Researchers have developed a mesoporous nanoplate network of two-dimensional (2D) layered nickel hydroxide (Ni(OH)2) intercalated with polyoxovanadate (POV) anions using a chemical solution deposition method. This technique allows precise control over the chemical composition and pore structure of the Ni(OH)2–POV nanohybrids. The ordered layer-by-layer growth of Ni(OH)2–POV is confirmed by powder X-ray diffraction and high-resolution transmission electron microscopy. The nanohybrids form a highly porous, interconnected network with a lateral size of approximately 400 nm and thicknesses ranging from 5 nm to 7 nm. These thin films function as highly active electrochemical capacitor electrodes, offering a maximum specific capacity of 1440 F g−1 at a current density of 1 A g−1 and maintaining 85% capacity retention over 2000 cycles. The superior electrochemical performance is attributed to the expanded mesoporous surface area and the intercalation of POV anions, highlighting their potential for use in highly efficient supercapacitor electrodes. / Journal cover design by scapiens