The invention relates to a method for detecting physicochemical properties of micro and nano structures on the surface of a material, in particular to an in-situ quasi synchronous detection method for detecting physicochemical properties of micro and nano structures by adopting an atomic force microscope-ion migration spectrometer (AFM-IMS) or atomic force microscope-high-field asymmetric waveform ion mobility spectrometer (AFM-FAIMS) combined technology under the atmospheric environment. The method comprises the following steps of: scanning and imaging a detected sample on an atomic force microscope (AFM) to acquire physical property data, desorbing the chemical substances of the sample by using corona discharge, ionizing the chemical substances into charged ions, sending the charged ions to an ion migration spectrometer (IMS) or a high-field asymmetric waveform ion mobility spectrometer (FAIMS) in a mode of migrating the electric field or using artificial airflow by using a micro electromechanical interface device, performing separation and detection, and determining the chemical components. The method can directly correspondingly analyze the physical properties of the sample and the chemical components, and has in-situ (quasi) synchronous fixed point analysis function of the micro and nano structures; and the whole process is performed under the atmospheric environment, themethod has low limit on the sample, the analysis efficiency and the test efficiency are greatly improved, the operation is convenient and flexible, the volume cost is low, and the method is convenient for popularization and application in the field of material analysis and test.