Wear 263 (2007) 1243–1248 Short communication Optimization of steel wool contents in non-asbestos organic (NAO) friction composites for best combination of thermal conductivity and tribo-performance Jayashree Bijwe ∗ , Mukesh Kumar Industrial Tribology Machine Dynamics and Maintenance Engineering Centre, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India Received 13 September 2006; received in revised form 4 January 2007; accepted 6 January 2007 Available online 23 May 2007 Abstract Thermal conductivity (TC) of friction composites plays a vital role in the performance of the composites. Low TC renders the tribo-surface vulnerable for degradation of organic ingredients and affecting the braking capability adversely. Too high TC, on the other hand, results in adverse effect on brake-fluid. The optimum TC as a result of tailoring the composite with right contents of metallic fillers is hence desired. However, hardly any in depth efforts are placed in this direction. Hence, in this work, three friction composites were developed using same ingredients in same proportion except steel wool and barite which were added in a complementary manner. The compositions containing 4, 8 and 12 wt.% of steel wool (and inert filler barite in 31, 27, and 23 wt.%) were developed as brake-pads and designated as S1 , S2 and S3 , respectively. The brake-pads were tested for their friction and wear behavior on a Krauss type RWDC 100, 450 V/50 Hz machine in simulated braking condition against a cast iron commercial disc and evaluated as per ECR 90 test schedule. It was observed that with increasing metal contents, mechanical properties decreased, TC increased slowly and other important friction properties including fade resistance improved. Wear properties however, did not show any correlation with amount of steel wool, TC or mechanical properties. Overall, composite S3 proved to be the best performer. SEM studies proved helpful in understanding the wear mechanism. © 2007 Elsevier B.V. All rights reserved. Keywords: Non-asbestos organic (NAO) friction composites; Thermal conductivity; Fade and recovery; Brake-pad materials 1. Introduction Non-asbestos organic composite friction materials are being increasingly used in automotive brake disc pads and clutch facing applications. They are essentially multi-ingredient systems in order to achieve the desired amalgam of performance properties [1] amongst which the coefficient of friction and its stability under various operating conditions, such as temperature, pressure and speed is most important. The four categories of ingredients, viz. binders, fibers, friction modifiers and fillers based on the major function they perform apart from contributing towards friction and wear performance are selected. Binders mainly from phenolics or modified phenolics provide mechanical integrity to the friction material while fibers, such as mineral, ceramics, organic and metallic types provide mainly the strength. ∗ Corresponding author. Tel.: +91 11 26591280; fax: +91 11 26591280. E-mail address: [email protected] (J. Bijwe). 0043-1648/$ – see front matter © 2007 Elsevier B.V. All rights reserved. doi:10.1016/j.wear.2007.01.125 Friction modifiers, such as abrasives and solid lubricants are used to achieve the desired range of friction. Fillers the fourth class is again subdivided as functional fillers (to enhance the specific function, such as resistance to fade, thermal conductivity, etc.) and space fillers/inert fillers (just to cut the cost without any adverse effect on performance properties). The effect of such ingredients on tribo-performance [2–4] and fade and recovery behavior [5–11] is extensively studied in the literature. Thermal properties, such as specific heat, thermal conductivity (TC), diffusivity, thermal expansion, etc. also play a vital role in performance of brake-pads, especially when braking is severe. Low TC renders the tribo-surface vulnerable due to accumulation of frictional heat which leads to the degradation of organic ingredients and affects the braking capability adversely. Too high TC on the other hand, results in adverse effect on brake-fluid because of conduction of heat towards piston and brake-fluid via back plate. The optimum TC as a result of tailoring the composite with right contents of metallic fillers is hence desired. In spite of this fact, literature pertaining either to the ideal range of these 1244 J. Bijwe, M. Kumar / Wear 263 (2007) 1243–1248 parameters or influence of such ingredients on these parameters is not available. Moreover, it is also important to note that an ingredient added to tailor a specific property of a composite may influence other important performance properties in a beneficial or undesirable manner and hence has to be monitored. Any research papers could not be available on the optimization of thermal conductivity and tribo-performance of friction composites. Hence, in the present work, three NAO composite were developed by varying steel wool and barite (inert filler) in compensatory manner keeping apparent composition unaltered. Since influence of thermal conductivity is best reflected in severe operating conditions, fade and recovery mode of performance testing was selected in the present work. The comparative studies along with worn surface analysis are reported in this paper. Fade indicates the loss in braking effectiveness of a material at elevated temperature (typically in the range 300–400 ◦ C) because of a reduction in the kinetic friction coefficient (μ). High fade is undesirable since it affects the deterioration in efficiency and reliability of brakings in severe operating conditions. The recovery term is used to quantify the revival of μ when the pad gets cooled after severe brakings. Since fade and recovery behavior indicates the potential of composites in very harsh operating conditions, it was selected for this research study. 2. Experimental 2.1. Fabrication of the composites The fabrication of composites containing twelve ingredients was based on keeping parent composition of 10 ingredients (65%, w/w) constant and varying two ingredients, viz. steel wool and barite (35%, w/w) in complementary manner as shown in Table 1 based on a systematic increase in steel wool (4, 8 and 12 wt.%). The parent composition contained straight phenolic resin (10%), functional fillers, such as alumina, graphite, vermiculite, cashew dust (27%, w/w) and fibers, such as glass, PAN, Lapinus, Aramid and brass (28%, w/w). The ingredients were mixed in a plough type shear mixer to ensure the macroscopic homogeneity using a chopper speed of 2800 rpm and feeder speed 1440 rpm. The addition of ingredients during mixing was in a particular sequence. Aramid and glass fibers were mixed initially for 2 min followed by other pulpy materials and finally by powdery materials. The mixing schedule was of ten minutes duration. The mixing sequence and time of mixing of each lot of ingredients lead to proper uniformity in the mixture. If mixing time is low, proper homogeneity cannot be achieved. If it is too high, it does not improve the homogeneity further. Hence, it has to be optimized which was done in the laboratory in earlier Table 1 lists the varying ingredients in composites Ingredients S1 (wt.%) S2 (wt.%) S3 (wt.%) BaSO4 Steel wool 31 4 27 8 23 12 Total 35 35 35 work [12]. The mixture was then placed into a four-cavity mould supported by the adhesive-coated back plates. Each cavity was filled with approximately 80 g of the mixture and heat cured in a compression-moulding machine under a pressure of 8 MPa for 7–8 min at curing temperature. Three intermittent ‘breathings’ were also allowed during the initiation of curing to expel volatiles. The pads were then removed and were then post-cured in an oven at 100 ◦ C for 8 h. The post curing operation is done to cure the residual resin. As per standard practice in the literature after optimization, it is done at 100 ◦ C for 8 h to ensure complete curing of the resin [12]. The surfaces of the pads were then polished with a grinding wheel to attain the desired thickness and smooth surface. Three composites were designed as S1 , S2 and S3 accordingly (Table 1). 2.2. Characterization of the composites For mechanical strength testing, test bars were fabricated as per ASTM standards. Composites were characterized for physical (density, water swelling, heat swelling, void contents) (details of the methods are given in Appendix A) and chemical properties (acetone execration). All the results are shown in Table 2. Thermal conductivity was measured as per ASTM-E1461-01 standard on FL-3000 Flash line instrument supplied by Anter Corporation, USA. Square samples of size 10 mm × 10 mm and thickness 2–3 mm were used for TC measurement at room temperature. Thermal conductivity of a commercial brake-pad (composite C) was also measured to compare with that of developed composites. (The Fade & Recovery study on this material, however, was not done because details of its ingredients were not available. The data on TC and Fade & Recovery studies could not be correlated with the composition.) 2.3. Test set-up and procedure for fade and recovery evaluation by ECR 90 test schedule The fade and recovery tests were conducted using a Krauss type RWDC 100 C (450 V/50 Hz) machine discussed elsewhere [11–12]. A gray cast iron rotor disc of the passenger car (Maruti Suzuki 1000 cc) with radius 0.12 m and average roughness (Ra ) value 3.28 m was used as a counterface. Details about testing method are explained elsewhere [13]. The software computes the various values (as shown in Table 3) as an essence of fade Table 2 Mechanical properties of the composites evaluated in the laboratory Properties S1 S2 S3 Density (g/cc) Acetone extraction (%) Water absorption (%) Void content (%) Heat swelling (%) Tensile strength (MPa) ASTM D638 %Strain (ASTM D638) Flexural strength (MPa) ASTM D790 Flexural modulus (GPa) (ASTM D790) %Strain (ASTM D790) 2.27 0.169 0.60 37 1.54 22.56 3.10 46.65 11 0.53 2.29 0.141 1.05 39 2.78 20.47 2.97 44.64 10.7 0.49 2.32 0.181 0.70 40 2.94 17.57 2.72 38.74 9 0.49 J. Bijwe, M. Kumar / Wear 263 (2007) 1243–1248 1245 and recovery plot. The various performance parameters derived from the plots are defined in Appendix B. Wear volume of the composites was calculated using weight loss and the density of the materials. The change in roughness of the discs after the test was also measured. SEM studies on worn surfaces were also carried out to understand the wear mechanisms. 3. Results and discussion As seen from Table 2, it was observed that the density of composites showed increasing trend because of addition of steel wool which is heavier than the filler barite. Acetone exaction indicates amount of uncured resin in the composites which was negligible in all the composites. Void contents increased with increase in steel wool. The heat swelling also showed the same trend as anticipated because of higher expansion of steel wool. All the mechanical properties, (tensile and flexural) decreased with increase in contents of steel wool and decrease in barite%. It could be because of the fact that barite being powdery filler has better binding capacity with the resin rather than steel wool. 3.1. Fade and recovery behavior Seven steps of friction assessment test are shown in a single graph. Three such graphs for selected composites (S1 , S2 and S3 ) are shown in Fig. 1(a–d). Following trends were observed from the seven step friction assessment test graphs for the composite. In composite S2 large fade was observed after fifth braking during cold cycle, while in S1 and S3 comparatively quite less amount of fade was observed after fifth and eighth brakings, respectively. During fade cycle S2 showed maximum fluctuations in μ which is not a desirable feature for friction materials. In other two composites, after first few braking cycles, fluctuations reduced drastically as seen in plateau regions. Such behavior is desirable for good friction material. The constant speed (660 rpm), constant interval (5 s) and constant pressure (1.82 MPa) R-90 frictional response of the three composites is summarized in Table 3. It incorporates the performance μ, the fade μ, the recovery μ, temperature rise in disc and wear volume of pads. A clear trend was observed in all composites with the increase of steel wool content in most of the properties. μperformance , μrecovery , μfade and μmax increased with increasing content of steel wool which a desirable feature. Percent of fade also showed fixed pattern. With increase in steel wool, tendency of fade decreased. In case of %recovery, however, no fixed trends were seen. The values did not vary much. Temperature rise in the disc should be as low as possible and termed as one of the important parameters called counterface friendliness. In this case, composite S1 (419 ◦ C) performed better than other two composites S3 (431 ◦ C) and S2 (456 ◦ C). Interestingly, wear behavior of composite S1 was also far superior to the other composite. In literature, general trends show that the friction and wear performance do not go together. If friction behavior is good, wear performance is poor and vice versa [11]. However, wear performance is of secondary importance than the friction performance. Based on above-mentioned discussion it was confirmed that increase in metal contents, led to Fig. 1. Fade and recovery cycles for composites: (a) S1 , (b) S2 and (c) S3 . improvement in friction performance (μperformance ) and fade tendency. μperformance improved from 0.371 to 0.407 while %fade decreased from 18 to 11% (Table 3). Thus, S3 proved to be the best performer followed by S1 . S1 though proved best in wear performance, it was poor in friction performance. It was also confirmed that wear and mechanical properties of the composites Table 3 ECR 90 frictional response of the composites Properties S1 S2 S3 μperformance μrecovery μfade μmin μmax %Fade %Recovery Wear of pads (×10−6 m3 ) Temperature rise of disc (◦ C) Ra (original-worn sample) (m) 0.371 0.370 0.304 0.250 0.446 18 100 2.5 419 2.723 0.386 0.411 0.329 0.193 0.499 14.7 106 6.7 456 2.755 0.407 0.416 0.361 0.246 0.482 11.4 102 3.4 431 2.815 1246 J. Bijwe, M. Kumar / Wear 263 (2007) 1243–1248 Table 4 Thermal properties of the composites S1 , S2 , S3 and C Properties (cm2 /s) Diffusivity Specific heat (J/kg K) Conductivity (W/m K) S1 S2 S3 C 0.0099 1039.2 2.39 0.0104 1116.2 2.43 0.0107 1233.8 2.51 0.0091 1001.3 2.15 did not show any correlation. Mechanical properties deteriorated with increase in steel wool while wear did not show any trend in this context. Table 4 shows the thermal properties of all composites at ambient temperature. Data on commercial sample in identical conditions are also included. As expected thermal conductivity increased with increasing content of steel wool. For commercial sample TC value was found 2.15 W/m K. For S1 almost 11% increase in TC value was observed while for S2 and S3 it was 13 and 16%, respectively. Thus, the increase in steel wool led to the increase in TC and hence more efficient dissipation of frictional heat. Higher the dissipation lower was the surface temperature and hence lower was the degradation of organic contents in the composite and hence lower tendency of fade. Though this was anticipated while tailoring the composites, effect of increasing contents of steel wool on other performance properties could not be anticipated. Present studies brought out interesting features. The increase in steel contents not only increased the TC and decreased the fade tendency, but also helped to improve other friction related parameters. The μperformance , μrecovery and μfade , increased which are desirable features of the good friction composites. The difference between μmax and μmin (μ) shows Fig. 2. SEM micrographs of composites S1 , S2 and S3 . J. Bijwe, M. Kumar / Wear 263 (2007) 1243–1248 1247 Fig. 3. SEM micrographs of corresponding discs D1 , D2 and D3 . undulations in friction behavior. This was best for S1 (0.196) and poorest for S2 (0.306). For S3 , it was moderate (0.236). Increase in temperature of the disc indicates counterface friendliness of the materials. It should be as low as possible. Table 3 shows that S3 was moderate in this respect while S1 was best. Thus, based on the studies, metallic contents up to 12% proved to be beneficial from most of the angles. However, the studies on composites with further increase in the amount of steel wool were not performed, which could lead to optimization of steel wool contents for best combination of friction and TC values. 3.2. Microscopy and wear mechanism Wear performance of the composites was in the order, S1 > S3 > S2 . The reasons for lowest and highest wear of S1 and S2 , respectively, could be observed in SEM studies of worn surfaces as shown in Fig. 2. Micrographs 2a1 , 2b1 and 2c1 are for worn surfaces of composites S1 , S2 and S3 at 500× magnification while 2a2 , 2b2 and 2c2 are for S1 , S2 and S3 at 1000× magnification. When micrographs 2a1 , 2b1 and 2c1 or 2a2 , 2b2 and 2c2 are compared, surface of S2 showed largest number of secondary plateaus of very big size. (Micrograph 2b2 shows half the portion filled with single secondary plateau.) Such plateaus originate from the back transfer of the degraded organic materials from the disc. They do not have load-bearing capacity and affect the wear performance adversely. These micrographs also show the primary plateaus which contain the original ingredients along with wear debris. These contribute in rejuvenating friction performance and controlling wear. When the micrographs are compared, extent of secondary and primary plateaus was lowest and highest, respectively, in S1 supporting its best wear behavior. In case of S2 , the situation was exactly reverse supporting its poorest wear performance. For S3 , which showed moderate wear behavior, the surface topography supported this since it showed moderate size and number of secondary plateaus. Fig. 3(3a1 , 3b1 and 3c1 ) shows the corresponding worn disc surfaces at 500× magnification. The surface was heavily covered with thick layer of friction film. In case of D2 worn against S2 which showed highest wear, the tribo-layer was thickest and patchy supporting heavy transfer of organic materials from the composite due to severe operating conditions. For composite S1 (lowest wear), on the other hand, tribo-layer was very thin and coherent (D1 ). Worn surface D3 showed totally different features. Hardly any patchy transfer was seen on the surface. A thin film of uniform thickness was observed through out the surface. Surface was covered with scorching marks (white spots) and not the patches of organic degraded materials. These are the spots appearing on the surface due to mild scratching followed by discoloration on micro-level (not apparent by naked eyes) in hot conditions. An additional micrograph of D3 (Fig. 3c2 ) at lower magnification (100×) was also included to show the different features on the disc. The friction layer/friction film/tribo-layer/secondary plateaus terms are used by the researchers to describe the effect of back transfer of organic materials from the disc to the pad. This back transferred materials is generally responsible for the deterioration of friction behavior by reducing the μ, 1248 J. Bijwe, M. Kumar / Wear 263 (2007) 1243–1248 which is undesirable feature. It influences wear behavior also in adverse way. The secondary plateaus are generated on the pad surface because of back transfer of organic material, such as resin (charred, degraded and softened), Aramid fibers, cashew nut shell liquid (CNSL) powder, graphite, etc. These plateaus do not have adhesion to the pad material as good as that of original ingredients. Hence, these do not have good load bearing properties resulting in deterioration in friction and increase in wear. A.3. Heat swelling Heat Swelling was measured by SAE J 160 JNU80 standard. Thickness of the sample (10 mm × 10 mm × 4 mm ) from the brake pad at six different places was measured accurately at room temperature. The process was repeated after heating the sample in oven at 200 ± 2 ◦ C for 2 h. The increase in thickness was recorded as heat swell & percentage was calculated. Appendix B 4. Conclusions Definitions of friction coefficient in fade and recovery studies. Based on studies on three composites containing increased amount of steel wool (4–12%, w/w) at the cost of inert filler (barite), it was confirmed that the higher the wool contents, better was the friction performance in fade and recovery mode, higher was the resistance to fade. However, wear did not show any correlation with wool contents. SEM studies indicated the tendency of secondary plateaus formation was maximum in the composite which showed highest wear and vice versa. Metal contents (12 wt.%) proved to be most beneficial for tailoring the tribo-properties. Thermal conductivity played a vital role in controlling friction and wear behavior. Higher the steel wool amount, higher was the TC and better was the performance. Acknowledgements Authors acknowledge funding by Department of Science and Technology (Govt. of India) to carry out this work and Mr. B.S. Tomar (Manager R&D) Allied Nippon Ltd. Sahibabad (India) for extending the facility of Krauss tester. Appendix A μmin : this is lowest coefficient of friction for cold, fade and recovery cycles. μmax : this is highest coefficient of friction for cold, fade and recovery cycles. μperformance : this is average of coefficient of friction taken after 1 s for fade and recovery cycles at temperature greater than 100 ◦ C. (The requirement of this varies from vehicle to vehicle. For a small sized car, μ in the range 0.4–0.45 is required while that for racing cars range of 0.5–0.6 is required. For heavier vehicles or medium sized cars, it should be in the range 0.3–0.35.) μfade : minimum coefficient of friction for the fade cycle taken after 270 ◦ C. %Fade: (μperformance − μfade ) × 100/μperformance (lower fade% is desirable for a good friction composite). μrecovery : maximum coefficient of friction for the recovery taken after 100 ◦ C. %Recovery: μrecovery × 100 /μperformance (desirable 100–120% for a good friction composite). 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