We have succeeded in nanoscale polymerization of Langmuir-Blodgett (LB) films of cadmium 10,12-pentacosadiynoate (CdPA) by near-field two-photon excitation with femtosecond pulses. The LB films of CdPA were excited locally through an aperture of a near-field optical fiber probe by femtosecond-pulsed near-infrared radiation. The formation of polydiacetylene (PDA) films has been confirmed by two-photon induced and ordinary (linear) luminescence and Raman measurements by using a scanning near-field optical microscope. The polymerization of CdPA to PDA was induced by the femtosecond-pulsed near-infrared radiation but not by continuous wave radiation. This result confirms that the polymerization was not induced by heat arising from the near-field irradiation. The number of photons involved in the polymerization reaction was estimated to be 2 from the dependence of photoluminescence intensities of PDA on the power of incident light for polymerization.
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