Open Access

Lubricating greases enclose oil in porous structures of aggregated thickener particles. Their tendency to separate oil under static conditions is evaluated according to DIN 51817 or DIN ISO 22285 in tests of up to 168 h with the mass fraction of separated oil as result. With an analytical photo-centrifuge, separated oil mass fractions can be tracked in real time in the instrument operating temperature range from 4–60 °C. Due to the higher mechanical load compared to standard tests, the grease samples separate more and faster oil, significantly speeding up the analysis process. Fitting the measured data from both methods with the function wO = wO,∞ exp(−t/tc), the parameters maximum oil separation wO,∞ and characteristic time tc are obtained as measures of oil separation extent and rate. Both parameters help to compare the two methods and to interpret the oil separation characteristics of greases. Using four commercial greases of NLGI classes 0–2, the analytical photo-centrifuge measuring method is presented in detail and its results are discussed in reference to those of standard DIN 51817.

According to the ASTM D97, the pour point is the temperature below which petroleum products cease to flow. To evaluate the relevance of pour point measurements for synthetic lubricating oils, we investigated the crystallization, melting temperature and low-temperature flow behavior of one mineral and five synthetic lubricating oils. The classification of three groups emerged from this process. The formation of paraffin crystals in mineral oils (I) below the crystallization temperature causes shear-thinning behavior and a yield point. The crystallization temperature determined in the thermal analysis and rheology correlates well with the pour point. Synthetic lubricating oils, which solidify glass-like (II), exhibit a steady viscosity increase with falling temperature. The temperature at which viscosity reaches 1000 Pas corresponds well to the pour point. Synthetic oils, especially esters, with complex crystallization behavior (III), exhibit supercooling depending on the shear rate and cooling conditions. For these lubricating oils, the pour point provides no information for low-temperature applicability.

The structure and flow behavior of lubricating greases depend on the base oil and the type and concentration of the dissolved thickener. In this study, the linear viscoelastic properties of greases were characterized by combining oscillatory shear and squeeze flow covering a broad frequency range (0.1–105 rad s−1). Multiple-particle tracking (MPT) microrheology and scanning electron microscopy (SEM) provided further insight into local viscoelastic properties and sample structure on a submicron-length scale. The type and viscosity of the base oil did not affect the absolute value of the complex viscosity and the filament shape formed by a given thickener. High-frequency shear modulus data, however, indicated that the thickener lithium 12-hydroxystearate formed stiffer networks/filaments in poly-α-olefins than in mineral oils. As expected, the viscosity increased with increased thickener concentrations, but microscopy and high-frequency rheometry revealed that the thickness, length, and stiffness of the individual filaments did not change. In mineral oil, the 12-hydroxystearate thickeners yielded higher viscosity than the corresponding stearates with the same metal ion. The filamentous lithium thickeners created stronger networks than the roundish aggregates formed by magnesium and zinc stearate. Network mesh sizes varying between approximately 100 nm and 300 nm were consistently determined from SEM image analysis and MPT experiments. The MPT experiments further disclosed the existence of gel-like precursors of approximately 130 µm at thickener concentrations far below the critical value at which a sample-spanning network resulting in a characteristic grease texture is formed.

Die Fakultäten Angewandte Chemie sowie Maschinenbau und Versorgungstechnik kooperieren eng in der Forschung zu Schmierfetten. Die Schwerpunkte dieser Zusammenarbeit liegen auf der Herstellung, Charakterisierung und Wirkung von Fetten. Um den Studierenden beider Fakultäten bereits im Bachelorstudium die Möglichkeit zu geben, sich mit dem Thema „Schmierfette" vertraut zu machen, ist die Einrichtung eines „virtuellen" fakultätsübergreifenden Labors geplant. In einem ersten Schritt wurden Versuche entwickelt, die es zukünftigen interdisziplinären Studierendengruppen ermöglichen, eigenständig Schmierfette herzustellen und zu prüfen. Diese fakultätsübergreifende Zusammenarbeit soll die interdisziplinären Kompetenzen der Studierenden fördern und den Zugang zu komplexen Inhalten erleichtern.