High-Pressure High-Temperature Nanodiamond-Modified ZnO Nanocomposites as Promising Photocatalysts: Synthesis and Characterization

Zinc oxide (ZnO) nanostructures suffer from fast electron–hole recombination, limiting their applicability in photocatalytic environmental remediation, and carbon additives such as detonation nanodiamonds (DNDs) are constrained by their high defect density. To address this, ZnO nanocomposites modified with high-pressure, high-temperature nanodiamonds (HPHT NDs) were synthesized to evaluate whether their intrinsically lower defect density—evidenced by a dominant diamond Raman peak at 1330 cm−1 and a low sp2 carbon fraction of 6.6% compared to oxidized DNDs with strong D/G bands (~1350/1580 cm−1) and ~25–35% sp2 carbon—can enhance charge separation and improve photocatalytic activity. Oxidized HPHT NDs bearing carbonyl, carboxyl, and hydroxyl groups enabled covalent attachment to ZnO, and the resulting ND–ZnO composites were characterized by SEM/EDX, ATR-FTIR, Raman spectroscopy, XPS, and cathodoluminescence (CL). EDX confirmed increasing carbon incorporation from 13.0 to 52.9 at.%, while XPS revealed a 0.5 eV shift in the Zn 2p3/2 peak and an increase in Zn–O–Zn lattice oxygen from 31.3% to 61.6% in ND–ZnO 10. CL showed enhanced near-band-edge emission and reduced Zni-related luminescence (~3.0 eV). ND–ZnO 10 achieved a nearly threefold-higher degradation rate constant (0.0251 min−1) than pristine ZnO (0.0087 min−1) and retained 88% efficiency after five cycles, demonstrating strong potential for durable wastewater treatment.