The letter reports a single-step method for fabrication of metal nanoparticle loaded mesoporous alumina through anodizing of a commercial aluminum alloy. The metal nanoparticles, with short dimensions of 2-4 nm and aspect ratios up to 8, display crystalline structures and are evenly dispersed in mesoporous alumina. The approach can easily be implemented on a large scale and extended to other alloy systems consisting of a valve metal and different alloying elements with Gibbs free energy of oxide formation less negative than that of the valve metal, benefiting nanoarchitecture design and nanostructure synthesis for applications in catalysis, ion exchange, sensing, etc.Mesoporous materials have attracted significant interest due to the great potential for applications in catalysis, ion exchange, sensing, etc. 1-3 However, the applications require the materials to have specific properties that are not intrinsic to most mesoporous materials. The required properties can be achieved by loading mesoporous materials with nanoparticles possessing specific properties, 3-9 e.g. Pd and Pt particles for catalytic capability, 4 iron/iron oxide particles for magnetic properties, 8 or Ag-Au alloy particles for optical properties. 9 However, uploading nanoparticles into mesoporous materials and preventing the nanoparticles from aggregation during fabrication and application processes remain a major challenge. 10, 11 Here we report a single-step method for fabrication of metal nanoparticle/mesoporous alumina composite, with tuned pore morphology and particle distribution, through anodizing of a commercial aluminum alloy. The approach can easily be implemented on a large scale and extended to other alloy systems consisting of a valve metal and different alloying elements with Gibbs free energy of oxide formation less negative than that of the valve metal, having potential impacts on nanoarchitecture design and nanostructure synthesis.AA2099-T8 aluminum alloy (1.62 wt.% Li; 2.83 wt.% Cu; 0.72 wt.% Zn; 0.30 wt.% Mg; 0.29 wt.% Mn; 0.04 wt.% Fe; 0.06 wt.% K; 985 ppm Zr; 180 ppm Si; 1.5 ppm Ag and remainder Al) was anodized in a mixed solution of 0.4 M sulfuric acid and 0.53 M tartaric acid at room temperature, by linearly increasing the voltage from the open circuit potential (OCP) to 3 V vs. saturated calomel electrode (SCE) at a sweep rate of 0.03 V/min, using a Solartron 1287 potentiostat. The anodizing conditions were chosen based on previous finding that copper could not be oxidized below 3 V (SCE). 12 Figure 1a shows a transmission electron micrograph of an utramicrotomed 13 cross section of the anodized alloy, revealing the porous anodic alumina attached to the alloy substrate. As a consequence of the increasing voltage with time during the potentiodynamic sweep, the pore diameter and interpore spacing increase toward the alloy/film interface, due to the linear relationship between the applied voltage and the pore diameter and the barrier layer thickness. 14 The pore diameter and interpore spacing near the alloy/film interface a...