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Two tungstates containing platinum nanoparticles (Pt Npts) were obtained by air-calcining α-Keggin-type diplatinum(II)-coordinated polyoxotungstates, Cs 3 [α-PW 11 O 39 { cis -Pt(NH 3 ) 2 } 2 ]⋅8H 2 O ( Cs-P-Pt ) and Cs 4 [α-SiW 11 O 39 { cis -Pt(NH 3 ) 2 } 2 ]⋅11H 2 O ( Cs-Si-Pt ), at 700–900 °C for 5 h. The polyoxotungstate  Cs-P-Pt  was transformed to a mixture of Pt Npts and Cs 3 PW 12 O 40  upon calcination, while the  Cs-Si-Pt  structures were transformed to Pt Npts and Cs 4 W 11 O 35 . The Pt Npts generated by air-calcining  Cs-P-Pt  at 700 °C for 5 h were uniform with an average particle size of 3.6 ± 1.1 nm, which was much smaller than that of the Pt Npts obtained by calcining  Cs-Si-Pt  (19.9 ± 9.9 nm) under identical conditions. This demonstrated the significant inhibitory effect of  Cs-P-Pt  on aggregation during high-temperature air-calcination at a high platinum content (10.6 wt.%) and in the absence of a support. During calcination at 700–900 °C,  Cs-P-Pt  exhibited higher activities than  Cs-Si-Pt  with respect to hydrogen evolution from aqueous triethanolamine solutions under visible light irradiation in the presence of Eosin Y, α-Keggin-type mono-aluminum-substituted polyoxotungstate, and titanium dioxide. When  Cs-P-Pt  was calcined at 800 °C for 100 h, no decrease in activity was observed in comparison with that upon calcination for 5 h. Graphical Abstract

catalysis letters

Two Tungstates Containing Platinum Nanoparticles Prepared by Air-Calcining Keggin-Type Polyoxotungstate-Coordinated Diplatinum(II) Complexes: Effect on Sintering-Resistance and Photocatalysis