therefore, softening of the composite probably account for the abrupt drop in the friction coefcient curves at the velocities of 0.06 and 0.08 m/s, and the slightly increased wear rate at 0.06 m/s (see Figs. 2b and 3). In addition, both the increase in surface ductility of the composite under wear and surface soften may lead to a reduction in the propagating rate of subsurface cracks, consequently reduces the thickness of tribolayer. 3.2. Effect of normal load 3.2.1. Friction and wear behavior Fig. 8a shows the relationship between SFC and the normal load. The inserted Fig. 8b is the typical friction coefcient curves at the loads of 25 and 35 N and the sliding velocity of 0.01 m/s. When the load is below 25 N, the SFC steadily decreases as the load increases. The friction coefcient curve becomes smoother at higher loads, and the uctuation of the friction coefcient at the initial stage becomes smaller (not all shown here) at higher loads. For instance, the SFC of the composite at 25 N is 0.66 0.03, which is 20% lower than that at 5 N (0.83 0.06). However, when the normal load increases up to 35 N, the SFC rapidly increase up to the value at 5 N. As can be seen in Fig. 8b, the friction coefcient curve at 35 N evidently uctuates with sliding duration until the time of 1300 s. Wear rate of the composite as a function of normal load was plotted in Fig. 9. Interestingly, the wear rate does not show significant increase at the range of 525 N. But when the load increases

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Fig. 6. SEM micrographs showing the cross-sectional morphologies of sub-surface, and the EDS line-scanning pattern of elements Al and O along the direction marked using black arrows, at the velocity of 0.01 m/s (a and b) and 0.04 m/s (c and d), respectively, and the load of 10 N.

up to 35 N, the wear rate steeply increases by about 4 times in compared to that at 25 N. This abrupt variation at 35 N is similar with the variation of SFC. It is inferred that a transition from steady-state wear to severe wear occurred between 25 and 35 N, which probably originates from a change of wear mechanism. Fig. 10a and b shows the full SEM view of the worn scars of the composite at loads of 10 and 35 N, respectively. The worn surface tested at loads below 25 N (including) has similar microstructural features: O-rich tribolayer covering large part area of worn surface (dark-contrast area). Also, micro-ploughing can be found on the tribolayer. In contrast, the worn surface under the load of 35 N is rougher than those at lower loads, and characterized as smaller tribolayer coverage. The ploughing tracks are wider at this load, shown by the black arrows in Fig. 10b. It is thought that the com-

posite underwent severe wear with a large amount of materials removal at 35 N. Fig. 11ac gives the typical cross-sectional micrographs of tribolayer formed on worn surface at the loads of 5, 15, and 35 N, respectively. Evidently, O-rich tribolayer is formed at all the loads, while the coverage is discontinuous at 35 N and much less than that at 5 and 15 N. Also, there is a visible interface between the tribolayer and the composite. Composition analysis by EDS indicates the layer has similar composition with that shown in Fig. 6a. It is important to note that cracks initiate within the O-rich tribolayer (Fig. 11b) or near the interface of tribolayer/composite (Fig. 11a) when the applied load is below 25 N. The area underneath the tribolayer is almost uninuenced by wear. But the cracks initiate within the non-oxygenated area underneath the tribolayer at 35 N

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Fig. 7. Thickness of the tribolayer varying as a function of sliding velocity.

Fig. 10. SEM micrographs revealing the full view of the worn scars of the composite at 10 N (a) and 35 N (b), respectively, and the sliding velocity of 0.01 m/s.

(Fig. 11c). These cracks are the direct origin of delamination damage of surface materials. The delaminating depth of the specimens is statistically measured by SEM observation and plotted in Fig. 11d as a function of load. The damage depth steadily increases with normal load, which is consistent with the proposal on delamination wear by Zhang and Alpas [28].
Fig. 8. (a) The SFC as a function of normal load, (b) the typical friction coefcient curve varying with sliding duration at 25 and 35 N for the composite at a sliding velocity of 0.01 m/s.

Fig. 9. The variation of wear rate of the composite as a function of the normal load at a sliding velocity of 0.01 m/s.

3.2.2. Transition of wear behavior with load The negative load dependence of SFC at loads below 25 N could be attributed to the increased coverage of worn surface by tribolayer at higher loads [13], as well as the increased effective contact area with applied load [15]. The distinct transition of friction coefcient and wear rate of the composite at 35 N is probably correlated with the change in wear mechanism. As mentioned above, oxidation plays an important role in the wear of AlN/Al nanocomposite. The tribolayer can prevent direct contact between the composite and the frictional pair, driving the wear to a steady state. As shown in Fig. 11ac, the thickness of tribolayer increases from about 57 m at 5 N to 10 m at 25 N, and no longer varies with the increase of load. Increase of the tribolayer thickness is helpful to protect the composite from big wear loss. On the other hand, however, the shearing stress on the contact surface increases with load, which consequentially increases the damage depth, as shown in Fig. 11d. When the load is below 25 N, the delamination occurs mainly within the tribolayer or the tribolayer/composite interface, the wear can be regarded as oxidation wear [29]. Therefore, the composite under the tribolayer is almost uninuenced by wear, give rising to ignorable variation in the wear rate in this load range. Whereas, the damage happens mainly in non-oxygenated matrix under the O-rich layer at 35 N, so the friction and wear of the composite no longer depends on the O-rich tribolayer, but is

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Fig. 11. SEM images of typical cross-sectional morphologies of tribolayer formed on the worn surface at normal loads of 5 N (a), 15 N (b), and 35 N (c), respectively, and the sliding velocity of 0.01 m/s, (d) delaminating depth within the subsurface as a function of normal load, measured statistically by using SEM images.

completely dominated by the hardness and toughness of the composite itself. This transition in delaminating position is the main reason of the steep increase in the steady-state friction coefcient and wear rate at 35 N. This phenomenon is similar with that reported by Cui et al. [30], who proposed that delaminating position immediately determine the level of wear rate when an oxide lm was formed. To sum up, tribo-oxidation and formation of O-rich layer have a signicant inuence on the friction and wear behavior of NC Al based composite, and should be an important clue used to understand the complex wear mechanism of NC Al based materials.

continuous tribolayer, as well as the transition of delaminating position from tribolayer to interior of the composite. Acknowledgements The authors would like to thank Prof. H.M. Cheng for his meaningful proposals in preparation and revision of the manuscript, and thank Dr. Z. Han for her help in wear experiments and enlightened discussion. References
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4. Conclusions (1) The friction coefcient increases with increasing the sliding velocity at 0.010.04 m/s. Particularly, the friction coefcient curves at 0.06 and 0.08 m/s underwent abrupt drops at duration of 1200 s. Wear rate of the composite reduces in a hyperbolicshape curve with increasing sliding velocity. (2) O-rich tribolayer was formed at all velocities, but its coverage on worn surface is larger at higher velocities than that at 0.01 m/s. Wear of the composite is dominated by micro-poughing and delamination of the tribolayer. Increase of sliding speed promotes the formation of O-rich tribolayer, therefore, the wear rate is much lower at high velocity. (3) The steady-state friction coefcient steadily reduces with increasing normal load from 5 to 25 N. Wear rate of the composite exhibits a weak load dependence in the load range of 525 N. Both the steady-state friction coefcient and wear rate sharply increase at 35 N. (4) Tribolayer is the most important feature on worn surface at various loads. Tribolayer coverage on the worn surface at 35 N is distinctly fewer than that at lower loads. Delamination happens within the tribolayer or tribolayer/composite interface at loads of 525 N, while it happens within the composite below the tribolayer at 35 N. The severe friction and wear as observed at 35 N originates from the lack of protection given by semi-

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