This experimental study was conducted to investigate macroscopic characteristics of the flash boiling spray with tow component mixing fuel. Homogeneous Charge Compression Ignition (HCCI) is a newer combustion method for internal combustion engines to reduce nitrogen oxide and particulate matter simultaneously. But it is difficult to put this combustion method to practical use in an engine because of such problems as instability of combustion in low load operating conditions and knocking in high load operating conditions. In HCCI, combustion characteristics and exhaust emissions depend on conditions of air/fuel mixture and chemical reactions of fuel molecules. The fuel design approach is achieved by mixing two components which differ in properties such as density, viscosity, volatility, ignitability and so on. We plan to apply the fuel design approach to HCCI combustion generated in a real engine, and examine the possibility of mixture formation control using the flash boiling spray. Spray characteristics of two component fuel with a flash boiling phenomenon was investigated using Shlieren and Mie scattering photography. Test fuel was injected into a constant volume vessel at ambient conditions imitated injection timing BTDC of a real engine. As a result, it was found that a flash boiling phenomenon greatly changed spray structure, especially in the conditions of lower temperature and density. Therefore, availability of mixture formation control using flash boiling spray was suggested.