2D and 3D TEM Characterisation of Benzene and Ethylene Soot

Abstract

Flame-generated soot particles from two different fuels, benzene (B) and ethylene (E), at different ageing conditions, were analysed to assess their morphological and structural features. Samples were collected at 6, 10 and 14 mm from the nozzle location. Traditional 2D transmission electron microscopy (TEM) and a novel 3D TEM were used to investigate morphology variations. High-resolution TEM (HRTEM) was used to capture structural characteristics. Samples were then placed on lacey carbon microgrids. A field emission gun TEM was used to capture images of the agglomerates. Tilt series of ±60 degrees were acquired at 1-degree steps to perform the 3D reconstruction. IMOD software and backwards projection were used to reconstruct the tomogram from the tilt series. The 2D analysis revealed that soot particles’ agglomerations for both fuels change from a bundle to a chain-like structure as they “age”, i.e., extracted at a higher “flame height”. In B, the primary particle diameter increases as they get “older,” whereas in E, the opposite happens, and overall, E particles are bigger than B ones. The nanostructure presents ordered regions with parallel-stacked layers of carbon lamellae. This is more evident in the aged soot samples, with the difference that in E a thick amorphous layer is present at the edge of the particles, which is not observable for B. A nanostructure analysis suggests a trend of increasing fringes length as the soot ages, going from 1.04 nm of B6 to 1.22 nm of B10 to 1.05 nm of B14 and from 1.139 nm of E6 to 1.20 nm of E14 (±0.02 nm). The tortuosity does not vary greatly across all the samples, ranging between 1.132 and 1.149 (±0.004). Separation is also quite similar everywhere, with 0.404 nm of B6, 0.392 nm of B10, 0.399 nm of B14, 0.397 nm of E6 and 0.396 nm of E14 (±0.002 nm). Ring structures and particle overlaps, two examples of geometrical characteristics concealed in 2D, can be seen in the 3D reconstructions. Furthermore, the comparison between 3D and 2D volume and surface area raises questions about the reliability of those parameters as derived from 2D measurements. This study advances knowledge of how soot structure can be affected by the fuel type and emphasises the significance of how soot is investigated.