Purpose This exploratory study evaluates the potential of nanothermal analysis (nTA) coupled with atomic force microscopy (AFM) of soil samples for understanding physicochemical processes in soil and for linking the nanospatial and microspatial distribution of thermal characteristics with the macroscopic properties of soil samples. Materials and methods Soil and reference samples were investigated by differential scanning calorimetry and AFMnTA. nTA was conducted on 16 points of each AFM image in two subsequent heating cycles (55-120°C and 55-300°C, respectively). Thermograms were subdivided into characteristic types and their spatial distribution was compared between sample replicates and materials. Results and discussion Thermogram types consisted of partly structured expansion and compression phases, suggesting material-specific thermal profiles. The distribution of thermogram types reflected sample-dependent nanoscale and microscale heterogeneity. Indications for water molecule bridge transitions were found by nTA in peat and soil. Organic materials generally revealed strong expansion and irreversible compression phases, latter probably due to the collapse of pore and aggregate structures. In contrast to charcoal and manure, peat shows strong expansion below 120°C and compression only above 120°C. Conclusions All investigated samples are heterogeneous on the nanoscale and microscale with respect to thermal behaviour. AFM-nTA allows distinguishing numerous different materials on nanometre and micrometre scales in soil samples. The material-dependent characteristics will help in understanding and learning more about the nanoscale distribution of different materials and properties. Related to the macroscopic thermal behaviour, this will allow studying links between the properties of biogeochemical interfaces and the processes governed by them.