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At least 1,531 records · Page 85

Force-extension curves for broken-rod macromolecules: Dramatic effects of different probing methods for two and three rods

We study force-extension curves of a single semiflexible chain consisting of several rigid rods connected by flexible spacers. The atomic force microscopy and laser optical or magnetic tweezers apparatus stretching these rod-coil macromolecules are discussed. In addition, the stretching by external isotropic force is analyzed. The main attention is focused on computer simulation and analytical results. We demonstrate that the force-extension curves for rod-coil chains composed of two or three rods of equal length differ not only quantitatively but also qualitatively in different probe methods. These curves have an anomalous shape for a chain of two rods. End-to-end distributions of rod-coil chains are calculated by Monte Carlo method and compared with analytical equations. The influence of the spacer’s length on the force-extension curves in different probe methods is analyzed. The results can be useful for interpreting experiments on the stretching of rod-coil block-copolymers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization and Application of a Hybrid Optical Microscopy/Laser Ablation Liquid Vortex Capture/Electrospray Ionization System for Mass Spectrometry Imaging with Sub-micrometer Spatial Resolution

Herein, a commercial optical microscope, laser microdissection instrument was coupled with an electrospray ionization mass spectrometer via a low profile liquid vortex capture probe to yield a hybrid optical microscopy/mass spectrometry imaging system. The instrument has bright-field and fluorescence microscopy capabilities in addition to a highly focused UV laser beam that is utilized for laser ablation of samples. With this system, material laser ablated from a sample using the microscope was caught by a liquid vortex capture probe and transported in solution for analysis by electrospray ionization mass spectrometry. Both lane scanning and spot sampling mass spectral imaging modes were used. The smallest area the system was able to ablate was ~0.544 μm × ~0.544 μm, achieved by oversampling of the smallest laser ablation spot size that could be obtained (~1.9 μm). With use of a model photoresist surface, known features as small as ~1.5 μm were resolved. The capabilities of the system with real world samples were demonstrated first with a blended polymer thin film containing poly(2-vinylpyridine) and poly(N-vinylcarbazole). Using spot sampling imaging, sub-micrometer sized features (0.62, 0.86, and 0.98 μm) visible by optical microscopy were clearly distinguished in the mass spectral images. A second real world example showed the imaging of trace amounts of cocaine in mouse brain thin tissue sections. Lastly, with use of a lane scanning mode with ~6 μm × ~6 μm data pixels, features in the tissue as small as 15 μm in size could be distinguished in both the mass spectral and optical images.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

AE (Acoustic Emission) for Flip-Chip CGA/FCBGA Defect Detection

C-mode scanning acoustic microscopy (C-SAM) is a nondestructive inspection technique that uses ultrasound to show the internal feature of a specimen. A very high or ultra-high-frequency ultrasound passes through a specimen to produce a visible acoustic microimage (AMI) of its inner features. As ultrasound travels into a specimen, the wave is absorbed, scattered or reflected. The response is highly sensitive to the elastic properties of the materials and is especially sensitive to air gaps. This specific characteristic makes AMI the preferred method for finding "air gaps" such as delamination, cracks, voids, and porosity. C-SAM analysis, which is a type of AMI, was widely used in the past for evaluation of plastic microelectronic circuits, especially for detecting delamination of direct die bonding. With the introduction of the flip-chip die attachment in a package; its use has been expanded to nondestructive characterization of the flip-chip solder bumps and underfill. Figure 1.1 compares visual and C-SAM inspection approaches for defect detection, especially for solder joint interconnections and hidden defects. C-SAM is specifically useful for package features like internal cracks and delamination. C-SAM not only allows for the visualization of the interior features, it has the ability to produce images on layer-by-layer basis. Visual inspection; however, is only superior to C-SAM for the exposed features including solder dewetting, microcracks, and contamination. Ideally, a combination of various inspection techniques - visual, optical and SEM microscopy, C-SAM, and X-ray - need to be performed in order to assure quality at part, package, and system levels. This reports presents evaluations performed on various advanced packages/assemblies, especially the flip-chip die version of ball grid array/column grid array (BGA/CGA) using C-SAM equipment. Both external and internal equipment was used for evaluation. The outside facility provided images of the key features that could be detected using the most advanced C-SAM equipment with a skilled operator. Investigation continued using in-house equipment with its limitations. For comparison, representative X-rays of the assemblies were also gathered to show key defect detection features of these non-destructive techniques. Key images gathered and compared are: Compared the images of 2D X-ray and C-SAM for a plastic LGA assembly showing features that could be detected by either NDE technique. For this specific case, X-ray was a clear winner. Evaluated flip-chip CGA and FCBGA assemblies with and without heat sink by C-SAM. Only the FCCGA package that had no heat sink could be fully analyzed for underfill and bump quality. Cross-sectional microscopy did not revealed peripheral delamination features detected by C-SAM. Analyzed a number of fine pitch PBGA assemblies by C-SAM. Even though the internal features of the package assemblies could be detected, C-SAM was unable to detect solder joint failure at either the package or board level. Twenty times touch ups by solder iron with 700degF tip temperature, each with about 5 second duration, did not induce defects to be detected by C-SAM images. Other techniques need to be considered to induce known defects for characterization. Given NASA's emphasis on the use of microelectronic packages and assemblies and quality assurance on workmanship defect detection, understanding key features of various inspection systems that detect defects in the early stages of package and assembly is critical to developing approaches that will minimize future failures. Additional specific, tailored non-destructive inspection approaches could enable low-risk insertion of these advanced electronic packages having hidden and fine features.

Ghaffarian, Reza↗

Influence of different sulfur to selenium ratios on the structural and electronic properties of Cu(In,Ga)(S,Se){sub 2} thin films and solar cells formed by the stacked elemental layer process

In this study, we investigate the effect of different elemental selenium to elemental sulfur ratios on the chalcopyrite phase formation in Cu(In,Ga)(S,Se){sub 2} thin films. The films are formed by the stacked elemental layer process. The structural and electronic properties of the thin films and solar cells are analyzed by means of scanning electron microscopy, glow discharge optical emission spectrometry, X-ray diffraction, X-ray fluorescence, Raman spectroscopy, spectral photoluminescence as well as current-voltage, and quantum efficiency measurements. The influence of different S/(S+Se) ratios on the anion incorporation and on the Ga/In distribution is investigated. We find a homogenous sulfur concentration profile inside the film from the top surface to the bottom. External quantum efficiency measurements show that the band edge of the solar cell device is shifted to shorter wavelength, which enhances the open-circuit voltages. The relative increase of the open-circuit voltage with S/(S+Se) ratio is lower than expected from the band gap energy trend, which is attributed to the presence of S-induced defects. We also observe a linear decrease of the short-circuit current density with increasing S/(S+Se) ratio which can be explained by a reduced absorption. Above a critical S/(S+Se) ratio of around 0.61, the fill factor drops drastically, which is accompanied by a strong series resistance increase which may be attributed to changes in the back contact or p-n junction properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Tailoring spectral properties for entangled photon generation

The linear intensity scaling of entangled two-photon absorption (ETPA) offers a fundamental mechanism to enable nonlinear optical spectroscopy and microscopy under a substantially lower excitation power than is currently feasible. However, the long data acquisition time and low signal-to-noise ratio in reported ETPA-based spectroscopic and microscopic studies prevent its widespread application. To gain the full potential of this novel quantum light approach, it is essential to optimize entangled photon generation for significantly enhanced ETPA responses. Here, we report a new quantum light source by combining entangled photon generation with free-space femtosecond pump-pulse shaping. Here, through measurements of singles and coincidence counts by varying the patterns applied to a spatial light modulator to control the spectral widths of the pump pulses, we reveal strong dependence of the singles and coincidence count rates as well as their ratios on the spectral widths of pump pulses. An optimal spectral width for the highest ratios between the coincidence photon and the signal or idler photon count rates is also determined. Identification of such optimal spectral widths for entangled photon generation in the presence of postgeneration spectral selection makes this quantum light source a promising choice for ETPA-based spectroscopy and imaging.

Photon pairs & parametric down-conversion↗

Ice cloud formation potential by free tropospheric particles from long-range transport over the Northern Atlantic Ocean

Long-range transported free tropospheric particles can play a significant role on heterogeneous ice nucleation. Using optical and electron microscopy we examine the physicochemical characteristics of ice nucleating particles (INPs). Particles were collected on substrates from the free troposphere at the remote Pico Mountain Observatory in the Azores Islands, after long-range transport and aging over the Atlantic Ocean. We investigate four specific events to study the ice formation potential by the collected particles with different ages and transport patterns. We use single-particle analysis, as well as bulk analysis to characterize particle populations. Both analyses show substantial differences in particle composition between samples from the four events; in addition, single-particle microscopy analysis indicates that most particles are coated by organic material. The identified INPs contained mixtures of dust, aged sea salt and soot, and organic material acquired either at the source or during transport. The temperature and relative humidity ( RH ) at which ice formed, varied only by 5% between samples, despite differences in particle composition, sources, and transport patterns. We hypothesize that this small variation in the onset RH may be due to the coating material on the particles. Finally, this study underscores and motivates the need to further investigate how long-range transported and atmospherically aged free tropospheric particles impact ice cloud formation.

54 ENVIRONMENTAL SCIENCES↗

Machine Learning-Enabled Correlation and Modeling of Multimodal Response of Thin Film to Environment on Macro and Nanoscale Using “Lab-on-a-Crystal”

To close the feedback loop between artificial intellegence-controlled materials synthesis and characterization, material functionality must be rapidly tested. A platform for high-throughput multifunctional materials characterization is developed using a quartz crystal microbalance with auxiliary in-plane electrodes and a custom gas/vapor flow cell, enabling simultaneous scanning probe microscopy and electrical, optical, gravimetric, and viscoelastic characterization on the same film under controlled environment. The lab-on-a-crystal in situ multifunctional output allows direct correlations between the gravimetric/viscoelastic, electrical, and optical responses of polymer film in response to environment. Finally, when multiple film properties are used to augment the training set for machine learning regression, prediction of material response to the environment improves by a factor of 13 when <5% of the total dataset is used for model training.

36 MATERIALS SCIENCE↗

IR Spectroscopy for the Analysis of Scattering Polymeric Materials{sup *}

An effective spectroscopic method for estimating the degree of filling (porosity) of polymeric materials, the average size and the size distribution of the scattering particles of the filler within the polymer matrix, their anisotropy and the degree of orientation is proposed. The obtained spectral data are in good agreement with the results of optical and electron microscopy methods.

36 MATERIALS SCIENCE↗

Using defects as a ‘fossil record’ to help interpret complex processes during additive manufacturing: as applied to raster-scanned electron beam powder bed additively manufactured Ti–6Al–4V

Abstract Defects in parts produced by additive manufacturing, instead of simply being perceived as deleterious, can act as important sources of information associated with the complex physical processes that occur during materials deposition and subsequent thermal cycles. Indeed, they act as materials-state ‘fossil’ records of the dynamic AM process. The approach of using defects as epoch-like records of prior history has been developed while studying additively manufactured Ti–6Al–4V and has given new insights into processes that may otherwise remain either obscured or unquantified. Analogous to ‘epochs,’ the evolution of these defects often is characterized by physics that span across a temporal length scale. To demonstrate this approach, a broad range of analyses including optical and electron microscopy, X-ray computed tomography, energy-dispersive spectroscopy, and electron backscatter diffraction have been used to characterize a raster-scanned electron beam Ti–6Al–4V sample. These analysis techniques provide key characteristics of defects such as their morphology, location within the part, complex compositional fields interacting with the defects, and structures on the free surfaces of defects. Observed defects have been classified as banding, spherical porosity, and lack of fusion. Banding is directly related to preferential evaporation of Al, which has an influence on mechanical properties. Lack-of-fusion defects can be used to understand columnar grain growth, fluid flow of melt pools, humping, and spattering events. Graphical abstract

36 MATERIALS SCIENCE↗

Relative Role of Particle Size and Shape on the Magnetic and Catalytic Behavior of Nanozinc Chromite

The purpose of this study is to define an effective synthesis for spinel-type zinc chromite (ZnCr{sub 2}O{sub 4}) nanoparticles by a simple microwave combustion method. The synthesized material was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and from optical properties. A magnetic property for the material was examined through the vibrating sample magnetism. The distribution of the external magnetic lines of force and the self-generated magnetic field of ferromagnetic materials was taken into account in the presence of an external magnetic field. Zinc chromite showed good performances in catalytic oxidation, and the role of particle size and shape is highlighted.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

On the Similarity of Deformation Mechanisms During Friction Stir Welding and Sliding Friction of the AA5056 Alloy

A comparative investigation of the structure of an aluminum-manganese alloy is performed after its friction stir welding and sliding friction. Using the methods of optical and electron microscopy, it is shown that during friction identical ultrafine-grained structures are formed in the weld nugget and in the surface layer, in which the grains measure ~ 5 μm irrespective of the initial grain size of the alloy. An assumption is made that the microstructure during both processes under study is formed by the mechanism of rotational plasticity.

36 MATERIALS SCIENCE↗

Influence of Thermomechanical Treatment on Structural-Phase Transformations and Mechanical Properties of the Cu–Al–Ni Shape-Memory Alloys

Using the methods of optical and electron microscopy and electron and X-ray diffraction analyses, the influence of thermomechanical treatment on the mechanical properties, average grain size, and structural and phase transformations is investigated in the Cu–Al–Ni triple alloys exhibiting a shape memory effect. In the alloys under study with a fixed content of 3wt% Ni the concentration of aluminum was varied from 9 to 14 wt%. It is shown that in the alloys subjected to thermal treatment, including forging and homogenizing annealing using controlled recrystallization in the austenitic state followed by quenching, the grain-boundary disintegration and segregation disappear. It is found out that the microstructure of the alloys in the hot-forged and hardened states with the content of aluminum 9–10 wt%. consists of the grains of the average dimensions within 60–80 μm, with the content of aluminum 10–12 wt% – 100–350 μm, while in the alloys with the content of aluminum up to 14 12 wt% the average grain size reaches 1 mm. According to the data of mechanical testing at room temperature, with a decrease in the content of aluminum the ultimate tensile strength (σ{sub UTS}), the yield strength (σ{sub М}) and the relative elongation (δ) increase. An improvement of the mechanical properties of the alloys is attributed to the grain structure refinement of the β{sub 2}-austenite and package substructure of the β'{sub 1}-and γ'{sub 1}-martensites as the content of aluminum in the alloys decreases. For instance, in the fine-grained alloys containing 9.2 and 9.5 wt% Al the value of relative elongation remains at a high level (>10%), while for the other alloys with 10–14 wt% Al it does not exceed 5%. As the content of aluminum in the alloys decreases, the character of the specimen fracture under uniaxial tension changes (from brittle to ductile).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Microstructure, Morphology, and Nanomechanical Properties Near Fine Holes Produced by Electro-Discharge Machining

Fine holes in metal alloys are employed for many important technological purposes, including cooling and the precise atomization of liquids. For example, they play an important role in the metering and delivery of fuel to the combustion chambers in energy-efficient, low-emissions diesel engines. Electro-discharge machining (EDM) is one process employed to produce such holes. Since the hole shape and bore morphology can affect fluid flow, and holes also represent structural discontinuities in the tips of the spray nozzles, it is important to understand the microstructures adjacent to these holes, the features of the hole walls, and the nanomechanical properties of the material that was in some manner altered by the EDM hole-making process. Several techniques were used to characterize the structure and properties of spray-holes in a commercial injector nozzle. These include scanning electron microscopy, cross-sectioning and metallographic etching, bore surface roughness measurements by optical interferometry, scanning electron microscopy, and transmission electron microscopy of recast EDM layers extracted with the help of a focused ion beam.

electro-discharge machining↗

Fabrication of AZ31/MWCNTs Surface Metal Matrix Composites by Friction Stir Processing: Investigation of Microstructure and Mechanical Properties

The surface metal matrix composites of AZ31 Mg alloy reinforced with multiwall carbon nanotubes (MWCNTs) have been fabricated through the friction stir processing by a conventional and two stepped tools. The microstructure and mechanical properties of fabricated composites were studied by optical and electron microscopy, microhardness and tensile tests, respectively. The processing has developed a fine-grain structure along with good distribution of reinforcements. The hardness and tensile strength of fabricated MWCNT/AZ31 composites are generally higher than as-received and FSPed samples. The accumulative effect of grain refinement and reinforcing nanotubes is assumed to be the reason for increasing the ductility after friction stir processing. The hardness is nearly doubled for FSPed samples and some more for nanocomposites compared with the as-received sample. The elongation of nanocomposites is about two times greater than that of the as-rolled sample. The speed ratio, pass number and CNT amount are three important factors influencing the resulting microstructure and mechanical properties. The stepped tools also give a more uniform distribution of reinforcement and higher grain refinement.

36 MATERIALS SCIENCE↗

Universal Mechanism of Viscoplastic Deformation of Metallic Materials Far from Thermodynamics Equilibrium

The article gives results of structure formation in metallic materials after different types of deformation: tungsten after rolling, nickel after thermal cycling and nickel single crystal after rolling, aluminum single crystal after cyclic tension and aluminum alloys (D16, 2024-T3) after impulsive load. We used optical and electron microscopy methods for investigation of deformation structure formation and molecular dynamics method for computer modeling of the processes of plastic deformation (LAMMPS software). The following quantitative parameters were calculated during the simulation: energy of pair interaction, temperature, total cumulative pressure, stress tensor and pressure tensor. The study shows that the plastic flow of metallic materials with any initial structure at certain loading stage can be carried out by homogeneous mass transfer through channels with a liquid-like structure, from which follows that the dislocation mechanism of plastic deformation of crystals has a limited field of application. The main role has a synergistic structure formation in the conditions of distance from thermodynamic equilibrium. The relaxation processes proceed intensively after and during the process of destruction. The results of modeling have shown the possibility of forming channels of hydrodynamic flow without the participation of defects in the initial material.

36 MATERIALS SCIENCE↗

The Influence of Galvanizing Parameters on the Structural Development of Zn-Al-Based Coatings

The evolution of some layers’ characteristics, deposited by galvanization, was monitored according to the technological parameters of the process. Two types of alloys from the Zn-Al and Zn-Al-Ti-B systems were used for deposition. The structure of the deposited layers was analyzed by optical and electron microscopy. The chemical composition, phases and compounds in the structures were identified. The mechanical properties of the structural constituents of the layers were determined by nanoindentation. These techniques highlighted the typical non-uniformities in terms of composition and properties in the layers, mainly due to the diffusion and distribution of iron from the steel substrate in the deposited layers. The evaluation of iron diffusion in the deposited layer was done by differential thermal analysis. The values of the critical temperatures (melting temperature, eutectic temperature and solidification temperature) were correlated with the parameters used during deposition. It was observed that the structure of the coatings is layered, with a specific order from the steel substrate to the edge. In these layers, the constituents are mixtures of soft solid solutions of Al in Zn (η and β) and hard intermetallic compounds. Moreover, increasing the immersion time in the galvanizing bath and the bath temperature leads to an increase in iron diffusion in the coating layer, which contributes to lower coating thickness, thus reducing its durability in operation.

36 MATERIALS SCIENCE↗

Listening to Radiation Damage In Situ: Passive and Active Acoustic Techniques

Knowing when, why, and how materials evolve, degrade, or fail in radiation environments is pivotal to a wide range of fields from semiconductor processing to advanced nuclear reactor design. A variety of methods, including optical and electron microscopy, mechanical testing, and thermal techniques, have been used in the past to successfully monitor the microstructural and property evolution of materials exposed to extreme radiation environments. Acoustic techniques have also been used in the past for this purpose, although most methodologies have not achieved widespread adoption. However, with an increasing desire to understand microstructure and property evolution in situ, acoustic methods provide a promising pathway to uncover information not accessible to more traditional characterization techniques. This work highlights how two different classes of acoustic techniques may be used to monitor material evolution during in situ ion beam irradiation. The passive listening technique of acoustic emission is demonstrated on two model systems, quartz and palladium, and shown to be a useful tool in identifying the onset of damage events such as microcracking. An active acoustic technique in the form of transient grating spectroscopy is used to indirectly monitor the formation of small defect clusters in copper irradiated with self-ions at high temperature through the evolution of surface acoustic wave speeds. Here, these studies together demonstrate the large potential for using acoustic techniques as in situ diagnostics. Such tools could be used to optimize ion beam processing techniques or identify modes and kinetics of materials degradation in extreme radiation environments.

36 MATERIALS SCIENCE↗

Microstructure and Residual Stress in Functionally Graded 316L Stainless Steel/Inconel 625 Alloys Fabricated by Direct Energy Deposition

Functionally graded materials (FGMs) provide a unique solution to combine distinct properties within a single component to enhance its overall performance. Understanding the microstructure and residual stress distribution is particularly important as the material dissimilarity in FGMs can result in high residual stress that affects the mechanical integrity of structural components. Here, this work aims to study the microstructure and residual stress of additively manufactured FGMs and the effects of isothermal annealing. In this study, 316L stainless steel/Inconel 625 FGMs were built by direct energy deposition, and characterized by optical and electron microscopy as well as synchrotron-based X-ray diffraction. Our study reveals that thermal annealing at 500°C for 3 h has minimal effects on the microstructure and chemistry of the graded materials, but effectively relieves the residual stress and leads to a uniform distribution of residual stress.

36 MATERIALS SCIENCE↗