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To obtain the relation between spark discharges and the topography of electrode surfaces, some models, such as a micro-initial model of cone and spherical head cylinder, generated from the scanning of a scanning electron microscope are introduced. Based on the principles of energy conservation and thermal equilibrium, the second-order non-homogeneous differential equation is established. The relationships between the temperature of the cathode surface and the distance from the top of micro-protrusions, the cone angle, and the radius of the ball head are derived from a set of second-order non-homogeneous differential equations. When introduced electron emission theory, the main emission type at the initial stage of the discharge is electron field emission. As the discharge progresses, the Joule heat generated by the emission current will cause thermionic emission. During this progress, the emission current density gradually increases. When the temperature of the cathode surface reaches the melting point of the cathode metal, the current density will increase sharply. Observed from the discharge, the temperature of the cathode surface is inversely proportional to the cone angle and the radius of the ball head maintains a gradually decreasing slope. It is proportional to micro-protrusions maintaining a gradually increasing slope. When the cone angle is less than 12° and the radius of the ball head is less than 0.04 µm, the temperature of the cathode surface changes more dramatically. Through this study, a further understanding of factors that affect the density of cathode current emission can be obtained, which is of great significance to improve the capacity of cathode emission. [ABSTRACT FROM AUTHOR]

In this paper, the effect of D0 temperature, Kappa factor and the final pH value on bleaching sulfate bleached pine wood pulp was studied. The results showed that the bleaching efficiency was better when the pH value was 4, and the amount of absorbable organic halogen (AOX) in the bleaching wastewater was decreased. The Kappa factor is linear with the whiteness in the range of 0–0.15. With the increase of the Kappa factor, the amount of AOX in bleaching wastewater of D0 and Ep gradually increases. High temperature bleaching can reduce AOX production, but some fibers are hydrolyzed, leading to a decrease in pulp viscosity. The effects of chlorine dioxide solution adding sodium dihydrogen phosphate (NaH2PO4) and dimethylsulfoxide (DMSO) on pulp bleaching were investigated. The results showed that both solutions could reduce the amount of AOX in bleaching wastewater. Among them, the addition of NaH2PO4 in chlorine dioxide increased pulp whiteness, while the addition of DMSO was the opposite. Scanning electron microscope showed that a small amount of hollow cracks and more voids appeared on the surface of pulp fibers after the addition of NaH2PO4. Pulp fibers bleached by the chlorine dioxide adding DMSO have more folds and less voids on the surface. The surface wrinkles of pulp fibers increased with the addition of DMSO and the voids were less. FT-IR showed that the number of chromophore groups in the pulp bleached by chlorine dioxide adding NaH2PO4 were decreased. However, the lignin characteristic absorption peak in the pulp bleached by chlorine dioxide adding DMSO increased at the intensity of 1062 and 1160 cm−1, which indicated that there were more residual chromophore groups. [ABSTRACT FROM AUTHOR]

Exploring novel materials with large magnetocaloric effect and excellent mechanical properties near room temperature (RT) are highly desired for Ni-Mn based Heusler alloys. In this work, the martensitic transformation, magnetic properties, and mechanical properties of Ni50-xCoxMn50-yTiy (x = 13–15, y = 13–16) alloys were systematically investigated by tuning Co or Ti contents. The magnetism of austenite was enhanced with an increase in Co or Ti content. 5M and 6M martensites were observed in Ni-Co-Mn-Ti alloys by transmission electron microscopy. The Ni36Co14Mn35Ti15 alloy with a large magnetocaloric effect was found near room temperature by tuning composition. The largest magnetization change (ΔM) and magnetic entropy change (ΔSm) in the Ni36Co14Mn35Ti15 non-textured polycrystalline alloy obtained during martensitic transformation under the magnetic field of 5 T were about 106 emu/g and 19.3 J kg−1 K−1, respectively. Furthermore, the maximum compressive strength and ductility for the Ni36Co14Mn35Ti15 as-cast alloy can exceed 1220 MPa and 15%, respectively. The fracture mechanism and bonding interaction were analyzed by a scanning electron microscope and first-principles calculations. [ABSTRACT FROM AUTHOR]

Graphite cathodes are widely used due to their good emission properties, especially their long lifetime. Some previous papers have researched their lifetime under certain conditions and uncovered some important phenomena. This paper is dedicated to research the lifetime of the graphite cathode under higher power. In the lifetime test, the voltage and current amplitudes are about 970 kV and 9.7 kA, respectively. The repetition rate is 20 Hz. An X-band relativistic backward wave oscillator is used to generate high power microwave by utilizing the electron beam energy. The experimental results demonstrate that the emission property of the graphite cathode remains quite stable during 105 pulses, despite some slight deteriorations regarding the beam and microwave parameters. The macroscopic morphology change of the cathode blade due to material evaporation is observed by a laser microscope. The mass loss of the graphite cathode is about 60 μg/C. Meanwhile, the observation by a scanning electron microscope uncovers that the original numerous flaky micro-structures are totally replaced by a relatively smooth surface at the mid region of the cathode blade and a large number of new micro-protrusions at the blade edges during the lifetime test. [ABSTRACT FROM AUTHOR]

Ionically conducting lanthanum fluoride (LaF3), displaying a nanoscopic lamellar structure, has been synthesized at the surface of an aqueous solution of LaCl3 and HF. The structure and the chemical composition of the conductor have been analyzed by SEM, electron probe microanalysis, X-ray powder diffraction, FTIR, and 19F magic angle spinning nuclear magnetic resonance (NMR) spectroscopy. The fluorine dynamics have been studied by NMR diffusometry and relaxometry in a temperature range from room temperature up to 875 K. The fluorine self-diffusion coefficient of the nanostructured LaF3 is about two orders of magnitude larger than that of bulk LaF3. This novel material is highly promising for many typical applications of fluorine ionic systems. [ABSTRACT FROM AUTHOR]

In this paper, we investigate the degradation mode and mechanism of AlGaN/GaN based high electron mobility transistors (HEMTs) during high temperature operation (HTO) stress. It demonstrates that there was abrupt degradation mode of drain current during HTO stress. The abrupt degradation is ascribed to the formation of crack under the gate which was the result of the brittle fracture of epilayer based on failure analysis. The origin of the mechanical damage under the gate is further investigated and discussed based on top-down scanning electron microscope, cross section transmission electron microscope and energy dispersive x-ray spectroscopy analysis, and stress simulation. Based on the coupled analysis of the failure physical feature and stress simulation considering the coefficient of thermal expansion (CTE) mismatch in different materials in gate metals/semiconductor system, the mechanical damage under the gate is related to mechanical stress induced by CTE mismatch in Au/Ti/Mo/GaN system and stress concentration caused by the localized structural damage at the drain side of the gate edge. These results indicate that mechanical stress induced by CTE mismatch of materials inside the device plays great important role on the reliability of AlGaN/GaN HEMTs during HTO stress. [ABSTRACT FROM AUTHOR]

GaN, with its wide bandgap of 3.4 eV, has emerged as an efficient material for designing high-efficiency betavoltaic batteries. An important part of designing efficient betavoltaic batteries involves a good understanding of the full process, from the behavior of the nuclear material and the creation of electron-hole pairs all the way through the collection of photo-generated carriers. This paper presents a detailed model based on Monte Carlo and Silvaco for a GaN-based betavoltaic battery device, modeled after Ni-63 as an energy source. The accuracy of the model is verified by comparing it with experimental values obtained for a GaN-based p-i-n structure under scanning electron microscope illumination. [ABSTRACT FROM AUTHOR]

The effect of filler aspect ratio on the electromagnetic properties of epoxy-amine resin reinforced with carbon nanofibers is here investigated. A heat treatment at 2500?°C of carbon nanofibers seems to increase their aspect ratio with respect to as-received ones most likely due to a lowering of structural defects and the improvement of the graphene layers within the dixie cup conformation. These morphological differences revealed by Raman's spectroscopy and scanning electron microscopy analyses may be responsible for the different electrical properties of the resulting composites. The DC characterization of the nanofilled material highlights an higher electrical conductivity and a lower electrical percolation threshold for the heat-treated carbon nanofibers based composites. In fact, the electrical conductivity is about 0.107?S/m and 1.36?×?10-3?S/m for the nanocomposites reinforced with heat-treated and as received fibers, respectively, at 1?wt.?% of nanofiller loading, while the electrical percolation threshold falls in the range [0.05-0.32]wt.?% for the first nanocomposites and above 0.64?wt.?% for the latter. Moreover, also a different frequency response is observed since the critical frequency, which is indicative of the transition from a resistive to a capacitive-type behaviour, shifts forward of about one decade at the same filler loading. The experimental results are supported by theoretical and simulation studies focused on the role of the filler aspect ratio on the electrical properties of the nanocomposites. [ABSTRACT FROM AUTHOR]

The structural, optical, and photocatalytic properties of TiO2 and Ag–TiO2 thin films grown by a hydrothermal method were studied by using an x-ray diffractometer, scanning electron microscope, energy-dispersive x ray, and UV–vis spectroscopy. The results indicated that all films were of single-phase and the Ag presence enhanced catalytic and water-splitting performances in the visible light region. In particular, the methylene blue solution was disintegrated up to 99% after 12 and 8 h for TiO2 and Ag–TiO2 films, respectively. Meanwhile, the splitting efficiency increased from 0.3% for TiO2 to 1% for Ag–TiO2. These performances demonstrate the great potential of Ag–TiO2 films in photocatalytic and water-splitting applications. [ABSTRACT FROM AUTHOR]

A large volume 3D dust cloud containing in situ grown nanometer-sized particles is produced in a newly developed versatile table-top experimental device. Carbonaceous nanoparticles having almost uniform size throughout the dust cloud are grown using capacitively coupled rf discharge in Ar–C2H2 gas mixture with a low precursor gas flow rate (∼2 sccm) and minimal rf power (∼1 W). The vertical and radial extensions of the dust cloud are 40 cm and 5 cm, respectively. The pure Ar plasma in the setup is characterized by measuring the discharge parameters as well as plasma parameters under different discharge conditions. The average particle size and its temporal growth profile are determined by analyzing the scanning electron microscope images of the particles. The dust density measured using the laser extinction method is found to be of the order of 1016–1012 m − 3 for the discharge duration of 2–10 min. A spontaneous dust density wave is also observed in the dust cloud. [ABSTRACT FROM AUTHOR]

Short-arc lamps are equipped with tungsten electrodes due to their ability to withstand a high thermal load during operation. Nominal currents of more than one hundred amperes lead to a cathode tip temperature near the melting point of tungsten. To reduce the electrode temperature and, thereby, to increase the maintenance of such lamps, ThO2 or tentatively La2O3 are added to the electrode material. They generate a reduced work function by establishing a monolayer of emitter atoms on the tungsten surface. Emitter enrichments on the lateral surface of doped cathodes are formed. They are traced back to transport mechanisms of emitter oxides in the interior of the electrode and on the electrode surface in dependence of the electrode temperature and to the redeposition of vaporized and ionized emitter atoms onto the cathode tip by the electric field in front. The investigation is undertaken by means of glow discharge mass spectrometry, scanning electron microscope images, energy dispersive x-ray spectroscopy, and through measurements of the optical surface emissivity. The effect of emitter enrichments on the stability of the arc attachment is presented by means of temporally resolved electrode temperature measurements and by measurements of the luminous flux from the cathode-near plasma. They show that the emitter enrichments on the lateral surface of the cathode are attractive for the arc attachment if the emitter at the cathode tip is depleted. In this case, it moves along the lateral surface from the cathode tip to sections of the cathode with a reduced work function. It induces a temporary variation of the cathode tip temperature and of the light intensity from the cathodenear plasma, a so-called flickering. In particular, in case of lanthanated cathodes, strong flickering is observed. [ABSTRACT FROM AUTHOR]

Sn whiskers are observed by scanning electron microscope on the Cu surface in Cu(top)-Sn(bottom) bilayer system upon room temperature aging. Only Cu6Sn5 phase appears in the X-ray diffraction patterns and no Sn element is detected in the Cu sublayer by scanning transmission electron microscopy. Based on the interfacial thermodynamics, the intermetallic Cu6Sn5 compound phase may form directly at the Sn grain boundary. Driven by the stress gradient during the formation of Cu6Sn5 compound at Sn grain boundaries, Sn atoms segregate onto the Cu surface and accumulate to form Sn whisker. [ABSTRACT FROM AUTHOR]

We experimentally demonstrate a multi-wavelength ultrafast erbium-doped fiber laser incorporating a lm-scale topological insulator: Bi2Se3/Polyvinyl Alcohol film as both an excellent saturable absorber for mode-locking and a high-nonlinear medium to induce a giant third order optical nonlinear effect for mitigating the mode competition of erbium-doped fiber laser and stabilizing the multi-wavelength oscillation. By properly adjusting the pump power and the polarization state, the single-, dual-, triple-, four-wavelength mode-locking pulse could be stably initiated. For the four-wavelength operation, we obtain its pulse width of ~22 ps and a fundamental repetition rate of 8.83 MHz. The fiber laser exhibits the maximum output power of 9.7 mW with the pulse energy of 1.1 nJ and peak power of 50W at the pump power of 155 mW. Our study shows that the simple, stable, low-cost multi-wavelength ultrafast fiber laser could be applied in various potential fields, such as optical communication, biomedical research, and radar system. [ABSTRACT FROM AUTHOR]

We have systematically studied the temperature dependence of incorporation characteristics of nitrogen (N) and indium (In) in growing GaInNAs films. With the implementation of Monte-Carlo simulation, the low N adsorption energy (0.10 eV) is demonstrated. To understand the atomic incorporation mechanism, temperature dependence of interactions between Group-III and V elements are subsequently discussed. We find that the In incorporation behaviors rather than that of N are more sensitive to the Tg, which can be experimentally verified by exploring the compositional modulation and structural changes of the GaInNAs films by means of high-resolution X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscope, and secondary ion mass spectroscopy. [ABSTRACT FROM AUTHOR]

In this study, we create a multifunctional metal surface by producing a hierarchical nano/microstructure with femtosecond laser pulses. The multifunctional surface exhibits combined effects of dramatically enhanced broadband absorption, superhydrophobicity, and self-cleaning. The superhydrophobic effect is demonstrated by a falling water droplet repelled away from a structured surface with 30% of the droplet kinetic energy conserved, while the self-cleaning effect is shown by each water droplet taking away a significant amount of dust particles on the altered surface. The multifunctional surface is useful for light collection and water/dust repelling. [ABSTRACT FROM AUTHOR]

We performed ultra-high-speed tests for purely opening spot welds using plane tensile pulses. A gun system generated a parallel impact of a projectile plate onto a welded plate. Induced by the interactions of the release waves, the welded plate opened purely under the plane tensile pulses. We used the laser velocity interferometer system for any reflector to measure the velocity histories of the free surfaces of the free part and the spot weld of the welded plate. We then used a scanning electron microscope to investigate the recovered welded plates. We found that the interfacial failure mode was mainly a brittle fracture and the cracks propagated through the spot nugget, while the partial interfacial failure mode was a mixed fracture comprised ductile fracture and brittle fracture. We used the measured velocity histories to evaluate the tension stresses in the free part and the spot weld of the welded plate by applying the characteristic theory. We also discussed the different constitutive behaviors of the metals under plane shock loading and under uniaxial split Hopkinson pressure bar tests. We then compared the numerically simulated velocity histories of the free surfaces of the free part and the spot weld of the welded plate with the measured results. The numerical simulations made use of the fracture stress criteria, and then the computed fracture modes of the tests were compared with the recovered results. [ABSTRACT FROM AUTHOR]

Suspended membranes of two-dimensional (2D) materials are of interest for many applications. Much of their characterization relies on scanning probe microscopy (SPM) techniques such as atomic force microscopy (AFM) or scanning tunneling microscopy (STM). Unlike rigid samples, the suspended atomically thin 2D membranes are, however, flexible and do not remain mechanically undisturbed during SPM measurements. Local deformations can occur at the location of the scanning tip and thus result in measurements that misrepresent actual membrane topography and nanomechanical properties. Exact levels of such SPM tip-induced deformations in 2D membranes remain largely unknown, as they are to date only indirectly accessible via dual probe microscope concepts that either are not mechanically independent (e.g., SPM-SPM setups resulting in complicated imaging crosstalk) or suffer from intrinsically limited lateral resolution (e.g., optical far-field techniques as the second probe). Circumventing these shortcomings, we here demonstrate that by coupling an AFM with a scanning electron microscope (SEM) as the second, mechanically independent probe, we can directly and in situ visualize by SEM at high resolution 2D membrane deformations that result from controllable AFM tip manipulations in the nN range. Employing few-layer graphene as model membranes, we discuss the experimental realization of our coupled in situ AFM-SEM approach. [ABSTRACT FROM AUTHOR]

This paper develops a robust edge-based template matching algorithm for displacement measurement of compliant mechanisms under a scanning electron microscope (SEM). The algorithm consists of three steps. First, the Sobel gradient operator and a self-adaptive segment strategy are used to establish the shape model in which the gradient directions of the object's edge points are calculated. Second, a similarity criterion based on image gradients that is robust to illumination change and image noise is utilized for template matching to obtain the coarse results. The third step is to refine the matching results by using an orientation-guided subpixel interpolation strategy. A series of simulations is conducted, and the results show that the proposed algorithm enjoys great robustness against strong image noise and gray-value fluctuation, as well as small rotations and background interferences, and thus is suitable for processing SEM images of compliant mechanisms. Finally, the application of the proposed algorithm in the measurement of the spring constant of the flexure hinges with a straight beam form under a SEM is demonstrated. [ABSTRACT FROM AUTHOR]

Digital holography has been proposed to fulfill a need for an imaging diagnostic capable of in situ monitoring of surface erosion caused by plasma–material interaction in nuclear fusion devices. A digital holography diagnostic for 3D surface erosion measurement has been developed at Oak Ridge National Laboratory with the goal of deployment on a plasma device. A proof-of-concept in situ demonstration is planned which would involve measurement of plasma erosion on targets exposed to an electrothermal arc source. This work presents the results of an ex situ characterization of the capability and limitations of holographic imaging of targets exposed to the arc source. Targets were designed to provide a fiducial for comparison of deformed and unaffected areas. The results indicated that the average net erosion was ∼150 nm/plasma exposure, which is expected to be within the diagnostic's measurement capacity. Surface roughness averages determined by holographic image analysis showed good agreement with measurements taken with a profilometer. The limit of the holography diagnostic's x–y spatial resolution was characterized by comparison with scanning electron microscope imaging. [ABSTRACT FROM AUTHOR]

Nanoscale thermometry, an approach based on non-invasive, yet precise measurements of temperature with nanometer spatial resolution, has emerged as a very active field of research over the last few years. In transmission electron microscopy, nanoscale thermometry is particularly important during in situ experiments or to assess the effects of beam induced heating. In this article, we present a nanoscale thermometry approach based on electron energy-loss spectroscopy in a transmission electron microscope to measure locally the temperature of silicon nanoparticles using the energy shift of the plasmon resonance peak with respect to the zero-loss peak as a function of temperature. We demonstrate that using non-negative matrix factorization and curve fitting of stacked spectra, the temperature accuracy can be improved significantly over previously reported manual fitting approaches. We will discuss the necessary acquisition parameters to achieve a precision of 6 meV to determine the plasmon peak position. [ABSTRACT FROM AUTHOR]

Superhydrophobic coatings have been applied in various fields. The materials used in the preparation of superhydrophobic coatings have attracted the attention of scholars. Due to the harm of fluorine-containing substances with low surface energy to the environment, fluorine-free superhydrophobic coatings have become a hotspot in the research field. Herein, a fluorine-free superhydrophobic coating with oil/water separation was made by a solution immersion way. The fluorine-free copolymer and polydimethylsiloxane (PDMS)/SiO2 nanoparticles (NPs) were mixed to prepare a composite solution, and the superhydrophobic surface was obtained on the paper by a dipping method. The scanning electron microscope, x-ray photoelectron spectrometer, 1H nuclear magnetic resonance, and Fourier transform infrared were used to study the surface characteristics and structural composition of the superhydrophobic material. The research proved that the copolymer and PDMS/SiO2 NPs were successfully coated on the paper surface, and the rough structure of the superhydrophobic surface was also attributed to the introduction of the copolymer and PDMS/SiO2 NPs. The evaluation of the coating has proved its excellent hydrophobicity, oil/water separation performance, and self-cleaning performance. The coating is a sustainable and environmentally friendly superhydrophobic material that can be used in packaging, construction, petrochemical, and other industries. [ABSTRACT FROM AUTHOR]

Motivated by the importance of magnetization dynamics in nanomagnets for the development and optimization of magnetic devices and sensors, we measured and modeled spin wave spectra in patterned elliptical nanomagnets. Ferromagnetic resonance spectra for multiple nanomagnets of Ni80Fe20, fabricated by electron-beam lithography to have nominal short-axes of 200 nm or 100 nm, were measured by use of heterodyne magneto-optical microwave microscopy. Scanning electron microscope images taken of the same nanomagnets were used to define element shapes for micromagnetic simulations. The measured spectra show significant differences between nominally identical nanomagnets, which could be only partially attributed to uncontrolled shape variations in the patterning process, as evidenced by the limited agreement between the measured and simulated spectra. Agreement between measurements and simulations was improved by including a zone of reduced magnetization and exchange at the edges of the nanomagnets in the simulations. Our results show that the reduction of shape variations between individual magnetic random-access memory elements can potentially improve their performance. However, unambiguous determination of materials parameters in nanomagnets based on analysis and modeling of spin wave spectra remains problematic. [ABSTRACT FROM AUTHOR]

For nanoparticles with sub-10 nm diameter, the electronic bandgap becomes size dependent due to quantum confinement; this, in turn, affects their electro-optical properties. Thereby, MoS2 and WS2 monolayers acquire luminescent capability, due to the confinement-induced indirect-to-direct bandgap transition. Rolling up of individual layers results in single wall inorganic nanotubes (SWINTs). Up to the present study, their luminescence properties were expected to be auspicious but were limited to theoretical investigations only, due to the scarcity of SWINTs and the difficulties in handling them. By optimizing the conditions in the plasma reactor, relatively high yields of WS2 SWINTs 3–7 nm in diameter were obtained in this work, compared to previous reports. A correlative approach, transmission electron microscopy coupled with a scanning electron microscope, was adapted to overcome handling obstacles and for testing individual nanotubes by low-temperature cathodoluminescence. Clear cathodoluminescence spectra were obtained from WS2-SWINTs and compared with those of WS2 multiwall nanotubes and the corresponding bulk material. Uniquely, the optical properties of INTs acquired from cathodoluminescence were governed by the opposite impact from quantum size effect and strain in the bent triple S-W-S layers. The experimental findings were confirmed by the Density Functional and Time-Dependent Density Functional theoretical modeling of monolayer and bilayer nanotubes of different chiralities and diameters. This study provides experimental evidence of the quantum confinement effect in WS2 SWINTs akin to WS2 monolayer. The ability to tune the electronic structure with morphology or number of layers may be exploited toward photoelectrochemical water splitting with WS2 catalysts, devising field effect transistors, photodetectors, and so on. [ABSTRACT FROM AUTHOR]

Observation at low voltage using scanning electron microscopes (SEMs) enables the characterization of surface details on specimens on a nanometer scale and is widely used in science and industry. However, the energy width of the electron source restricts the spatial resolution of SEMs at low voltage, but it can be narrowed by lowering the work function of the emitter material. Here, we developed a cold field emitter using a cerium hexaboride single crystal (CeB6-CFE) as a monochromatic electron source. The work function of the CeB6 (310) plane was estimated to be as low as 2.25 ± 0.17 eV, and the energy width ranged from 0.17 to 0.26 eV for angular current densities ranging from 0.10 to 80 μA/sr. This energy width was 20% to 30% narrower than that of conventional W(310)-CFEs. Using the CeB6-CFE, the spatial resolution of the SEM at an acceleration voltage of 0.5 kV was improved by 11% compared with that of an SEM using the W(310)-CFE. [ABSTRACT FROM AUTHOR]

Double perovskite La2-xCaxCoMnO6 (x=0, 0.1, 0.2, 0.5) ceramics samples were synthesized by the standard solid-state reaction method. The crystal structures have been confirmed to be monoclinic perovskite structure with space group of P21/n at room temperature by the powder x-ray diffraction (Cu-Ka). The grains of the samples are relatively dense and distribute in random directions from the scanning electron microscope patterns. Holes are doped into La2CoMnO6 with the substitution of the Ca2+ ions in La-site, and further lead to the valences of Mn ions and Co ions transforming from Mn4+ and Co2+ to Mn3+ and Co3+, respectively. Ferromagnetic coupling of Mn4+-O2--Co2+ and antiferromagnetic coupling of Mn3+-O2--Co3+ are coexistent in La2-xCaxCoMnO6 system, which correspond to two transitions existed in field-cooling magnetization versus temperature curves. Curie temperature of La2-xCaxCoMnO6 system decreases with the increasing of Ca-substitution amount. The coexistence of different magnetic phases leads to the exchange bias effect. [ABSTRACT FROM AUTHOR]

In this paper, a paper-based ultracapacitors were fabricated by the rod-rolling method with the ink of carbon nanomaterials, which were synthesized by arc discharge under various magnetic conditions. Composites of carbon nanostructures, including high-purity single-walled carbon nanotubes (SWCNTs) and graphene flakes were synthesized simultaneously in a magnetically enhanced arc. These two nanostructures have promising electrical properties and synergistic effects in the application of ultracapacitors. Scanning electron microscope, transmission electron microscope, and Raman spectroscopy were employed to characterize the properties of carbon nanostructures and their thin films. The sheet resistance of the SWCNT and composite thin films was also evaluated by four-point probe from room temperature to the cryogenic temperature as low as 90 K. In addition, measurements of cyclic voltammetery and galvanostatic charging/discharging showed the ultracapacitor based on composites possessed a superior specific capacitance of up to 100 F/g, which is around three times higher than the ultracapacitor entirely fabricated with SWCNT. [ABSTRACT FROM AUTHOR]

In the present work, CaCu3Ti4O12 (CCTO) nanoceramics with different grain sizes were prepared by spark plasma sintering (SPS) at different temperatures (SPS-800, SPS-900, SPS-975, and SPS-1050) of the mechanosynthesized nano-powder. Structural and microstructural properties were studied by XRD and field-emission scanning electron microscope measurements. The grain size of CCTO nanoceramics increases from 80 nm to ∼200 nm for the ceramics sintered at 800 °C and 975 °C, respectively. Further increase of SPS temperature to 1050 °C leads to micro-sized ceramics of 2-3 lm. The electrical and dielectric properties of the investigated ceramics were studied by impedance spectroscopy. Giant dielectric constant was observed in CCTO nanoceramics. The dielectric constant increases with increasing the grain size of the nanoceramics with values of 8.3×103, 2.4×104, and 3.2×104 for SPS-800, SPS-900, and SPS-975, respectively. For the micro-sized SPS-1050 ceramics, the dielectric constant dropped to 2.14×104. The dielectric behavior is interpreted within the internal barrier layer capacitance picture due to the electrical inhomogeneity of the ceramics. Besides the resistive grain boundaries that are usually observed in CCTO ceramics, domain boundaries appear as a second source of internal layers in the current nanoceramics. [ABSTRACT FROM AUTHOR]

In this paper, we present our results of experimental and numerical pull-out tests on carbon nanotubes (CNTs) embedded in palladium. We prepared simple specimens by employing standard silicon wafers, physical vapor deposition of palladium and deposition of CNTs with a simple drop coating technique. An AFM cantilever with known stiffness connected to a nanomanipulation system was utilized inside a scanning electron microscope (SEM) as a force sensor to determine forces acting on a CNT during the pull-out process. SEM-images of the cantilever attached to a CNT have been evaluated for subsequent displacement steps with greyscale correlation to determine the cantilever deflection. We compare the experimentally obtained pull-out forces with values of numerical investigations by means of molecular dynamics and give interpretations for deviations according to material impurities or defects and their influence on the pull-out data. We find a very good agreement of force data from simulation and experiment, which is 17 nN and in the range of 10-61 nN, respectively. Our findings contribute to the ongoing research of the mechanical characterization of CNT-metal interfaces. This is of significant interest for the design of future mechanical sensors utilizing the intrinsic piezoresistive effect of CNTs or other future devices incorporating CNT-metal interfaces. [ABSTRACT FROM AUTHOR]

We have systematically analyzed the effect of strain on the electrical properties of flexible field effect transistors with a single-walled carbon nanotube (SWCNT) network on a polyethersulfone substrate. The strain was applied and estimated at the microscopic scale (<1 μm) by using scanning electron microscope (SEM) equipped with indigenously designed special bending jig. Interestingly, the strain estimated at the microscopic scale was found to be significantly different from the strain calculated at the macroscopic scale (centimeter-scale), by a factor of up to 4. Further in-depth analysis using SEM indicated that the significant difference in strain, obtained from two different measurement scales (microscale and macroscale), could be attributed to the formation of cracks and tears in the SWCNT network, or at the junction of SWCNT network and electrode during the strain process. Due to this irreversible morphological change, the electrical properties, such as on current level and field effect mobility, lowered by 14.3% and 4.6%, respectively. [ABSTRACT FROM AUTHOR]

SrFe12O19/La1-xCaxMnO3 (SFO/LCMO) composites with x = 0.1 and 0.5 were synthesized via a two stage combined citrate precursor sol-gel and hydrothermal method. The structure and composition of the samples were refined from the X-ray diffraction patterns. The morphologies of the composites were investigated using transmission and scanning electron microscopies, which revealed micron-sized hexagonal platelets of SFO with LCMO particles with average diameters of 110-130 nm formed at the surface. An investigation of the temperature and field dependence of the magnetization found that the SFO phase with a ferrimagnetic characteristic up to 720 K dominates the magnetic properties of the composite samples. The SFO/LCMO composite samples showed a reduction in saturation magnetization and coercivity when compared with pure SFO. However, low temperature hysteresis loops recorded after cooling in applied fields up to 5 T revealed the absence of exchange bias in the SFO/LCMO composite, ruling out the possibility of significant interfacial magnetic coupling between SFO and LCMO. [ABSTRACT FROM AUTHOR]

The indium supplied on c-plane GaN templates using Metal organic vapor phase epitaxy was studied by in situ X-ray reflectivity (XRR) at 800 °C. The presence of liquid indium layers on the GaN (0001) surface was demonstrated using data-fitting of XRR measurements, ex situ atomic force microscope, auger electron spectroscopy, and cross-sectional scanning electron microscope. These measurements demonstrated that a liquid indium layer coexisted with indium droplets on top of the GaN (0001) surface at 800 °C. The liquid indium film thicknesses increased with increasing TMIn supply time and did not change during cooling from 800 °C to room temperature. [ABSTRACT FROM AUTHOR]

In this paper, we investigate the tendency of porous low-K dielectrics (also named Ultra Low-K, ULK) behavior to shrink when exposed to the electron beam of a scanning electron microscope. Various experimental electron beam conditions have been used for irradiating ULK thin films, and the resulting shrinkage has been measured through use of an atomic force microscope tool. We report the shrinkage to be a fast, cumulative, and dose dependent effect. Correlation of the shrinkage with incident electron beam energy loss has also been evidenced. The chemical modification of the ULK films within the interaction volume has been demonstrated, with a densification of the layer and a loss of carbon and hydrogen elements being observed. [ABSTRACT FROM AUTHOR]

W-doped/undoped TiO2 nanotube array (TNAs) photoelectrodes with different nanostructures were successfully fabricated using the anodization method. Their morphology and characteristics were studied using scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and ultra violet/visible light diffuse reflectance spectra (UV/vis/DRS). Their electronic structure and optical properties were studied by means of first-principle. Photocatalytic (PC) performance of W-TNAs photoelectrodes with different crystal structures was evaluated using the decomposition rates of Rhodamine B (Rh.B) under xenon light illumination. The results demonstrated that W substituting Ti broadened the width of conduction band (CB) and valence band (VB) of anatase and rutile TiO2, reduced the band gap of rutile TiO2 and even caused its red-shift. W incorporated into TNAs photoelectrodes extended light absorption threshold and enhanced its utilization of solar light and PC activity, particularly, the PC performance of W-TNAs photoelectrodes with mixed crystal and rutile crystal structure. [ABSTRACT FROM AUTHOR]

We investigate the role of grain constraint upon martensitic transformation through in situ scanning electron microscope tensile experiments on shape memory microwires with a small number of grains and grain junctions. The martensite transformation morphology becomes more complex with increasing grain constraint: In unconstrained monocrystalline regions, the transformation is simple, single variant, and complete; near grain boundaries, the transformation is only partial, containing regions of untransformed austenite; near a triple junction, the morphology is complex, the transformation is partial and also multi-variant. These observations speak of transformation-induced stress concentrations that are more severe around triple junctions than around grain boundaries. Finite element modeling also provides an estimate for constraint effects on martensitic transformation yielding higher stresses near triple junctions than near grain boundaries. Towards the goal of developing polycrystalline Cu-based shape memory alloys that avoid intergranular fracture, our results support three design objectives: (1) Removal of triple junctions, (2) reduction of the total grain boundary area, and (3) geometry design containing unconstrained regions where the transformation can be most easily accommodated. [ABSTRACT FROM AUTHOR]

To cool a high mobility two-dimensional electron gas (2DEG) at a GaAs–AlGaAs heterojunction to milliKelvin temperatures, we have fabricated low resistance Ohmic contacts based on alloys of Au, Ni, and Ge. The Ohmic contacts have a typical contact resistance of R C ≈ 0.8 Ω at 4.2 K, which drops to 0.2 Ω below 0.9 K. Scanning electron microscope images establish that the contacts have the same inhomogeneous microstructure that has been observed in previous studies. Measurements of the contact resistance R C , the four-terminal resistance along the top of a single contact, and the vertical resistance RV all show that there is a superconductor in the Ohmic contact, which can be turned completely normal with a magnetic field of 0.15 T. We briefly discuss how this superconductivity may be affecting the electrical transport measurements of 2DEGs, especially how it may hinder the cooling of electrons in a 2DEG below 0.1 K. [ABSTRACT FROM AUTHOR]

AlN/GaN/AlN quantum disks (Q-disks) embedded in self-assembled hexagonally shaped GaN nanowires have been grown on the Si (111) substrate by plasma-assisted molecular beam epitaxy. To correlate the structural and optical properties of individual Q-disks inside the nanowire, highly spatially resolved cathodoluminescence (CL) spectroscopy in a scanning transmission electron microscope has been performed at 18 K. CL spectrum linescans along a single nanowire clearly identify the emission from the GaN base around 354 nm as well as two recombination channels at 347 nm and 330 nm directly correlated with the AlN/GaN/AlN Q-disk. A detailed characterization of these individual quantum objects is presented. [ABSTRACT FROM AUTHOR]

For insulators, the deposited charge on the surface after electron bombardment interferes with the total electron emission yield (TEEY) measurement. The key to measuring the TEEY of insulators is to eliminate the surface deposited charge. Being different from traditional measurement methods, we develop and demonstrate a new method for measuring the TEEY of insulators in a scanning electron microscope by preparing the micro-patterned metal on the surface of the insulators as a conducting channel. The TEEY of the insulators is measured based on the TEEY of the metal part and the metal–insulator periodic structure. By theoretical analysis, we get a criterion for judging whether the deposited charge is eliminated. The result shows that this method is reliable by measuring the TEEY of Si. Then, we obtained the TEEY of SiO2 by this method with an energy of up to 3000 eV. The measured TEEY characteristics of SiO2 are consistent with the data from the references. Moreover, the surface charge diffusion distance of the insulators can also be estimated under this measuring condition. We get that the maximum value of the TEEY of SiO2 is ∼4.2, and the surface charge diffusion distance of SiO2 is ∼1 µm. In this work, the criterion for judging whether the deposited charge is eliminated is obtained, which has not been proposed in traditional measurement methods. [ABSTRACT FROM AUTHOR]

GaN-based nanorod light-emitting diodes (LEDs) with multilayer graphene (MLG) transparent electrodes have been fabricated. Two types of nano-LEDs with graphene on and under the metal pads are fabricated and their performances are investigated. And LEDs with graphene on the metal-pads exhibiting lower forward voltage and higher electroluminescence intensity are obtained. Using scanning electron microscope and Raman spectroscopy, we have demonstrated that graphene transferred after the metal deposition remains intact and has much less damages than graphene under the metal during the fabrication of LEDs with nanorods. [ABSTRACT FROM AUTHOR]

Lead Telluride (PbTe) with bismuth secondary phase embedded in the bulk has been prepared by matrix encapsulation technique. X-Ray Diffraction results indicated crystalline PbTe, while Rietveld analysis showed that Bi did not substitute at either Pb or Te site, which was further confirmed by Raman and X-Ray Photoelectron Spectroscopy. Scanning Electron Microscopy showed the expected presence of a secondary phase, while Energy Dispersive Spectroscopy results showed a slight deficiency of tellurium in the PbTe matrix, which might have occurred during synthesis due to higher vapor pressure of Te. Transmission Electron Microscopy results did not show any nanometer sized Bi phase. Seebeck coefficient (S) and electrical conductivity (σ) were measured from room temperature to 725 K. A decrease in S and σ with increasing Bi content showed an increased scattering of electrons from PbTe-Bi interfaces, along with a possible electron acceptor role of Bi secondary phase. An overall decrease in the power factor was thus observed. Thermal conductivity, measured from 400 K to 725 K, was smaller at starting temperature with increasing Bi concentration, and almost comparable to that of PbTe at higher temperatures, indicating a more important role of electrons as compared to phonons at PbTe-Bi interfaces. Still, a reasonable zT of 0.8 at 725 K was achieved for undoped PbTe, but no improvement was found for bismuth added samples with micrometer inclusions. [ABSTRACT FROM AUTHOR]

The SnO2:F transparent conductive oxide (TCO) layers with submicron-size textured structures have been characterized using spectroscopic ellipsometry (SE). By applying the Drude model to the SE analysis, the optical carrier concentration, mobility, and sheet resistance of the textured SnO2:F layers have been estimated, in addition to the detailed layered structures. The excellent agreement has been observed between the results obtained from SE and other characterization techniques including scanning electron microscope, atomic force microscope, and Hall measurements, confirming that SE is a reliable measurement technique even for the textured structures. Nevertheless, the electron mobility obtained from SE is lower than that deduced electrically from the Hall measurement, although the carrier concentrations estimated from these techniques are quite similar. From the SE analysis, the optical constants of the textured SnO2:F layers have been extracted, and the free carrier absorption in the SnO2:F layers increases drastically with decreasing optical mobility. The SE technique developed in this study can be applied further to perform the nondestructive mapping characterization of large-area TCO textures incorporated into thin-film solar cell modules. [ABSTRACT FROM AUTHOR]

In this study, the influences of reflow time and strain rate on interfacial fracture behaviors of the Sn-4Ag/Cu solder joints were investigated through in-situ observation. The interfacial microstructures of the solder joints reflowed for different times were first observed by scanning electronic microscope and measuring laser confocal microscope. Then tensile tests of the solder joints were conducted using in-situ tensile stage at different strain rates, and the interfacial fracture processes were in-situ observed. The observation results reveal that the thickness and surface roughness of the interfacial Cu6Sn5 layers increase linearly with increasing square root of the reflow time. Due to the serious strain concentration, fractures of the solder joints occur around the solder/Cu6Sn5 interface. The solder joints reflowed for a short time usually fracture inside the solder close to the joint interface, while the long-time reflowed solder joints are more apt to fracture in the interfacial Cu6Sn5 layer, because the stress applied on the Cu6Sn5 grains increases with increasing reflow time and grain size of Cu6Sn5. The solder joints reflowed for moderate time have the highest fracture resistance. At higher strain rate, the solder can apply a higher stress on Cu6Sn5 layer prior to its fracture, making the latter more apt to fracture. [ABSTRACT FROM AUTHOR]

The charge transport in sulfonated multi-wall carbon nanotube (sMWNT)-Nafion composite is reported. The scanning electron microscope images of the composite, at 1 and 10 wt % of sMWNT, show that the nanotubes are well dispersed in polymer matrix, with conductivity values of 0.005 and 3.2 S/cm, respectively; and the percolation threshold is nearly 0.42 wt. %. The exponent (∼0.25) of the temperature dependence of conductivity in both samples indicates Mott's variable range hopping (VRH) transport. The conductance in 1 wt. % sample increases by three orders of magnitude at high electric-fields, consistent with VRH model. The negative magnetoresistance in 10 wt. % sample is attributed to the forward interference scattering mechanism in VRH transport. The ac conductance in 1 wt. % sample is expressed by σ(ω)∝ωs, and the temperature dependence of s follows the correlated barrier hopping model. [ABSTRACT FROM AUTHOR]

The success of a microtube hydroforming (μTHF) process heavily depends on the material properties of microtubes, which can reveal the material response under multiaxial stress and influence the formability of hydroformed products. However, these material properties are not well understood because of the limited availability of material testing apparatus that would permit control of axial force and internal pressure simultaneously to mimic realistic μTHF loading. The main purpose of this study is to develop a set of grippers that can transfer required testing loads under fully coupled combinations of axial force and internal pressure. The grippers are designed so that they may be kept at the safe working temperature even when tests are carried out at higher temperatures. The grippers are also designed to fit in a load frame that is integrated in a scanning electron microscope for in situ material testing. The capabilities of the grippers are demonstrated by performing uniaxial and multiaxial material tests on SS304 microtubes with 1 mm outside diameter and 0.15 mm nominal tube wall thickness. The finite element simulations and experimental results show that the designed grippers can firmly hold the specimen and thus enable tensile, compression, torsion, and microtube bulge material tests to be accurately performed. [ABSTRACT FROM AUTHOR]

In this study, a femtosecond laser etching method is proposed to pattern an aluminum nitride (AlN) film, grown by metal-organic chemical vapor deposition on sapphire. Via control of typical pulse energies, the designed pattern was precisely written in the AlN film. The morphology of the patterned structures was characterized using a three-dimensional laser scanning confocal microscope and a scanning electron microscope; crystalline quality and film strain were analyzed using a Raman spectrometer and a transmission electron microscope. The results indicate that consistent morphologies were achieved with only slight changes to the crystalline quality. The tensile stress of the AlN film was released, and the film surface was slightly compressed after laser patterning. Thus, femtosecond etching has the potential to be an in situ patterning method during film growth. [ABSTRACT FROM AUTHOR]

An in situ hydrogen (H) plasma charging and in situ observation method was developed to continuously charge materials, while tensile testing them inside a scanning electron microscope (SEM). The present work will introduce and validate the setup and showcase an application allowing high-resolution observation of H-material interactions in a Ni-based alloy, Alloy 718. The effect of charging time and pre-straining was investigated. Fracture surface observation showed the expected ductile microvoid coalescence behavior in the uncharged samples, while the charged ones displayed brittle intergranular and quasi-cleavage failure. With the in situ images, it was possible to monitor the sample deformation and correlate the different crack propagation rates with the load-elongation curves. H-charging reduced the material ductility, while increasing pre-strain decreased hydrogen embrittlement susceptibility due to the possible suppression of mechanical twinning during the tensile test and, therefore, a reduction in H concentration at grain and twin boundaries. All the presented results demonstrated the validity of the method and the possibility of in situ continuously charging of materials with H without presenting any technical risk for the SEM. [ABSTRACT FROM AUTHOR]

High temperature materials usually serve under extreme conditions. In order to ensure the safety and reliability of industrial application, it is very significant to clarify the microstructural evolution and mechanical properties at high temperature. The in situ experiment combining mechanical tensile testing and heating in the scanning electron microscope (SEM) is a feasible method to study the relationship between the microstructure, mechanical properties, and temperature. However, it was challenging to acquire images of high quality when the temperature exceeded 800 °C due to the effect of thermal electrons and the instability of loading conditions at high temperature. In this study, a mini-tensile apparatus was devised and installed in an ordinary SEM, which can achieve a stable loading of 0–2200 N and obtain high quality images in the temperature range of 1150 °C. A highly efficient heat source with multi-layer thermal insulation was designed to prevent the other parts of the apparatus from being affected by high temperature. A symmetrical tensile structure was developed to ensure that the region of interest was always within the field of view of the microscope during testing. Thermal electrons were suppressed to ensure that the sample can be clearly distinguished at 1150 °C. In order to ensure the testing reliability, standard carbon steel was used to calibrate the instrument. Finally, a Ni-based single crystal superalloy, as an example, was tested using this in situ tensile testing system at 1150 °C to verify the main functions and reliability of the apparatus. [ABSTRACT FROM AUTHOR]

van der Waals forces, electrostatic interactions, and capillary forces are the dominant force interactions at the micro- and nanoscale. This complex ensemble of surface forces is oftentimes summarized as adhesion and is important for various applications and research fields. So far, numerous measurement techniques have evolved in this field. However, there is still a lack of experimental insight into the complex interplay of van der Waals, electrostatic, and capillary forces for small force ranges below 10 nN, as this is the order of magnitude of the latter, which can shadow other interactions in ambient and even inert gas environments. To exclude capillary forces and thus to turn the van der Waals and electrostatic forces into the most significant interactions, we develop an interferometric force spectroscopy setup based on a scanning probe technique, featuring a sub-nanonewton resolution, and integrate it into the vacuum chamber of a scanning electron microscope. In this work, we describe the setup integration, show the long-term drift behavior and resolution capabilities, and conduct first measurements of adhesion energies between a silica colloidal probe and a silicon substrate. The presented setup shows its capability to reliably measure adhesive interactions in vacuum and an ambient environment with a sub-nanonewton resolution proving its potential to allow for the investigation of the separate contribution of capillary, van der Waals, and electrostatic interactions to adhesion and for a systematic experimental validation of the established adhesion theories and approximations on the micro- and nanoscale. [ABSTRACT FROM AUTHOR]

In this research, we have explored the structural, morphological, electrical, and magnetic properties of Mn2+ substituted polycrystalline Ba0.4Ca0.4Sr0.2MnxTi1−xO3 (where x = 0.0, 0.05, 0.10, 0.15, and 0.20) ceramic samples prepared by the standard solid-state reaction system. The x-ray diffraction pattern of the 20% Mn-doped BCSMTO sample has confirmed a cubic to tetragonal structural phase transition. The lattice parameter is found to increase at 15% and 20% Mn concentrations, which is caused due to the inequality in ionic radii of cations. Scanning electron microscope analysis exhibited that, with the increase in Mn contents (x = 0.0–0.15), the average grain size of the samples gets bigger but then significantly decreased at 20% Mn substitution. Dielectric constants for all the samples are higher for lower frequency regions and remain independent at a higher frequency domain. The initial permeability remains almost constant at lower frequencies and then sharply falls at the cut-off frequency, which is in agreement with the Globus model. Among all the studied samples, the 10% Mn-doped ceramic sample shows the highest relative quality factor with significantly demolished loss (tan δM). At room temperature, the M–H loop for the 10% Mn-doped sample demonstrates a domination of diamagnetic nature at a higher magnetic field. The decrement in saturation magnetization with Mn addition suggests that the double-exchange interactions in tetragonal BaTiO3 may have been weakened. The outcome of this analysis emphasizes the impact of Mn as a doping element with 10% concentration in Ba0.4Ca0.4Sr0.2MnxTi1−xO3 that provides enhanced structural and electrical properties, which are associated with homogeneous grain size, reduced porosity, and lower tangent loss. [ABSTRACT FROM AUTHOR]

Supercapacitors or electrochemical capacitors are receiving greater interest because of their high-power density, long life, and low maintenance. We have synthesized CuS nanoparticles and graphene oxide (CuS–GO) nanocomposites for supercapacitor applications because of their low cost and excellent electrochemical properties. The phase purity of each material was determined using powder XRD studies. The bandgap was determined by UV-visible spectrophotometric studies. Scanning electron microscope and transmission electron microscope images revealed the nano-scale morphology of the synthesized particles. All the electrochemical measurements were conducted in a standard three-electrode configuration, using a platinum wire as the counter electrode and Hg/HgO as the reference electrode. CuS and its composites with graphene oxide on nickel foam were used as working electrodes. All the electrochemical measurements were performed in 3M KOH solution. The CuS–GO nanocomposite electrode showed a specific capacitance of 250 F/g, 225 F/g, 182 F/g, 166 F/g, 161 F/g, and 158 F/g at a current density of 0.5 A/g, 1 A/g, 5 A/g, 10 A/g, 15 A/g, and 20 A/g, respectively. CuS–GO electrodes showed a specific capacitance retention of 70% after 5000 charge–discharge cycles at a current density of 5 A/g. [ABSTRACT FROM AUTHOR]

Thin films of polycrystalline gallium antimonide (GaSb) were grown on widely available mica substrates using the physical vapor deposition method. The as-grown films contain grains of nano-scale with regular symmetries, as identified by x-ray diffraction and scanning electron microscope analysis. Two-terminal devices with coplanar electrodes were fabricated from the polycrystalline GaSb films; thus, the time dependent photoresponse property of the films was investigated by measuring the current density–voltage characteristics of devices. A significant photoresponse of the device was revealed by the linear dependence of the applied bias. Additionally, the transient behavior of the GaSb thin films was used to optimize growth temperatures of the films. This study shows that polycrystalline GaSb thin films on mica at 500 °C are suitable for high photoresponse and low noise IR photodetectors, thus proving to be a low cost solution for IR photodetectors. [ABSTRACT FROM AUTHOR]