Scalable High-Yield Exfoliation of Hydrophilic h-BN Nanosheets via Gallium Intercalation

Hexagonal boron nitride (h-BN) possesses a unique combination of a wide bandgap, high thermal conductivity, and chemical inertness, making it a key insulating and thermal management material for advanced electronics and nanocomposites. However, its intrinsic hydrophobicity and strong interlayer van der Waals forces severely limit exfoliation efficiency and dispersion stability, particularly in scalable liquid-phase processes. Here, we report a synergistic exfoliation strategy that integrates acid-induced hydroxylation with gallium (Ga) intercalation to achieve high-yield (>80%) production of ultrathin (<4 nm) hydrophilic h-BN nanosheets. Hydroxylation introduces abundant -OH groups, expanding interlayer spacing and significantly increasing surface polarity, while Ga intercalation leverages its native Ga2O3 shell to form strong interfacial interactions with hydroxylated basal planes. This oxide-mediated adhesion facilitates efficient layer separation under mild sonication, yielding nanosheets with well-preserved lateral dimensions and exceptional dispersion stability in polar solvents. Comprehensive characterization confirms the sequential chemical and structural modifications, revealing the crucial roles of hydroxylation-induced activation and Ga2O3 assisted wettability enhancement. This combined chemical activation–soft metallic intercalation approach provides a scalable, solution-processable route to high-quality h-BN nanosheets, opening new opportunities for their integration into dielectric, thermal interface, and multifunctional composite systems.