The invention discloses a method for testing SEM (scanning electron microscope) and TEM (transmission electron microscope) by collecting fine particulate matters through TGDSC, which comprises the following steps: step 1, installing a gas sampling clamp containing a gas filter membrane on a pipeline of a gas outlet of a TGDSC instrument, and then fixing a monocrystalline silicon wafer and a copper mesh with a carbon membrane on the filter membrane through a double faced adhesive tape; according to the invention, many experiment parameters can be changed in the TGDSC experiment process, so that the temperature range, the sample amount, the heating rate, the gas type, the atmosphere and the gas flow of the sample can be adjusted, and the TGDSC experiment can be carried out by changing the chemical components of the sample to obtain thermal reaction processes under different experiment conditions; meanwhile, the fine particulate matters in the corresponding reaction process can be collected for SEM and TEM analysis, and finally combustion dynamics and a fine particulate matter generation rule are established, so that an effective laboratory solution is provided for controlling the generation of the fine particulate matters.