To clarify the microcrystal structure of soot particulate in the combustion chamber, we examined sampling methods which freeze the reaction of sample specimens from the combustion chamber and collected the soot particulates on microgrids. We investigated the microcrystal structure with a high resolution transmission electron microscope.The results were: the particle size distribution and the microcrystal structure of the soot particulates is little different for the cooled freezing method and room temperature sampling. The typical layer plane structure which characterizes graphite carbon is not observed in the exhaust of diesel engines, but some particulates display a somewhat similar layer plane structure. The structure of soot particulate is a turbostratic structure as the electron diffraction patterns show polycrystals. The soot particulates in the combustion chamber is similar to exhaust soot particulates. In the initial stage of combustion, the particulate shows similar layer planes, but after the heat release there is no clear layer plane structure.