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Characterization of soot nanoparticle morphology can be used to develop understanding of nanoparticle interaction with engine lubricant oil and its additives. It can be used to help direct modelling of soot-induced thickening, and in a more general sense for combatting reductions in engine efficiency that occur with soot-laden oils. Traditional 2D transmission electron microscopy (TEM) characterization possesses several important shortcomings related to accuracy that have prompted development of an alternative 3D characterization technique utilizing electron tomography, known as 3D-TEM. This work details progress made towards facilitating semi-automated image acquisition and processing for location of structures of interest on the TEM grid. Samples were taken from a four cylinder 1.4 L gasoline turbocharged direct injection (GTDI) engine operated in typically extra-urban driving conditions for 20,284 km, with automatic cylinder deactivation enabled.

Formation of soot is a known phenomenon for diesel engines, however, only recently emerged for gasoline engines with the introduction of direct injection systems. Soot-in-oil samples from a three-cylinder turbocharged gasoline direct injection (GDI) engine have been analysed. The samples were collected from the oil sump after periods of use in predominantly urban driving conditions with start-stop mode activated. Thermogravimetric analysis (TGA) was performed to measure the soot content in the drained oils. Soot deposition rates were similar to previously reported rates for diesel engines, i.e. 1 wt% per 15,000 km, thus indicating a similar importance. Morphology was assessed by transmission electron microscopy (TEM). Images showed fractal agglomerates comprising multiple primary particles with characteristic core-shell nanostructure. Furthermore, large amorphous structures were observed. Primary particle sizes ranged from 12 to 55 nm, with a mean diameter of 30 nm and mode at 31 nm.

Morphology plays an important role in determining behaviour and impact of soot nanoparticles, including effect on human health, atmospheric optical properties, contribution to engine wear, and role in marine ecology. However, its nanoscopic size has limited the ability to directly measure useful morphological parameters such as surface area and effective volume. Recently, 3D morphology characterization of soot nanoparticles via electron tomography has been the subject of several introductory studies. So-called ‘3D-TEM’ has been posited as an improvement over traditional 2D-TEM characterization due to the elimination of the error-inducing information gap that exists between 3-dimensional soot structures and 2-dimensional TEM projections. Little follow-up work has been performed due to difficulties with developing methodologies into robust high-throughput techniques.

The size and morphology of soot particles and agglomerates extracted from lubricating oil drawn from the sump of a diesel engine have been investigated and compared using Transmission Electron Microscopy (TEM) and Nanoparticle Tracking Analysis (NTA). Samples were prepared for electron microscopy imaging by both centrifugation and solvent extraction to investigate the impact of these procedures on the morphological characteristics, such as skeleton length and width and circularity, of the obtained soot. It was shown that centrifugation increases the extent of agglomeration within the sample, with 15% of the agglomerates above 200 nm compared to only 11% in the solvent extracted soot. It was also observed that the width of centrifugation extracted soot was typically 10 nm to 20 nm larger than that of solvent extracted soot, suggesting that centrifugation forces the individual agglomerate chains together.

The effect of legislation in driving towards lower emissions has seen significant changes in injector design, (common- rail) and fuel composition (ULSD). This has led to numerous reports of deposits throughout the vehicle diesel system, filters, tanks, pumps and injectors. In recent examples, deposits internal to the fuel injector on the needle have become prevalent and characterisation of the deposits on the injector needle has become an industry priority. A number of studies have made progress on this but the deposits have proven difficult to fully characterise and often have an ineradicable nature, which makes analysis other than in situ difficult. This paper will describe for the first time the application of a number of surface techniques, in combination which not only provide characterisation data but also the ability to provide cross-sectional lifts out of the sample, which may then be the subject of further analysis.

The determination of size distribution of soot particles and agglomerates in oil samples using a Nanosight LM14 to perform Nanoparticle Tracking Analysis (NTA) is described. This is the first application of the technique to sizing soot-in-oil agglomerates and offers the advantages of relatively high rates of sample analysis and low cost compared to Transmission Electron Microscopy (TEM). Lubricating oil samples were drawn from the sump of automotive diesel engines run under a mix of light duty operating conditions. The oil samples were diluted with heptane before analysing. Results from NTA analysis were compared with the outputs of a more conventional analysis based on Dynamic Light Scattering (DLS). This work shows that soot-in-oil exists as agglomerates with average size of 115 nm. This is also in good agreement with TEM analysis carried out in a previous work. NTA can measure soot particles in polydisperse oil solutions and report the size distribution of soot-in-oil aggregates.