This study exploits the nanoscale resolution of scanning thermal microscopy (SThM) to reveal inhomogeneous nature of thermal properties of carbon-derived materials issued from thermal conversion of the most commonly known polyimide, Kapton®. This information is otherwise inaccessible if conventional thermal characterization techniques are used due to their limited spatial resolution. Kapton films were pyrolyzed in an inert atmosphere to produce carbon-based residues with varying degree of conversion to free sp2 disordered carbon. The thermal conductivity of carbon materials ranges from 0.2 to 2 W m−1 K−1, depending on the temperature of the carbonization process (varied between 500 and 1200 °C). For quantitative measurements of thermal conductivity, the Null Point SThM (NP-SThM) technique is used in order to avoid unwanted effects as the parasitic heat flows through the air and the probe cantilever. It was found that NP SThM data for bulk materials are in excellent agreement with results obtained through more traditional techniques, namely, photo-thermal radiometry, flash laser analysis, and micro-Raman thermometry. This allowed us to use the NP-SThM technique to differentiate structural heterogeneities or imperfections at the surface of the pyrolyzed Kapton on the basis of the measured local thermal conductivity.