The effects that both soap concentration and base oil viscosity exert on the rheology of lubricating greases and its relationship with grease microstructure are discussed in this work. With this aim, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and the viscosity of the base oil, according to an RSM statistical design. These lubricating greases were rheologically characterized through small-amplitude oscillatory shear (SAOS) and viscous flow measurements. In addition to these, scanning electronic microscopy (SEM) observations and mechanical stability tests were also carried out. It has been found that the structural skeleton (size and shape of the disperse phase particles) was highly influenced by the base oil viscosity. In this sense, the values of the viscoelastic functions in the linear viscoelastic region and the mechanical stability of the lubricating greases increase as the viscosity of the base oil decreases. An opposite tendency was observed during viscous flow tests at high shear rates, when the grease microstructure was mostly destroyed. On the other hand, the microstructural network of these greases becomes stronger as soap concentration increases. These results have been explained taking into account the balance between the solvency of the thickener in the base oil and the level of entanglements formed by soap fibers, which influence the lubricating grease network.
Thermal-induced changes in the viscous and viscoelastic responses of lubricating greases have been investigated through different rheological techniques in a temperature range of 0-175°C. Small-amplitude oscillatory shear and viscous flow measurements were carried out on a model conventional lithium lubricating grease prepared by inducing the in situ saponification reaction between 12-hydroxystearic acid and hydrated lithium hydroxide. The linear viscoelasticity functions dramatically decrease above 110°C, but not below this critical temperature, which determines the maximum recommended operating temperature in relation to its durability and resistance under working conditions. Two different regions, below and above this critical temperature, in the plateau modulus versus temperature plot have been detected. From this thermal dependence, a much larger thermal susceptibility of the lubricating grease at temperatures above 110°C is apparent. The thermo-mechanical reversibility of this material has been studied by applying different combined stress-temperature protocols. Regarding the viscous flow, a minimum in the shear stress versus shear rate plots appeared at temperatures above 60°C, more pronounced as temperature increases, resulting from material instabilities. The experimental results obtained have been explained on the basis of the thermo-mechanical degradation of the lubricating grease microstructure.
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