In Situ Rheology–SAXS Experiments for Correlating Structural and Mechanical Properties of Amphiphilic Copolymer Hydrogels

Alternating amphiphilic copolymers self-assemble into hydrogels with exceptional elasticity, self-healing, and tunable viscoelasticity. SAXS/WAXS and rheology reveal concentration- and temperature-dependent structural transitions (micelles → BCC → lamellae) directly linked to mechanical performance. Yet, their structural dynamics under applied stress remain unexplored. We propose in-situ rheology–SAXS/WAXS experiments at ID02 to capture nanoscale rearrangements during controlled shear. ID02 offers unique advantages: high flux, broad q-range (0.1–25 nm⁻¹), and millisecond time resolution, enabling detection of both micellar ordering and PEG crystallization while correlating with rheological response. Systematic studies across concentrations, temperatures, and compositions will reveal structure–property relationships governing elasticity, toughness, and recovery in AAP hydrogels, guiding the design of robust, stimuli-responsive materials for biomedical, soft robotics, and drug delivery