Flexural tests: 160 mm x 40 mm x 6 mm thick samples. Based upon international standards BS EN 12390‑5:2019 section 7.2, specimens were subjected to a three-point bending test with a 50 kN load cell in an Instron 3366 Universal testing machine, which applied a displacement-controlled point load central to the specimen at a rate of 0.2 mm/minute. 

Compression tests: 40 mm x 40 mm samples. Loading was applied to the platens at the rate of 0.5 mm/minute until specimen failure in line with international standards BS EN 1015-11:1999. The Instron 3366 Universal testing machine was used.

Tensile Wads tests:  2704-522 hydraulic grips were used to hold the wad specimens in place, such that the gauge volume was 75 mm above the lower grip. In-situ tensile loading, CT and XRD were performed at I12-JEEP in the external building experimental hutch 2 (EH2).  Each specimen was loaded using a maximum 10 kN load cell uniaxial servo-hydraulic test rig on the Large Sample Table. X-Ray Computed Tomography (CT) was performed at initial 0 mm displacement (with a small preload of 0.04 kN applied to ensure the newly-loaded sample was ready to test), as well as at further distinct load increments in the elastic, plastic, and post-fracture regimes controlled by displacement at 0.5 mm, 1 mm, 2 mm, 4mm and 8 mm. Loading was applied at a rate of 1 mm / min to help reduce strain rate effects, and the sample was held stationary at each displacement value while CT data collection took place. There were five stacked CT scans per displacement level, with scans moving from the base of the ROI rising at 15 mm increments (y = 111 mm – base of the region of interest (ROI), 96 mm, 81 mm, 66 mm and 51 mm) and covering the entire ROI.  A script was written by the beamline scientist to reduce the CT data down to 8-bit for further analysis at the University of Bath using Avizo software, with the resulting 8-bit files being 2560 x 2560 x 1188 voxels and the little Indian and x-fastest default settings used.