The measurements were carried out at the ISIS Neutron and Muon Spallation Source, UK at the neutron imaging beamline IMAT (Imaging and Materials Science & Engineering).34,35 The neutron radiographies were collected with an optical camera box36 based on a 2048 × 2048 pixels Andor’s Zyla sCMOS 4.2 Plus camera. The chamber was positioned as close as possible to the ZnS/LiF scintillator to reduce penumbra blurring. An L/D of 250 was used, where L (10 m) is the distance between the pinhole selector and the chamber and D (40 mm) is the pinhole’s diameter. The beam was shaped by using five pairs of jaws available on IMAT to the chamber size (50 × 50 mm2) to avoid the electronics radiation. The exposure time was set to 30 s per image, and a spatial resolution of 53 μm was achieved.

The software IBEX Instrument Control software37 from ISIS was modified in collaboration with Lacerta Technology to ensure that simultaneous RH readings were obtained with the corresponding beam images. This was a novel addition to the IBEX software, which permitted the correlation of RH readings with neutron image data a much more straightforward task, and removed possible errors in the synchronization of the data streams from two independent devices.

Prior to mounting, the samples were pre-dried for at least 24 h. During the experiment, the samples were subjected to one or two RH cycles (20–75–20%), consisting of 30 min RH equilibration at 20%RH followed by an increase in RH at 4%RH/min to 75%RH. The RH remained at 75% for 90 min for the experiments before being reduced at 4%RH/min to 20%RH.

Image processing was automated using a macro written for ImageJ (version 1.53) specifically for the images obtained from these measurements and setup.18

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