This section details the different behaviors of the contact resistance for both the dry or unlubricated and PFPE- and PAO- lubricated contacts at the set test conditions, and mechanisms responsible for the test failures per contact case. COF experienced by the contacts during the micromotions, and their surface conditions, i.e., the surface degradation resulting from the fretting mechanisms are used to assess the effects of lubricants. Additionally, the influence of factors such as the lubricant’s chemistry, kinematic viscosity, and applied lubricant film thickness on the contact’s fretting performance are also discussed.
3.1 Effect of Lubricant Chemistry
3.1.1 Unlubricated Contact
Unlubricated contacts generally met the test end criteria prior to a million fretting cycles, with one test ending at a maximum of 1.67 million cycles. All the tests demonstrated a similar trend of ECR and COF. Fig. 2 shows the variation in ECR and COF experienced in the test ending at 1.67 million cycles and the corresponding surface condition of the contacts at the end of the test. The ECR trend for unlubricated contacts involved two regions: (1) region LW, indicative of low wear and characterized by a low and stable ECR and lower values of COF, and (2) region HW, indicative of high wear and following region LW, exhibiting a decrease in ECR, and presenting intermittent ECR spikes and an increase in COF. It was observed that ECR in region LW was close to the values measured during stationary test conditions at the beginning of the test.
The introduction of two wear regions gives a quantitative estimation of the expected number of cycles, after which the rate of wear increases between the contacts when observing both the ECR and COF behavior. Region LW has comparatively little wear and is indicated by a COF less than 1 and accompanied by stable ECR. A censored test performed during this region showed the contacts experienced mostly adhesion surface wear with gold-on-gold interaction; the surface wear volume and area were low. However, region HW showed the onset of unstable ECR with intermittent ECR spikes due to the reactive contact metal oxides interfering between the surfaces and direct reactive metal asperity interaction. Additionally, COF went high, indicating higher surface wear due to increased contact friction and subsequent shear, leading to the exposure of underlayers at some wear sites or zones. The continuous occurrence of intermittent ECR spikes above 10 Ω eventually led to the contact failure as per the test end condition.
Two parameters were used to differentiate the wear regions: (1) the in-situ ECR measured at the set contact load during the fretting test and (2) the ECRinit acquired at 10 gf during the stationary test. Among all the tests performed for the unlubricated case, for a region to be termed LW the variation between ECR during the fretting test and ECRinit was within ± 5 mΩ, resembling stable ECR. Consequently, when the ECR variation went outside the ± 5 mΩ bounds, it indicated region HW with ECR dropping below ECRinit - 5 mΩ. As per this condition, unlubricated contacts showed an average duration of 10,000 cycles (23,000 cycles for this test) until the onset of region HW.
The effects of fretting; wear, and corrosion in unlubricated contacts resulted in the wearing of protective gold-plating and the exposure of underlayers on both the pin and the flat surface. EDS analysis of the pin and the flat in Fig. 3 showed the absence of gold in most of the wear regions, the presence of nickel and copper on the pin surface, and nickel-palladium alloy and copper on the flat. Surface mapping of both the contacts detected copper, which is the substrate metal; however, point analysis at several wear locations on the pin detected nickel as well. This was indicative of nickel underlayer thinning at some wear sites, while at other locations, even the underlayer was worn off to expose the copper. For the flat, point analysis at various locations confirmed the presence of a nickel-palladium underlayer where copper was detected as well, indicating underlayer thinning. Due to the exposure of reactive metals—nickel, palladium, and copper—the pin was found to be oxidized with the metal-oxide debris collected primarily at the central dimple, as seen in the pin’s SEM image. Additionally, the flat showed some oxygen mapping where nickel was present, indicating metal-oxide formation. The oxides were primarily observed as wear debris around the wear zone periphery. The exposure of underlayers and reactive metal oxidation resulted in the observed high values of ECR.
3.1.2 PFPE-Lubricated Contact
The tests that did not terminate in region LW progressed toward region HW, marked by a significant decrease in ECR below the stationary test condition value for the respective cases, the appearance of intermittent ECR spikes, and severe surface wear. Contacts in this region operated primarily in the boundary lubrication regime and were characterized by higher COF (above 0.4) and increased contact surface degradation. Fig. 4 shows ECR, COF, and surface wear of a test on a PFPE–A lubricated contact that stopped after entering region HW. Fig. 5 and Fig. 6 show the same for a test on PFPE–B and PFPE–C (2%) lubricated contacts. The duration of region LW was found using the same criteria as in the case of the unlubricated contact. PFPE–A showed an average of around 172,000 cycles, PFPE–B around 69,000 cycles, and PFPE–C (2%) around 81,000 cycles before entering region HW. The PFPE lubricants delayed the start of region HW by 11 times on average compared to the unlubricated contacts. As a result, PFPE–A lubricated contacts completed around 1.5 million fretting cycles on average, with one test lasting for 2.26 million fretting cycles; PFPE–B completed around 1.2 million fretting cycles, and PFPE–C (2%) completed close to 643,000 cycles (maximum completed cycles was 877,250) before meeting the test end criteria.
For the tests that did not terminate in region LW but rather in region HW, EDS analysis of the flat and pin surfaces for PFPE-lubricated contacts detected the presence of the nickel underlayer on the pin surface and the nickel-palladium underlayer on the flat surface; the analysis resulted in occasional detection of copper on either surface at some regions of the wear track. Fig. 7 shows SEM images of the pin and the flat surface and the respective EDS mapping for the PFPE–A test. On both the contact surfaces, the wear zone reveals the underlayer metals; however, concentrations of both the PFPE elements—oxygen and fluorine—were minimal at those locations, indicating the removal of the lubricant, effective metal-metal interaction, and eventual material wear. Point analysis of the pin confirmed the presence of a very thin gold layer over the regions where nickel was detected and the minute presence of nickel-palladium as a result of the underlayer’s material transfer from the flat. The absence of nickel exposure on the pin’s surface ruled out nickel’s oxidation and its oxide debris formation. Similarly, point analysis for the flat confirmed a thin gold layer over the exposed areas where nickel-palladium was detected and the presence of underlayer materials where copper was present. For the PFPE–B and PFPE–C cases, the flat and pin showed similar surface analysis with a thin gold layer over the underlayer metals and the absence of any oxidation. However, for PFPE–C, both the element mapping and point analysis on the pin confirmed the detection of nickel and oxygen and the absence of fluorine and carbon at some wear sites, indicating the probable oxidation of the pin.
Some PFPE-lubricated contact tests terminated in region LW since the rise in ECR during the instability was higher than 10 Ω multiple times and caused the tests to fail. For those cases, the surfaces were observed to have minimum wear, gold-over-gold wear condition, and considerable lubricant film between them. Fig. 8 shows the test with a PFPE–A lubricated contact that stopped in region LW. It was found that the high ECR did not sustain when the measurements were taken at 0.5 Hz, and COF increased between the contacts as well. Figure 8’s ECR and COF vs. displacement graph shows the reduction in ECR measured over the 80-micron wear track at 0.5 Hz (slow speed) immediately after the contact failed at 153,100 cycles (i.e., when ECR at 50 Hz was observed to be higher than 10 Ω for the fifth time). High values of ECR during 50 Hz (i.e., at high speed) and lower ECR measurements at 0.5 Hz demonstrated the effect of hydrodynamic lubrication at increased sliding velocities. Accordingly, an increase in COF from a value of around 0.1 during the start of the displacement along the wear track to 0.2 upon the displacement’s completion was also observed due to the reduction in velocity. As a result, the lubricating film could bear the contact load at a high speed of 50 Hz and minimized effective asperity contact. However, its load-bearing capability reduced as the speed decreased to 0.5 Hz, often allowing more metal-to-metal interaction (Stribeck’s effect). Hence, some PFPE-lubricated tests failed in region LW due to the onset of hydrodynamic lubrication, which increased ECR abruptly while minimizing the surface degradation.
3.1.3 PAO-Lubricated Contact
In general, the PAO-based lubricants demonstrated low and stable electrical contact resistance for longer durations when compared to the unlubricated and PFPE-lubricated contacts, except for PAO–B, which initially showed unstable ECR behavior for about 10,000 cycles only. However, the ECR instability was minimized or eliminated when a 2% (w/w) solution of PAO–B in mineral spirits was deposited onto the flat to obtain a reduced lubricant thickness. All PAO-based lubricated contacts had a similar range of cycles during which the in-situ ECR while fretting decreased to the ECR measured at the stationary test condition, ECRinit, analogous to the unlubricated contact case. This region, also called region LW, was followed by a transition region (TR) characterized by low and stable ECR with decreasing ECR behavior as the cycles increased. TR—defined by an increasing rate of surface wear, wear volume, and COF than region LW—was present for at least four million cycles in all the tests before the contacts failed. In some cases, it continued until the test end condition of 15 million cycles. For both PAO–A and PAO–B lubricated contacts, one test out of four failed. Fig. 9 and Fig. 10 show ECR, COF, and contact surface conditions at the end of tests for PAO–A and PAO–B lubricated contacts, respectively. Each of the remaining three tests for each case ran until 15 million fretting cycles without showing any significant increase in ECR throughout the tests. For the PAO–B (2%) case, all four tests failed at less than one million fretting cycles.
For quantification analysis analogous to the unlubricated contact case, a region HW was defined as well. It was characterized by a sharp decrease in the ECR behavior while fretting and COF shooting beyond a value of 1 during the HW onset, often extending in the range of 1.5 and 2.5 on average before the test end conditions were met. It was observed that all the PAO-lubricated contact tests that did not fail in TR experienced a drop in ECR of around 10 mΩ compared to ECRinit before entering region HW. Hence, an ECR change of more than 10 mΩ during the in-situ fretting determined the onset of region HW, often characterized by increased surface wear compared with contacts failing in TR. This was also confirmed by the increasing COF and decreasing ECR trends and surface analysis post-test end. On average, among all the tests, PAO–A showed six million cycles, PAO–B showed four million cycles, and PAO–B (2%) showed around one million cycles before entering region HW.
EDS analysis of both the pin and the flat surfaces shown in Fig. 11 ruled out the oxidation of the reactive underlayer metals (nickel and nickel-palladium) since the oxygen mapping was absent at locations where the reactive metals mapping was detected for both surfaces. Additionally, no copper was exposed by wear on either of the contacts; this finding was confirmed using point analysis. For the pin, nickel was exposed due to the major gold transfer to the flat surface; however, point analysis confirmed the presence of a thin gold layer over nickel mapping (which supported the absence of oxidation) and stable ECR during region LW and TR. As for the flat, point analysis detected nickel-palladium alloy at a few locations, but it was heavily covered with gold, primarily due to the material transfer phenomenon. The carbon map for both surfaces pointed to the oil’s adherence around the wear zone and throughout the wear tracks.
3.2 Comparison between Lubricants: Reliable Contact Life
Two-parameter Weibull analysis was used to compare the cycles to failure data for all the lubricated and unlubricated tests, as shown in Fig. 12. The analysis indicated that PAO-based lubricated contacts represented a higher contact life and were the most reliable, with survival probabilities of 99.9% for PAO–A, 87.5% for PAO–B, and 62.5% for PAO–B (2%) at 10 million fretting cycles. The survival probability of all the PFPE-lubricated contacts and the unlubricated ones was less than 1% calculated at 10 million cycles; however, at two million cycles, PFPE–A had 41.7%, PFPE–C had 30%, and PFPE–B had 25% as their respective survival estimates. PFPE–C (2%) was the least reliable, even at one million cycles. The evaluation of reliable performance at two million cycles was performed to compare the PFPE-lubricated contacts among themselves and with the unlubricated contact case. It shall be noted that the means of the different lubricated cases were not statistically significant, and the analysis was based on a small sample dataset.
3. 3 Effect of Lubricant Thickness on Fretting Performance
Two different film thicknesses of PFPE–C and PAO–B lubricants were achieved by preparing a solution capable of dissolving the respective lubricant type and altering the solution’s net concentration with dilution. For a fixed solution volume, increasing the lubricant concentration increased the obtained film thickness on the flat after the spin coating process. Two 2% solutions were made, one containing PFPE–C and the other containing PAO–B, the thicknesses of which were confirmed once the solutions were applied. Although the applied film thickness was different from the actual film thickness when the surfaces mated, the difference in film thickness due to change in concentration affected the contact’s performance. On average, thicker lubricating films close to 1 micron resulted in delaying the contacts entering region HW, where contact failure later occurred. Fig. 13 shows how using different lubricant thicknesses can affect the average number of cycles required by the coated contacts before entering region HW for each case. The error bars show the minimum and maximum cycles observed.
The film thickness deposited on the flat for PFPE–C (100%) without any dilution was 30 times thicker than the thickness of PFPE–C (2%). All of the PFPE–C (100%) lubricated contacts failed in region LW due to a surge in ECR, with no significant wear on the surfaces, whereas PFPE–C (2%) lubricated contacts resulted in one failed test in region LW while the remaining contacts failed in region HW. The PFPE–C (100%) lubricated contacts endured five times as many cycles before entering region HW, on average, compared to the PFPE–C (2%) lubricated contacts—although the difference was not statistically significant for the limited set of data. The film thickness obtained for the PAO–B (100%) lubricated contact was about 32 times thicker than PAO–B (2%), and the former contacts underwent four times the average number of cycles before entering the region HW. Thicker PAO–B lubricant film introduced ECR instability for about 10,000 initial fretting cycles, as seen in Fig. 14, which was not observed for PAO–B (2%) cases.
3.4 Effect of Viscosity
The kinematic viscosities of PAO-based lubricants were at least one-third of the PFPEs. While PAO lubricants showed higher contact life and larger duration of cycles during which ECR was stable compared to the PFPE lubricants, kinematic viscosity itself cannot solely account for the observed contact’s fretting performance. While the PAOs’ lower kinematic viscosities improved the contacts’ performance and their useful life, this was not the case when the different PAOs were compared. PAO–A had a higher viscosity among the three tested; however, they also showed higher reliability and increased cycles to failure. This suggests that a lubricant’s chemistry has a significant role to play in the observed differences in contact performances. On the other hand, kinematic viscosity was found to influence the occurrence of the hydrodynamic effect in PFPE-lubricated contacts. PFPE-based lubricant with a higher viscosity, like PFPE–C (2%), would show hydrodynamic behavior sooner than a lubricant like PFPE–B having a lower viscosity value. For quantification of the effect, the hydrodynamic behavior was observed when ECR was greater than 100 mΩ. During the initial 1,000 fretting cycles, ECR instabilities beyond 100 mΩ threshold were not considered to contribute to this effect since the instabilities resulted due to less effective contact area and an initial thick lubricant layer present between the mated contacts causing the ECR to increase. The fretting motion during 1,000 cycles dispersed the lubricant at the contact site and increased the effective contact area, which was also seen from the decreasing ECR values post the starting of the test. This was confirmed from the PAO–B lubricant that a thicker film could introduce such ECR instabilities at the beginning of the test for the initial 1,000 cycles, which over time reduced once the effective contact area increased. Fig. 15 shows how kinematic viscosities of PFPE-based lubricants influence the number of cycles completed before the hydrodynamic behavior of the film appears.
Kinematic viscosity is a lubricant property that is indicative of the resistance to relative motion between adjacent layers in a liquid. Its effect is primarily observed during the hydrodynamic mode of lubrication. A lubricant with higher viscosity possesses a larger load-bearing capacity under the same conditions of speed and load. In the case of PFPE-lubricated contacts, PFPE–C was more viscous, making the lubricated contacts susceptible to shift from boundary lubrication to the hydrodynamic mode of lubrication in shorter time periods than the other two PFPEs having lower kinematic viscosities. Less viscous PAO-based lubricants did not show any hydrodynamic effect later once the initial ECR instability was minimized after a few thousand cycles, as in the case of PAO–B (100%).