Materials and Design 32 (2011) 45284536

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Materials and Design

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Dry sliding wear behaviour of organo-modied montmorillonite lled epoxy nanocomposites using Taguchis techniques
Rashmi a, N.M. Renukappa a,, B. Suresha b, R.M. Devarajaiah c, K.N. Shivakumar d
a

Department of Electronics and Communication, Sri Jayachamarajendra College of Engineering, Mysore 570 006, India Department of Mechanical Engineering, The National Institute of Engineering, Mysore 570 008, India c Department of Mechanical Engineering, Acharaya Institute of Technology, Bengaluru 560 090, India d Center for Composite Materials Research, Department of Mechanical Engineering, NC A&T State University, Greensboro, NC-27411, USA
b

a r t i c l e

i n f o

a b s t r a c t
The aim of the research article is to study the dry sliding wear behaviour of epoxy with different wt.% of organo-modied montmorillonite (OMMT) lled nanocomposites. An orthogonal array (L9) was used to investigate the inuence of tribological parameters. The results indicate that the sliding distance emerges as the most signicant factor affecting wear rate of epoxy nanocomposites. Experimental results showed that the inclusion of 5 wt.% OMMT nanoller increased the wear resistance of the epoxy nanocomposite signicantly. Furthermore, the worn surfaces of the samples were analyzed by scanning electron microscopy (SEM) to study the wear mechanisms and to correlate them with the wear test results. 2011 Elsevier Ltd. All rights reserved.

Article history: Received 10 November 2010 Accepted 11 March 2011 Available online 21 March 2011 Keywords: A. Composites E. Wear H. Weighting and ranking factors

1. Introduction In recent years, polymer is extensively utilized in tribological components such as cams, brakes, bearings and gears because of their self-lubrication properties, lower friction and better wear resistance. The inherent deciency of polymers could be altered successfully by using various special llers (micro to nano sized particles). More and more polymer composites are now being used as sliding components, which were formerly composed only of metallic materials. Nevertheless, new developments are still under way to explore other elds of application for these materials and to tailor their properties for extreme load-bearing and environmental temperature conditions. The current global nanocomposite market size is around US$ 300 million and is expected to exceed US$ 1billion within the next 5 years [1,2]. Currently, clay lled nanocomposites account for almost 25% by volume of total nanocomposites usage and their market share is rapidly increasing. Much research has been carried out in the development of nanoparticles lled composites through the incorporation of nano-scaled materials such as ceramics and carbon in polymer matrices. For instance organoclays [3], carbon nanotubes [4], alumina nanoparticles [5] and nano ZnO and nano SiC nanoparticles [6] have been added to polymers. Most studies on the inuence of ller material in case of polymer composites sliding against metallic countersurface have been reported on the reduction of
Corresponding author. Tel.: +91 821 2548285; fax: +91 821 2548290.
E-mail addresses: renunijagal@gmail.com, renunijagal@sjce.ac.in (N.M. Renukappa). 0261-3069/$ - see front matter 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.matdes.2011.03.028

wear rate and coefcient of friction, in addition to higher mechanical strength obtained due to the addition of llers in polymer composites. The wear was considerably reduced by the addition of different llers in thermoplastic polymers [710]. In recent years the mechanism of ller action in reducing the wear rate of polymers has recently been a subject of intense study. However the microller lled polymer composites usually need quite a large amount of llers to achieve better wear resistance, but in these composites some inherent defects are inevitable. Considering the disadvantages caused by microllers, utilization of nanoparticles would be an optimum alternative. Since the predominant feature of nanoparticles lies in their ultra-ne dimension, ller atoms can reside at the interface and lead to a strong interfacial interaction if the nanollers are well dispersed. As a result, the nanocomposites coupled with a great number of interfaces could be expected to provide exceptional tribological performance [11]. Since nanollers can bring value added properties to the polymers, nanocomposites can become an important member in the family of wear-resistant and friction reducing materials. In lled polymer composites, the particle size plays an important role in the improvement of wear resistance. Recent investigations on the tribological behaviour of organoclay lled polyamide6 (PA6) by Srinath and Gnanmoorthy [12] and Dasari et al. [13] show a low friction and high wear resistance since the size of nano additives is of the order of surrounding polymer chains and increases the bonding of particle to the polymer matrix. Nanoparticles tend to produce a tenacious transfer layer on the counterface, which protects the composite surface from direct contact with the counterface thereby reducing friction and

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wear of nanocomposites. The addition of nanoclay to form a polymer nanocomposite is another means to modify the properties of material. The addition of 25% by weight of exfoliated clays can lead to improvement in thermal and mechanical properties in comparison to unlled polymer [1416]. Layered montmorillonite (MMT) or nanoclays (NCs) are newly invented nanollers in polymers for extraordinary improvements in mechanical behaviors of polymer matrix. Fig. 1 shows three typical forms of MMT inside polymer matrix. MMT is composed by stacks of nanoclay platelets. They can provide signicant improvement to the mechanical properties of polymer matrix due to their high aspect ratio of the nanoclay platelets and thus provide better interaction between the NCs and the matrix. The hydrophilic nature of the clay could lead to incompatibility with most hydrophobic polymeric materials. Thus, chemical modication on the clay or polymer resin or both has been carried out to enhance the interaction between the clay and the polymer [17]. The surface of the MMT is commonly modied with a cation exchange technique to expand the basal spacing and make the layered silicate compatible with most hydrophobic polymer matrices [18]. Modication of the hydrophilic clay surface was also carried out using a silane coupling agent. According to Dean et al. [19] the inter-gallery spacing of 3-(acryloxy)propyldimethylmethoxysilane (APDMMS) modied MMT was increased effectively. Ha et al. [20] demonstrated that the tensile strength and elastic modulus of 3-aminopropyltriethoxysilane (3-APS) modied MMT/E nanocomposites are higher than those of unmodied MMT/E. Ha et al. [21] also reported that modifying MMT using APS causes expansion in the interlayer galleries, which improves the dispersion of MMT into the E matrix. According to Wang et al. [22] improvements in the modulus and fracture toughness of E were achieved by incorporating silanemodied clay. Lam et al. [23,24] have studied the effects of nanoclay clusters in NCs and the results showed that there was an optimum nanoclay wt.% inside NCs in order to possess the highest mechanical reinforcement. It was found that the maximum hardness can be achieved for the nanoclay content at 4 wt.%. Further increasing the amount of nanoclays resulted in decreasing the hardness of the NCs. MMT as ller in thermoplastic/thermoset polymers has already been a matter of study [2532]. Recently many attempts were made to develop epoxy resin composites modied by nanollers to improve the mechanical and tribological performance of the epoxy matrix [33]. Clay has received much attention as a reinforcing material for polymers because of their potentially high aspect ratio ranging from 100 to 1500 and unique intercalation/exfoliation characteristics. MMT frequently exhibits unexpected properties including reducing gas

permeability, improved solvent resistance, and superior mechanical and enhanced ame retardant properties [31]. Researchers continue to show increased interest in the study of epoxy-layered silicate nanocomposites mainly because these nanocomposites exhibit a wide range of improved properties after modication. Wang et al. [34] found that the wear resistance of unsaturated polyester/ MMT was better than that of unsaturated polyester, but the reduction of friction coefcient is not obvious. Wang and Pinnavaia [35] used a special surface treatment for nanoclay and studied the mechanical properties of nanoclay/Epon 828 nanocomposites. Yasmin et al. [36] used three-roll mill for high-shear mixing and dispersion of Cloisite 30B nanoclay in a DGEBA based Ciba-Geigy GY 6010 epoxy resin and observed an improvement of about 80% in the modulus with 10 wt.% nanoclay. Zunjarao et al. [37] studied the effect of two types of processing IKA high-shear mixing and ultrasonication on the mechanical properties of Nanomer 1.30E/Epon 862/ Epikure 3274 nanocomposites. They reported a higher modulus ($40% for 6% by weight of nanoclay) for nanocomposite processed by IKA high-shear mixing than those processed by ultrasonication. Keeping these aspects in mind, it was decided to study the dry sliding wear behaviour of OMMT lled epoxy nanocomposites. The objective of this work is to study the dry sliding wear behaviour of OMMT lled epoxy nanocomposites and explore the tribological parameter and mechanisms that account for the change in the wear behaviour in the presence of OMMT as ller. A plan of experiments, to acquire the data in a controlled way has been designed on the basis of Taguchi technique. 2. Experimental procedure 2.1. Materials The epoxy resin (Epon 828) with an epoxy equivalent weight of 188 g/mol and the curing agent (diethyl toluene diamine (Epikure W)) with an amine hydrogen equivalent weight of 45 g/mol were supplied by M/s MillerStephenson Chemical Company, Inc. USA. The OMMT used was Nanomer 1.30E supplied by M/s Nanocor, Inc USA. This organo-modied montmorillonite (OMMT) was surface treated with octadecylamine surfactant for good dispersion in an amine cured epoxy resin. The physical properties of the OMMT used in the present study are listed in Table 1. 2.2. Nanocomposite fabrication Pre-calculated amount of the epoxy resin, OMMT, and curing agent were mixed using IKA high-shear mixer (T-T18 ULTRA

Fig. 1. Scheme of different structure of composite arising from the intercalation of layered silicates and polymers: (a) phase separated microcomposite, (b) intercalated nanocomposite, and (c) exfoliated nanocomposite.

4530 Table 1 Physical properties of OMMT particles. Physical properties Color d(001) (nm) Average particle size (lm) Organic modier Bulk density (g/cm3) Cationic exchange capacity Aspect ratio Surface area (m2/g) Youngs modulus (GPa) Tensile strength (GPa)

Rashmi et al. / Materials and Design 32 (2011) 45284536 Table 2 Summary of experimental conditions. Montmorillonite (nanomer 1.30E) Off white 2.34 810 Octadecylamine 1.90 130 meq/100 g 2001000 750 175 1 Sample name (designation) Neat epoxy (Ep) 2 wt% OMMTEpoxy (2OMMT-Ep) 5 wt% OMMTEpoxy (5OMMT-Ep) 7 wt% OMMTEpoxy (7OMMT-Ep) Sliding distance (m) 1000 1000 1000 1000 2000 2000 2000 2000 3000 3000 3000 3000 4000 4000 4000 4000

Table 3 Control factors and levels used in the experiment. Control factors Levels I II 1 20 2 2000 III 1.5 30 5 3000

TURRAX Basic) at an operating speed of 24,000 RPM for 45 min. The temperature during mixing was maintained at about 60 C. After mixing, the mixture was degassed in a vacuum chamber for about 45 min. Then, the mixture was poured into aluminum moulds and degassed for 30 min. After degassing, the aluminum moulds were placed in an oven and the materials were cured at 177 C for 150 min. Based on the literature [23,24], the present work of OMMT/epoxy samples were fabricated by high-shear mixing process with different amounts of OMMT namely 0 wt.% (0OMMT-Ep), 2 wt.% (2OMMT-Ep), 5 wt.% (5OMMT-Ep) and 7 wt.% (7OMMT-Ep) respectively. 2.3. X-ray diffraction and transmission electron microscopy The interlayer distance of OMMT in the epoxy nanocomposites were studied by wide angle X-ray diffraction (XRD). XRD was recorded for both OMMT and OMMT lled epoxy nanocomposites, using X-ray diffractometer (RIGHKU-Make) and copper Ka target was used. The basal spacing reection of samples was calculated from Braggs equation by monitoring the diffraction angle 2h from 26 at scanning rate of 0.5/min. Transmission electron microscopy (TEM) images of neat epoxy, 2 and 5 wt.% OMMT lled epoxy nanocomposites were prepared to understand the extent of the intercalation/exfoliation of OMMT in epoxy. 2.4. Microhardness test Microhardness test was conducted to all the samples and a total of ve indentations were measured on the sample surface as per ISO 6507 [38]. Microhardness tester (Zwick 3212) of the Zwick GmbH & Co., Germany, was used in the test. To increase the accuracy of measurement, all sample surfaces were polished using high-grade sand paper prior to the test. 2.5. Dry sliding wear test A pin-on-disk setup, (ASTM G99 standard, Make: Magnum Engineers, Bangalore) was used for the dry sliding wear tests [39]. A surface (6 mm 6 mm 2.5 mm) of the composite specimen, glued to a pin of 6 mm diameter and 22 mm length has contact with a hardened alloy steel disc with hardness value of 62 HRC and surface roughness (Ra) of 0.250.30 lm. The summary of the experimental conditions and plan of experiments by Taguchi method for the present work are listed in Tables 2 and 3 respectively. The test samples were polished against a 600 grade SiC paper to ensure proper contact with the countersurface. The surfaces of both the sample and the disc were cleaned with a soft paper soaked in acetone and thoroughly dried before the test. The pin assembly was initially weighed to an accuracy of 0.0001 g in an electronic balance (Mettler Toledo). The difference between the initial and nal weights is the measure of sliding wear loss. Three

A: Sliding velocity (m/s) B: Normal load (N) C: Filler content (wt.%) D: Sliding distance (m)

0.5 10 0 1000

samples were run for each combination of the test parameters employed. The results reported are thus the average of three readings and the relative deviation in wear loss was below 12%. The wear was measured by the loss in weight, which was then converted into wear volume using measured density data. The specic wear rate (ks) was calculated from the following equation:

ks

V d L

where V is the volume loss in m3, L is the load in Newton and d is the sliding distance in meters. 2.6. Scanning electron microscopy The surfaces of the worn out samples were examined directly by a scanning electron microscope (JSM 840A model of JEOL make). Before the examination, a thin gold lm was coated on the worn out surface by sputtering to get a conducting layer. 2.7. Experimental design In this study, using Taguchi method, a powerful tool for parameter design of the performance characteristics was used to determine optimal parameters settings for minimization of sliding wear [4042]. Taguchis parameter design can optimize performance characteristics through the setting of design parameters and reduce the sensitivity of the system performance to the source of variation [43]. The wear tests on the composites are carried out under different operating conditions considering four parameters, viz., sliding velocity, normal load, ller content and sliding distance each at three levels as listed in Table 3 in accordance with L9 (313) orthogonal array as per the design of experiments. The impact of these four parameters were studied using L9 (34) orthogonal design. The tests were conducted as per experimental design given in Table 3 at room temperature. In conventional full factorial experiment design, it would require 34 = 81 runs to study four parameters each at three levels, whereas, Taguchis factorial experiment approach reduces it to only nine runs offering a great advantage in terms of experimental time and cost. The characteristic is that the lower value represents a desired response, such as sliding wear, lower the better (LB) is used. The S/N ratio can be calculated as a logarithmic transformation of the loss function from the following equation.

S=N ratio 10 log 10

  1 2 y n

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where y represents response sliding wear and n denotes the number of experiments. The plan of the experiments is as follows: the rst column is assigned to sliding velocity (A), the second column to normal load (B), third column to ller content (C) and the fourth column to sliding distance (D). 3. Results and discussion 3.1. X-ray diffraction and transmission electron microscopy Fig. 2 shows the XRD pattern in the range of 2h = 0 6 for OMMT, neat epoxy and OMMT lled epoxy nanocomposites. The XRD pattern of the OMMT shows a broad intense peak at around 2h = 3.8 corresponding a basal spacing 23.0 (By using Braggs law 2d sinh = nk, where k is the X-ray wave length (1.54 ), 2h = 4.2). However they show shoulder at 2h = 2. This is a clear indication that only a portion of nanoclay is intercalated. Becker et al. [44] and Chin et al. [45] have reported a similar observation in the case of Epoxy/layered silicate (MMT) nanocomposites. The

absence of the characteristic clay d(001) peak indicates the exfoliation of the clay platelets in the epoxy matrix. The TEM images of the prepared samples for neat epoxy, 2 and 5 wt.% OMMT lled epoxy nanocomposites are shown in Fig. 3ac respectively to understand the extent of the intercalation/exfoliation achieved. Fig. 3b reveals that in 2 wt.% of OMMT lled epoxy nanocomposites, we observe completely delaminated and uniformly dispersed ller in the epoxy matrix with minimum interlayer spacing. However, in 5 wt.% OMMT epoxy nanocomposite, the interlayer spacing of at least 10 nm is observed.

3.2. Microhradness and wear volume Fig. 4 shows the experimental measurements of microhardness of neat epoxy and epoxy nanocomposites with different OMMT ller loading. From the gure, it is clear that the microhardness (Hv) increased from 14.5 of the neat epoxy to 19.6 in 5 wt.% of OMMT lled epoxy nanocomposites. This implies a maximum increment of 35%. It has been shown that a composite with a higher hardness value will be accompanied with lower wear rate and friction coefcient [46]. Note that the hardness increment is more signicant up to 5 wt.% of ller loading. The higher Hv for 5 wt.% lled epoxy composite is thought to result partly from the intrinsic hardness of OMMT and these nanoparticles might impose better resistance against epoxy segment motion under indention. However, further loading of ller from 5 to 7 wt.%, the increase in hardness is marginal suggesting that higher ller loading gives rise to poor dispersion and agglomeration in the epoxy matrix. Further, it might not be able to elaborate the full strengthening capability in hardness improvement. It seems that the 5 wt.% nano-OMMT particles could be more uniformly distributed and contributed to the continuous hardness improvement. Plots of wear volume and specic wear rate (ks) as a function of sliding distance for neat epoxy and OMMT lled epoxy nanocomposites are shown in Figs. 5 and 6 respectively. From the plot shown in Fig. 5, it was noticed that the wear volume loss increases with increase in sliding distance for all the samples. The sliding between neat epoxy and a at steel countersurface ground to

Fig. 2. XRD pattern of OMMT and OMMT lled epoxy nanocomposites.

Fig. 3. TEM images of (a) neat epoxy, (b) 2 wt.% OMMT lled epoxy, and (c) 5 wt.% OMMT lled epoxy nanocomposites.

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Fig. 4. Micro-hardness of OMMT lled epoxy nanocomposites.

Fig. 7. Scanning electron micrograph of neat epoxy at 30 N, 1 m/s. (a) Lower magnication, and (b) higher magnication. Fig. 5. Wear volume as a function of sliding distance of neat epoxy and OMMT lled epoxy nanocomposites.

obvious from the wear data (Fig. 6) that the ks of neat epoxy is linear up to 2000 m and increases nonlinearly up to 4000 m. The OMMT lled epoxy nanocomposites except 7 wt.%, the ks decreases almost linearly with increase in sliding distance. Epoxy containing 5 wt.% of OMMT had the smallest ks, while the ks of neat epoxy increased to some extent at an excessive content of OMMT particles (>5 wt.%), possibly owing to the poor adhesion of the nano-particles by the epoxy matrix and the conglomeration of the nanoparticles at a too high ller content. With the addition of 5 wt.% OMMT in epoxy, the ks decreased by 7080% (Fig. 6). This behaviour is in agreement with that of the tensile strength and hardness (shore-D) results listed in Table 4. It is already known that majority microllers are more effective in reducing the wear of different polymers. There is scientic and technological need to develop an understanding of the action of nanollers reducing the wear. In the case of neat epoxy, wear
Fig. 6. Specic wear rate as a function of sliding distance of neat epoxy and OMMT lled epoxy nanocomposites. Table 4 Physico-mechanical nanocomposites. Samples

properties

of

neat

epoxy

and

OMMT

lled

epoxy

arithmetic average surface roughness of 0.250.30 lm, under a load of 30 N and at 1 m/s, resulted in a specic wear rate of 10.54 105 mm3/Nm for 1000 m sliding distance (Fig. 6). Wear volume loss showed an upward trend in the gradient, as the sliding distance increased, noted for neat epoxy (Fig. 5). This result may be due to an increase in temperature which occurred during the wear process. The order of wear resistance behaviour of epoxy nanocomposites is as follows; 5 > 2 > 7 > 0% by weight of OMMT as ller. It is

Tensile strength (MPa) 47.50 31.56 37.95 33.79

Tensile modulus (GPa) 1.44 1.73 1.90 2.09

Elongation at break (%) 10.39 10.50 11.30 9.35

Hardness (Shore-D) 76 80 83 85

Density (g/cm3) 1.1699 1.1768 1.1819 1.1828

Ep 2OMMT-Ep 5OMMT-Ep 7OMMT-Ep

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Fig. 8. Scanning electron micrograph of 5 wt.% OMMT lled epoxy at 30 N, 1 m/s. (a) Lower magnication, and (b) higher magnication.

debris consists of shear deformed polymer matrix containing broken pulverized matrix particles and wear powder of the metallic countersurface. The particles can either be lost from the contact zone or remains there for a xed time as a transfer layer. In such cases, their polymer component can cushion the countersurface asperities and reduce the effective toughness, but the pulverized matrix particles and wear powder of the metallic countersurface can act as a third body abrasive leading to enhanced roughening of the countersurface. Thus, ks of the neat epoxy depend on the account of various particles in the wear debris. During wear process, no transfer lm was formed on the countersurface leading to higher ks for neat epoxy. The wear volume loss is low for OMMT lled epoxy nanocomposites compared to neat epoxy. At the start of sliding, the two surfaces of all the asperities were in contact with each other. As shear forces were applied, the asperities deformed. The OMMT particles protrude out from the surface of the sample. Initially, epoxy matrix wears out and only OMMT nanoparticles remain in contact with the countersurface. As sliding distance increases the wear rate decreases. The OMMT nanoparticles wear out the steel countersurface. Due to extreme hardness of the countersurface, OMMT nanoparticles adhere to the matrix and excess ller concentration was noticed on the composite surface after prolonged sliding. During sliding, a rolling effect of nanoparticles could reduce the shear stress, the frictional coefcient, and the contact temperature. For the OMMT lled epoxy nanocomposites, a three-body contact condition was induced by the addition of nanoparticles between the contact surfaces, which is evidenced by the grooves on the worn surfaces (Figs. 8a and b). Hence, it was proposed that during the sliding process many of the hard particles were embedded in the soft polymeric transfer lms on the countersurface and grooved the sample surface. In this way, the distance between the countersurface and the sample was also enhanced i.e., the particle acted as spacers. This in turn, can cause a reduction in the adhesion

between the contacting surfaces. Therefore, the coefcient of friction of OMMT lled epoxy was always less than that of neat epoxy. Moreover, as the nanoparticles were free to move, they tend to be dispersed uniformly over the transfer lms during the wear process, which would result in a more uniform contact stress between the contact surfaces and in turn minimizes the stress concentration. This ensured that the specic wear rate of OMMT lled epoxy was lower under higher sliding distance. The addition of nanoparticles into epoxy changed the contact conditions for OMMT lled epoxy versus countersurface and effectively reduced the friction force. Due to the abrasiveness of hard nanoparticles, a polishing effect on the worn surface could be expected. The ability of nanoOMMT to improve the tribological behavior is increased with decreasing particle size of nanometer-OMMT. In the present work, the wear-resistant epoxy nanocomposite which was lled with small size OMMT particles (<40 nm) transferred well to the counterface and its transfer lm was thin, uniform and adhered strongly to the countersurface. Thus, the improvement in the tribological behavior of nanometer-OMMT lled epoxy composite is related to the improved characteristics of the transfer lm. In general, the friction and wear properties do always describe the whole tribological system rather than a material property alone. Suresha et al. [4751] examined the inuence of microstructure on the tribological performance of various ller lled glass epoxy composites. They conformed that the dispersion state of the microparticles and micro-structural homogeneity of the llers improve the wear resistance signicantly. When the micro-structural homogeneity of the microcomposites was improved, their wear resistance could be increased signicantly. The graphite akes dispersed in the epoxy and glass fabric reinforced epoxy composite lead to interfacial strengthening and increased wear resistance [4749]. The high interfacial adhesion between the matrix and graphite is due to more uniform dispersion of microparticles. Ravikumar et al. [50] and Suresha et al. [51] studied the abrasive wear of graphite/SiC lled in glass fabric reinforced epoxy composites and concluded that the graphite ller increased the specic wear rate and SiC decreased the specic wear rate of glassepoxy composite. The phenomenon reported in the present work is similar to what is reported in Refs. [4751]. However, a further increase in ller loading leads obviously to a deterioration of the specic wear rate. A change in wear mechanism could be involved which may be ascribed to the large amount of OMMT particles causing a higher abrasive wear. Some aspects of the reinforcing role that ceramic microparticles can play in the tribological behaviour were studied by Durand [52], who found that large particles protect the matrix better than smaller ones because they can shield the polymer if they are not pulled out. Small particles, on the other hand, were removed and then involved in an abrading wear process. Hardness contribution also plays a vital role in wear property improvement as reported elsewhere [53]. Important characteristics of nanocomposites have to be considered in order to explain this phenomenon. The quality of the interface in nanocomposites, usually play a very vital role in the materials capability to transfer stresses and elastic deformation from the matrix to the llers [54]. If the llermatrix interaction is poor, the nanoparticles are unable to carry any part of the applied load. In that case, the wear resistance cannot be greater than that of neat polymer matrix. If the bonding between the polymer matrix and llers is instead strong enough, the yield strength of the lled composite can be higher than that of the neat matrix [55]. In the same way, the difference in reducing the friction coefcient and improving the wear resistance ability of neat epoxy and OMMT lled epoxy composites should result mainly from the adhesion strength of the llermatrix. Based on the experience from various studies, Friedrich et al. [56] concluded that ne particles contribute better to the property improvement under sliding

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Rashmi et al. / Materials and Design 32 (2011) 45284536 Table 6 Response table for signal to noise ratios. S/N ratio (db) 89.34 90.54 106.55 94.00 91.90 101.51 90.48 101.41 86.91 Level 1 2 3 Delta Rank Velocity (A) 95.48 95.80 92.94 2.86 4 Load (B) 91.27 94.62 98.33 7.05 2 Filler content (C) 97.42 90.48 96.32 6.94 3 Distance (D) 89.94 94.18 100.65 11.26 1

Table 5 Experimental design (L9 orthogonal array) with output and S/N ratio. Test run 1 2 3 4 5 6 7 8 9 Velocity (A) (m/s) 0.5 0.5 0.5 1.0 1.0 1.0 1.5 1.5 1.5 Load (B) (N) 10 20 30 10 20 30 10 20 30 Filler content (C) (%) 0 2 5 2 5 0 5 0 2 Distance (D) (m) 1000 2000 3000 3000 1000 2000 2000 3000 1000 ks (mm3/Nm)

3.41 10 2.97 105 4.70 105 2.00 105 2,54 105 8.40 105 2.99 105 8.50 105 4.51 105

wear conditions than larger particles. A similar trend was conrmed by Xing and Li [57] recently on the spherical silica particles lled epoxy when particle size varied from 0.12 to 0.51 lm. In the present work, the results are showing the similar trend. In view of this, the bulk of the load is supported by the ller, resulting in increased wear resistance of the composite. Also, the nanoller improved the adhesion of the transfer lm to the countersurface and thereby suppressed the wear process. When epoxy comes in contact, adhesive wear occurs and the wear rate increases. The wear rate decreases at a faster rate after the sliding distance of 2000 m. Better wear resistance was obtained by the addition of 5 wt.% OMMT particles. During sliding the OMMT particles get smeared at the interface forming a thin lm which reduced the specic wear rate. In the present case, OMMT nanoparticles had polishing effect on the hard steel, reducing the abrasive effect on the nanocomposite wear. 3.3. Worn surface morphology The SEM examination of worn surfaces of neat epoxy and OMMT lled epoxy nano composite samples against steel countersurface under 30 N load and at 1 m/s sliding velocity are given in Figs. 7a and b and 8a and b. Fig. 7a and b presents the features of worn surfaces of neat epoxy. Arrow lines marked show the sliding direction. At lower

magnication, the worn surface was relatively rough and associated with microcracks in the matrix (Fig. 7a). At higher magnied SEM (Fig. 7b), damage to the matrix is higher resulting in more matrix removal from the surface. The wear loss and consequently the contact temperature were greatly increased, which caused an accelerative breakage of the matrix especially in the interfacial region. As a result, the surface damage remarkably increased with grooves left by the matrix removal (Fig. 7b). Fig. 8a and b shows the worn surfaces of 5 wt.% of OMMT lled epoxy nanocomposites tested under 30 N and 1 m/s. In comparison with Fig. 7a and b, it was clear that the worn surfaces were much smoother at the same sliding conditions and the matrix detachment was greatly limited with the addition of OMMT nanoparticles. It should be noted that from Fig. 8 that the wear debris size and shape also change for OMMT lled epoxy. The debris becomes rounder and ner compared to that seen in Fig. 7 when the ller is absent. These ne particles develop patches of compacted material as seen in Fig. 8a and b. Fig. 8b shows at a high magnication the makeup of the compacted material formed by the accumulation of the wear debris. The worn surface preformed was relatively smooth and characterized by micro-surface damage due to fatigue wear, which normally occurs at high temperatures and removes the surface layer by microcracks. A patch consist of worn particles held together by thermo-mechanical processes involved in sliding, specically hardening owing to frictional heat, and further compression owing to the normal applied load. Therefore, with the addition of OMMT nanoparticles, surface integrity was maintained in the matrix with a very gradual wear process even at high load and velocity conditions and led to an enhanced load-carrying capacity of the nanocomposite. Further, for selected samples, the wear trace widths of the samples during sliding process were

Fig. 9. Effect of control factors on specic wear rate.

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measured using scanning electron microscope. The maximum and minimum trace width for the neat epoxy is 50 lm and 25.35 lm respectively. However, in 5 wt.% OMMT lled epoxy nanocomposite the trace width is 27.69 lm18.46 lm respectively. From the trace width data, it can be concluded that OMMT lled epoxy nanocomposite has minimum trace width and hence enhanced the wear resistance. 3.4. Wear characteristics analysis by Taguchi method The experimental results were also analyzed using Taguchi method and the signicant parameters affecting material wear, identied. The results of the Taguchi analysis are as follows: From Table 5, the overall mean for the S/N ratio of the wear rate is found to be 85.264 db. Fig. 9 shows graphically the effect of the three control factors on specic wear rate. The analyses were made using MINITAB 15, a popular software specically used for design of experiment applications. The possible interactions between the control factors must be considered, before any attempt is made to use this simple model as a predictor for the measurement of performance. Thus factorial design incorporates a simple means of testing for the presence of the interaction effects. The S/N ratio response are given in Table 6, from which it can be concluded that among all the factors, sliding distance is the most signicant factor followed by normal load and ller content while the sliding velocity has the least or almost no signicance on wear rate of the OMMT lled epoxy composite. Analysis of these results leads to the conclusion that combination of factors A2, B3, C1 and D3 gives minimum specic wear rate as shown in Fig. 9. 4. Conclusions The study shows the successful fabrication of neat epoxy and OMMT lled epoxy nanocomposites. XRD and microstructure analysis (TEM) of neat epoxy and its nanocomposites were performed. The dry sliding wear of the neat epoxy and OMMT lled epoxy nanocomposites were examined by routine experiments and also by using Taguchis design of experiment method. The following conclusions can be drawn:  The dry sliding wear performance of neat epoxy and OMMT lled epoxy nanocomposites are in the following order: Ep < 7OMMT-Ep < 2OMMT-Ep < 5OMMT-Ep. This can be explained from an examination of the variation of wear volume loss and specic wear rate.  At higher sliding distance, the abrasive wear mechanisms could govern the interaction between the surfaces in contact. In this condition the wear resistance of neat epoxy could be increased by lling the matrix with OMMT nanoparticles. In particular, from the tests conducted, the dry sliding wear behaviour of 5 wt.% OMMT lled epoxy nanocomposites are better compared to neat epoxy and with higher OMMT ller lled epoxy nanocomposites.  Dry sliding wear response of these nanocomposites under different loads and sliding velocities can be successfully analyzed using Taguchis experimental design method. Taguchis method provides a simple, systematic and efcient methodology for the optimization of the control factors. While sliding distance emerges as the most signicant factor affecting wear rate of OMMT lled epoxy nanocomposites, other factors like load, ller content and sliding velocity have been found to play a significant role in determining the specic wear rate.  OMMT nanoller play an important role to improve the wear resistance of polymer composites. According to SEM observations, the worn surfaces of nanocomposite should have a nanoscale rolling effect of nanoparticles which may govern the significant enhancement of the wear resistance of the epoxy.

 The present experimental results indicate that in the context of application as a bearing material (journal bearings and sliding components), the performance of OMMT lled epoxy nanocomposite is good and possibly superior to neat epoxy.

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