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Aberration‐corrected microscopy and spectroscopy analysis of pristine, nitrogen containing detonation nanodiamond
Author(s) -
Turner Stuart,
Shenderova Olga,
Da Pieve Fabiana,
Lu Yinggang,
Yücelen Emrah,
Verbeeck Jo,
Lamoen Dirk,
Van Tendeloo Gustaaf
Publication year - 2013
Publication title -
physica status solidi (a)
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.532
H-Index - 104
eISSN - 1862-6319
pISSN - 1862-6300
DOI - 10.1002/pssa.201300315
Subject(s) - nanodiamond , electron energy loss spectroscopy , spectroscopy , materials science , high resolution transmission electron microscopy , transmission electron microscopy , diamond , nitrogen , analytical chemistry (journal) , carbon fibers , detonation , nanotechnology , chemistry , explosive material , physics , composite material , organic chemistry , chromatography , quantum mechanics , composite number
Aberration‐corrected transmission electron microscopy, electron energy‐loss spectroscopy, and density functional theory (DFT) calculations are used to solve several key questions about the surface structure, the particle morphology, and the distribution and nature of nitrogen impurities in detonation nanodiamond (DND) cleaned by a recently developed ozone treatment. All microscopy and spectroscopy measurements are performed at a lowered acceleration voltage (80/120 kV), allowing prolonged and detailed experiments to be carried out while minimizing the risk of knock‐on damage or surface graphitization of the nanodiamond. High‐resolution TEM (HRTEM) demonstrates the stability of even the smallest nanodiamonds under electron illumination at low voltage and is used to image the surface structure of pristine DND. High resolution electron energy‐loss spectroscopy (EELS) measurements on the fine structure of the carbon K‐edge of nanodiamond demonstrate that the typical π* pre‐peak in fact consists of three sub‐peaks that arise from the presence of, amongst others, minimal fullerene‐like reconstructions at the nanoparticle surfaces and deviations from perfect sp 3 coordination at defects in the nanodiamonds. Spatially resolved EELS experiments evidence the presence of nitrogen within the core of DND particles. The nitrogen is present throughout the whole diamond core, and can be enriched at defect regions. By comparing the fine structure of the experimental nitrogen K‐edge with calculated energy‐loss near‐edge structure (ELNES) spectra from DFT, the embedded nitrogen is most likely related to small amounts of single substitutional and/or A‐center nitrogen, combined with larger nitrogen clusters.