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C−H terminated nanometer scale diamonds (d = 1 to 15 nm) are synthesized from 1-fluoroadamantane at high pressure (6−8 GPa) and high temperature (500−1500 °C) in a multianvil press. High resolution transmission electron microscopy, X-ray diffraction, Raman, diffuse reflectance Fourier transform infrared, and X-ray absorption spectroscopies demonstrate the excellent crystallinity and atomically flat C−H terminated surfaces of nanodiamonds with (111) and (110) facets. The importance of hydrogen to the synthesis of nanodiamond and its faceting is discussed. Following vacancy generation, annealing and oxidation of the nanodiamonds, optically detected magnetic resonance and electron spin resonance coherence times (T2 = 0.9 and 2.1 μs) of nitrogen vacancy (NV) centers are measured. The obtained T2 values are equivalent to the shallow NV centers (depth <10 nm) in bulk diamond crystals and larger nanocrystals prepared by mechanical milling. 

Abstract Understanding the behavior of confined water at liquid–solid interfaces is central to numerous physical, chemical, and biological processes, yet remains experimentally challenging. Here, shallow nitrogen‐vacancy (NV) centers in diamond serve as sensors to investigate the nanoscale dynamics of interfacial water confined between the diamond surface and an overlying fluorinated oil droplet. With the help of nuclear magnetic resonance (NMR) protocols selectively sensitive to¹H and¹⁹F, NVs are used to probe water and oil near the interface under ambient conditions. Comparing opposite sides of a doubly‐implanted diamond membrane — one exposed to oil, the other not — a slow, multi‐day process is uncovered in which the interfacial water layer is gradually depleted. This desorption appears to be driven by sustained interactions with the fluorinated oil and is supported by molecular dynamics simulations and surface‐sensitive X‐ray spectroscopies. These findings provide molecular‐level insight into long‐timescale hydration dynamics and underscore the power of NV‐NMR for probing liquid–solid heterointerfaces with chemical specificity. 

Disorder and many body interactions are known to impact transport and thermalization in competing ways, with the dominance of one or the other giving rise to fundamentally different dynamical phases. Here we investigate the spin diffusion dynamics of 13 C in diamond, which we dynamically polarize at room temperature via optical spin pumping of engineered color centers. We focus on low-abundance, strongly hyperfine-coupled nuclei, whose role in the polarization transport we expose through the integrated impact of variable radio-frequency excitation on the observable bulk 13 C magnetic resonance signal. Unexpectedly, we find good thermal contact throughout the nuclear spin bath, virtually independent of the hyperfine coupling strength, which we attribute to effective carbon-carbon interactions mediated by the electronic spin ensemble. In particular, observations across the full range of hyperfine couplings indicate the nuclear spin diffusion constant takes values up to two orders of magnitude greater than that expected from homo-nuclear spin couplings.