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At least 109 records · Page 6

Study of the self-organization processes in lead sulfide quantum dots

A procedure is described for the synthesis of nanoparticles based on lead chalcogenides. The procedure combines the synthesis of colloidal quantum dots (QDs) in aqueous solutions with simultaneous organization of the QDs into ordered arrays. The processes of the self-organization of QDs are analyzed at the nano- and microscopic levels by the photoluminescence method, atomic-force microscopy, and optical microscopy.

36 MATERIALS SCIENCE↗

Light-Induced Macroscopic Peeling of Single Crystal Driven by Photoisomeric Nano-Optical Switching

Single-crystal optical actuators are emerging as a prospective material form for nano-optical mechanical switching, sensing, or transduction device applications in nano-technology and quantum technology. Crystal-lattice strain effects lie at the molecular origins of their macroscopic optical behavior, and linkage photoisomerization is an attractive source of optical actuation if only suitably functioning materials of this ilk could be found. In this work, we discover η 1 -SO 2 to η 1 -OSO single-crystal linkage photoisomerization in [Ru(NH 3 ) 4 (SO 2 )(3-phenylpyridine)]Cl 2 ·H 2 O, which behaves macroscopically as a single-crystal optical actuator, whereby the crystal peels in response to light-induction at 100 K. It thermally recovers, whereupon the crystal exhibits remarkable restorative properties. We apply photocrystallography alongside concerted optical microscopy and optical absorption spectroscopy to reveal how the molecular origins of photoisomerization induce crystal-lattice strain that engenders this macroscopic crystal peeling effect. Finally, linking structure and function across molecular and macroscopic length scales showcases a means by which single-crystal optically actuating materials could be systematically designed.

36 MATERIALS SCIENCE↗

Ultrasound – A new approach for non-woven scaffolds investigation

In this study we verified the method of impulse acoustic microscopy as a tool for scaffold evaluation in tissue engineering investigation. Cellulose diacetate (CDA) non-woven 3D scaffold was used as a model object. Scanning electron microscopy and optical microscopy were used as reference methods in order to realize feasibility of acoustic microscopy method in a regenerative medicine field. Direct comparison of the different methods was carried out.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Simultaneous differential spinning disk fluorescence optical sectioning microscopy and nanomechanical mapping atomic force microscopy

Combined microscopy techniques offer the life science research community a powerful tool to investigate complex biological systems and their interactions. Here, we present a new combined microscopy platform based on fluorescence optical sectioning microscopy through aperture correlation microscopy with a Differential Spinning Disk (DSD) and nanomechanical mapping with an Atomic Force Microscope (AFM). The illumination scheme of the DSD microscope unit, contrary to standard single or multi-point confocal microscopes, provides a time-independent illumination of the AFM cantilever. This enables a distortion-free simultaneous operation of fluorescence optical sectioning microscopy and atomic force microscopy with standard probes. In this context, we discuss sample heating due to AFM cantilever illumination with fluorescence excitation light. Integration of a DSD fluorescence optical sectioning unit with an AFM platform requires mitigation of mechanical noise transfer of the spinning disk. We identify and present two solutions to almost annul this noise in the AFM measurement process. The new combined microscopy platform is applied to the characterization of a DOPC/DOPS (4:1) lipid structures labelled with a lipophilic cationic indocarbocyanine dye deposited on a mica substrate.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Role of different compatibilizing approaches on the microstructure and mechanical properties of polypropylene/talc composites

Since in a highly filled polymer, a major problem arises from non-uniformity of properties due to the poor dispersion of filler, the application of coupling agents have been directed to overcome this problem and also to enhance the mechanical performance of the composites by improving the adhesion at the interface. In this study, a comparison between two major coupling approaches is conducted: 1) Using PPgMA as a kind of compatibilizer which changes the nature of the matrix, 2) Using titanate coupling agent which takes action at the interface and reacts with hydroxyl groups at the inorganic filler surface, resulting in the formation of monomolecular layer on the inorganic surface to increase compatibility of filler/matrix interface. The comparison is made based on the mechanical properties of the composites by means of elastic modulus, yield stress, impact strength and percentage of strain-to-fracture and evaluation of their effects on both the dispersion and adhesion of talc plates in the matrix through the microscopy. Transmission optical microscopy (TOM) and scanning electron microscopy (SEM) are used to observe the deformation micromechanism and the fracture surface of the composites, respectively.

36 MATERIALS SCIENCE↗

Thermoelectric properties of Bi{sub 2}Te{sub 2.4}Se{sub 0.6} solid solutions of different particle-size composition

The thermoelectric properties of n-type Bi{sub 2}Te{sub 2.4}Se{sub 0.6} solid solution prepared by the vacuum hot pressing of powder mixtures with different particle sizes are investigated. The powders were prepared by the mechanical grinding of ingots and melt spinning. The microstructure and fracture pattern of a sample cleavage surface are analyzed using scanning electron microscopy and optical microscopy. The thermoelectric characteristics (the Seebeck coefficient, electrical conductivity, and thermal conductivity) are measured at room temperature and in the temperature range of 100–700 K.

36 MATERIALS SCIENCE↗

Microstructure of surface cerium hydride growth sites

Samples of cerium were exposed to hydrogen under controlled conditions causing cerium hydride sites to nucleate and grow on the surface. The hydriding rate was measured in situ, and the hydrides were characterised using secondary ion mass spectrometry, scanning electron microscopy, and optical microscopy. The results show that the hydriding rate proceeded more quickly than earlier studies. Characterisation confirmed that the hydrogen is confined to the sites. The morphology of the hydrides was confirmed to be oblate, and stressed material was observed surrounding the hydride, in a number of cases lathlike features were observed surrounding the hydride sites laterally with cracking in the surface oxide above them. It is proposed that during growth the increased lattice parameter of the CeH{sub 2} induces a lateral compressive stress around the hydride, which relieves by the ca. 16% volume collapse of the γ-Ce to α-Ce pressure induced phase transition. Cracking of the surface oxide above the laths reduces the diffusion barrier to hydrogen reaching the metal/oxide interface surrounding the hydride site and contributes to the anisotropic growth of the hydrides.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of Cooling Rate on Microsegregation During Solidification of Superalloy INCONEL 718 Under Slow-Cooled Conditions

The solidification sequence, microstructural evolution, solid-liquid interface variation, interdendritic segregation, and elemental distribution of as-cast IN718 alloy at three slow-cooling rates (5, 10, and 20 °C/min) were investigated by differential scanning calorimetry (DSC), confocal laser scanning microscopy (CLSM), optical microscopy (OM), field-emission scanning electron microscopy (FESEM), and electron-probe microanalysis (EPMA) techniques. The results indicate that as the cooling rate decreases, the constitutional supercooling at the solidification front affects the solid-liquid interface more significantly, and the size and quantity of the Laves phase increase. However, the composition of the Laves phase is insensitive to the cooling rate in the range of conditions studied here. In dendrite core, the contents of Ni, Cr, Fe, and Al follow a slight downward trend with an increasing cooling rate, whereas the Nb, Mo, and Ti contents show an upward trend. Additionally, Mo shows a stronger propensity to segregate under slow-cooling conditions because its effective partition coefficient almost linearly decreased with decreasing cooling rate, which is same as Nb. Using the parameters experimentally determined in this study and the Clyne–Kurz equation, we achieved reasonable agreement between the calculated and measured liquid composition change during the solidification process at different cooling rates. All experimental and theoretical programs in this research were undertaken with the aim of gaining further understanding of the microsegregation behaviors in large-scale IN718 ingots, whose cooling rates are within a lower range.

36 MATERIALS SCIENCE↗

Microstructure and Mechanical Characterization of Friction-Stir-Welded Dual-Phase Brass

Friction stir welding (FSW) is an ideal process to join brass to avoid the evaporation of zinc. In the present investigation, 6-mm-thick dual-phase brass plates were joined efficiently using FSW at various tool rotational speeds. The microstructures were studied using optical microscopy, electron backscattered diffraction and transmission electron microscopy. The optical micrographs revealed the evolution of various zones across the joint line. The microstructure of the heat-affected zone was similar to that of base metal. The weld zone exhibited finer grains due to dynamic recrystallization. The recrystallization was inhomogeneous and the inhomogeneity reduced with increased tool rotational speed. The dual phase was preserved in the weld zone due to the retention of zinc. The severe plastic deformation created a lot of dislocations in the weld zone. The weld zone was strengthened after welding. The role of tool rotational speed on the joint strength is further reported.

36 MATERIALS SCIENCE↗

Viewing Optical Processes at the Nanoscale: Combining Scanning Tunneling Microscopy and Optical Spectroscopy

The combination of optical spectroscopy and scanning tunneling microscopy techniques has the potential to yield the unambiguous single-molecule level insight required to fully understand the complex structure–property relationship of emerging material systems. In this Perspective, we highlight the recent progress of single-molecule absorption detected by scanning tunneling microscopy (SMA-STM) to investigate light–matter interactions of supported (nano)particles, quantum dots, and molecular and thin films at the nanoscale. We further show how the SMA-STM technique has been recently extended to expand the classes of materials that can be investigated as well as recent design modifications that enable both time-resolved imaging and tomography. Finally, we hypothesize how these modifications can be further leveraged to advance our current knowledge of light–matter interactions and how the resulting nanoscale insight can be implemented for future material applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electrical current leakage and open-core threading dislocations in AlGaN-based deep ultraviolet light-emitting diodes

Electrical current transport through leakage paths in AlGaN-based deep ultraviolet (DUV) light-emitting diodes (LEDs) and their effect on LED performance are investigated. Open-core threading dislocations, or nanopipes, are found to conduct current through nominally insulating Al{sub 0.7}Ga{sub 0.3}N layers and limit the performance of DUV-LEDs. A defect-sensitive phosphoric acid etch reveals these open-core threading dislocations in the form of large, micron-scale hexagonal etch pits visible with optical microscopy, while closed-core screw-, edge-, and mixed-type threading dislocations are represented by smaller and more numerous nanometer-scale pits visible by atomic-force microscopy. The electrical and optical performances of DUV-LEDs fabricated on similar Si-doped Al{sub 0.7}Ga{sub 0.3}N templates are found to have a strong correlation to the density of these nanopipes, despite their small fraction (<0.1% in this study) of the total density of threading dislocations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Investigations of Polymethacrylate Tribochemical Films Using X-Ray Spectroscopy and Optical Profilometry

This study investigates the elemental composition and surface morphology of solid tribochemical films formed on steel surfaces. The reversible addition-fragmentation chain transfer (RAFT) method was used to synthesize nine different metal-free polymers, which were blended into commercial base oils. The polymers were either homopolymers of dodecyl methacrylate and ethylhexyl methacrylate or were co-polymers of these monomers with six polar monomers. After tribological testing at 100 degrees C using the ball-on-flat geometry, the resulting tribochemical films were imaged using scanning electron microscopy (SEM) and optical microscopy. The resulting tribochemical films have thicknesses around 50-100 nm. Two of the films corresponding to small (P1-imidazole-containing copolymer) and large (P3-less polar homopolymer) wear were cross-sectioned using focused ion beam (FIB) and analyzed for elemental composition using energy-dispersive X-Ray (EDX) mapping. Oxygen and nitrogen enrichment was observed, consistent with the relative chemical composition of the precursor polymers. Transmission electron microscopy (TEM) evidence suggests that at the worn surface, some organic elements penetrate or are mixed into the steel substrate giving an interlocking appearance. The two samples examined with TEM showed that P1 tribofilm is diffused or mixed with the steel substrate more so than P3, suggesting a stronger affinity and contact during tribofilm formation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Two-Photon Fluorescence Microscope for Microgravity Research

A two-photon fluorescence microscope has been developed for the study of biophysical phenomena. Two-photon microscopy is a novel form of laser-based scanning microscopy that enables three-dimensional imaging without many of the problems inherent in confocal microscopy. Unlike one-photon optical microscopy, two-photon microscopy utilizes the simultaneous nonlinear absorption of two near-infrared photons. However, the efficiency of two-photon absorption is much lower than that of one-photon absorption, so an ultra-fast pulsed laser source is typically employed. On the other hand, the critical energy threshold for two-photon absorption leads to fluorophore excitation that is intrinsically localized to the focal volume. Consequently, two-photon microscopy enables optical sectioning and confocal performance without the need for a signal-limiting pinhole. In addition, there is a reduction (relative to one-photon optical microscopy) in photon-induced damage because of the longer excitation wavelength. This reduction is especially advantageous for in vivo studies. Relative to confocal microscopy, there is also a reduction in background fluorescence, and, because of a reduction in Rayleigh scattering, there is a 4 increase of penetration depth. The prohibitive cost of a commercial two-photon fluorescence-microscope system, as well as a need for modularity, has led to the construction of a custom-built system (see Figure 1). This system includes a coherent mode-locked titanium: sapphire laser emitting 120-fs-duration pulses at a repetition rate of 80 MHz. The pulsed laser has an average output power of 800 mW and a wavelength tuning range of 700 to 980 nm, enabling the excitation of a variety of targeted fluorophores. The output from the laser is attenuated, spatially filtered, and then directed into a confocal scanning head that has been modified to provide for side entry of the laser beam. The laser output coupler has been replaced with a dichroic filter that reflects the longer-wavelength excitation light and passes the shorter-wavelength fluorescence light. Also, the confocal pinhole has been removed to increase the signal strength. The laser beam is scanned by a twoperpendicular- axis pair of galvanometer mirrors through a pupil transfer lens into the side port of an inverted microscope. Finally, the beam is focused by a 63-magnification, 1.3-numerical- aperture oil-immersion objective lens onto a specimen. The pupil transfer lens serves to match the intermediate image planes of the scanning head and the microscope, and its location is critical. In order to maximize the quality of the image, (that is, the point spread function of the objective lens for all scan positions), the entire system was modeled in optical-design software, and the various free design parameters (the parameters of the spatial-filter components as well as the separations of all of the system components) were determined through an iterative optimization process. A modular design was chosen to facilitate access to the optical train for future fluorescence correlation spectroscopy and fluorescence-lifetime experiments.

Fischer, David G.↗

Characterization of TiN, TiC and Ti(C,N) in titanium-alloyed ferritic chromium steels focusing on the significance of different particle morphologies

Titanium-alloyed ferritic chromium steels are a competitive option to classical austenitic stainless steels owing to their similar corrosion resistance. The addition of titanium significantly influences their final steel cleanliness. The present contribution focuses on the detailed metallographic characterization of titanium nitrides, titanium carbides and titanium carbonitrides with regard to their size, morphology and composition. The methods used are manual and automated Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy as well as optical microscopy. Additional thermodynamic calculations are performed to explain the precipitation procedure of the analyzed titanium nitrides. The analyses showed that homogeneous nucleation is decisive at an early process stage after the addition of titanium. Heterogeneous nucleation gets crucial with ongoing process time and essentially influences the final inclusion size of titanium nitrides. A detailed investigation of the nuclei for heterogeneous nucleation with automated Scanning Electron Microscopy proved to be difficult due to their small size. Manual Scanning Electron Microscopy and optical microscopy have to be applied. Furthermore, it was found that during solidification an additional layer around an existing titanium nitride can be formed which changes the final inclusion morphology significantly. These layers are also characterized in detail. Based on these different inclusion morphologies, in combination with thermodynamic results, tendencies regarding the formation and modification time of titanium containing inclusions in ferritic chromium steels are derived. - Graphical abstract: Display Omitted - Highlights: • The formation and modification of TiN in the steel 1.4520 was examined. • Heterogeneous nucleation essentially influences the final steel cleanliness. • In most cases heterogeneous nuclei in TiN inclusions are magnesium based. • Particle morphology provides important information on inclusion formation.

36 MATERIALS SCIENCE↗

Doppler optical coherence microscopy and tomography applied to inner ear mechanics

While it is clear that cochlear traveling waves underlie the extraordinary sensitivity, frequency selectivity, and dynamic range of mammalian hearing, the underlying micromechanical mechanisms remain unresolved. Recent advances in low coherence measurement techniques show promise over traditional laser Doppler vibrometry and video microscopy, which are limited by low reflectivities of cochlear structures and restricted optical access. Doppler optical coherence tomography (DOCT) and Doppler optical coherence microscopy (DOCM) both utilize a broadband source to limit constructive interference of scattered light to a small axial depth called a coherence gate. The coherence gate can be swept axially to image and measure sub-nanometer motions of cochlear structures throughout the cochlear partition. The coherence gate of DOCT is generally narrower than the confocal gate of the focusing optics, enabling increased axial resolution (typically 15 μm) within optical sections of the cochlear partition. DOCM, frequently implemented in the time domain, centers the coherence gate on the focal plane, achieving enhanced lateral and axial resolution when the confocal gate is narrower than the coherence gate. We compare these two complementary systems and demonstrate their utility in studying cellular and micromechanical mechanisms involved in mammalian hearing.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Preparation and characterization of novel foamed porous glass-ceramics

Foamed glass-ceramics without using foaming agent have been synthesized in a novel glass system of SrO-CaO-Al{sub 2}O{sub 3}-TiO{sub 2}-B{sub 2}O{sub 3}-SiO{sub 2}-P{sub 2}O{sub 5}-M{sub x}O{sub y} (where M = Ba, Mg, La, Ce and Ni) by a simple process of powder sintering. The glass and glass-ceramics are characterized by dilatometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), optical microscopy and Fourier transformed infrared spectroscopy (FTIR). All the glasses formed are amorphous and the glass transition temperature and dilatometric softening temperature of these glasses are found to be in the range 673–678 °C and 706–728 °C respectively. The glasses are highly stable as indicated by the DSC evaluated glass stability parameters of the range 195–240 °C. Quantitative sintering study of glass powder compacts revealed swelling in the samples with NiO and CeO{sub 2} corresponding to a geometry change of 75 and 108% around 900 °C respectively. With reference to this finding the glass powder compacts are heated to 900 °C and the foamed glass-ceramics are obtained. Characteristic crystalline silicate phases have been identified in the XRD studies and their microstructures are recorded by FESEM. Optical microscope study of the foamed samples revealed formation of bigger foamed cavity with residual pores in samples with NiO and CeO{sub 2} in comparison to samples with BaO, MgO and La{sub 2}O{sub 3}. The mean pore diameters of the samples with NiO and CeO{sub 2} are determined to be 43 and 32 μm, and their respective porosities are 2.34 and 1.82 cm{sup 3}/g respectively. Thus NiO and CeO{sub 2} are found to be very effective to obtain foamed glass-ceramics without using foaming agent by the viscous flow sintering of fine glass powder compacts along with the reduction of the respective polyvalent ions. - Highlights: • Synthesis of foamed porous glass-ceramics without foaming agent by sintering method • Only powder compact yielded foamed porous glass-ceramics but bulk glass did not. • Glasses containing NiO and CeO{sub 2} exhibited significant foaming efficiency. • Bloating of entrapped gas during viscous flow sintering is the origin of foaming. • Residual void created pores in the sintered glass-ceramics as evidenced in FESEM.

36 MATERIALS SCIENCE↗

Strontium‐Enriched Barite for Enhanced PbSO 4 Nucleation in Lead‐Acid Batteries

Abstract Barite (BaSO 4 ) crystals are an important additive in lead acid batteries due to their ability to promote the controlled nucleation and growth of anglesite (PbSO 4 ) during battery cycling. This is due to BaSO 4 ’s isostructural match with PbSO 4 , which facilitates epitaxial nucleation. However, BaSO 4 ’s efficacy as a nucleation promoter is limited by lattice mismatches between the two phases of 1–5%. Here, strontium‐enriched barite, (Ba,Sr)SO 4 , is synthesized to produce a nucleating promoter that displays an improved lattice match with PbSO 4 . Nucleation of PbSO 4 from Pb‐rich sulfuric acid solutions on strontium‐free and strontium‐enriched barite (up to 17 mol% Sr) is investigated using in‐situ atomic force microscopy and optical microscopy. At low strontium concentrations, PbSO 4 forms by the Stranski–Krastanov growth pathway (monolayer + island formation), with most nucleation occurring on edges and surface defects. At higher concentrations, the layer‐by‐layer growth mechanism known as Frank van‐der‐Merwe growth is observed, which allows for facile growth of continuous PbSO 4 films across the BaSO 4 surface. These films are successfully re‐dissolved on exposure to Pb‐free sulfuric acid. The results show that strontium incorporation fundamentally alters the mechanism of PbSO 4 nucleation on BaSO 4 , and thus provides a potential avenue for creating improved nucleation promoters in lead‐acid batteries.

Campbell, Colin T. [Pacific Northwest National Lab↗

Synthesis of porous Ti–50Ta alloy by powder metallurgy

Highlights: • The proposed preview milling with the next sintering enables the homogeneous porous Ti50Ta (wt).% alloy to be obtained • The α and β nanocrystalline phases were prepared by ball milling. • For the longest sintering time there is complete diffusion of preview milled initial powders • The press and sinter route is proved to be a promising alternative for melted Ti-based biomaterials. - Abstract: The aim of the present study was to assess the possibility of producing porous Ti50Ta (wt%) alloys using powder metallurgy by characterizing the material properties. The influence of the sintering time on the microstructure, mechanical properties, and corrosion behaviour of the produced alloy was investigated. The samples were examined using scanning electron microscopy (SEM), transmission electron microscopy (TEM), optic microscopy, X-ray diffraction (XRD) and nanoindentation methods. The XRD results confirmed that nanocrystalline α and β phases were formed during high-energy ball milling. A longer sintering time of 72 h allowed complete interdiffusion of the elements in the pre-milled initial powders. The sintering time significantly influenced the microstructure and porosity. Additionally, the corrosion resistance of the Ti-Ta samples in Ringer's solution was characterized and differences were observed between the samples sintered at different temperatures. The open-circuit potential (E{sub OCP}) and the corrosion potential (E{sub CORR}) of all samples were similar. The sintered Ti50Ta (wt%) alloy showed better corrosion resistance than equivalent Ti or Ta reference samples. We concluded that these alloys had suitable properties for medical implant applications in the future.

77 NANOSCIENCE AND NANOTECHNOLOGY↗