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This paper presents investigations on the tribological behaviour of PTFE composites against steel at cryogenic temperatures. The results showed that the friction coefficient decreases with temperature down to 77 K, but did not follow a linear evolution further down to extreme low temperatures. It can be stated that the cryogenic environment has a significant influence on the tribological performance of the polymer composites. The effect of low temperatures was more clearly detected at low sliding speed, where friction heat is reduced. A change in wear mechanism from adhesive to abrasive was observed in this case. SEM and AFM analyses showed that the PTFE matrix composites investigated under these experimental conditions have transferred material onto the disc down to very low temperatures. Chemical analyses indicate the presence of iron fluorides.
Friction systems running in cryogenic environment are critical in respect to wear and frictional heat generation because in this temperature range, conventional lubricants can't be applied. In order to test the friction and wear behaviour of appropriate solid lubricants and wear resistant material combinations in cryogenic environment, including liquid hydrogen, special test rigs have been constructed. These devices provide test conditions for tribological investigations at temperatures ranging from 4.2K to room temperature in liquid or gaseous environment at pressures between 10-3 mbar and 20 bar. Investigations on polymers, composites and metals with and without coatings show that there is a broad variety of appropriate materials for cryogenic friction units, but the behaviour of austenitic steels in such systems gives an example of non sufficient knowledge in this field.
Windings in superconducting magnets operating at 4.2 K are highly susceptible to quenching caused by small frictional heat inputs. Small movements in the magnet system are inevitable during ramping due to the increasing electromagnetic forces. Friction pairs of polymer based materials have been investigated at 4.2 K to gain an understanding of their sliding behavior in conditions representative of superconducting MRI systems. The results indicate that polymer-polymer pairs experience unstable sliding behavior with repeated stick-slip whereas polymer-aluminum couples have stable sliding behavior up to high contact pressures of 20 MPa.
In a future energy supply system based on renewable sources hydrogen technology will play a key role. Because the amount of energy from renewable sources, such as wind or solar power, differs seasonally and regionally, an energy storage method is necessary.
Hydrogen, as an environmentally friendly energy carrier, can fill this gap in an ideal way, in particular for mobile applications (Wurster et al., 2009). Already today, in Germany the amount of hydrogen as a byproduct in chemical industry is enough for fuelling about 1 Mio passenger cars1. Excess electrical power can be used to produce hydrogen by electrolysis. On demand, this hydrogen can be used for mobile or stationary fuel cells. Beside this new developing technology, hydrogen is used as fuel for rocket engines and in chemical industry since a long time. Table 1 comprises some physical parameters of hydrogen. It can be seen that hydrogen gas has a very low density which makes storage at high pressure or in liquid form (LH2) necessary.
This paper presents the mechanical and tribological properties of
Polytetrafluoroethylene (PTFE) and Polyetheretherketone (PEEK)
matrix composites filled with short carbon fibers in cryogenic
environments. Tensile tests were performed at room temperature (RT)
in air and in LN2. Tribological experiments were carried out with a
pin-on-disc configuration at RT, in LN2, in LH2 and in LHe. PEEK
composites have a better tribological performance than PTFE materials
especially regarding the wear resistance.
Supporting elements between large superconducting magnets like the field coils in WENDELSTEIN 7-X have to sustain high loads while allowing a certain amount of tangential movement without any stick-slip motion. In model tests with reciprocating friction in liquid helium and vacuum a PVD-MoS2-coating has proven its suitability for these components. It showed a very stable sliding behaviour with a friction coefficient below 0.1 without coating failure under all test conditions.
For tribological components working under extreme
conditions, such as vacuum, or broad temperature
ranges, it is often a problem to achieve acceptable
durability of their friction parts. Thus, new material
requirements are involved for these tribo-systems, in
particular regarding operability and reliability. At BAM,
several projects were conducted in the recent years,
dealing with the tribological properties of friction
couples at cryogenic temperature and in vacuum
environment. This paper describes the vacuum and ultra
high vacuum tribometers constructed at BAM and
presents experiments carried out with polymer
composites. The experiments presented were performed
with PEEK, filled with solid lubricants, against 304
steel with a pin-on-disc configuration in oscillating
sliding. Friction tests were carried out in vacuum in the
temperature range between -40°C and +160°C and in
ultra high vacuum at room temperature.
Influence of the Temperature on the Tribological Behaviour of PEEK Composites in Vacuum Environment
(2008)
This paper describes tribological experiments carried out with polyetheretherketone (PEEK), filled with carbon fibres and solid lubricants (polytetrafluoroethylene (PTFE), graphite or MoS2), against steel discs. Oscillating sliding tests were performed in high vacuum environment in the temperature range between -40°C and +160°C. Results indicate that MoS2 filled PEEK show the best tribological performance in vacuum. Particularly, in the lower temperature range and at higher loads the friction behaviour is improved by the MoS2 content.
Spacers and supports belong to the critical elements in the structure of a nuclear fusion device, particularly, when they are installed in the vacuum or superconducting magnet system of the reactor. These supports have to sustain high loads while allowing a certain amount of tangential movement with low friction and without any stick-slip motion. Vacuum and cryogenic environments are extremely hostile for smooth sliding systems, because conventional liquid lubricants cannot be employed, and only a very limited number of materials for dry sliding systems under these conditions are available. In order to test the friction behaviour of support elements in the field coils of the fusion experiment WENDELSTEIN 7-X, a test rig was build which allows testing in liquid helium environment at 4.2 K, with a normal force up to 150 kN, and a sliding velocity of 0.1 mm/s in oscillating motion. First tests have shown that the apparatus is appropriate for simulating the sliding behaviour of support elements. As an example, a result of an earlier model test of an MoS2-coating is shown.
In the development of hydrogen technology, special attention is paid to the technical problems of
hydrogen storage. One possible way is cryogenic storage in liquid form. Generally cryotechnical
machines need components with interacting surfaces in relative motion such as bearings, seals or
valves, which are subjected to extreme conditions. Materials of such systems have to be resistant to
friction-caused mechanical deformation at the surface, low temperatures and hydrogen environment.
Since materials failure can cause uncontrolled escape of hydrogen, new material requirements are
involved for these tribo-systems, in particular regarding operability and reliability. In the past few
years several projects dealing with the influence of hydrogen on the tribological properties of friction
couples were conducted at the Federal Institute for Materials Research and Testing, (BAM), Berlin.
This paper reports some investigations carried out with polymer composites. Friction and wear were
measured for continuous sliding and analyses of the worn surfaces were performed after the
experiments. Tests were performed at room temperature in hydrogen as well as in liquid hydrogen.
Cryogenic solid lubrication
(2013)
The main part of a narrow support element (NSE) of the W7-X superconducting coil system is an aluminium bronze pad, PVD coated on its spherical surface with MoS2, which slides against the flat surface of the stainless steel coil housing, coated with MoS2 spray. The operational requirements of the NSEs are: vacuum of p < 10-6 mbar, temperature T ~4 K, maximum load P ~1500 kN, typical displacement ≤5 mm, smooth sliding and no stick-slip events. The paper describes test results obtained with a downscaled NSE at T = 4.2 and 77 K. During the test the NSEs were submerged in liquid helium and nitrogen, respectively. Whereas the LN2 test ran smoothly for up to ~15,000 cycles, the test in LHe showed stick-slip from the very first cycle. The stick-slip disappeared after ~50 cycles. Post mortem analysis of the tested parts revealed that in case of LHe the sprayed MoS2 film was removed during the first 30-100 cycles by blistering and flaking. The reason for the loss of adhesion at LHe temperature is not known, several possible causes are under discussion. Further experiments under vacuum and at T ~4 K are being prepared which are expected to help in clarifying the issue.
The tribological behaviour of MoS2/ta-C double layer coatings deposited by Laser-Arc technology was investigated in vacuum and air. In vacuum environment, the friction coefficient against steel balls varies between 0.005 and 0.02 depending on the contact pressure. At high contact pressures, the friction coefficient is as low as 0.005 and the life time between 340,000 and 500,000 cycles. Furthermore, it is shown that a ta-C base layer improves the performance of MoS2 coating.
Surface analyses were performed before and after the tribological tests by means of SEM, EDX, XRD, and TEM. They show that in the top layer beneath the sliding surface crystallization of the initially quasi-amorphous MoS2 took place. TEM images also verified an orientation of the basal MoS2-lattice planes parallel to the surface.
MoS2 is a suitable solid lubricant for environments free of oxygen or water vapor (i.e. vacuum). Humid air degrades film properties due to oxidation accompanied by high wear and increasing coefficients of friction. The present study aims at the further development of sputtered pure MoS2 coatings, extending their applicability to varying environmental conditions by increasing the resistance against humidity. The systematic coating development process is supported by using an experimental Box–Behnken design with variations of the deposition parameters cathode voltage, target/substrate distance, temperature and argon gas pressure. In contrast to common one-factor-at-a-time (OFAT) studies, this approach enables a determination of interactions between deposition process parameters and tribological–mechanical MoS2 film properties. The tribological improvement focuses on a maximization of wear resistance in air and vacuum measured in ball-on-disk experiments. The evaluated mechanical properties are hardness, elastic modulus and residual stresses. These stresses were determined by the substrate curvature method. The study reveals that the residual stress state in the films and the hardness-to-modulus ratio are crucial for their tribological performance in humid air and vacuum environments. After a detailed determination of the relationships between deposition conditions and film properties, some selected microstructural analyses are presented which show that a substantially basal orientation of the lattice has positive effects on wear but also causes anisotropic film properties which result in fissile fracture of the coating if strong shock or point loads occur.
Due to the rapidly increasing price of tungsten carbide and the significant health risks associated with the wear products of WC-Co (Co3O4 and Wo3), an alternative is required. Niobium carbide (NbC) is well suited as a cutting tool due to its high melting point and low solubility in iron. So far, NbC-Ni cermets best met the requirements of high hardness and toughness. Various secondary carbides such as VC, Mo2C, TiC, but also WC were added to further improve the hardness.
In this presentation tribological investigations on steels, polymers and coatings in gaseous and liquid hydrogen are shown. For steels the results of show that although martensitic steel may suffer from hydrogen embrittlement, application e.g. in roller bearings is possible. On the other hand, martensitic transformation of austenitic steels may cause problems in the application of these materials. Furthermore, the tribological performance of polymer composites with and without solid lubricant fillers in gaseous and liquid hydrogen was investigated. In particular, PEEK- and PTFE-matrix compounds showed low friction and sufficient low wear under these conditions. Among the solid lubricants, carbon-based materials are appropriate for hydrogen applications. Several variants of DLC and ta-C materials were tested. Beside the results for hydrogen, also a comparison with CH4-environment is shown.
The focus of this study is to evaluate the influence of hydrogen on the friction and wear behavior of a wide range of polymer materials. Thereby, the tribological performance of filled und unfilled polymers from different suppliers were compared at room temperature in air and hydrogen gas (H2) as well as in liquid hydrogen at -235°C (LH2).
Increasing demand for alternatives to tungsten carbide (WC) cemented carbides as cutting tools, due to the health risks of their wear products WO3 and Co3O4. Niobium carbide (NbC) has a high potential, due to its high wear resitance, high hot hardness and melting point (3520°C), and low solubility in iron alloys.
A modified pin-on-disc test was applied to determine tribological properties of typical brake pad constituents. Ball-milling of these ingredients together with iron oxide and graphite provided model materials displaying the main features of real third bodies. Solid lubricants like graphite affected the friction and wear behaviour of Fe3O4 powders considerably whereas further addition of hard nanoparticles induced only minor effects. This was corroborated by comparison with modelling results. MoS2 played a dual role. Depending on special conditions, this ingredient either reduced or increased friction. The latter could be explained, after nanoscopic characterization, by oxidation and destruction of the wear-protecting tribofilm.
Superconducting magnets are susceptible to quenching, even with the smallest amounts of energy disturbances due to the extremely low thermal capacity of materials at 4.2 K. Hence, small mechanical disturbances resulting in frictional heating can be sufficient to exceed the wire’s critical temperature, causing it to quench. Unfortunately, relative motion between surfaces in the magnet System is inevitable due to various forces present in the System, including winding pretension, differences in material thermal contraction and the large electromagnetic forces. Typically insulating polymers are present at this interface to achieve the required electrical insulation requirements.
Ensuring a sustainable energy supply is currently one of the most important areas for industry and research institutions. Hydrogen technology is a promising candidate, but its broad extension requires extremely high reliability and safety in all areas for common applications as automobiles and stationary fuel cells. Particularly components containing tribosystems are critical parts.
The sliding performance of PEEK composites was investigated in vacuum environment. Tests were performed with carbon fibre reinforced PEEK composites filled with PTFE, and MoS2 or graphite as further solid lubricant. Polymer samples were tested in a pin-on-disc configuration continuously sliding against CrNi-steel. Depending on sliding speed and temperature, the MoS2 filled composites showed high wear resistance and friction coefficients as low as PVD coatings.
Influence of solid lubricant fillers on the tribological behaviour of peek composites in vacuum
(2009)
For further development of hydrogen technology, it is necessary to have a sufficient number of materials for safe and reliable operation available. Frictional contacts exposed to hydrogen, are critical because of vanishing protective oxide layers in the presence of a chemical reducing environment. Furthermore, liquid lubricants are often not applicable, because of purity requirements, or very low temperatures in the case of liquid hydrogen. Thus, for numerous tribosystems in hydrogen technology, solid lubrication is the only possible method for reducing friction and wear. Therefore, investigations on the tribological behaviour of friction reducing materials, such as PTFE, graphite, DLC and MoS2, in inert and hydrogen environment were carried out. The results show that solid lubricants, applied as coatings or as components in polymer composites, are able to reduce friction and wear in gaseous as well as in liquid hydrogen. However, some materials are very sensitive to the environmental medium.
Besides carbon, metal sulphides are used in every standard brake pad formulation as friction stabilisers. In order to investigate their impact, various powder mixtures were tribologically stressed in a pin-on-disc device in order to produce and test artificial third bodies. containing the three main components of a real friction film, namely magnetite, graphite and a metal sulphide of interest. Since the sliding behaviour is influenced by the relative humidity the powder mixtures are tested at low, medium and high moisture levels. The tests revealed that the presence of graphite dominates the friction behaviour as well as the humidity sensitivity.
The powders were prepared by either manual mixing or high energy ball-milling. Interestingly, all ball-milled blends provided coefficients of friction within the desired range for braking, which was attributed to the effect of zirconia particles from wear debris of the milling balls. The zirconia particles prevent the formation of solid lubricant films on the surfaces and support a homogeneous mixture of all constituents of the powder. Optimum brake performance is gained by an optimum combination of solid lubricants and abrasives.
Molybdenum disulfide (MoS₂) is a well-known solid lubricant for tribosystems running in vacuum or dry gases. Problems arise due to its sensitivity to humidity, which is a drawback for its application under ambient conditions. However, by using a physical vapor deposition (PVD) process, deposition parameters can be optimized not only to gain a coatings structure with favorable frictional properties but also to minimize the sensitivity to attack by water molecules. Therefore, an improved tribological behavior even under moist conditions can be achieved. MoS₂coatings are also candidates for being applied at cryogenic temperatures. They already have proven their suitability, e.g., for sliding support elements between superconducting magnets of the nuclear fusion-experiment Wendelstein 7-X. However, these coatings were exclusively produced for this particular application and the utilization for more common tribosystems may be precluded due to cost considerations. In view of a wider range of applications, pure and Cr containing PVD-MoS₂ coatings with an optimized structure were tested under varying environments including hydrogen gas and cryogenic temperatures. Results of the most promising variant are presented in this paper.
The magnetic plasma confinement system of the nuclear fusion experiment “Wendelstein 7-X”, which recently produced the first plasma, consists of 20 planar and 50 non-planar superconducting coils. To keep them precisely in position, these coils contact each other at special support elements. The supports are operated in high vacuum at a temperature of about 4 K, and when the magnetic field is ramped up, forces up to 1500 kN and sliding motion of some mm occurs. Because mechanical disturbances may cause severe failures, only low friction without any stick-slip behaviour is tolerable. In pre-tests a PVD-MoS2-coating had proven to be the optimum solution. It was tested with downsized samples in reciprocating motion in liquid nitrogen (T = 77 K) and liquid helium (T = 4,2 K). In long-term tests in liquid nitrogen this coating showed stable sliding for up to 14.900 friction cycles without coating failure. However, in liquid helium an unexpected stick-slip effect occurred, whose origin could not be clarified so far.
We applied a combination of Raman spectroscopy (RS) and cross-sectional transmission electron microscopy (X-TEM) to identify silicone oil residues and tribofilms at steel disc surfaces after tribological testing. Neither chemical cleaning nor mechanical removal of a 50 µm thick surface layer produced a surface without any silicone residue. Nevertheless, long-term tribological properties are not affected due to silicone degradation which has been proved by Raman spectroscopy. Excellent anti-wear and anti-friction properties of a nanocomposite at severe stressing conditions correlated with the formation of a silica-based tribofilm containing amorphous and graphite-like carbon nanoparticles. Since reliable carbon quantification by analytical TEM is difficult, RS is a useful complementary method for carbon identification at wear scars.
In order to obtain a better understanding of the role of tribofilms during automotive braking, their structures were investigated and the essential features identified.
Next, different ingredient combinations were studied by preparing some model materials with simpler compositions than real tribofilms. A test method was developed for verifying the tribological properties of the model materials and for comparison with results obtained with numerical sliding simulations of such structures. Prerequisites of good brake Performance properties were identified. Although the coefficient of friction could be varied in a wide ränge, smooth sliding conditions could only be achieved with values smaller than 0.4. Tests with artificial third body powders turned out to be useful as screening method for the selection of raw materials for brake pad formulations.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
The tribological characteristics of pure and graphite filled polymers were investigated in gaseous hydrogen at ambient temperatures and in LH2 at -253°C. It could be shown that the tribological properties of PI and PEEK materials is related to the formation of a transfer film. The influence of both hydrogen and cryogenic temperatures will be discussed in the presentation.
The development of hydrogen technologies is a key strategy to reduce greenhouse gas emission worldwide. Power-to-Gas is a challenging solution, in which hydrogen and methane can be used in mobility, industry, heat supply and electricity generation applications. This presentation deals with the tribological behaviour of polymer materials in hydrogen and methane, both in gas and in liquefied form.
High performance polymer composites have been intensively investigated for tribological applications in air, but rarely in hydrogen environment. Author's previous benchmark of composites in liquid hydrogen (LH2) showed that graphite filled polymers have beneficial friction behaviour in this extreme condition. Therefore, further investigations have been undertaken in hydrogen environment. This paper presents first results obtained with polyimide composites filled with different types (natural, synthetic) and amounts of graphite in air, vacuum and hydrogen environments. A particular attention is taken to the influence of hydrogen on graphite as well as on the polymer matrix.
The influence of hydrogen environment on the friction and wear behavior of polyimide (PI) composites was investigated for two different PI-types (PI1 and PI2) filled with natural or synthetic graphite. Sliding tests were run against AISI 52100 steel and the worn surfaces as well as the transfer film were analyzed by means of SEM, EDX and Infrared Spectroscopy. Results indicate that the chemical structure of the polyimide has a major influence on the tribological behavior. While the friction of PI2 remains rather stable in all environments, PI1 showed very low friction in hydrogen without any lubricant. The lubricity of graphite was found to be more effective in hydrogen than in moist air.