It was tried to microencapsulate camellia oil using heterocoagulation between fatty acid dissolved in camellia oil and chitosan dissolved in the continuous water phase. Oleic acid as a fatty acid was dissolved in camellia oil in order to certainly form the microcapsule shell made from oleic acid and chitosan. The microcapsules were observed with optical microscope and characterized about the diameters, ζ-potential, FTIR analysis and adhesion feature on human hair. Microcapsules with the mean diameter in the range from ca. 1.5 μm to 4.5 μm could be prepared with the preparation method presented in this study. The oil droplets of camellia oil charged negatively to be -54.6 mV and the microcapsules charged positively to be 59.6 mV. The microcapsules adhered well on the negatively charged human hair and were kept stably before and after drying at room temperature for 24 h and blowing.