Challenges and solutions of environmental scanning electron microscopy characterisation of biomaterials: Application to hygro‐expansion of paper

Most methodologies to measure the moisture‐induced deformation (hygro‐expansion) of paper microconstituents, including fibres and interfibre bonds, are low resolution or time‐consuming. Hence, here, a novel method is proposed and validated to measure high‐resolution full‐field strain maps of paper microconstituents during hygro‐expansion, based on environmental scanning electron microscopy (ESEM). To this end, a novel climate stage enables accurate control of the relative humidity (RH) near the specimen in the ESEM from 0%–100%. The fibre surface, which is decorated a priori with a microparticle pattern, is captured during RH change. Subsequently, correlating the fibre surface using a dedicated global digital image correlation algorithm enables high‐resolution hygro‐expansion strain maps. Method optimisation involved performing contrast enhancement, scan‐correction to reduce ESEM artefacts and a background correction, resulting in a strain resolution of 6·10−4 . Method validation revealed that the fibres' crystallinity is affected by the electron beam, even for minimal invasive electron beam settings. Interestingly, however, the fibres consistently exhibit conventional hygro‐expansion behaviour during the drying slopes. Using the optimised procedure, hygro‐expansion characterisation of two interfibre bonds and four interfibre bond cross‐sections revealed the competition between the low longitudinal and large transverse fibre hygro‐expansion in the bonded area.