Intriguing Carbon Flake Formation during Microwave-Assisted Hydrothermal Carbonization of Sodium Lignosulfonate

Elongated carbon structures, here denoted as carbon flakes (CF), are revealed after microwave-assisted hydrothermal carbonization of sodium lignosulfonate. The morphology of formed CF is investigated by transmission electron microscopy and atomic force microscopy. Interestingly, a wide range of length distributions (between 100 and 700 nm) and a relatively constant aspect ratio and thickness are observed, indicating structures clearly different from the carbon spheres commonly formed during hydrothermal carbonization of lignocellulosic biomass. Moreover, X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy provide further information of the chemical structure, which consist mainly of nanographitic domains with a high degree of defects such as oxygenated functional groups, hybridized sp³ carbon, and aliphatic side chains. Furthermore, new insights into the formation mechanisms are uncovered and the formation is speculated to proceed through the combined effect of microwave irradiation and a heterogeneous solid–solid conversion. The formed CF are anticipated as highly interesting products for a variety of material applications.