Micronewton shear rheometer performing SAOS using 2 mg of sample

Abstract

Rheological measurements typically require at least 20–50 mg of sample. We set up a miniaturized sliding-plates shear rheometer (mgRheo) that requires only 2 mg sample or even less. We designed a flexure-based force-sensing device that could measure force ranging from the micronewton to millinewton scale, e.g., 40 μN–400 mN for one particular spring constant. The setup was strain-controlled by a piezostage and could perform standard rheological tests such as small amplitude oscillatory shear, step strain, and stress relaxation. The accuracy and consistencies were evaluated on polydimethylsiloxane viscoelastic standard, entangled poly(hexyl methacrylate), and polystyrene. The obtained phase angles quantitatively agreed with those from commercial rheometers. The exact values of the modulus are prone to the overfilling of the sample. The storage G′ and loss G″ moduli from the mgRheo were systematically higher than those from commercial rheometers (i.e., within 5% with careful trimming or 30% with excessive overfilling). Between 102 and 106 Pa, G′ and G″ were in good agreement with commercial rheometers. Such a setup allowed for general rheometric characterizations, especially obtaining linear viscoelasticity on soft matters that are synthetically difficult to obtain in a large quantity.