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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.

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.

Studies of diesel system deposits continue to be the subject of interest and publications worldwide. The introduction of high pressure common rail systems resulting in high fuel temperatures in the system with the concomitant use of fuels of varying solubilizing ability (e.g. ULSD and FAME blends) have seen deposits formed at the tip of the injector and on various internal injector components. Though deposit control additives (DCAs) have been successfully deployed to mitigate the deposit formation, work is still required to understand the nature and composition of these deposits. The study of both tip and internal diesel injector deposits (IDID) has seen the development of a number of bench techniques in an attempt to mimic field injector deposits in the laboratory. One of the most used of these is the Jet Fuel Thermal Oxidation Tester or JFTOT (ASTM D3241).

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.