This review covers literature published up to June 2026. Detecting various water pollutants quickly and reliably remains a challenge. Boron-doped diamond (BDD) electrodes, particularly when fabricated as nanostructured thin films such as nanocones or nanowalls, offer a wide electrochemical window, low background current,
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This review covers literature published up to June 2026. Detecting various water pollutants quickly and reliably remains a challenge. Boron-doped diamond (BDD) electrodes, particularly when fabricated as nanostructured thin films such as nanocones or nanowalls, offer a wide electrochemical window, low background current, and excellent chemical stability, making them promising tools for electrochemical sensing. However, unmodified BDD electrodes face an inherent trade-off among conductivity, active site density, and interfacial stability, a phenomenon termed herein the “sensitivity-selectivity-stability triangle bottleneck”, which severely limits practical performance. In this review, we demonstrate how multi-scale structural regulation can circumvent this bottleneck. Specifically, a triple strategy comprising boron doping, surface modification, and post-annealing treatment is proposed and evaluated. First, the effect of boron doping level on conductivity and active site density is discussed. Second, two common surface modification approaches are examined: carbon nanomaterials (which increase surface area and form conductive networks) and metal nanoparticles (which enhance catalytic activity and interfacial charge transfer). Third, post-annealing is highlighted as a key synergistic step that locks the modified layer and stabilizes the interface. Together, these three components form an integrated framework. To provide concrete guidance, the performance of each strategy is compared for representative water pollutants, including heavy metal ions, phenolic compounds, and emerging contaminants such as antibiotics and pesticides, with emphasis on sensitivity, selectivity, and stability. Representative detection limits achieved include 0.01 μg/L for Pb
2+, 5 nM for acetaminophen, and 0.32 fM for PCB-77, demonstrating the effectiveness of the triple structural regulation strategy. Finally, in line with the theme of this Nanomaterials Special Issue on nanostructured thin films, current challenges in structural regulation are summarized, and future directions, including multi-parameter optimization, AI-assisted high-throughput screening, and real-world testing, are outlined. The goal is to offer practical structure-performance guidelines for designing BDD-based electrochemical sensors that are both high-performing and durable.
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