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This work reports the template- and etching-free fabrication of hollow bimetallic nickel-cobalt benzenetricarboxylic acid (Ni-Co BTC) hexagonal nanoplates by a polyvinylpyrrolidone (PVP)-assisted approach. The incorporation of PVP can reduce the stacking of these nanoplates along the vertical direction and generate depletion forces between them to reduce aggregation. When employed for the quartz crystal microbalance (QCM) sensing of ammonia (NH₃), the hollow Ni-Co BTC hexagonal nanoplates exhibit 1.6, 3.8, and 7.5 times higher sensitivity to 69.5 ppm of NH₃ than non-hollow Ni-Co BTC nanoplates, Ni-BTC nanobelts, and Co-BTC microrods, respectively, and a low limit of detection (LOD) of 1.53 ppm. Additionally, they show good selectivity to NH₃ in the presence of other interfering compounds and excellent stability with only a very small decrease of 2.86 % in sensitivity after 6 months. The NH₃ …