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1. Morphology and kinetics of asphalt binder microstructure at gas, liquid and solid interfaces

   https://doi.org/10.1111/jmi.12842  

   RAMM, A. ; DOWNER, M. C. ; SAKIB, N. ; BHASIN, A. ( November 2019 , Journal of Microscopy)

   We combined optical and atomic force microscopy to observe morphology and kinetics of microstructures (typically referred to as bees) that formed at free surfaces of unmodified Performance Graded (PG) 64‐22 asphalt binders upon cooling from 150°C to room temperature (RT) at 5°C min^–1, and changes in these microstructures when the surface was terminated with a transparent solid (glass) or liquid (glycerol) overlayer. The main findings are: (1) at free binder surfaces, wrinkled microstructures started to form near the crystallization temperature (∼45°C) of saturates such as wax observed by differential scanning calorimetry, then grew to ∼5 µm diameter, ∼25 nm wrinkle amplitude and 10–30% surface area coverage upon cooling to RT, where they persisted indefinitely without observable change in shape or density. (2) Glycerol coverage of the binder surface during cooling reduced wrinkled area and wrinkle amplitude three‐fold compared to free binder surfaces upon initial cooling to RT; continued glycerol coverage at RT eliminated most surface microstructures within ∼4 h. (3) No surface microstructures were observed to form at binder surfaces covered with glass. (4) Submicron bulk microstructures were observed by near‐infrared microscopy beneath the surfaces of all binder samples, with size, shape and density independent of surface coverage. No tendency of such structures to float to the top or sink to the bottom of mm‐thick samples was observed. (5) We attribute the dependence of surface wrinkling on surface coverage to variation in interface tension, based on a thin‐film continuum mechanics model.

   Asphalt binder, or bitumen, is the glue that holds aggregate particles together to form a road surface. It is derived from the heavy residue that remains after distilling gasoline, diesel and other lighter products out of crude oil. Nevertheless, bitumen varies widely in composition and mechanical properties. To avoid expensive road failures, bitumen must be processed after distillation so that its mechanical properties satisfy diverse climate and load requirements. International standards now guide these mechanical properties, but yield varying long‐term performance as local source composition and preparation methods vary.In situdiagnostic methods that can predict bitumen performance independently of processing history are therefore needed. The present work focuses on one promising diagnostic candidate: microscopic observation of internal bitumen structure. Past bitumen microscopy has revealed microstructures of widely varying composition, size, shape and density. A challenge is distinguishing bulk microstructures, which directly influence a binder's mechanical properties, from surface microstructures, which often dominate optical microscopy because of bitumen's opacity and scanning‐probe microscopy because of its inherent surface specificity. In previously published work, we used infrared microscopy to enhance visibility of bulk microstructure. Here, as a foil to this work, we use visible‐wavelength microscopy together with atomic‐force microscopy (AFM) specifically to isolatesurfacemicrostructure, to understand its distinct origin and morphology, and to demonstrate its unique sensitivity to surface alterations. To this end, optical microscopy complements AFM by enabling us to observe surface microstructures form at temperatures (50°C–70°C) at which bitumen's fluidity prevents AFM, and to observe surface microstructure beneath transparent, but chemically inert, liquid (glycerol) and solid (glass) overlayers, which alter surface tension compared to free surfaces. From this study, we learned, first, that, as bitumen cools, distinctly wrinkled surface microstructures form at the same temperature at which independent calorimetric studies showed crystallization in bitumen, causing it to release latent heat of crystallization. This shows that surface microstructures are likely precipitates of the crystallizable component(s). Second, a glycerol overlayer on the cooling bitumen results in smaller, less wrinkled, sparser microstructures, whereas a glass overlayer suppresses them altogether. In contrast, underlying smaller bulk microstructures are unaffected. This shows that surface tension is the driving force behind formation and wrinkling of surface precipitates. Taken together, the work advances our ability to diagnose bitumen samples noninvasively by clearly distinguishing surface from bulk microstructure.

    

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2. Investigation of the flexural and thermomechanical properties of nanoclay/graphene reinforced carbon fiber epoxy composites

   https://doi.org/10.1557/jmr.2019.302  

   Tareq, Md Sarower ; Zainuddin, S. ; Woodside, E. ; Syed, F. ( November 2019 , Journal of Materials Research)

   null (Ed.)

   Flexural and thermomechanical properties of the epoxy-based carbon fiber composites (CFCs) on addition of single and binary nanoparticles (nanoclay and graphene) have been investigated. It was found that nanoclay acts more effectively in increasing the stiffness of the CFCs, whereas graphene is more effective in achieving higher strength. Nanoclay-added samples exhibited highest flexural (64.5 GPa) and storage (25.3 GPa) modulus among all types. Graphene-added samples showed highest improvement (by 21%) in flexural strength and exhibited most stable thermomechanical properties with highest energy dissipation capability (3.1 GPa loss modulus) in flexural test and dynamic mechanical analysis (DMA), respectively. By contrast, addition of binary nanoparticles reduced the stiffness and significantly increased the strain to failure (42%) of the composites. Optical microscopy and scanning electron microscopy indicated that addition of nanoparticles significantly reduced delamination and matrix cracking of the CFCs because of strong interfacial bonding and toughened matrix, respectively. 

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3. Can AFM be used to measure absolute values of Young's modulus of nanocomposite materials down to the nanoscale?

   https://doi.org/10.1039/D0NR02314K  

   Liu, Yuke ; Sokolov, Igor ; Dokukin, Maxim E. ; Xiong, Yongqiang ; Peng, Ping'an ( June 2020 , Nanoscale)

   At present, a technique potentially capable of measuring values of Young's modulus at the nanoscale is atomic force microscopy (AFM) working in the indentation mode. However, the question if AFM indentation data can be translated into absolute values of the modulus is not well-studied as yet, in particular, for the most interesting case of stiff nanocomposite materials. Here we investigate this question. A special sample of nanocomposite material, shale rock, was used, which is relatively homogeneous at the multi-micron scale. Two AFM modes, force-volume and PeakForce QNM were used in this study. The nanoindentation technique was used as a control benchmark for the measurement of effective Young's modulus of the shale sample. The indentation rate was carefully controlled. To ensure the self-consistency of the mechanical model used to analyze AFM data, the model was modified to take into account the presence of the surface roughness. We found excellent agreement between the average values of effective Young's modulus calculated within AFM and the nanoindenter benchmark method. At the same time, the softest and hardest areas of the sample were seen only with AFM. 

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4. Post-synthesis modification of slide-ring gels for thermal and mechanical reconfiguration

   https://doi.org/10.1039/D0SM02260H  

   Dikshit, Karan ; Bruns, Carson J. ( May 2021 , Soft Matter)

   Ring-sliding behavior in polyrotaxanes imbues gels, elastomers, and glasses with remarkable stress-dissipation and actuation properties. Since these properties can be modulated and tuned by structural parameters, many efforts have been devoted to developing synthetic protocols that define the structures and properties of slide-ring materials. We introduce post-synthetic modifications of slide-ring gels derived from unmodified α-cyclodextrin and poly(ethylene glycol) polyrotaxanes that enable (i) actuation and control of the thermo-responsive lower critical solution temperature (LCST) behavior of ring-modified slide-ring hydrogels, and (ii) chemically bonding separate gels into hybrid or shape-reconfigured macro-structures with a slide-ring adhesive solution. The mechanical properties of the post-modified gels have been characterized by shear rheology and uniaxial tensile tests, while the corresponding xerogels were characterized by wide-angle X-ray scattering. These demonstrations show that post-synthetic modification offers a practical solution for re-configuring the properties and shapes of slide-ring gels. 

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5. Settling of barite particles in oil-based drilling fluids

   Kalaga, D. V. ( May 2019 , 10th International Conference on Multiphase Flow, ICMF 2019)

   Controlling the downhole pressure is an important parameter for successful and safe operation of the drilling operation. The drilling fluid density is an important design parameter for preventing the fluid formation and gas entering the wellbore. Several types of weighting agents, barite in the present work, are added to maintain the desired density of the drilling fluid. The uneven density distribution of the barite, which can lead to a density variation as high as 0.5 kg/L (4 lbs/gal) (Tehrani et al. 2011), is caused by the settlement of barite or other weighting materials in the well bore. This paper presents the rheological properties of the drilling fluid measured using a rheometer and estimated rates of barite particle settlement in an oil-based drilling fluid using gamma-ray densitometry for the first time. Experiments were performed in a static cell (with no shear) and in a Taylor Couette cell (with low shear stress). Further, an attempt has also been made to relate the rate of barite particle settling to the rheological properties of the drilling fluid. 

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