Investigation of the bulk and surface microstructure of bitumen by atomic force microscopy

Bitumen, the heavy residue of crude oil, can display a rich microscale morphology, including so-called Bee structures. The use of Atomic Force Microscopy (AFM) measurements in literature strongly indicates that the appearance of Bee structures is related to the presence of paraffin wax crystals. Most studies have investigated standard bitumen surfaces when cooling bitumen in an air atmosphere. Only a few investigations have analysed surfaces formed in other media or have analysed fractured surfaces which relate to the bulk morphology. Although considerable research has focussed on identifying Bee structures, less attention has been paid to the Bee structure morphology of different bitumen types and the relations to other binder parameters. The comparison between the micro morphology of the air-oil interface compared to the bulk phase volume has been studied even less. In this experimental study, five bitumen samples were selected based on differences in their natural wax content. Both the air-cooled surface interface and fractured surfaces were characterised using AFM in tapping mode. All the air-cooled surfaces revealed Bee structures, except the wax-free bitumen, which did not display the presence of any Bee structure. None of the fracture surfaces revealed Bee structures. Reheating a fractured surface of a wax-containing bitumen transformed the morphology into Bee structures. The experiments demonstrate that Bee structures are present in different binders but display very different shapes and sizes. Flowever: image analysis indicates that the unit cell inside these structures is rather constant and independent of the binder type. This work confirms a relationship between natural wax and Bee structures and it also shows that Bee structures, as such, are a surface phenomenon which is not present in the bulk phase volume of samples. (C) 2018 Elsevier Ltd. All rights reserved.