Provincial papers. A. S. Batchellor makes suggestions for their treatment. To make them immediately valuable they should be indexed, and some missing parts should be transcribed from other sources ... A. S. Batchellor. Editor of state papers. [1

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Domain Structures of Ni and NiFe (Oxy)Hydroxide Oxygen-Evolution Catalysts from X‑ray Pair Distribution Function Analysis

Ni–Fe (oxy)­hydroxides, Ni_{(1–<i>z</i>)}Fe_<i>z</i>O_<i>x</i>H_<i>y</i>, are among the fastest-known water oxidation catalysts in alkaline media on a per-cation basis. At current densities relevant for electrolysis (e.g., >0.5 A/cm^–2), mass and electron transport through catalyst films with high mass loading are critical and depend substantially on the extended and intermediate catalyst architecture. Here we use X-ray pair distribution function (PDF) analysis to determine the intermediate nanostructures of electrodeposited Ni_{(1–<i>z</i>)}Fe_<i>z</i>O_<i>x</i>H_<i>y</i> films. We report the effects of electrodeposition technique (pulsed versus continuous), electrochemical cycling, and Fe content on the structure of the catalyst film. The PDF patterns for Ni_{(1–<i>z</i>)}Fe_<i>z</i>O_<i>x</i>H_<i>y</i> films are best simulated by model structures consisting of brucite-like β-Ni­(OH)₂ fragments 1 to 3 layers in thickness. Only the oxidation state of the film significantly affects the intralayer scattering behavior (i.e., metal–oxygen bond distance). The interlayer interactions, however, are affected by Fe content and deposition conditions. The domain size of many of the systems are similar, extending to ∼5 nm, which are best modeled by sheets containing upward of ∼250 metal cations. Smaller domains were found for films deposited through a larger number of electrochemical cathodic current pulses. Films can be cycled between as-deposited, oxidized, and reduced states, with minimal loss of intrasheet coherence, indicating a degree of structural stability. We estimate heterogeneity in the domain structures by modeling the PDF data to linear combinations of oxyhydroxide fragments with different sizes and numbers of layers

Advanced and In Situ Analytical Methods for Solar Fuel Materials.

In situ and operando techniques can play important roles in the development of better performing photoelectrodes, photocatalysts, and electrocatalysts by helping to elucidate crucial intermediates and mechanistic steps. The development of high throughput screening methods has also accelerated the evaluation of relevant photoelectrochemical and electrochemical properties for new solar fuel materials. In this chapter, several in situ and high throughput characterization tools are discussed in detail along with their impact on our understanding of solar fuel materials

Advanced and In Situ Analytical Methods for Solar Fuel Materials

In situ and operando techniques can play important roles in the development of better performing photoelectrodes, photocatalysts, and electrocatalysts by helping to elucidate crucial intermediates and mechanistic steps. The development of high throughput screening methods has also accelerated the evaluation of relevant photoelectrochemical and electrochemical properties for new solar fuel materials. In this chapter, several in situ and high throughput characterization tools are discussed in detail along with their impact on our understanding of solar fuel materials