Vergelijkend AFM Onderzoek: Microstructuur van bitumen in relatie tot healing

In this report we present the background, the scientific and experimental approach and the results of AFM experiments performed on two different batches of bitumen. The specific bitumen researched in this project has also been studied in the context of the InfraQuest project ‘Pragmatisch Healing Onderzoek’. It has been known for quite some time already that bitumen posessess a microstructure at the typical length scale of micrometers. This can be shown experimentally by imaging the bitumen surface with Atomic Force Microscopy (AFM). As is the case for many other engineering materials (e.g. steel), the microstructure will manifest itself by the macroscopic mechanical response of the material; thus on the typical length scales where it performs its load bearing function in pavement structures. Together with the hitherto not precisely specified properties of the many available bitumen grades, this justifies further research into the origin and properties of this microstructure. Here we also anticipate that a better understanding about the origin and properties of the bitumen microstructure will lead to improved bitumen grades (material appraisal) and possibly to better criteria for selecting a bitumen for a specific application. In the context of this research first the objectivity of the AFM imaging technique has to be established. Therefore two independent laboratories (TNO and CiTG, TU Delft) have prepared and conditioned bitumen samples for the AFM. All samples have been prepared from the same batch of bitumen. Then each laboratory has imaged its ‘home made ‘samples’ as well as the samples prepared at the other lab. The results appear to be qualitatively identical. Thus one may conclude that the microstructure of bitumen is a reproducible quantity. It was also found that the (thermal) conditioning of the bitumen (prior to imaging) has a significant impact on the microstructure observed. One may conclude from this that the sample conditioning procedure is a very important aspect in the AFM imaging process. In other words: an AFM image of bitumen is meaningless, unless the conditioning procedure of the samples is reported extensively. The next step was to find the influence of temperature on the observed bitumen microstructure. Identical samples have been prepared by TU Delft and both laboratories have imaged the microstructure as a function of temperature. A similar observation as stated before has been made: the microstructures observed by both laboratories were very similar. Moreover, it has been observed that the microstructure gradually disappears when the temperature is raised. However, even at the highest (experimental) temperatures (70 °C) traces of the microstructure remain visible. Apparently the ordering process that governs the bitumen microstructure has an associated interaction energy in the order of 400 kB, i.e. 30-40 meV (kB, Boltzmann constant). It was also found that (chemically) reclaimed bitumen (from an asphalt test beam) does show a microstructure as well. Surprisingly however, it was found that the microstructure of harder bitumen grades disappears at lower temperatures compared to softer bitumen grades. This is against the intuition that in harder bitumen molecules are more tightly bound together than in softer grades, and that for harder bitumen the microstructure would ‘melt’ (disappear) at higher temperatures. The molecular mobility appears to be higher in harder bitumen grade, hence they are anticipated to be better ‘healers’. Macroscopic fatigue test have shown similar trends.Structural EngineeringCivil Engineering and Geoscience

Proceedings 2nd workshop KPE-CEAB 2022: KPE-CEAB Characterization and Evaluation of Asphalt Binder Properties (CEAB)

Pavement Engineerin

Insights into Polymerization-induced Phase Separation of Epoxy-Bitumen Systems and Strategies to Tailor High-Performance Bituminous Materials

The utilization of epoxy-based polymers as bituminous modifiers in developing durable and long-lasting pavement structures have gained increasing interest over the last years showing evidence of high performing materials (1-8). It has been noticed that the addition of epoxy-based modifier into bitumen lead to materials with superior characteristics against oxidative aging (1, 3, 8). Next to aging resistance, the incorporation of epoxy modifiers in bituminous materials has added functional benefits, such as improved resistance to moisture damage and fatigue cracking (5, 6). Despite the evidence of aging resistance in epoxy-asphalt concrete mixes, the influence of the epoxy-based polymers on the bitumen aging and the microstructure morphology of newly formed systems have not been fundamentally evaluated yet. Within the scope of this research, the aging susceptibility of epoxy modified bitumen has been investigated. The extent of aging has been probed by using a Fourier Transform Infrared spectrometer and also rheologically evaluated using a dynamic shear rheometer. Furthermore, an improved compatibility between epoxy and bitumen at the microstructural level defines the long-term chemo-mechanical performance of EB systems in a controlled manner. Thus, another aspect of this study was to investigate the morphological and interfacial characteristics of EB microstructure.Pavement Engineerin

The role of rejuvenators in embedded damage healing for asphalt pavement

Rejuvenator encapsulation technique showed great potential for extrinsic asphalt pavement damage healing. Once the capsules are embedded within asphalt pavement, the healing is activated on-demand via progressing microcrack. When the microcrack encounters the capsule, the fracture energy at the tip opens the capsule and releases the rejuvenator. Then the released rejuvenator wets the crack surfaces, diffuses into and softens the aged bitumen, allowing two broken edges to come in the contact, preventing further asphalt pavement deterioration. The quality and speed of the damage repair process strongly depend on the quality of rejuvenator, thus it is important to choose a proper rejuvenator with good abilities to restore the lost properties of bitumen from ageing and show a sustainable performance after healing. To this aim, three different rejuvenators were studied and ranked based on the performance of their rejuvenated bitumen, including physical properties, rheological properties, chemical properties and the performance after re-ageing. Furthermore, these rejuvenators were encapsulated in calcium alginate capsules and the tests on these capsules indicate the diameter, mechanical resistance and thermal stability of the capsules are influenced by the encapsulated rejuvenator. The findings will benefit the development of rejuvenator encapsulation technique and the optimization of the capsule healing system towards a better healing effect in asphalt pavement.Materials and EnvironmentPavement Engineerin