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Multiscale monitoring of oleogels during thermal transition

Sebastian Mannweiler,Dominic Oppen,Simon Hilbig,Marcel Mundhenk,Jochen Weiss,J. R. Agudo

Published 2025 in Applied Rheology

ABSTRACT

Abstract Thermal transitions, such as crystallization or relaxation, in heterogeneous materials are complex and occur at different length and time scales. Several devices are necessary for their analysis, leading to varying boundary conditions and multiple specimens across measurements. This study investigated the thermal transitions of oleogels, designed to replace animal products, composed of rapeseed oil with 20% w/w oleogelator. Three oleogels with either rice bran wax (RBX), ethyl cellulose (EC), or a 1:1 mixture of both were analyzed. To capture dynamic mechanisms at multiple length and time scales, a simultaneous multiscale experiment was conducted on a single sample under the same conditions. Accordingly, Raman and dielectric spectroscopy were coupled with dynamic mechanical analysis (DMA) over a temperature range of 150 to −10°C. Differential scanning calorimetry was also performed to validate the results. DMA revealed a gradual glass transition in EC oleogels at ∼120°C. Raman spectroscopy complemented these findings, providing detailed molecular insights into RBX crystallization starting at ∼60°C until ∼5°C, not detectable with DMA. Dielectric spectroscopy extended the frequency range of DMA and revealed a temperature-activated relaxation process > 500 Hz at ∼5°C in RBX-containing samples. This study demonstrated the potential of multiscale analyses to link mechanical, dielectric, and chemical processes to complex thermal processes occurring in soft materials such as oleogels. Furthermore, these results provide a basis for improving the applicability of plant-based fat substitutes.

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