Time-resolved rheometry of drying liquids and suspensions

TL;DR

This paper introduces a zero normal-force rheometry method that enables real-time, bulk rheological measurements of drying liquids and suspensions by maintaining constant contact area despite volume loss.

Contribution

The study presents a novel zero normal-force protocol for time-resolved rheometry, effectively measuring properties during solvent evaporation and suspension dehydration.

Findings

Accurately monitors viscosity during evaporation with up to 70% volume loss.

Tracks viscoelastic changes in suspensions approaching glass transition.

Maintains constant contact area despite sample volume decrease.

Abstract

From paints to food products, solvent evaporation is ubiquitous and critically impacts product rheological properties. It affects Newtonian fluids by concentrating any non-volatile components and viscoelastic materials, which hardens up. In both of these cases, solvent evaporation leads to a change in the sample volume, which makes any rheological measurements particularly challenging with traditional shear geometries. Here we show that the rheological properties of a sample experiencing `slow' evaporation can be monitored in a time-resolved fashion by using a zero normal-force controlled protocol in a parallel-plate geometry. Solvent evaporation from the sample leads to a decrease of the normal force, which is compensated at all times by a decrease of the gap height between the plates. As a result, the sample maintains a constant contact area with the plates despite the significant decrease of its volume. We validate the method under both oscillatory and continuous shear by accurately monitoring the viscosity of water-glycerol mixtures experiencing evaporation and a relative volume decrease as large as 70%. Moreover, we apply this protocol to dehydrating suspensions. Specifically, we monitor a dispersion of charged silica nanoparticles undergoing a glass transition induced by evaporation. While the decrease in gap height provides a direct estimate of the increasing particle volume fraction, oscillatory and continuous shear measurements allow us to monitor the suspension's evolving viscoelastic properties in real-time. Overall, our study shows that a zero normal-force protocol provides a simple approach to bulk and time-resolved rheological characterization for systems experiencing slow volume variations.