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Acidic oxygen evolution reaction (OER) electrocatalysts that provide high activity, lower costs, and long-term stability are needed for the wide-scale adoption of proton-exchange membrane (PEM) water electrolyzers for generating hydrogen through electrochemical water splitting. We report the effects of chromium substitution and temperature treatments on the structure, OER activity, and electrochemical stability of ruthenium oxide (RuO2) aerogel OER electrocatalysts. RuO2 and Cr-substituted RuO2 aerogels (Ru0.6Cr0.4O2) were synthesized using sol–gel chemistry and then thermally treated at different temperatures. Introducing chromium into the synthesis increased the surface area (7–11 times higher) and pore volume (5–6 times higher) relative to RuO2 aerogels. X-ray diffraction analysis is consistent with s that Cr was substituted into the rutile RuO2 structure. X-ray photoelectron spectroscopy showed that trivalent Cr substitution altered the surface electronic structure and ratio of surface hydroxides. The specific capacitance values of Cr-substituted RuO2 aerogels were consistent with charge storage within a hydrous surface. Cr-substituted RuO2 aerogels exhibited 26 times the OER mass activity and 3.5 times the OER specific activity of RuO2 aerogels. Electrochemical stability tests show that Cr-substituted RuO2 aerogels exhibit similar stability to commercial RuO2. Understanding how metal substituents can be used to alter OER activity and stability furthers our ability to obtain highly active, durable, and lower-cost OER electrocatalysts for PEM electrolyzers.