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NIR‐sensitized cationic polymerization proceeded with good efficiency, as was demonstrated with epoxides, vinyl ether, and oxetane. A heptacyanine functioned as sensitizer while iodonium salt served as coinitiator. The anion adopts a special function in a series selected from fluorinated phosphates ( a : [PF 6 ] − ,  b : [PF 3 (C 2 F 5 ) 3 ] − ,  c : [PF 3 ( n ‐C 4 F 9 ) 3 ] − ), aluminates ( d : [Al(O‐ t ‐C 4 F 9 ) 4 ] − ,  e : [Al(O(C 3 F 6 )CH 3 ) 4 ] − ), and methide [C(O‐SO 2 CF 3 ) 3 ] −  ( f ). Vinyl ether showed the best cationic polymerization efficiency followed by oxetanes and oxiranes. DFT calculations provided a rough pattern regarding the electrostatic potential of each anion where  d  showed a better reactivity than  e  and  b . Formation of interpenetrating polymer networks (IPNs) using trimethylpropane triacrylate and epoxides proceeded in the case of NIR‐sensitized polymerization where anion  d  served as counter ion in the initiator system. No IPN was formed by UV‐LED initiation using the same monomers but thioxanthone/iodonium salt as photoinitiator. Exposure was carried out with new NIR‐LED devices emitting at either 805 or 870 nm.

NIR‐Sensitized Cationic and Hybrid Radical/Cationic Polymerization and Crosslinking