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Multiple interval thixotropic test (miTT)—an advanced tool for the rheological characterization of emulsions and other colloidal systems

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Abstract

In the last years, the 3iTT protocol—a dynamic-mechanical test (DMT) at low deformation and constant frequency, followed by a start-up flow (SUF) at constant shear-rate, and a DMT—was developed as an alternative to check for changes in material behavior, which was extended to form the multiple interval thixotropic test protocol (miTT), differing in modifying the shear rates systematically. The results of this test routine are a viscosity function η(\(\dot{\gamma }\)) with increasing and decreasing \(\dot{\gamma }\) and the dependence of G’ and G” on \(\dot{\gamma }\) previous test. More importantly, the G’ and G” are strongly influenced by the previously applied shear rate. While regular emulsions show a decrease of G’ and G” upon a higher shear rate \(\dot{\gamma }\) in the previous shear step, the pickering emulsions with graphene oxide show an increase. In both cases, the change is approximately reversible. The changes in G’ and G” correlate well with the emulgel composition.

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Acknowledgements

GM Zhu and WQ Li would like to acknowledge financial support from the National Science Foundation of China (Grant No. 51978410).

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Authors and Affiliations

  1. College of Materials Science and Engineering, Shenzhen Key Laboratory of Polymer Science and Technology, Guangdong Research Center for Interfacial Engineering of Functional Materials, Nanshan District Key Laboratory for Biopolymers and Safety Evaluation, Shenzhen University, Shenzhen, 518055, People’s Republic of China

    Florian J. Stadler, Shuming Cui, Wenqiang Li, Shichang Wang, Zhi-Chao Yan & Guangming Zhu

  2. Department of Polymer and Petrochemical Engineering, NED University of Engineering & Technology, University Road, Karachi, 75270, Pakistan

    Saud Hashmi

  3. College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen, 518055, People’s Republic of China

    Stephan Handschuh-Wang

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  1. Florian J. Stadler
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Correspondence to Florian J. Stadler or Guangming Zhu.

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Appendix

Appendix

Comments on applying the miTT protocol

In general, a fresh sample was used for the miTT protocol, which was not used for further experiments (except polarized optical microscopy). The results for the GO emulgel suggest that it would be possible to reuse the samples for other test profiles as the miTT protocol does not change the rheological properties very much, while this is not the case for the CNF emulgels. Therefore, it is suggested that utmost caution should be exercised that the samples’ rheological properties are not changed too much when reusing the samples for other setups after miTT or using previously strongly sheared samples before starting miTT.

The best way would be to compare the G’(\(\dot{\gamma }\) prev) for rising and decreasing shear rate branch. If the differences are quite severe, such as in Fig. 8a (CNF emulgels), it would be better not to use the sample for further rheological tests; if the differences are minimal like in Fig. 8b (GO emulgels), and the stability of the system is sufficient (e.g., the water evaporation does not influence the results), using the sample for other purposes should be unproblematic.

More details are given in supplementary information along with the evaluation script for the miTT test (for use at your own risk).

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Stadler, F.J., Cui, S., Hashmi, S. et al. Multiple interval thixotropic test (miTT)—an advanced tool for the rheological characterization of emulsions and other colloidal systems. Rheol Acta 61, 229–242 (2022). https://doi.org/10.1007/s00397-021-01323-y

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