The morphology of the composites PHB/PBT-PTMG polymerized using in situ polymerization method has been investigated by atomic force microscopy. The results suggest that the polymerization time and matrix solvent could have an appreciable influence on the morphology and properties of composite PHB/PBT-PTMG. The interactions between rigid polymer PHB particles and the matrix copolymer PBT-PTMG are stronger in a good solvent than that in a poor solvent. For longer polymerization times, the interaction between PHB/PBT-PTMG composites is also stronger. In addition, the adhesive force between the AFM tip and the PHB/PBT-PTMG composites was analyzed. The magnitudes of the adhesive forces between the tip and composites which were polymerized in a good solvent or for a long polymerization time were larger. It is demonstrated that by comparing the interaction between the AFM tip and the composites one can investigate qualitatively variations of the properties of the composites and can distinguish the components in composites.Using the in situ direct polycondensation method [1], rigid rod-like monomers could be dispersed and polymerized in a flexible matrix polymer solution at room temperature, giving rise to polymer microcomposites containing nanoparticles. It was suggested that the monomers of the rigid polymer are polymerized in the free volume of the matrix polymer and that the rigid polymer particles can be obtained by controlling the quality of the matrix polymer, namely by controlling the free volume of the matrix polymer [1].In in situ polycondensation, the interactions between the matrix polymer in different solvents and a rigid polymer are different [2][3][4]. If the rigid polymer has a strong interaction with the matrix polymer it will not separate and the corresponding composite can become a good composite coating. Otherwise, the rigid polymer microparticles can be separated from the matrix and can be used as medical or chemical materials. * Corresponding author In recent years, great developments have been seen in the field of scanning force microscopy (SFM), also known as atomic force microscopy (AFM) [5]. In addition to topographic imaging, the force between the AFM tip and the surface can also provide unique localized chemical and physical information about the sample surface on the nanometer scale which could not readily be obtained by other techniques [6]. By using the force-distance curve [7], one can directly measure the surface force, elasticity, friction and adhesion, which are dependent on the probe, contact surface and surrounding medium. When the AFM tip withdraws from contact with a sample surface, an adhesion force develops between the tip and the sample. In the absence of capillary forces (for example, in liquid media), the adhesion force could arise from chemical bonds between the tip and sample surfaces [5]. Analysis of the adhesion forces can thus produce localized chemical information about the sample-liquid interface, such as the nature of the surface functional group. However, the complexit...