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We present a novel method to measure transient photovoltage at nanointerfacesusing ultrafast electron diffraction. In particular, we report our results onthe photoinduced electronic excitations and their ensuing relaxations in ahydroxyl-terminated silicon surface, a standard substrate for fabricatingmolecular electronics interfaces. The transient surface voltage is determinedby observing Coulomb refraction changes induced by the modified space-chargebarrier within a selectively probed volume by femtosecond electron pulses. Theresults are in agreement with ultrafast photoemission studies of surface statecharging, suggesting a charge relaxation mechanism closely coupled to thecarrier dynamics near the surface that can be described by a drift-diffusionmodel. This study demonstrates a newly implemented ultrafast diffraction methodfor investigating interfacial processes, with both charge and structureresolution.

Photovoltage Dynamics of the Hydroxylated Si(111) Surface Investigated by Ultrafast Electron Diffraction