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Simple, fast, and versatile methods for the quantification of thiol groups are of considerable interest not only for protein analysis but also for the characterization of the surface chemistry of nanomaterials stabilized with thiol ligands or bearing thiol groups for the subsequent (bio-) functionalization via maleimide−thiol chemistry. Here, we compare two simple colorimetric assays, the widely used Ellman’s assay performed at alkaline pH and the aldrithiol assay executed at acidic and neutral pH, with respect to their potential for the quantification of thiol groups and thiol ligands on different types of nanoparticles like polystyrene nanoparticles, semiconductor nanocrystals (SC NC), and noble metal particles, and we derive criteria for their use. In order to assess the underlying reaction mechanisms and to obtain stoichiometry factors mandatory for reliable thiol quantification, both methods were studied photometrically and with electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS), thereby demonstrating the influence of different thiols on the reaction mechanism. Our results underline the suitability of both methods for the quantification of directly accessible thiol groups or ligands on the surface of 2D- and 3D-supports, here exemplarily polystyrene nanoparticles. Moreover, we could derive strategies for the use of these simple assays for the determination of masked (i.e., not directly accessible) thiol groups like disulfides such as lipoic acid and thiol stabilizing ligands coordinatively bound to Cd and/or Hg surface atoms of II/VI and ternary SC NC and to gold and silver nanoparticles.
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.
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.
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.
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.
The solid lubricant molybdenum disulfide is a well known material for extreme conditions where conventional oil or grease lubrication is not feasible (vacuum, high pressures). However, under reactive environments e.g. high humidity or hydrogen MoS2 is prone to premature failure. By using a PVD process, deposition parameters can be optimized to gain coatings with a more textured structure orienting the basal planes parallel to the Substrate surface, A similar concept has been used by Koch et al. for coatings developed to withstand the extreme operational conditions of the WENDELSTEIN W7-X fusion experiment. Therefore, an improved tribological behavior even under adverse conditions can be achieved.
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.
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.