Journal Article

Multi-instrument characterization of five nanodiamond samples: a thorough example of nanomaterial characterization

Farrer, Jeffrey K, Farnsworth, Paul B, Linford, Matthew R, Jones, Hodge F, Singh, Bhupinder, Smith, Stacey J, Vanfleet, Richard, Jensen, David S, Dadson, Andrew E

2016

Overview

Here, we report the most comprehensive characterization of nanodiamonds (NDs) yet undertaken. Five different samples from three different vendors were analyzed by a suite of analytical techniques, including X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS), inductively coupled plasma mass spectrometry (ICP-MS), diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), Brunauer-Emmett-Teller (BET) surface area measurements, and particle size distribution (PSD) measurements. XPS revealed the elemental compositions of the ND surfaces (83–87 at.% carbon and 12–14 at.% oxygen) with varying amounts of nitrogen (0.4–1.8 at.%), silicon (0.1–0.7 at.%), and tungsten (0.3 at.% only in samples from one vendor). ToF-SIMS and ICP showed metal impurities (Al, Fe, Ni, Cr, etc. with unexpectedly high amounts of W in one vendor’s samples: ca. 900 ppm). Principal component analyses were performed on the ToF-SIMS and ICP data. DRIFT showed key functional groups (–OH, C=O, C–O, and C=C). BET showed surface areas of 50–214 m²/g. XRD and TEM revealed PSD (bimodal distribution and a wide PSD, 5–100 nm, for one vendor’s samples). XRD also provided particle sizes (2.7–27 nm) and showed the presence of graphite. EELS gave the sp²/sp³ contents of the materials (37–88 % sp³). PSD measurements were performed via differential sedimentation of the particles (mean particle size ca. 17–50 nm). This comprehensive understanding should allow for improved construction of nanodiamond-based materials. Graphical Abstract Five different nanodiamond samples were exhaustively characterized using a suite of analytical techniques.

• Publisher: Springer Berlin Heidelberg,Springer,Springer Nature B.V
• Subject: aluminum / Analysis / Analytical Chemistry / Biochemistry / Characterization and Evaluation of Materials / Chemistry / Chemistry and Materials Science / Chromatography / chromium / Diffraction / Drift / Electron energy loss spectroscopy / Electrons / elemental composition / energy / Energy loss / Food Science / Fourier transforms / graphene / Inductively coupled plasma / iron / Laboratory Medicine / Mass spectrometry / Monitoring/Environmental Analysis / nanodiamonds / Nanomaterials / Nanoparticles / Nanostructure / nickel / nitrogen / oxygen / Particle size / particle size distribution / reflectance / Research Paper / Scientific imaging / silicon / Spectroscopy / Surface area / Transmission electron microscopy / Tungsten / X-ray diffraction / X-ray photoelectron spectroscopy / X-rays