Temperature induced healing in strained bituminous materials observed by atomic force microscopy

Bitumen is the binder in the composite material named asphalt concrete. Under cyclic mechanical loading of traffic passing over the pavement, eventually damage will initiate in the pavement, leading to eventual structural failure. This damaging process is accelerated by time dependent change of the mechanical properties of asphalt concrete due to ageing mechanisms like oxidation. Bitumen displays spatial heterogeneity at the micrometer scale, which has been observed by atomic force microscopy (AFM). The mechanical properties of the elliptical, microstructural domains of bitumen are distinct from those of the continuous phase. This introduces stiffness discontinuities in the material, which under mechanical loading will concentrate stresses at the interfaces, and thus the locations where early stages of damage will develop. This work aims at in situ probing of the crack healing of bituminous materials as a function of moderate temperature changes. The bitumen was prepared on a flexible substrate which was mechanically strained to induce damage. AFM measurements of the strained bitumen specimen provides evidence of the crack initiation at the interface and the predominant propagation of cracks through the elliptical domain phases. Healing of these cracks was observed after applying modest amounts of heat to the material. Meanwhile the process was monitored in situ with AFM. With increase of temperature one of the phases starts softening, while the material as a whole remains solid. This allows the phases to rearrange and meanwhile eliminating micro cracks at the interface

Extracting hysteresis from nonlinear measurement of wavefront-sensorless adaptive optics system

In many scientific and medical applications wavefront-sensorless adaptive optics (AO) systems are used to correct the wavefront aberration by optimizing a certain target parameter, which is nonlinear with respect to the control signal to the deformable mirror (DM). Hysteresis is the most common nonlinearity of DMs, which can be corrected if the information about the hysteresis behavior is present. We report a general approach to extract hysteresis from the nonlinear behavior of the adaptive optical system, with the illustration of a Foucault knife test, where the voltage–intensity relationship consists of both hysteresis and some memoryless nonlinearity. The hysteresis extracted here can be used for modeling and linearization of the AO system.Delft Center for Systems and ControlMechanical, Maritime and Materials Engineerin

Microstructural Changes in Bitumen at the onset of Damage-healing

Self-healing of bitumen is a property that positively contributes to the sustainability, maintenance requirements and cost effectiveness of asphalt pavements. Ideally one would like to design an asphalt mix with a well-defined healing potential. Although substantial research efforts have been dedicated to the healing mechanism in bitumen, complete understanding of the fundamental mechanisms that govern the property of healing is still lacking. Here we investigate the manifestation of damage and healing of bitumen at the microstructural level. Three distinct bitumen grades are subjected to mechanical loading conditions, and the damage is investigated at the microstructural level by atomic force microscopy combined with finite element simulations. One of the bituminous phases appears to display visible signs of cracks, which are found to (partly) disappear at moderate temperature changes. Simulations of mechanical loading of experimentally derived finite element meshes are corresponding well with these experimental observations. Moreover, the simulations provide a measure of mechanical response, i.e. stiffness, of the material as a function of strain level. From this it is found that the microstructural cracks lead to diminished structural response properties, whereas after healing these properties are partly recovered. The experimental observations, together with the simulations, support earlier ideas that relate the phenomenon of self-healing in bitumen to their rheological property of thixotropy. Moreover, the work presented hints that the property of self-healing is governed by processes at the microstructural length scale.Pavement Engineerin

Model-based aberration correction in a closed-loop wavefront-sensor-less adaptive optics system

In many scientific and medical applications, such as laser systems and microscopes, wavefront-sensor-less (WFSless) adaptive optics (AO) systems are used to improve the laser beam quality or the image resolution by correcting the wavefront aberration in the optical path. The lack of direct wavefront measurement in WFSless AO systems imposes a challenge to achieve efficient aberration correction. This paper presents an aberration correction approach for WFSlss AO systems based on the model of the WFSless AO system and a small number of intensity measurements, where the model is identified from the input-output data of the WFSless AO system by black-box identification. This approach is validated in an experimental setup with 20 static aberrations having Kolmogorov spatial distributions. By correcting N = 9 Zernike modes (N is the number of aberration modes), an intensity improvement from 49% of the maximum value to 89% has been achieved in average based on N +5 = 14 intensity measurements. With the worst initial intensity, an improvement from 17% of the maximum value to 86% has been achieved based on N + 4 = 13 intensity measurements.Delft Center for Systems and ControlMechanical, Maritime and Materials Engineerin

Automated spherical aberration correction in scanning confocal microscopy

Mismatch between the refractive indexes of immersion media and glass coverslips introduces spherical aberrations in microscopes especially for high numerical aperture objectives. This contribution demonstrates an automated adjustment of the coverslip correction collar in scanning confocal microscopy to compensate for spherical aberrations due to coverslip thickness mismatch. With a motorized coverslip correction collar, the adjustment procedure consists of xz image scans, image processing, correction quality evaluation, the mismatch estimation, and eventually the optimal adjustment of the correction collar. For fast correction with less photodamage, coarse-fine Gaussian fitting algorithms are proposed and evaluated with various specimen for their estimation accuracy. The benefits of the proposed automated correction are demonstrated for various coverslips with biological specimens, showing the optimized resolution of the confocal microscope.Delft Center for Systems and ControlMechanical, Maritime and Materials Engineerin

Is Atomic Force Microscopy suited as Tool for fast Screening of Bituminous Materials? An Inter-laboratory Comparison Study

Bituminous binders are known to have microstructures at typical length scales of micrometers. This microstructure can be probed with Atomic Force Microscopy (AFM). Now that worldwide several research groups are reporting AFM results on bitumen, it is becoming important to improve the understanding of the reproducibility and objectivity of the technique for studying bituminous samples. When reproducibility and stability are proven, AFM can be a tool for asphalt professionals to rapidly screen bituminous binders. In this context two independent laboratories have developed a standard method for preparing and conditioning bitumen for AFM imaging. By means of an inter-laboratory comparison of independently imaged specimen, the reproducibility of microstructure measurements was investigated. A quantitative comparison on different microstructures was developed, and the consistency of independently obtained results was confirmed. The results from both labs were comparable: the microstructural properties were found to be randomly distributed within a 5% interval. Also the influence of temperature on the microstructure was demonstrated to be reproducible and consistent. With the increase of temperature, the microstructure gradually disappeared, however traces of the microstructure remained visible up to the highest measurement temperature of 60°C. It is concluded that given well defined sample preparation and measurement procedures, the microstructure of bitumen can be reproducibly imaged by AFM from room temperature up to temperatures where bitumen has become soft and too sticky to be probed by the same setup as used for lower temperatures.Structural EngineeringCivil Engineering and Geoscience

Adaptive optics for confocal laser scanning microscopy with adjustable pinhole

The pinhole plays an important role in confocal laser scanning microscopy (CLSM) for adaptive optics (AO) as well as in imaging, where the size of the pinhole denotes a trade-off between out-of-focus rejection and wavefront distortion. This contribution proposes an AO system for a commercial CLSM with an adjustable square pinhole to cope with such a trade-off. The proposed adjustable pinhole enables to calibrate the AO system and to evaluate the imaging performance. Experimental results with fluorescence beads on the coverslip and at a depth of 40 μm in the human hepatocellular carcinoma cell spheroid demonstrate that the proposed AO system can improve the image quality by the proposed calibration method. The proposed pinhole intensity ratio also indicates the image improvement by the AO correction in intensity as well as resolution.Team Raf Van de Pla

Turning Back Time: Rheological and Microstructural Assessment of Rejuvenated Bitumen

Countermeasures to the ageing of bituminous asphalt binders is a highly important topic, both for service-life extension of asphalt ‘in the field’ and for recycling old pavements (RAP) into new structures with similar functional requirements as the original structure. Usually this is achieved by applying additives that restore the adhesive and mechanical properties of the original bituminous binder. These additives are commonly termed (asphalt) rejuvenators. Here we examine the performance of two very distinct rejuvenating agents. Usually the effectiveness of rejuvenators is measured by comparing the penetration and softening point of the rejuvenator-aged bitumen blend to reference values of the virgin binder. First, the rejuvenating capabilities of the two additives are evaluated in terms of rheology using a dynamic shear rheometer. Then the microstructures of the virgin binder and the rejuvenated blends are obtained by means of atomic force microscopy. Subsequently the rheological results are related to the microstructure morphologies. One finds from rheology that both rejuvenators exhibit the desired softening and property restoring performance. Though, one rejuvenator does so at much lower dose rates. By correlating rheology to the microstructural observations one finds that the effect of both rejuvenators is very distinct at microscopic length scales: rejuvenation is achieved by distinct chemo-physical mechanisms. One of the rejuvenators restores the virgin microstructure, whereas the other rejuvenator generates a new morphology. Thus, it is demonstrated that by combining rheological and microstructural techniques, the mechanism and performance of rejuvenation can be understood. This may guide future designs and optimization of asphalt rejuvenating agents.Structural EngineeringCivil Engineering and Geoscience