Recently, the Langmuir-Blodgett Method¹⁾ is receiving much attention as a means to obtaining functional organic super thin films in the electric field. This method can control rearrangement in molecular dimensions while retaining highly orderly structure. New diversified applications utilizing the method are being developed in a variety of fields such as molecular electronics, bioelectronics, etc..²⁾ Amphiphilic diacetylene monocarboxylic acids are readily polymerised by heat, light³⁾ and radiation while polymerized films^3,4) are thermally and mechanically stable. As a result, application to photoresist material⁵⁾ having a high degree of resolving power and nonlinear optical material⁶⁾ are expected.