The gelation procedure and the gelation time of gelatin gels may lead to apparently similar materials, however, with different rheological fingerprints under small and large oscillatory shear deformations. Here, in the first paper of this series, gelation of 3 and 5% w/w gelatin solutions at 5 °C was performed in situ on the rheometer plate and in custom-made casting modules to obtain individual gel layers. Large amplitude oscillatory shear (LAOS) tests were performed. The nonlinear deformation regime was qualitatively analyzed using normalized Lissajous-Bowditch curves. The MITlaos software was employed to decompose the total intracycle stress response and to calculate the Chebyshev coefficients ratios. The dynamic moduli of the fresh gels were measured directly after the in situ preparation and within a time frame until 1.5 h. In the strain sweeps, we observed intense stiffening followed by yielding above 200% strain. However, the individual gel layers aged for 24 and 48 h show different LAOS fingerprints. The extensive loops in the viscous Lissajous-Bowditch curves indicate an elastoplastic material response. Based on the overall nonlinear rheological response, we propose a structural formation that describes the behavior of the gels for the conditions studied here. In the second paper of this series, we give the impact of hard micro-fillers (glass beads) and we describe the nonlinear characteristics of the filled gels.
Keywords: Chebyshev coefficients ratios; Gelatin; Large amplitude oscillatory shear (LAOS); Nonlinear viscoelasticity; Strain stiffening.
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