High-Energy Surface X-ray Diffraction for Fast Surface Structure Determination

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Science  14 Feb 2014:
Vol. 343, Issue 6172, pp. 758-761
DOI: 10.1126/science.1246834

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Understanding the interaction between surfaces and their surroundings is crucial in many materials-science fields, such as catalysis, corrosion, and thin-film electronics, but existing characterization methods have not been capable of fully determining the structure of surfaces during dynamic processes, such as catalytic reactions, in a reasonable time frame. We demonstrate an x-ray-diffraction–based characterization method that uses high-energy photons (85 kiloelectron volts) to provide unexpected gains in data acquisition speed by several orders of magnitude and enables structural determinations of surfaces on time scales suitable for in situ studies. We illustrate the potential of high-energy surface x-ray diffraction by determining the structure of a palladium surface in situ during catalytic carbon monoxide oxidation and follow dynamic restructuring of the surface with subsecond time resolution.

Speeding Up Surface Diffraction

Surface diffraction methods can determine the atomic structure of the topmost layer of a crystal and also subsurface structures. However, many surface diffraction methods either require ultrahigh vacuum conditions, which limits the reaction conditions that can be studied, or require long data acquisition times, which limits temporal resolution. Using high x-ray energies, Gustafson et al. (p. 758, published online 30 January; see the Perspective by Nicklin) were able to measure the intensities of surface-diffracted beams to follow the surface oxidation that accompanies the changes in a palladium surface during the catalytic oxidation of CO with O2.

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