3.1. Wear Investigation
3.1.1. Lip Seal Specimen
Due to the weight of the embedded particles in the polymer sample adding to the total measured mass, the mass loss does not give an accurate representation of the wear rate. In the wear test, results not only from the material loss from the specimen but also the gain from the embedded particles are evaluated together. The specific wear rate of polymers was calculated by dividing the measured mass loss by the density of the polymer, with the applied normal load and the sliding distance. The results are shown in
Figure 3.
Similar to the research by Amenta et al. [
33] in the case of two-body abrasion tribosystems, the wear rate of the reinforced PTFE is above the neat PTFE. However, when testing on the steel counterface with Martian regolith, this was not the case. LHS-1 and MGS-1 regoliths have a more significant impact on the wear rate of PTFE-based materials than the reference quartz sand. PEEK counterface seemed to cause more wear on the seal specimen than 34CrNiMo6. It could be possibly explained by the more pronounced regolith particle embedding in the softer counterface, acting as a two-body system. It was confirmed from the visual inspection of the counterfaces that the PEEK was more covered with embedded regolith particles. Furthermore, in the case of PEEK, adhesion also contributes to the wear process, further degrading the seal material. Although it would result in a more prevalent tribo-layer, it is damaged by the third-body abrasive particles, and the beneficiary effects are mitigated.
The specimen height was continuously registered during the sliding.
Figure 4 shows the different test cases. The specimen height is not only influenced by the wear of the sample but also by the infiltrated and embedded third-body particles, as well as the formed tribo-layer on the counterface.
The initial height increase at the start of the tests was the highest (~10–180 µm) in the case of the LHS-1 regolith, suggesting that the specimen was running on a layer of particles. The quartz sand had a reduced effect on the initial run setting. Not only the particle size and angularity are responsible for this, but also the packing density of the external regolith. In the case of the steel counterface tests, a clear decreasing trend could be established for the seal specimen height with increasing sliding distance.
For the PEEK counterfaces, the trend is not so straightforward due to the additional adhesion mechanism, e.g., in the case of LHS-1 regolith on PEEK with PTFE seal specimen, around ~380 m, the specimen height starts to increase. This could be attributed to the dynamic three-body mechanism, with a balance of constant adhering transfer layer formation with particle embedding compensated with wear and tear-off of the layer. In the case of lunar regolith and steel counterface, the general three-body abrasion process was observed on a smaller scale. The process starts with a short running-in period of ~10–20 m, where the micro geometry of the softer specimen is transformed, and the roughness peaks are adjusted. The third-body particles enter the contact zone, leading to an increase in wear (displacement between counterface and pin sample). This converges into a dynamic process, a cyclic equilibrium state (steady state). The particles slide and roll between the contacting surfaces and may get embedded. Then, they abrade the surface material to the point where it breaks apart, allowing new particles to enter the contact zone and embed again.
In the case of Martian regolith, the wear does not increase substantially before decreasing again, as with the LHS-1 particles. Rather, it displays a logarithmic decreasing trend. After the running-in period, a tribofilm is formed, decreasing the wear rate. The formed tribo-layer lowers the wear rate by reducing direct contact between the pin and counterface by protecting the polymer from the counterface asperities [
34]. The transfer layer is formed during the running-in phase by depositing polymer material in the roughness valleys of the counterface. Hence, the contact transitions from a polymer/steel contact to a polymer/partial polymer/partial steel contact. Research shows that MoS
2 as a filler has a beneficial effect on the formation and durability of the transfer layer [
35,
36], which could be confirmed by comparing the results of neat PTFE with MGS-1 on steel counterface (
Figure 4a) and with PTFE+GF+MoS
2 specimen with MGS-1 on steel counterface (
Figure 4b).
When investigating the tests on the PEEK counterface with lunar/Martian regolith, the increase in specimen height is more significant than with a steel counterface. This shows that the PEEK countersurface allowed particles to enter the contact zone, which embeds more easily in the PEEK surface than in steel, making it easier to embed in the pin samples. As a result, a thicker regolith layer lifts the pin from the PEEK disc more permanently than on the steel surface.
Figure 5 shows an example of the Martian regolith-covered PTFE seal surface, indicating a formed transfer layer, as well as embedded external particle agglomerates.
3.1.2. Wear of Packings
The packings have an uneven surface topography, which allows particles to be easily introduced in the contact zone, and this could explain the experienced fluctuations in the wear graphs. The trapped particles contribute to the increased mass of the samples after the test. For this reason, the wear rate is not representative of the wear of the PTFE and PTFE+AF packings and will not be taken into account. A wear analysis will be based on the online registered height of the specimen and the post-test surface analysis.
Figure 6 shows the effect of external abrasive particles on the wear of packing specimens. The wear of the packing samples on steel counterfaces (
Figure 6a,b) varies more compared to the lip seal samples in
Figure 4. The range of height loss extends from 20–60 µm for lip seal to 250–400 µm for packing materials. Some graphs show a sudden increase/decrease in the specimen height, indicating a sudden layer removal from the packing due to abrasion. An example of this is visible in the case of neat PTFE packing tests on steel counterface with quartz particles (
Figure 6a), where a sudden drop in specimen height occurred at ~300 m sliding distance, indicating loss of material. It could be linked to the partial removal of the top layer of the packing sample, as shown in
Figure 7. Also, the dislocated fibers might roll under the packing sample, causing the registered height to rise. When the fibers and soil particles are removed from the contacting area, the packing sample height lowers again.
The data from the PTFE+AF specimen tested on steel with MGS-1 regolith and the PTFE+AF specimen tested on PEEK with LHS-1 are incomplete. The tests have been attempted more than three times, but the specimen was always torn apart immediately after start or after reaching a maximum of ~30–50 m sliding; therefore, these packing seal materials are not considered suitable for Martian or lunar conditions. The data are shown until the point of failure indicated by a sudden drop of >1000 µm in the specimen height. The lines show an increase in displacement just before the point of failure, suggesting that many particles were suddenly introduced in the contact zone. This led to an increase in the CoF and, ultimately, the failure of the pin sample with a torn top layer. The term failure rather than the wear of the two packing specimens gives a more accurate approach to the nature of the failure. When comparing the braided structure of natural PTFE with its composite version, it was observed that the disintegration and slipping of the braided fibers in the composite specimens occurred more rapidly. This accelerated degradation is attributed to the impregnation of the composite fibers with a mixture of solid lubricant and wax, which reduced inter-fiber friction compared to natural PTFE fibers. The enhanced sliding behavior of the composite resulted in an increased specific surface area, facilitating the accumulation of regolith within the impregnated lubricant.
Figure 6c,d indicate the result with the PEEK counterface. Similar to the conclusion concerning the range of the height loss in the case of steel counterface, testing on PEEK resulted in more broad values compared to the lip seal specimen. The range increases from 100–200 µm to 250–400 µm for the lip seals and packing samples, respectively. When testing PTFE+AF with MGS-1 on the PEEK counterface, the particles were immediately introduced in the contact area at the start of the test, increasing the height (wear) displacement to ~180 µm. In general, LHS-1 regolith caused more fluctuations and particle embedding (
Figure 6b) or wear (
Figure 6c) than other external particles.
3.2. Friction Analysis
Figure 8 shows the influence of external abrasive particles on the coefficient of friction of the lip seal specimen. The friction curves showcase the main friction components: adhesion and surface deformation, which are influenced by the embedding and erratic movement of regolith particles. These effects vary according to the properties of the contacting surfaces and the tribological system. This complex third-body phenomenon has been extensively described in the literature [
37]. In the initial stages of the sliding in all test systems, during the running-in, the regolith particles enter the contact zone with varying dynamics. Subsequently, a macro-trend emerges, representing the dynamic equilibrium of friction. This equilibrium is characterized by localized transient behaviors influenced by the specific attributes of the tribological system. On steel surfaces, quartz sand resulted in a relatively uniform third-body mechanism. The distinct compositions and adhesion characteristics of LHS-1 and MGS-1 regoliths led to contrasting friction patterns between the natural and composite PTFE lip seal specimens. The lower grain-embedding capability of the harder composite PTFE resulted in more consistent friction with MGS-1 regolith compared to natural PTFE pin. In the case of the PEEK countersurface, the higher adhesion tendency between the polymers prevailed, particularly in the presence of quartz sand, while in the case of LHS-1, the process was characterized by friction instability.
Figure 9 shows the effect of external abrasive particles on the coefficient of friction for packing specimens. The tests with packing specimens were only partially suitable for studying friction differences since the structural integrity of the braided structure is broken during sliding. Unlike the block sealing material tests, these experiments were influenced by the complex, inhomogeneous 3D surface formed by the woven fibers. These fibers, with micro- and macro-grooves, deform differently under normal loads depending on whether they are natural or composite PTFE braids. The gaps between the fibers act as localized traps, effectively retaining regolith particles and slowing their movement through the contact zone, similar to the principle of a labyrinth seal. While beneficial for sealing purposes, these trapped abrasive particles intensify countersurface cutting and friction instability, depending on the type of regolith.
Figure 9a,c illustrate these phenomena, which are particularly pronounced with natural PTFE braided pins on PEEK surfaces when LHS-1 regolith was applied. On the steel surfaces, the integrity of the composite packing pins was prematurely lost due to the fiber separation, preventing the completion of the measurements.
3.3. Surface Analysis
The post-mortem 3D topography analysis revealed a reduction in surface height within the wear track of the counterface disc materials attributed to abrasion caused by the polymer sample with the external particles. An example is shown in
Figure 10, where the blue region represents the wear track with reduced surface height.
The scale bar in the 3D images highlights the difference in height between the wear track and the unaffected surface. Across all steel counterfaces, the lip seal samples resulted in a surface height reduction of approximately 0.01 to 0.02 mm, regardless of the regolith type. In comparison, the packings caused a larger reduction between 0.02 and 0.03 mm. Within the wear track, the average surface roughness of Ra of the steel counterfaces also decreased by approximately 0.1 µm. Abrasion likely removed the roughness peaks, smoothing the surface and lowering roughness compared to the unaffected areas. Furthermore, adhesion may have facilitated the formation of a polymer transfer layer on the steel counterface, with possible compaction of regolith particles deposited in surface valleys. The reduction of ~25% in the mean roughness depth (Rz) values on the steel surfaces indicates this phenomenon. For the steel counterfaces, the wear tests produced an evenly distributed wear track with no distinct grooves or peaks. Both lip seal and packing samples exhibited minimal transfer layers. No significant differences were observed between the pure PTFE and PTFE+GF+MoS
2 lip seal samples or between the pure PTFE and PTFE+AF packing samples. The observed visible discoloration of the wear track is likely due to the adhesion of regolith particles, as the color of the wear tracks closely matched that of the respective regoliths. This effect was more noticeable on PEEK counterfaces than on steel. While the steel counterfaces showed limited wear, the pin samples, especially the lip seal samples, displayed clear signs of abrasion (
Figure 11).
The steel counterfaces showed no clear evidence of embedded particles, regardless of regolith or seal material. As the PTFE lip seal samples are softer, hard particles tend to create grooves or are embedded in the lip seal surface rather than in the steel. This caused significant wear on the lip seal surface with visible grooves, adhesion of small dust particles, and embedding of larger particles. Quartz soil caused only minor abrasion and adhesion on the lip seal samples, resulting in slight scratches and discoloration. Lunar regolith produced deeper grooves and small embedded particles on the lip seal surface. The Martian regolith resulted in the most severe effect, with large cuts and visible embedded particles on the lip seal surface (
Figure 11).
The PEEK counterface was more susceptible to abrasion than steel. Embedded particles and adhesion of smaller dust particles were observed. Moreover, PEEK had a notable impact on the embedding of abrasive particles in the lip seal surfaces. Larger particles from lunar and Martian regoliths were often embedded in the lip seal samples, as shown in
Figure 12 and
Figure 13. The PTFE+GF+MoS
2 composite displayed larger embedded particles than pure PTFE. The PTFE/PEEK sliding tests clearly demonstrated the three-body abrasion mechanism, where abrasive particles penetrated the lip seal surface and subsequently cut into the PEEK surface. Unlike steel, the PEEK surface exhibited signs of embedded and adhered quartz soil particles.
Figure 12a,b show the combined effects of abrasion and adhesion within the wear track on a PEEK counterface tested with PTFE+GF+MoS
2 with LHS-1 regolith. Abrasion had a more pronounced impact on the PEEK counterface material due to its lower hardness compared to 34CrNiMo6 steel. Clear, distinct grooves could be identified on the pin surface, formed by harder lunar regolith particles embedded in the PTFE composite pin, as shown in
Figure 12c,d.
The abrasion and adhesion zones on PEEK counterfaces were more pronounced in the case of the PTFE+GF+MoS
2 lip seal samples tested with Martian regolith, as shown in
Figure 13a,b. Hard abrasive particles penetrated the surface of the PTFE composite more easily than the virgin PTFE lip seal samples when sliding on the PEEK counterface, regardless of the regolith type. The surface of the PTFE+GF+MoS
2 pin is shown in
Figure 13c,d.
The Martian regolith caused limited embedding of hard particles on the PEEK surface, as the larger particles were primarily embedded in the lip seal samples. This resulted in an uneven surface, with distinct zones of abrasion and adhesion on the PEEK counterface. The adhesive zones had smooth surfaces with no embedded particles, whereas the abrasive zones on the PEEK surface contained embedded hard particles. The opposite was true for the lunar regolith, where the adhesive zones along the edges of the wear track had a higher concentration of embedded particles (discoloration in optical images) compared to the abrasive zones in the center of the wear track. The extraterrestrial regolith particles were embedded in the lip seal surface, creating grooves in the PEEK counterface. The edges of the lip seal samples were also worn off. 3D surface topography of PEEK counterface tested with PTFE and quartz sand and the embedded several quartz particles in the PTFE pin are highlighted in
Figure 14.
The packing samples caused similar effects on the PEEK counterface as on the steel surfaces. Regolith particle adhesion to the PEEK surface was less significant with packing samples. The transfer layer was minimal, and no significant roughness peaks or valleys formed due to abrasion or adhesion. Only the PTFE+AF/PEEK/Quartz tribosystem showed clear graphite adhesion on the PEEK surface, as shown in
Figure 15. The packing samples did not produce significant grooves on the PEEK surface. This indicates that while particles entered the packing/PEEK contact zone more easily, they did not penetrate deeply enough to form grooves on either surface. The packing samples seemed to provide some protection to both the PEEK and steel shaft surfaces from abrasion and particle embedding. However, the packing material itself showed limited wear resistance, as evident from clear signs of layer removal and fiber detachment.
The results further highlight the benefit of incorporating external packing materials in the tribosystem. Overall, the wear behavior of the seals was significantly influenced by the material composition and environmental conditions. PTFE filled with 15 wt% glass fiber and 5 wt% molybdenum disulfide (PTFE+GF+MoS2) enhances wear resistance and reduces friction compared to unfilled PTFE under similar abrasive conditions. PEEK counterfaces exhibited greater susceptibility to embedded particles, facilitating three-body abrasion mechanisms. The inclusion of fillers, e.g., glass fiber in PTFE, was observed to improve the formation of protective tribo-layers, mitigating direct material loss and enhancing durability under dynamic contact conditions. The effect of the specific abrasive environment is further investigated. The quartz sand, characterized by its larger particle size, caused increased vibrations during sliding but resulted in minimal particle embedding. Its spherical shape particles likely rolled between the surfaces, reducing wear and penetration. Neither steel nor PEEK counterfaces showed significant grooves or particle embedding, and the wear rates for both seals were the lowest among all tested conditions.
The LHS-1 regolith exhibited greater adhesion than quartz, causing dust to adhere to surfaces and particles to embed in lip seals and PEEK counterfaces. This led to the formation of grooves and higher material removal, particularly on PEEK, which, combined with lunar regolith, resulted in the highest wear rate for the PTFE+GF+MoS2 samples. Steel counterfaces, in contrast, had relatively low wear rates. An adhesive layer formed at the edges of the wear tracks in lip seal tests, with less pronounced effects in packings.
The Martian MGS-1 regolith was the most adhesive, causing significant adhesion on both counterfaces and seals. Particle embedding was more prominent in lip seals than packings. Steel counterfaces showed minimal effects, while PEEK had uneven zones with distinct areas of abrasion and adhesion. MGS-1 regolith caused the highest wear rates for pure PTFE lip seals sliding on steel. The CoF was similarly influenced by the lunar and Martian regolith.