Structure evolution of nanodiamond aggregates: a SANS and USANS study

J Appl Crystallogr. 2022 Mar 25;55(Pt 2):353-361. doi: 10.1107/S1600576722002084. eCollection 2022 Apr 1.

Abstract

Ultra-small-angle neutron scattering (USANS) and small-angle neutron scattering (SANS) measurements, covering length scales from micrometres to nanometres, were made to investigate the structure of nanodiamonds (NDs) and their suspensions. These nanodiamonds were produced by two different techniques, namely by the detonation method and by the laser ablation of a carbon-hydro-carbon mixture. The (U)SANS results indicated the presence of structures four orders of magnitude larger than the dimensions of a single ND particle, consisting of aggregations of ND particles. This aggregation of the ND particles was studied by employing the contrast variation technique. Two different solvents, namely H2O and dimethyl sulfoxide (and their deuterated counterparts), were used to understand the role of hydrogen in the shape and size of the aggregates. The analysis of experimental data from SANS measurements also reveals the ND particles to have an ellipsoidal structure. Using a defined shape model and the SANS contrast variation technique, it was possible to characterize the non-diamond outer shell of the particles and determine the outer layer thickness. This clarification of the structure of the NDs will allow better preparation of suspensions/samples for various applications. Understanding the structure of NDs at multiple length scales also provides crucial knowledge of particle-particle interaction and its effect on the aggregation structures.

Keywords: cold neutron sources; detonation NDs; laser synthesis technique; nanodiamonds; small-angle neutron scattering.