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1.
This paper offers important insights on the development of the microstructure in asphalt binders as a function of the treatment temperature. Different treatment temperatures are useful to understand how dispersed domains form when different driving energies for the mobility of molecular species are provided. Small and flat dispersed domains, with average diameter between 0.02 and 0.70 μm, were detected on the surface of two binders at room temperature, and these domains were observed to grow with an increase in treatment temperature (up to over 2 μm). Bee‐like structures started to appear after treatment at or above 100°C. Moreover, the effect of the binder thickness on its microstructure at room temperature and at higher treatment temperatures was investigated and is discussed in this paper. At room temperature, the average size of the dispersed domains increased as the binder thickness decreased. A hypothesis that conciliates current theories on the origin and development of dispersed domains is proposed. Small dispersed domains (average diameter around 0.02 μm) are present in the bulk of the binder, whereas larger domains and bee‐like structures develop on the surface, following heat treatment or mechanical disturbance that reduces the film thickness. Molecular mobility and association are the key factors in the development of binder microstructure. 相似文献
2.
The observation of asphalt binder with the environmental scanning electron microscope (ESEM) has shown the potential to observe asphalt binder microstructure and its evolution with binder aging. A procedure for the induction and identification of the microstructure in asphalt binder was established in this study and included sample preparation and observation parameters. A suitable heat‐sampling asphalt binder sample preparation method was determined for the test and several stainless steel and Teflon sample moulds developed, finding that stainless steel was the preferable material. The magnification and ESEM settings conducive to observing the 3D microstructure were determined through a number of observations to be 1000×, although other magnifications could be considered. Both straight run binder (PG 58‐28) and an air blown oxidised binder were analysed; their structures being compared for their relative size, abundance and other characteristics, showing a clear evolution in the fibril microstructure. The microstructure took longer to appear for the oxidised binder. It was confirmed that the fibril microstructure corresponded to actual characteristics in the asphalt binder. Additionally, a ‘bee’ micelle structure was found as a transitional structure in ESEM observation. The test methods in this study will be used for more comprehensive analysis of asphalt binder microstructure. 相似文献
3.
This paper presents findings on the evolution of the surface microstructure of two asphalt binders, one unmodified and one polymer modified, directly exposed to aging agents with increasing durations. The aging is performed using an accelerated weathering tester, where ultraviolet radiation, oxygen and an increased temperature are applied to the asphalt binder surface. Ultraviolet and dark cycles, which simulated the succession of day and night, alternated during the aging process, and also the temperature varied, which corresponded to typical summer day and night temperatures registered in the state of Qatar. Direct aging of an exposed binder surface is more effective in showing microstructural modifications than previously applied protocols, which involved the heat treatment of binders previously aged with standardized methods. With the new protocol, any molecular rearrangements in the binder surface after aging induced by the heat treatment is prevented. Optical photos show the rippling and degradation of the binder surface due to aging. Microstructure images obtained by means of atomic force microscopy show gradual alteration of the surface due to aging. The original relatively flat microstructure was substituted with a profoundly different microstructure, which significantly protrudes from the surface, and is characterized by various shapes, such as rods, round structures and finally ‘flower’ or ‘leaf’ structures. 相似文献
4.
In an effort to better understand the structure and behaviour of bitumen in low temperature, we describe the first use of cryogenic atomic force microscopy and phase detection microscopy to characterize bitumen nano‐ and micro‐structures. The results were interpreted in light of glass transition temperatures (Tgs) for bitumen fractions. The domains visible by microscopy, the catana, peri and para phases, were attributed to domains rich in asphaltenes, naphthene and polar aromatics, and saturates, respectively. Between ?10°C and ?30°C, atomic force microscopy images revealed topographic features not visible in atomic force microscopy images acquired at room temperature. According to phase detection microscopy and Tgs, the features were assigned to viscous unfrozen saturates. Upon cooling to ?72°C, unfrozen domains of 20–400 nm were observed. These domains were found in the paraphase rich in saturates and in the periphase rich in naphthene aromatics and polar aromatics. The findings indicate that new viscous domains form upon cooling to low temperatures owing to phase segregation, and that some bitumens are never entirely rigid in low temperatures. 相似文献
5.
We introduce noncontact optical microscopy and optical scattering to characterize asphalt binder microstructure at temperatures ranging from 15°C to 85°C for two compositionally different asphalt binders. We benchmark optical measurements against rheometric measurements of the magnitude of the temperature‐dependent bulk complex shear modulus . The main findings are: (1) Elongated (~5 × 1 μm), striped microstructures (known from AFM studies as ‘bees’ because they resemble bumble‐bees) are resolved optically, found to reside primarily at the surface and do not reappear immediately after a single heating–cooling cycle. (2) Smaller (~1 μm2) microstructures with no observable internal structure (hereafter dubbed ‘ants’), are found to reside primarily in the bulk, to persist after multiple thermal cycles and to scatter light strongly. Optical scattering from ‘ants’ decreases to zero with heating from 15°C to 65°C, but recovers completely upon cooling back to 15°C, albeit with distinct hysteresis. (3) Rheometric measurements of reveal hysteresis that closely resembles that observed by optical scatter, suggesting that thermally driven changes in microstructure volume fraction cause corresponding changes in . 相似文献
6.
SERGEI MAGONOV JOHN ALEXANDER MARKO SURTCHEV ALBERT M. HUNG ELHAM H. FINI 《Journal of microscopy》2017,265(2):196-206
In recent years, many researchers have investigated bitumen surface morphology, especially the so‐called bee‐like structures, in an attempt to relate the chemical composition and molecular conformation to bitumen micromechanics and ultimately performance properties. Even though recent studies related surface morphology and its evolution to stiffness and stress localization, the complex chemical nature of bitumen and its time‐ and temperature‐dependent properties still engender significant questions about the nature and origin of the observed morphological features and how they evolve due to exposure to various environmental and loading conditions. One such question is whether the observed surface features are formed from wax or from the coprecipitation of wax and asphaltene. Our prior work was mainly theoretical; it used density functional theory and showed that the coprecipitation theory may not stand, mainly because wax–asphaltene interactions are not thermodynamically favourable compared to wax–wax interactions. This paper presents a comprehensive approach based on experiments to study surface morphology of bitumen and conduct compositional mapping to shed light on the origin of the bee‐like surface morphological features. We used Atomic Force Microscopy (AFM), with the main focus being on single‐pass detection and mapping of local electric properties, as a novel approach to enhance existing compositional mapping techniques. This method was found to be highly effective in differentiating various domains with respect to their polarity. The results of our study favour the hypothesis that the bee‐like features are mainly composed of wax, including a variety of alkanes. 相似文献
7.
New direct observations of asphalts and asphalt binders by scanning electron microscopy and atomic force microscopy 总被引:2,自引:0,他引:2
Observations made using AFM and SEM have been combined in order to study the structure of asphalts. Fluorescence microscopy was used to aid in understanding the structural changes occurring when polymer is added to the asphalts. With the atomic force microscope we are able to study the structure of the asphalts without any pre-preparation. Despite very low resolution, our study reveal ed a network of asphaltene molecules with regard to asphalt gel. The same result is obtained by SEM observation but with a much better resolution. SEM observation, however, needs an adequate preparation method. In the presence of polymer we observed a rearrangement of the initial asphaltene association which leads to the assumption that polymer can aggregate the asphaltene phase. 相似文献
8.
9.
Atomic Force Microscopy was employed in order to relate the features observed on the surface of a 50/70 asphalt binder according to its local stiffness and elastic recovery. Indentations were performed in different points of the surface and a significant variation of elasticity was observed between the points on the so-called bee structure and the matrix. Also, indentations varying the maximum force were performed on similar white spots in the bee structure and the recovery was followed up to 1 h after indentation. It was observed that the elastic recovery is very much dependent on the colloidal structure of the bee. The final surface state of the binder, close to the bee for usual bees is not the same as the initial one indicating severe plastic deformation. Also, permanent phase change could be observed for bright spots presented in not well-structured bee arrangements. A surface hardening was observed in the bee region. 相似文献
10.
ERICO R. DOURADO BIANCA S. PIZZORNO LAURA M. G. MOTTA RENATA A. SIMAO LENI F.M. LEITE 《Journal of microscopy》2014,254(3):122-128
Samples of unmodified and modified asphalt binders containing 1% polyphosphoric acid were studied. Fourier‐transform infrared spectroscopy was used to evaluate the structural indices of the functional groups present in the samples and the results indicated there was a strong interaction between the polyphosphoric acid and oxygenated species. Contact angle measurements indicated that adhesion of the binder to the aggregate depended on the polyphosphoric acid content. Atomic force microscopy was used to relate features observed on the surface of the asphalt binder 50/70, with their local mechanical properties such as stiffness and elasticity. It was observed that the surface of the sample containing 1% polyphosphoric acid provides stiffness values lower than the unmodified asphalt binder. 相似文献
11.
The resonant frequencies and flexural sensitivities of an atomic force microscope (AFM) with assembled cantilever probe (ACP) are studied. This ACP comprises a horizontal cantilever, a vertical extension and two tips located at the free ends of the cantilever and the extension, which makes the AFM capable of simultaneous topography at top surface and sidewalls of microstructures especially microgears, which consequently leads to a time-saving swift scanning process. In this work, the effects of the sample surface contact stiffness and the geometrical parameters such as the ratio of the vertical extension length to the horizontal cantilever length and the distance of the vertical extension from clamped end of the horizontal cantilever on both flexural and torsional resonant frequencies and sensitivities are assessed. These geometrical effects are illustrated in some figures. The results show that the low-order vibration modes are more sensitive for low values of the contact stiffness, but the situation is reversed for high values. 相似文献
12.
The mechanical properties of bitumen, such as elasticity/Young's modulus, stickiness/adhesion, hardness and energy loss, and sample deformation were acquired quantitatively and simultaneously with the topology at the microscale, discriminating clearly two separate phases within the bitumen. Temperature‐dependent measurements revealed detailed and specific data about the changes of these properties with temperature, enabling the development of predictive models for the performance and durability of asphalt. 相似文献
13.
We report a local crystal structure analysis with a high precision of several picometers on the basis of scanning transmission electron microscopy (STEM). Advanced annular dark-field (ADF) imaging has been demonstrated using software-based experimental and data-processing techniques, such as the improvement of signal-to-noise ratio, the reduction of image distortion, the quantification of experimental parameters (e.g., thickness and defocus) and the resolution enhancement by maximum-entropy deconvolution. The accuracy in the atom position measurement depends on the validity of the incoherent imaging approximation, in which an ADF image is described as the convolution between the incident probe profile and scattering objects. Although the qualitative interpretation of ADF image contrast is possible for a wide range of specimen thicknesses, the direct observation of a crystal structure with deep-sub-angstrom accuracy requires a thin specimen (e.g., 10 nm), as well as observation of the structure image by conventional high-resolution transmission electron microscopy. 相似文献
14.
This paper uses self-assembled monolayers (SAMs) on an Au(111) substrate to detect the unique characteristics of viologen molecules using scanning tunneling microscopy (STM), and reports the orientation and surface changes of molecules at the nanolevel in real-time. In particular, the rectification characteristics of the viologen molecule were observed at the molecular level using scanning tunneling spectroscopy (STS). After verifying the rectification characteristics of viologen molecules, an experiment was carried out to demonstrate the possibility of applying viologen to photodiodes and switching devices by forming a thin film of chlorophyll a on the viologen SAMs using the Langmuir–Blodgett (LB) method. This material mimics the photoinduced electron transport phenomenon in the early stage of photosynthesis in living plants. This study demonstrates the applicability of viologen to bioelectronic photodiodes and switching devices based on photo effects by observing the topography, current sensing, and current–voltage (I–V) characteristics using current-sensing atomic force microscopy (CS-AFM) by introducing light to the AFM-tip/chlorophyll a/viologen/Au(1 1 1) substrate structure. 相似文献
15.
Effect of aging on the morphology of bitumen was investigated. Two bitumens were aged according to the thin film oven test (TFOT), pressure aging vessel (PAV) test and ultraviolet (UV) radiation, respectively. The morphology of the binders before and after aging was characterized by atomic force microscopy. The physical properties and chemical compositions of the binders were also measured. The results showed that aging affected the bitumen morphology significantly. Aging increased the overall surface stiffness of the bitumen and made the bitumen surface more solid-like. The extent of these changes was dependent on aging conditions. TFOT decreased the contrast between the dispersed domains and the matrix, which contributed to the single-phase trend of the binders. The effect of PAV aging on morphology of the binders was dependent on the base bitumen. In one case, it further accelerated the single-phase trend of bitumen in comparison with that after TFOT. In the other case, it caused the phase separation of bitumen. In both cases, PAV aging increased the surface roughness of the binders obviously. As a result of UV aging, the contrast between the matrix phase and dispersed phase was increased due to the difference in sensitivity to UV radiation of the bitumen molecules, which caused or further promoted the phase separation in the binders. Regardless of the aging procedure carried out, a strong correlation was observed between the changes in morphology and physical properties as well as chemical compositions of the binders before and after aging. 相似文献
16.
The structure of the asphaltene phase in the bitumen is believed to have a significant effect on its rheological properties. It has traditionally been difficult to observe the asphaltene phase in unaltered samples of bitumen. The maltenes are thought to form a continuous phase in which the asphaltenes are ‘dispersed’. In this study, confocal laser‐scanning microscopy (CLSM) operating in fluorescence mode was used to examine the structure of paving‐grade Safaniya and San Joaquin bitumen. The asphaltene fraction fluoresces in the 515–545 nm wavelength range when irradiated with light with a wavelength of 488 nm. The major advantages of CLSM are that the bitumen sample requires little pretreatment or preparation that may affect the original dispersion of asphaltenes and the bitumen is observed at ambient temperature and pressure. This reduces the possibility of producing images that are not representative of the original material. CLSM was able to show the distribution of maltene and asphaltene components in bitumen. The asphaltene aggregates in the bitumen were observed to be 2–7 µm in size and formed a dispersed ‘sol’ structure in the continuous maltene matrix rather than a network ‘gel’ structure. Surprisingly, the structure and fluorescence of the asphaltene phase does not appear to alter radically upon oxidative ageing. The structure of the asphaltene phase of an AR4000 San Joaquin bitumen was found to be more homogeneous than that of Safaniya bitumen, illustrating the range of structures that can be observed in bitumens by this method. 相似文献
17.
M. POČUČA Z. BRANKOVIĆ G. BRANKOVIĆ D. VASILJEVIĆ‐RADOVIĆ 《Journal of microscopy》2008,232(3):585-588
LaNiO3 thin films were successfully prepared by a chemical method from citrate precursors. The LNO precursor solution was spin‐coated onto Si (100) and Si (111) substrates. To obtain epitaxial or highly oriented films, the deposited layers were slowly heated in a gradient thermal field, with a heating rate of 1° min?1, and annealed at 700°C. The influence of different substrate orientations on the thin film morphology was investigated using atomic force microscopy and X‐ray diffraction analysis. Well‐crystallized films with grains aligned along a certain direction were obtained on both substrates. Films deposited on both substrates were very smooth, but with a different grain size and shape depending on the crystal orientation. Films deposited on Si (100) grew in the (110) direction and had elongated grains, whereas those on Si (111) grew in the (211) direction and had a quasi‐square grain shape. 相似文献
18.
Interfacial microstructure and phase composition of PtTiGePd ohmic contacts to heavily C-doped AlGaAs were investigated as a function of annealing temperatures. Results of the material analyses were used to explain the specific contact resistances measured for each thermal treatment. Evidence of interdiffusion and compound formation between AlGaAs and Pd was visible in a Ga-rich Pd-Ga-As reaction zone prior to heat treatment. As the annealing temperature was raised from 530 to 600°C, As began to out-diffuse. At 600°C, this As out-diffusion, which is critical to the formation of good p-type ohmic contacts, contributed to the creation and development of the laterally continous two-phase interfacial region, TiAs/Pd12Ga2Ge5, overlying the AlGaAs substrate. The minimum specific contact resistance was also achieved at this temperature. As the annealing temperature was elevated to 650°C, the specific contact resistance degraded in response to intensive chemical diffusion and development of a broad, nonuniform multiphased interfacial region. 相似文献
19.
Dark-field imaging modes have attracted less interest in biological confocal microscopy than the extensive applications of immunofluorescence imaging. There are, however, certain biological and materials science applications where it is necessary to use a confocal imaging mode that is capable of partial or full rejection of light specularly reflected from coverslips, microscope slides or specimen surfaces. In this paper we present a simple modification of a commercial confocal microscope to incorporate dark-field imaging. We discuss theoretical aspects of the resulting dark-field imaging mode and also give experimental examples. 相似文献
20.
Effect of montmorillonite organic modification on microstructures and ultraviolet aging properties of bitumen 总被引:2,自引:0,他引:2
The effect of montmorillonite (MMT) organic modification on microstructures and ultraviolet (UV) aging properties of bitumen was investigated. The microstructures of MMT modified bitumen were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and atomic force microscopy (AFM), respectively. The binders were aged by UV radiation. The UV aging properties of MMT modified bitumen was studied by determining physical properties and AFM analysis. XRD and FTIR analyses show that the sodium montmorillonite (Na(+) -MMT) modified bitumen forms a phase-separated structure, whereas the organo-montmorillonite (OMMT) modified bitumen forms an intercalated structure. After Na(+) -MMT modification, the contrast between the matrix and the dispersed domains is inverted according to AFM analysis. However, this contrast inversion is prevented with the introduction of OMMT due to the good compatibility between the OMMT and the bitumen. As a result of UV aging, both viscosity aging index and softening point increment of OMMT modified bitumen are lower than that of the unmodified bitumen and Na(+) -MMT modified bitumen. Furthermore, the association interactions and single-phase trend in OMMT modified bitumen are further prevented in comparison with Na(+) -MMT modified bitumen during UV aging, indicating the good aging resistance of OMMT modified bitumen after organic modification of MMT. 相似文献