Description:
<jats:title>Abstract</jats:title><jats:p>The assembly of 3D nanoscale structures of plasmonic nanoparticles (NPs) holds great promise for achieving enhanced optical and electronic properties. This type of materials exhibits a large number of surface hot spots, while offering the possibility for synergetic effects to be observed. Herein, a facile, yet powerful, strategy to fabricate 3D mesoporous networks of copper NPs decorated with graphite layers (denoted as Cu/G) is demonstrated by using a polymer‐assisted self‐assembly method. After thermal processing, the resulting Cu/G‐linked networks retain an open and interconnected porosity with a large surface area (up to 90 m<jats:sup>2</jats:sup> g<jats:sup>−1</jats:sup>) and narrow pore size distribution (ca. 4.3 nm in size). Owing to these characteristics, Cu/G assemblies behave as high‐performance surface‐enhanced Raman scattering (SERS) probes for the detection of analytes in very low concentrations. The substrates comprise low‐cost, environmentally benign materials and show promise for chemical and biological sensing applications.</jats:p>