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At least 1,351 records · Page 75

Property Improvement in CZT via Modeling and Processing Innovations . Te-particles in vertical gradient freeze CZT: Size and Spatial Distributions and Constitutional Supercooling

A section of a vertical gradient freeze CZT boule approximately 2100-mm 3 with a planar area of 300-mm 2 was prepared and examined using transmitted IR microscopy at various magnifications to determine the three-dimensional spatial and size distributions of Te-particles over large longitudinal and radial length scales. The boule section was approximately 50-mm wide by 60-mm in length by 7-mm thick and was doubly polished for TIR work. Te-particles were imaged through the thickness using extended focal imaging to locate the particles in thickness planes spaced 15-µm apart and then in plane of the image using xy-coordinates of the particle center of mass so that a true three dimensional particle map was assembled for a 1-mm by 45-mm longitudinal strip and for a 1-mm by 50-mm radial strip. Te-particle density distributions were determined as a function of longitudinal and radial positions in these strips, and treating the particles as vertices of a network created a 3D image of the particle spatial distribution. Te-particles exhibited a multi-modal log-normal size density distribution that indicated a slight preference for increasing size with longitudinal growth time, while showing a pronounced cellular network structure throughout the boule that can be correlated to dislocation network sizes in CZT. Higher magnification images revealed a typical Rayleigh-instability pearl string morphology with large and small satellite droplets. This study includes solidification experiments in small crucibles of 30:70 mixtures of Cd:Te to reduce the melting point below 1273 K (1000°C). These solidification experiments were performed over a wide range of cooling rates and clearly demonstrated a growth instability with Te-particle capture that is suggested to be responsible for one of the peaks in the size distribution using size discrimination visualization. The results are discussed with regard to a manifold Te-particle genesis history as 1) Te-particle direct capture from melt-solid growth instabilities, 2) Te-particle formation from dislocation core diffusion and the formation and breakup of Te-tubes, and 3) Te-particle formation due to classical nucleation and growth as precipitates.

36 MATERIALS SCIENCE↗

Quaternary 2D Transition Metal Dichalcogenides (TMDs) with Tunable Bandgap [Quaternary Two-Dimensional (2D) Transition Metal Dichalcogenides (TMDs) with Tunable Bandgap]

Alloying/doping in 2D material is important due to wide range bandgap tunability. Increasing the number of components would increase the degree of freedom which can provide more flexibility in tuning the bandgap and also reduces the growth temperature. Here, synthesis of quaternary alloys Mo x W 1– x S 2 y Se 2(1– y ) is reported using chemical vapor deposition. The composition of alloys is tuned by changing the growth temperatures. As a result, the bandgap can be tuned which varies from 1.61 to 1.85 eV. In conclusion, the detailed theoretical calculation supports the experimental observation and shows a possibility of wide tunability of bandgap.

2D materials↗

Size‐Tunable Synthesis of Hollow Gold Nanospheres through Control of Reaction Temperature

Here, it is demonstrated that the size tunable hollow gold nanospheres (HGNs) of ≈24–122 nm in diameter can be facilely achieved by controlling a signal parameter, reaction temperature, in the synthesis. The varied particle sizes of HGNs result in highly tunable surface plasmon resonance (SPR) absorption in the entire visible to near infrared region of the spectrum, with maximum peak position from 565 to 850 nm when the reaction temperature is varied from 80 to 10 °C. The particle size and structural properties are determined using dynamic light scattering, transmission‐mode scanning electron microscopy, and high‐resolution transmission electron microscopy. The optical properties are characterized using UV–vis spectroscopy. A mechanism behind the temperature‐dependent HGN synthesis is explained by the thermodynamics of homogeneous nuclei formation of the cobalt scaffold. Discrete dipole approximation calculations are performed to simulate the SPR spectrum and provide insight into the relation between the SPR absorption and structural details of the HGNs. This study demonstrates a simple yet effective method based on temperature control for synthesizing produce size tunable HGNs with varying properties of interest for different applications.

Pu, Ying‐Chih↗

Effects of Laser-Cutting and Spark Erosion Techniques and Heat Treatment on the Magnetic Properties of Grain-Oriented Transformer Steels

Spark erosion and laser-cutting processes were examined in terms of their effects on the magnetic properties of grain-oriented electrical steels at working frequencies. The maximum permeability value in each case was considered a reference to determine the quantitative effect of cutting and eroding methods as well as the effects of heat treatment. To minimize the deterioration that appears after the piercing process is implemented, the specimens were subjected to heat treatment at the most appropriate temperature. The influence of stress-relief annealing could be observed throughout the domain refinement on the surface by using magneto-optical Kerr microscopy. Additionally, it was clearly seen that the domain contrast at the cut edge of the spark-eroded sample was more uniform than that provided by laser cutting upon applying a high AC-field amplitude.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Transient Oxidation of a γ-Ni-28Cr-11Al Alloy

γ-NiCrAl alloys with relatively low Al contents tend to form a layered oxide scale during the early stages of oxidation, rather than an exclusive α-A l2 O 3 scale, the so-called 'thermally grown oxide' (TGO). A layered oxide scale was established on a model γ-Ni-28Cr-11Al (at.%) alloy after isothermal oxidation for several minutes at 1100 °C. The layered scale consisted of an NiO layer at the oxide/gas interface, an inner Cr 2 O 3 layer, and an α-Al 2 O 3 layer at the oxide/alloy interface. The evolution of such an NiO/Cr 2 O 3 /Al 2 O 3 layered structure on this alloy differs from that proposed in earlier work. During heating, a Cr 2 O 3 outer layer and a discontinuous inner layer of Al 2 O 3 initially formed, with metallic Ni particles dispersed between the two layers. A rapid transformation occurred in the scale shortly after the sample reached maximum temperature (1100°C), when two (possibly coupled) phenomena occurred: (i) the inner transition alumina transformed to α-Al 2 O 3 , and (ii) Ni particles oxidized to form the outer NiO layer. Subsequently, NiO reacted with Cr 2 O 3 and Al 2 O 3 to form spinel. Continued growth of the oxide scale and development of the TGO was dominated by growth of the inner α-Al 2 O 3 layer.

36 MATERIALS SCIENCE↗

Enhancing the Range and Reliability of the Spacer Layer Imaging Method

The spacer layer imaging method (SLIM) is widely used to measure the thickness of additive and lubricant films, in lubricant development and evaluation, and for fundamental research into elastohydrodynamic lubrication and tribofilm formation mechanisms. The film thickness measurement, as implemented on several popular tribometers, provides powerful, non-destructive in-situ mapping of film topography with nanometre-scale height sensitivity. However, the results can be highly sensitive to experimental procedure, machine condition, and image analysis, in some cases reporting unphysical film thickness trends. The prevailing image analysis techniques make it challenging to interrogate these errors, often hiding their multivariate nonlinear behaviour from the user by spatial averaging. Herein, several common ‘silent errors’ in the SLIM measurement, including colour matching to incorrect fringe orders, and colour drift due to the optical properties of the system or film itself, are discussed, with examples. A robust suite of novel a priori and a posteriori methods to address these issues, and to improve the accuracy and reliability of the measurement, are also presented, including a novel, computationally inexpensive circle-finding algorithm for automated image processing. In combination, these methods allow reliable mapping of films up to at least 800 nm in thickness, representing a significant milestone for the utility of SLIM applied to elastohydrodynamic contact.

EHL film geometry↗

Acquisition of Real-Time Operation Analytics for an Automated Serial Sectioning System

Mechanical serial sectioning is a highly repetitive technique employed in metallography for the rendering of 3D reconstructions of microstructure. While alternate techniques such as ultrasonic detection, micro-computed tomography, and focused ion beam milling have progressed much in recent years, few alternatives provide equivalent opportunities for comparatively high resolutions over significantly sized cross-sectional areas and volumes. To that end, the introduction of automated serial sectioning systems has greatly heightened repeatability and increased data collection rates while diminishing opportunity for mishandling and other user-introduced errors. Unfortunately, even among current, state-of-the-art automated serial sectioning systems, challenges in data collection have not been fully eradicated. Therefore, this paper highlights two specific advances to assist in this area; a non-contact laser triangulation method for assessment of material removal rates and a newly developed graphical user interface providing real-time monitoring of experimental progress. Furthermore, both are shown to be helpful in the rapid identification of anomalies and interruptions, while also providing comparable and less error-prone measures of removal rate over the course of these long-term, challenging, and innately destructive characterization experiments.

36 MATERIALS SCIENCE↗

Tribological behavior of N-doped ZnO thin films by metal organic chemical vapor deposition under lubricated contacts

N-doped ZnO thin films were deposited on 304L stainless steel through the pyrolysis of zinc acetate and ammonium acetate in different ratios at a temperature of 420 degrees C using metal organic chemical vapor deposition. Compositional and structural analyzes of the films were performed by using Rutherford backscattering spectroscopy and X-ray diffraction. The frictional behavior of the thin films and 304L stainless steel substrate was evaluated using a ball-on-flat configuration with reciprocating sliding under marginally lubricated and fully flooded conditions. Al alloy (2017) was used as ball counterface, while basestock synthetic polyalfaolefin oil (PAO10) without additives was used as lubricant. The flat and ball counterface surfaces were examined to assess the wear dimension and failure mechanism. Under marginally lubricated condition, N-doped ZnO thin films provided significant reduction in friction, whereas the films have minimal or no effect in friction under fully flooded condition. N-doped ZnO thin films showed a significant effect in protecting the ball counterface as wear volume was reduced compared with that of the substrate under the marginally lubricated condition. Under the fully flooded condition, with the exception of one of the films, the wear volume of the N-doped ZnO thin films ball reduced compared with that of the substrate. In all the ball counterfaces for N-doped ZnO thin films under both conditions, wear occurred through abrasive mechanism of various degrees or mild polishing. Thus, superfluous lubrication of N-doped ZnO thin films is not necessary to reduce friction and wear.

36 MATERIALS SCIENCE↗

Effect of microstructure on air oxidation resistance of nuclear graphite

Oxidation resistance in air of three grades of nuclear graphite with different structures was compared using a standard thermogravimetric method. Differences in the oxidation behavior have been identified with respect to both (i) the rate of oxidation in identical conditions and the derived apparent activation energy and pre-exponential factor and (ii) the penetration depth of the oxidant and the development of the oxidized layer. These differences were ascribed to structural differences between the three graphite grades, in particular the grain size and shape of the graphite filler, and the associated textural properties, such as total BET surface area and porosity distribution in the un-oxidized material. It was also found that the amount of strongly bonded surface oxygen complexes measured by thermodesorption significantly exceeds the amount afforded by the low BET surface area, and therefore low temperature oxygen chemisorption is not a reliable method for determining the amount of surface sites (re)active during air oxidation. The relationship between nuclear graphite microstructure and its oxidation resistance demonstrated in this work underlines the importance of performing comprehensive oxidation characterization studies of the new grades of nuclear graphite considered as candidates for very high temperature gas-cooled reactors.

36 MATERIALS SCIENCE↗

Application of Electron Backscatter Diffraction to evaluate the ASR risk of concrete aggregates

Alkali-Silica Reaction (ASR) is a frequent cause of reduced concrete durability. Eliminating the application of alkali reactive aggregates would reduce the quantity of ASR concrete deterioration in the field. This study introduces an Electron Backscatter Diffraction (EBSD) technique to distinguish the ASR risk of slow-late reacting aggregates by measuring microstructural properties of quartz. Quantifying the amount of quartz grain boundaries and the associated misorientation of grains can thereby be used to differentiate microstructures bearing an ASR risk. It is also shown that dissolution of quartz in high pH environments occurs along quartz grain and subgrain boundaries. Results of EBSD analysis are compared with ASR performance testing on concrete prisms and optical light microscopy characterization of quartz microstructure. EBSD opens new possibilities to quantitatively characterize microstructure of quartz in concrete aggregates with respect to ASR. This leads to a better understanding on the actual cause of ASR.

36 MATERIALS SCIENCE↗

Metallurgical alloy approach to two-dimensional supramolecular materials

Alloys are normally mixtures of metallic elements used to search for superior functional properties compared with their individual components. Although a quintessential approach to better materials in metallurgy, the concept of alloying has been expanded to other inorganic materials and covalent polymers. In this work, we report on alloy formation of small organic molecules structured as amphiphilic chromophores in water. Using X-ray scattering, microscopy, and optical spectroscopy, we unambiguously demonstrate the formation of supramolecular alloys with changes in physical, photophysical, and mechanical properties. Additionally, we identify single-crystalline, two-dimensional supramolecular polymers containing multiple molecular species, analogous to intermetallic compounds. The mechanism of alloy formation suggests the possibility of controlled growth in these supramolecular assemblies to create emergent functional structures.

36 MATERIALS SCIENCE↗

In situ characterization of phase transformations in petroleum pitch by high temperature X-ray diffraction

The phase transformation from isotropic to mesophase of a petroleum-derived pitch was monitored by in situ X-ray diffraction at 410 °C. The kinetics of the transformation were characterized by monitoring the growth of a broad peak at 2θ~24° and could be described by Avrami’s equation. The volatilization of low molecular weight components originally present in the pitch, or produced during the condensation reaction, was assessed by thermal gravimetry analysis, following the same thermal history. Ex situ characterizations of the pitch precursor before and after thermal treatment provided insight into the evolution of the molecular structure associated with mesophase generation (optical polarized microscopy, molecular weight distribution by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, X-ray photoelectron spectroscopy, Auger spectroscopy, and thermal stability). Here, this investigation demonstrates the value of using complementary in situ and ex situ experimental techniques to characterize complex mechanisms during the processing of organic materials.

02 PETROLEUM↗

Friction and wear behavior of nitrogen-doped ZnO thin films deposited via MOCVD under dry contact

Most researches on doped ZnO thin films are tilted toward their applications in optoelectronics and semiconductor devices. Research on their tribological properties is still unfolding. In this work, nitrogen-doped ZnO thin films were deposited on 304 L stainless steel substrate from a combination of zinc acetate and ammonium acetate precursor by MOCVD technique. Compositional and structural studies of the films were done using Rutherford Backscattering Spectroscopy (RBS) and X-ray Diffraction (XRD). The frictional behavior of the thin film coatings was evaluated using a ball-on-flat configuration in reciprocating sliding under dry contact condition. After friction test, the flat and ball counter-face surfaces were examined to assess the wear dimension and failure mechanism. In conclusion, both friction behavior and wear (in the ball counter-face) were observed to be dependent on the crystallinity and thickness of the thin film coatings.

36 MATERIALS SCIENCE↗

Evaluation of post-weld heat treatments applied to FeCrAl alloy weldments

The nuclear incident at the Fukushima Daiichi nuclear power plant has created a strong push for accident-tolerant fuel cladding to replace current zirconium-based cladding. A current near-term focus on iron-chromium-aluminum (FeCrAl) alloys. Laser-welded FeCrAl samples (C35MN, C37M, and C35M10 TC) were subjected to three different post-weld heat treatment regimes: 650 °C for 5 h, 850 °C for 1 h, and 850 °C for 5 h. Here, the samples were then analyzed using optical light microscopy, micro-hardness indentation, and scanning electron microscopy coupled with energy-dispersive spectroscopy and electron backscatter diffraction. The base microstructure of C37M and C35M10 TC experienced significant grain coarsening outside the fusion zone due to the applied post-weld heat treatments, whereas Nb-rich precipitation in C35MN limited grain growth compared with the other alloys studied.

36 MATERIALS SCIENCE↗

Surface composition, microstructure and corrosion resistance of AZ31 magnesium alloy irradiated by high-intensity pulsed ion beam

High-intensity pulsed ion beam (HIPIB) irradiation of AZ31 magnesium alloy is performed and electrochemical corrosion experiment of irradiated samples is carried out by using potentiodynamic polarization technology in order to explore the effect of HIPIB irradiation on corrosion resistance of magnesium alloy. The surface composition, cross-sectional morphology and microstructure are characterized by using electron probe microanalyzer, optical microscope and transmission electron microscope, respectively. The results indicated that HIPIB irradiation leads to a significant improvement in corrosion resistance of magnesium alloy, in terms of the considerable increase in both corrosion potential and pitting breakdown potential. The microstructural refinement and surface purification induced by HIPIB irradiation are responsible for the improved corrosion resistance. - Research Highlights: {yields} A modified layer about 30 {mu}m thick is obtained by HIPIB irradiation. {yields} Selective ablation of element/impurity phase having lower melting point is observed. {yields} More importantly, microstructural refinement occurred on the irradiated surface. {yields} The modified layer exhibited a significantly improved corrosion resistance. {yields} Improved corrosion resistance is ascribed to the combined effect induced by HIPIB.

36 MATERIALS SCIENCE↗

Sol-gel preparation and characterization of Er3+ doped TiO2 luminescent nanoparticles

Highlights: • Sol-gel derived Er{sup 3+} doped TiO{sub 2} nanoparticles for potential use in solar cells and bio imaging. • Influence of Er{sup 3+} doping into TiO{sub 2} with various Er{sup 3+} concentration on structural, optical, and luminescence properties. • Down-and up-conversion luminescence behaviour of Er{sup 3+} doped titanium dioxide. - Abstract: The present paper reports on down-and up-conversion luminescence behaviour of sol-gel derived erbium doped titanium dioxide with anatase structure. Through combined structural, optical and electron microscope analysis, effective and influence of Er{sup 3+} doping into TiO{sub 2} lattice has been demonstrated using X-Ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and optical reflectance spectra. XRD results showed only anatase diffraction peaks of TiO{sub 2}, indicating the formation of a pure anatase phase even after Er{sup 3+} incorporation into TiO{sub 2} lattice. Selected Area Electron Diffraction (SAED) confirmed that the synthesized TiO{sub 2} nanoparticles are polycrystalline in nature which correlated well with XRD findings. Upon excitation at 320 nm, two down-conversion contributions at 378 nm and 435 nm attributed to indirect band gap and defect-related emissions, respectively were observed from both pure and Er{sup 3+} doped TiO{sub 2} nanoparticles. On the other hand, strong green up-conversion emission centred at 544 nm ascribed to {sup 4}S{sub 3/2 }→ {sup 4}I{sub 15/2} transition of Er{sup 3+} was observed under 980 nm laser excitation for all Er{sup 3+} doped TiO{sub 2} samples. This result analysis brings insight on understanding of structural, optical and luminescence properties of Er{sup 3+} doped TiO{sub 2} nanoparticles for use in solar cells and bio imaging devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗