Oxygen-sensitive and near-infrared (NIR) luminescent Yb
III coordination polymers incorporating ligands based on pyrene derivatives were synthesized: Yb
III–TBAPy and Yb
III–TIAPy (TBAPy: 1,3,6,8-tetrakis(
p-benzoate)pyrene; TIAPy: 1,3,6,8-tetrakis(3,5-isophthalic acid)pyrene). The coordination structures of these materials have been characterized by means of electrospray ionization mass spectrometry, X-ray diffraction analysis, and thermogravimetric analysis. Moreover, the porous structure of Yb
III–TIAPy has been evaluated by measuring its N
2 adsorption isotherm. The NIR luminescence properties of Yb
III–TBAPy and Yb
III–TIAPy have been examined by acquiring emission spectra and determining emission lifetimes under air or argon and in vacuo. Yb
III–TIAPy exhibited high thermal stability (with a decomposition temperature of 400 °C), intense luminescence (with an emission quantum yield under argon of 6.6 %), and effective oxygen-sensing characteristics. These results suggest that NIR luminescent Yb
III coordination polymers prepared using pyrene derivatives could have applications in novel thermo-stable oxygen sensors.
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