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We describe here the preparation and characterization of a photocathode assembly for CO 2 reduction to CO in 0.1 M LiClO 4 acetonitrile. The assembly was formed on 1.0 μm thick mesoporous films of NiO using a layer-by-layer procedure based on Zr(iv)-phosphonate bridging units. The structure of the Zr(iv) bridged assembly, abbreviated as NiO|-DA-RuCP 2  2+ -Re(i), where DA is the dianiline-based electron donor ( N , N , N ', N '-((CH 2 ) 3 PO 3 H 2 ) 4 -4,4'-dianiline), RuCP 2+ is the light absorber [Ru((4,4'-(PO 3 H 2 CH 2 ) 2 -2,2'-bipyridine)(2,2'-bipyridine)) 2 ] 2+ , and Re(i) is the CO 2 reduction catalyst, Re I ((4,4'-PO 3 H 2 CH 2 ) 2 -2,2'-bipyridine)(CO) 3 Cl. Visible light excitation of the assembly in CO 2 saturated solution resulted in CO 2 reduction to CO. A steady-state photocurrent density of 65 μA cm -2 was achieved under one sun illumination and an IPCE value of 1.9% was obtained with 450 nm illumination. The importance of the DA aniline donor in the assembly as an initial site for reduction of the RuCP 2+ excited state was demonstrated by an 8 times higher photocurrent generated with DA present in the surface film compared to a control without DA. Nanosecond transient absorption measurements showed that the expected reduced one-electron intermediate, RuCP + , was formed on a sub-nanosecond time scale with back electron transfer to the electrode on the microsecond timescale which competes with forward electron transfer to the Re(i) catalyst at t  1/2 = 2.6 μs ( k  ET = 2.7 × 10 5 s -1 ).

A donor-chromophore-catalyst assembly for solar CO2 reduction

A donor-chromophore-catalyst assembly for solar CO₂ reduction