In this paper, we report the synthesis and characterization of pyrolyzed lignin compacts reinforced with 50 wt % wheat straw (WS) or sugar beet pulp (SBP) fibers. The compacts were pyrolyzed at 300, 500, 700, and 900 °C in an Ar atmosphere. Detailed thermogravimetric analysis (TGA), thermomechanical analysis (TMA), Fourier transform infrared (FTIR) spectroscopy, and microstructure analysis were performed on these samples. FTIR analysis showed that pyrolysis of lignin–WS and lignin–SBP resulted in aromatic char. Scanning electron microscope (SEM) studies showed that foams obtained by pyrolyzing both lignin–50 wt % SBP and lignin–50 wt % WS composites have a cellular structure. X-ray tomography and energy-dispersive spectrometry (EDS) studies showed that pyrolysis of wheat straw caused the formation of mineral-rich nodules in the pyrolyzed lignin matrix, which was responsible for the denser and uniform microstructure of the lignin–WS composites. Due to this reason, the lignin–WS composites were denser and had a better mechanical strength as compared to the lignin–SBP composites. Both the compositions also showed temperature-dependent wettability behavior.

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