We report on the first nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) study of the high-temperature nanodiamond-to-onion transformation. (1)H, (13)C NMR and EPR spectra of the initial nanodiamond samples and those annealed at 600, 700, 800 and 1800 ° C were measured. For the samples annealed at 600 to 800 ° C, our NMR data reveal the early stages of the surface modification, as well as a progressive increase in sp(2) carbon content with increased annealing temperature. Such quantitative experimental data were recorded for the first time. These findings correlate with EPR data on the sensitivity of the dangling bond EPR line width to air content, progressing with rising annealing temperature, that evidences consequent graphitization of the external layers of the diamond core. The sample annealed at 1800 ° C shows complete conversion of nanodiamond particles into carbon onions.
We report on EPR
and 13C and 1H NMR studies
of detonation nanodiamond particles with surface grafted by paramagnetic
gadolinium ions obtained by ion exchange with hydrogen atoms of carboxyl
groups through the reaction of aqueous nanodiamond suspension with
an aqueous solution of gadolinium nitrate. Our findings give clear
evidence that Gd3+ ions are chemically bound to the nanodiamond
surface and interact with electron and nuclear spins of the diamond
nanoparticle, which results in acceleration of electron and nuclear
spin–lattice relaxations. A model of positioning of Gd3+ ions on the DND surface terminated by oxygen-containing
groups is suggested. The distance between the Gd ion and nanodiamond
surface is estimated by relaxation measurements as 0.32 nm. Biomedical
applications of the studied nanomaterials are discussed.
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