“…The small diffraction peaks at 27.5°and 28°for the HB-r60 and HB-r90 samples, respectively (Figure S1b, Supporting Information), might originate from unknown by-products and/or stacked HB sheets. [29] The temperature-programmed desorption (TPD) curves (Figure 2a) contain a broad peak up to 1400 K for all samples, consistent with previous reports of HB sheets, [17,21,22,23,24] as well as peaks at 430, 500, and 550 K. The intensity of the 400 K peak was higher for samples with larger XRD peaks, suggesting that the 400 K peak originates from the unknown byproduct and/or stacking of the HB sheets. The TPD peak intensity at 500 K slightly decreased with the volume of resin, whereas the peak at 550 K slightly increased, indicating that the B-H bond becomes stronger in samples prepared with higher volumes of resin.…”