Hydrogen intercalation in solids is common, complicated, and very difficult to monitor. In a new approach to the problem, we have studied the profile of hydrogen diffusion in singlecrystal nanobeams and plates of VO2, exploiting the fact that hydrogen doping in this material leads to visible darkening near room temperature connected with the metalinsulator transition at 65 °C. We observe hydrogen diffusion along the rutile c-axis but not perpendicular to it, making this a highly one-dimensional diffusion system. We obtain an activated diffusion coefficient, ~.
− ./ cm 2 sec -1 , applicable in metallic phase. In addition, we observe dramatic supercooling of the hydrogen-induced metallic phase and spontaneous segregation of the hydrogen into stripes implying that the diffusion process is highly nonlinear, even in the absence of defects. Similar complications may occur in hydrogen motion in other materials but are not revealed by conventional measurement techniques.KEYWORDS: vanadium dioxide, hydrogen doping, metal-insulator transition, 1D diffusion, optical microscopy TEXT Hydrogen dissolves in many solids, with effects on their physical properties which are relevant to storage 1 , catalysis, sensing 2 , and material degradation 3 . Understanding how hydrogen moves within a solid is thus important, but is very challenging because of the combination of the difficulty of detecting hydrogen, the complexity of the transport processes, and the sensitivity of kinetics and energetics to microscopic nonuniformity and defects 4 . It has traditionally been studied, predominantly in metals and semiconductors, by neutron scattering 5 , nuclear 6 and muon magnetic resonance 7 , and other techniques which do not yield spatial profiles. It is thus hard to know when deviations from a simple Fick's law behavior are relevant, such as when diffusion is guided by dislocations, grain boundaries or strain fields associated with twinning or structural modifications, or if there is spontaneous segregation. Recently, information on the spatial profile has been obtained using the change in color on hydrogenation of thin yttrium 8 and vanadium