Transmission Electron Microscopy Investigations Research Articles

Creep-induced redistribution of alloying elements in CZ1 zirconium alloys

Introducing minor alloying elements is an effective strategy to improve the corrosion and mechanical properties of zirconium alloys for nuclear applications. During in-reactor service, external environment and stress can affect the distribution of alloying elements, substantially changing the degradation process of zirconium alloys. To date, there is a lack of in-depth understanding of the interaction between creep and microchemistry changes. Here, we conducted systematic transmission electron microscopy (TEM) and atom probe tomography (APT) investigations to address creep-induced redistribution of alloying elements in CZ1 (Zr-Sn-Nb-Fe-Cr-Cu) zirconium alloy with different initial microstructures. Nb, Fe, Sn, and Cu are found to co-segregate at grain boundaries. The higher the intermediate annealing temperature, the larger the Gibbsian interfacial excesses of solute elements are. We further demonstrate that creep can reduce the excess value of Fe at grain boundaries due to the coarsening of Zr-Fe-Cr second phase particles via grain boundary and dislocation pipe diffusion. At the same time, the excess value of Sn is increased by diffusing from the matrix to grain boundaries. Moreover, Cu as a minor element in the concentration range of 0.05–0.3 wt.% is found to segregate at dislocations to form the Cottrell atmosphere and develop Cu-rich nanoclusters for suppressing dislocation motion. The new understanding of the segregation and clustering of minor alloying elements provides guidance for developing zirconium alloys with enhanced creep resistance.

Exsolution of oxygen impurity from diamond lattice and formation of pressurized CO2-I precipitates

Diamond single crystals showing Infra-red features of pressurized CO2-I phase were studied using Transmission Electron Microscopy (TEM) and tomography. Numerous O-containing precipitates with sizes up to 45 nm are observed. The absolute majority of these precipitates decorate dislocation loops or are located inside them; individual scattered precipitates are also present. Morphology of the precipitates varies from quasi-isometric octahedra to highly flattened elongated ones. Close association of the precipitates with the dislocation loops implies their formation by exsolution of oxygen impurity from diamond lattice; the size distribution of the precipitates suggests that the equilibrium state is not yet reached. Presumably, the morphology and precise chemical composition depend on P-T-t evolution of the diamond crystal and corresponding changes in oxygen supersaturation in the lattice. The CO2-containing diamonds often contain micron-sized hexagonal lamellar inclusions. TEM investigation of a lamellae reveals that it consists of high quality graphite showing partial epitaxial relation with comprising diamond. The gap between the graphite and diamond may be enriched with oxygen impurity.

Reverse Engineering Analysis of Optical Properties of (Ti,Cu)Ox Gradient Thin Film Coating

Analysis of the optical properties of a gradient (Ti,Cu)Ox thin film is presented in this paper. The thin film was prepared using reactive co-sputtering of Ti and Cu targets. The desired elemental concentration profiles of Cu and Ti versus the thin film thickness were obtained by changing the power delivered to the magnetron equipped with Cu, while the powering of the magnetron equipped with the Ti target was maintained at a constant level during the film deposition. Optical properties were analysed using the reverse engineering method, based on simultaneously measured optical transmittance and reflectance. Detailed microstructure analysis performed using transmission electron microscopy investigations revealed that the thin film consisted of at least four areas with different structural properties. Finding a satisfying fit of theoretical to experimental data required taking into account the heterogeneity in the material composition and microstructure in relation to the depth in the prepared gradient thin film. On the basis of the built equivalent layer stack model, the composition profile and porosity at the cross-section of the prepared gradient film were evaluated, which agreed well with the obtained elemental and microscopy studies.

Green Synthesis of Au-doped SnO 2 Nanoparticles Using Teucrium Polium Plant Extract for the Evaluation of Their Physicochemical and Antibacterial Properties

Background & Objective: The biological production of nanoparticles (NPs) is a technique that has garnered a lot of interest because it is inexpensive, straightforward, and friendly to the natural environment. This study explores the green synthesis of Au-doped SnO 2 NPs using Teucrium polium plant extract and evaluates their antimicrobial properties in comparison with two commonly used antibiotics.
 Materials & Methods: Initially, an extract of Teucrium polium was made using water, and then it was combined with solutions of tin (II) chloride dehydrate [SnCl 2 .2H 2 O] and gold (III) chloride trihydrate [HAuCl 4 .3H 2 O]. The crystal structure was studied using X-ray diffraction (XRD). The form, structure, and grain size of the NPs were analyzed using scanning electron microscope (SEM) and transmission electron microscope (TEM). The synthesized NPs were tested for their antibacterial properties.
 Results: The XRD and EDS analyses revealed that the SnO 2 : Au phase formed an average crystallite size of 22 nm and an Au dopant content of around 2%. The SEM and TEM investigations demonstrated that the NPs were formed in a regular and nanoscale manner, with diameters ranging from 25 to 30 nm. MIC and MBC of SnO 2 : Au NPs against the studied bacteria (S.aureus ATCC 43300, P.aeruginosa PAO1) were reported 9.6±0.13- 9.6±0.07 μg/mL and 25.9±11.5- 32.5±11.2 μg/mL.
 Conclusion: Green-synthesized NPs exhibit significant antimicrobial activity against both Gram-positive and Gram-negative bacteria, even at low concentrations. The NPs effectively eliminate bacteria and prevent biofilm formation.

Optimal Concentration and Duration of Endotracheal Tube Coating to Achieve Optimal Antimicrobial Efficacy and Safety Balance: An In Vitro Study

Ventilator-associated pneumonia (VAP) is a common and genuine complication in fundamentally sick patients accepting mechanical ventilation. Silver nitrate sol-gel (SN) has been proposed as a potential preventative measure against VAP. Be that as it may, the arrangement of SN with distinctive concentrations and pH values remains a basic factor influencing its effectiveness. Silver nitrate sol-gel was arranged with distinctive concentrations (0.1852%, 0.03496%, 0.1852%, and 0.01968%) and pH values (8.5, 7.0, 8.0, and 5.0) separately. The antimicrobial action of the silver nitrate and NaOH arrangements were assessed against Escherichia coli as a reference strain. The thickness and pH of the arrangements were measured, and biocompatibility tests were performed on the coating tube. The auxiliary changes in the endotracheal tube (ETT) tests after treatment were analyzed utilizing electron microscopy (SEM) and transmission electron microscopy (TEM). The pH estimations of the diverse arrangements showed that the pH values shifted depending on the test conditions, with pH values extending from 5.0 to 8.5. The consistency estimations of the arrangements showed that the thickness values expanded as the pH values drew closer to 7.5 and diminished when the pH values went over 7.5. The antimicrobial action of the silver nitrate and NaOH arrangements were successful against Escherichia coli, with microbial checks decreasing in concentration (0.03496%, 0.1852% (pH: 8), and 0.01968%). The biocompatibility tests revealed tall cell reasonability rates, demonstrating that the coating tube was secure for therapeutic utilization and did not hurt typical cells. The SEM and TEM investigation gave visual proof of the antibacterial impacts of the silver nitrate and NaOH arrangements on the bacterial surface or interior of the bacterial cells. Moreover, the investigation revealed that a concentration of 0.03496% was the foremost successful in hindering the development of ETT bacterial colonization at the nanoscale level. We propose that cautious control and alteration of the pH and thickness of the arrangements are essential to guaranteeing the reproducibility and quality of the sol-gel materials. The silver nitrate and NaOH arrangements may serve as a potential preventative degree against VAP in sick patients, with a concentration of 0.03496% appearing to show the most elevated viability. The coating tube may serve as a secure and viable preventative measure against VAP in sick patients. Further investigation is required to optimize the concentration and introduction time of the arrangements to maximize their adequacy in avoiding VAP in real-world clinical settings.

Molten salt synthesis and formation mechanism of Ti3AlC2: A new path from Ti2AlC to Ti3AlC2

AbstractFine, pure Ti3AlC2 powder is prepared in a very mild condition via Ti3Al alloy and carbon black with the assistance of molten salts. X‐ray diffraction, scanning electron microscopy, TG‐DSC, and transmission electron microscopy (TEM) characterizations show that the high purity, nanosized Ti3AlC2 can be obtained at 900°C with the 1:1 salt‐to‐material ratio. The formation mechanism of Ti3AlC2 through this strategy of alloy raw material is fully studied under further TEM investigations, showing that the reaction process can basically be described as Ti3Al and C → TiAl and TiC → Ti2AlC and TiC → ψ and TiC → Ti5Al2C3 and TiC → Ti3AlC2, where the key ψ, a modulated Ti2AlC structure, is determined for the first time containing alternate‐displacement Al layers along (0 0 0 2) of Ti2AlC phase with a distinct selected area electron diffraction pattern. Such alternant displacement is considered a precondition of forming Ti5Al2C3 through topotactic transition, followed by Ti5Al2C3 converting into Ti3AlC2 by the diffusion of Ti, C atoms in the outside TiC. Several parallel orientations can be observed through the phase transition process: Ti2AlC (0 0 0 2)//ψ (0 0 0 1), ψ (0 0 0 1)//Ti5Al2C3 (0 0 0 3), Ti5Al2C3 (0 0 0 3)//Ti3AlC2 (0 0 0 2). Such parallel orientations among these phases apply an ideal condition for the topotactic reaction. The distinct path of the phase transition brings a significant change of heat effect compared with the traditional method, leading to a fast reaction rate and a mild reaction condition.

Irradiation-enhanced Interactions at UO2/Al2O3/Al Interfaces

Combustion synthesis is used to prepare thin UO2 films on aluminum alloy substrates. This simple preparation method involves electrospraying uranyl nitrate + acetylacetone + 2-methoxyethanol solution on the substrate, followed by a short annealing at 350 or 550 °C. The irradiation of films with a 40Ar2+ ion beam (energy of 1.7 MeV and fluences of 7.7 × 1016 and 1.3 × 1017 ions/cm2) is conducted to investigate irradiation-induced restructuring processes. High-resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) investigations show that the annealing temperature significantly influences the crystallinity and stability of materials during irradiation. A small amount of Mg in the alloy substrate diffuses into the amorphous Al2O3 interfacial layer between the film and the substrate. Local thermal spikes from the incoming ions facilitate the irradiation-induced mixing of immiscible Al2O3 and UO2 for the materials prepared at 350 °C. This mass diffusion produces relatively large cavities at the interface. Selective diffusion of a more significant amount of Mg for the materials prepared at 550 °C suppresses the mixing of the Al2O3 interlayer with the film but forms MgyU1–yO2±x solid solutions during irradiation. Local thermal heating triggers the precipitation of a discontinuous crystalline MgO layer close to the film surface. The enhanced and selective diffusion of Mg into the film makes the materials prepared at 550 °C more robust and mechanically stable than those prepared at 350 °C.

Hot-rolled Al-added medium Mn steel (Fe-8Mn-2.85Al-1Si-0.2C): Microstructural evolution and tensile behavior

In this study, a low Al (<3%) added medium manganese steel has been developed through melting casting route in an open-air induction furnace. The cast steel ingot has been intercritical annealed at 720 °C after hot deformation, that includes hot forging and hot rolling treatment, respectively. Microstructure characterization coupled with X-ray diffraction (XRD) has been performed after each processing step to understand the extent of austenite formation and its subsequent transformation to ferrite/martensite. The processed steel possesses the ultimate tensile strength, yield strength and ductility of 1000±20 MPa,700±10 MPa and 18.5 ± 0.5, respectively. To understand the possible cause of enhanced strength and deformation mode rietveld analysis has been carried out. It reveals that developed (final processed) steel possesses ∼18% (volume%) of austenite that subsequently reduced to ∼6.139% after tensile testing, indicating significant transformation of austenite to martensite (continuous and enhanced TRIP effect). The morphological characteristic of martensite in developed steel has been investigated using transmission electron microscopy (TEM). It reveals lath morphology of martensite due to low carbon content. The TEM and 3D atom probe analysis reveals the precipitation of intergranular type kappa (k) carbide in intercritically annealed specimens due to probable segregation of C and Al. However, volume fraction of the same is low. The SFE of the steel has been found to be ∼16 mJ m− 2, calculated by the modified Olson and Cohen method that also concludes TRIP is the preferred deformation mechanism in the developed steel.

Quercetin-loaded Liposomes Effectively Induced Apoptosis and Decreased the Epidermal Growth Factor Receptor Expression in Colorectal Cancer Cells: An In Vitro Study.

Quercetin is a flavonoid having anti-cancer properties; however, it has low stability, insufficient bioavailability, and poor solubility. This study aimed to load quercetin on nanoliposomes to enhance its efficiency against SW48 colorectal cancer cells. The cytotoxicity of free-quercetin and quercetin-loaded nanoliposomes on the expression of the epidermal growth factor receptor (EGER) gene was investigated. This present in vitro study was conducted at Yasuj University of Medical Sciences (Yasuj, Iran) in 2021. In this in vitro study, the lipid thin-film hydration method was used to synthesize quercetin-loaded liposomes. Additionally, high-performance liquid chromatography (HPLC) analyses, dynamic light scattering (DLS), and transmission electron microscopy (TEM) investigations were used to characterize nanomaterials. Following that, MTT, flow cytometry, and real-time PCR were used to investigate the cytotoxicity of quercetin-loaded liposomes on the colorectal cancer cells SW48 cell line, the incidence of apoptosis, and the expression of the EGFR gene in these cells. Statistical analysis was performed using the SPSS (version 26.0), and the graphs were created with the GraphPad Prism version 8.4.3. P<0.05 was considered statistically significant. The nanoparticles were spherical, homogenous, and 150±10 nm in size. According to HPLC, Quercetin had a 98% loading capacity. Although both free quercetin and quercetin-loaded liposomes indicated significant cytotoxicity against cancer cells (P˂0.001), the combined form was significantly more active (P=0.008). 50 µg/mL of this compound reduced the viability of SW48 cells by more than 80% (IC50 10.65 µg/mL), while the viability of cells treated with free quercetin was only 66% (IC50 18.74 µg/mL). The apoptosis was nearly doubled in the cells treated with quercetin-loaded nanoliposomes compared to free quercetin (54.8% versus 27.6%). EGFR gene expression, on the other hand, was significantly lower in cells treated with quercetin-loaded liposomes than the quercetin alone (P=0.006). When combined with nanoliposomes, quercetin had greater anti-proliferative, apoptotic, and anti-EGFR expression than free quercetin.

Formation of nanocrystalline AZ31B Mg alloys via cryogenic rotary swaging

A bulk nanocrystalline AZ31B Mg alloy with extraordinarily high strength was prepared via cryogenic rotary swaging in this study. The obtained alloy shows finer grains, higher strength, and a negligible tension-compression yield asymmetry, compared with that prepared via room-temperature rotary swaging. Transmission electron microscopy investigations showed that at the initial stage, multiple twins, mostly tension twins, were activated and intersected with each other, thereby refining the coarse grains into a fine lamellar structure. Then, two types of nanoscale subgrains were generated with increasing swaging strain. The first type of nanoscale subgrain contained twin boundaries and low-angle grain boundaries. This type of subgrain appeared at the twin-twin intersections and was mainly driven by high local stress. The second type of nanoscale subgrain was formed within the twin lamellae. The boundaries of this type of subgrain did not contain twin boundaries and were transformed from massive dislocation arrays. Finally, randomly oriented nanograins were obtained via dynamic recrystallization, under the combined function of deformation heat and increased stored energy. Compared with room-temperature rotary swaging, cryogenic rotary swaging exhibits a slower grain refinement process but a remarkably enhanced grain refinement effect after the same five-pass swaging.

Influence of thermo-mechanical treatment in austenitic and ferritic field condition on microstructural and mechanical properties of reduced activation ferritic-martensitic steel

Abstract 9Cr-1W-0.06Ta reduced activation ferritic-martensitic (RAFM) steel has been investigated in normalized and tempered (N + T) condition and in thermo-mechanically treated (TMT) in austenitic and ferritic field conditions. RAFM steel in N + T condition has a tempered martensitic structure (body-centred tetragonal, bct). It is unstable and will transfer into a stable body-centered cubic (bcc) in the structure during a long period subjected to high temperatures. To make it stable structure, the steel was subjected to austenitization at 1423 K for 10 min, and then cooled in still air (≈−1 K s−1) to 973 K and this temperature was maintained for 2 h in furnace to fully convert austenite into ferritic phase then the steel was subjected to 25% reduction in thickness by hot rolling. Optical, scanning and transmission electron microscopic investigations have been carried out to assess the microstructural changes of the steel N + T and TMT conditions. Hardness, tensile and creep studies are carried out and the results were correlated with the microstructural studies. TMT processed steel resulted in coarser prior austenite grains and exhibited ferrite in phase with fine distribution of M 23C6 and MX precipitates whereas N + T condition is subjected to tempered martensitic structure with coarser M 23C6 and MX precipitates. Even though ferrite phase present in TMT processed steel it exhibits higher tensile and creep strengths due to the presence of high dislocations and finer distribution of precipitates than the N + T condition.

Impedance Spectroscopy on Hafnium Oxide‐Based Memristive Devices

AbstractMemristive devices for neuromorphic computing have been attracting ever growing attention over the last couple of years. In neuromorphic electronics, memristive devices with multi‐level resistance states are required to accurately reproduce synaptic weights. Here, a memristive device based on a multilayer oxide system (Nb/NbOx/Al2O3/HfO2/Au), which features a filamentary‐free, homogenous interfacial resistive switching mechanism, is investigated. To gain a deeper insight into the switching mechanism, impedance spectroscopy (ImpSpec), X‐ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) are exploited. While this work focuses on the analysis of impedance and current‐voltage characteristics, XPS and TEM investigations can be found in a companion paper (Zahari et al.). In the course of this investigation, potentiodynamic impedance spectroscopy (PD‐ImpSpec) and time resolved impedance spectroscopy (TR‐ImpSpec) in combination with transient analysis are used. Evidence is presented of switching kinetics at voltages above 2.1 V directly related to changes in Schottky barrier resistance. These switching kinetics can in turn be interpreted by the charging and discharging of double positively charged oxygen vacancies ≈ 0.9 eV. The results of the impedance analysis are translated into a more general model for memristive devices to map the physical processes during switching.

Electron Ptychographic Phase Imaging of Beam-sensitive All-inorganic Halide Perovskites Using Four-dimensional Scanning Transmission Electron Microscopy.

Halide perovskites (HPs) are promising candidates for optoelectronic devices, such as solar cells or light-emitting diodes. Despite recent progress in performance optimization and low-cost manufacturing, their commercialization remains hindered due to structural instabilities. While essential to the development of the technology, the relation between the microscopic properties of HPs and the relevant degradation mechanisms is still not well understood. The sensitivity of HPs toward electron-beam irradiation poses significant challenges for transmission electron microscopy (TEM) investigations of structure and degradation mechanisms at the atomic scale. However, technological advances and the development of direct electron cameras (DECs) have opened up a completely new field of electron microscopy: four-dimensional scanning TEM (4D-STEM). From a 4D-STEM dataset, it is possible to extract not only the intensity signal for any STEM detector geometry but also the phase information of the specimen. This work aims to show the potential of 4D-STEM, in particular, electron exit-wave phase reconstructions via focused probe ptychography as a low-dose and dose-efficient technique to image the atomic structure of beam-sensitive HPs. The damage mechanism under conventional irradiation is described and atomically resolved almost aberration-free phase images of three all-inorganic HPs, CsPbBr3, CsPbIBr2, and CsPbI3, are presented with a resolution down to the aperture-constrained diffraction limit.

Transmission electron microscopy investigation of phase transformation and fuel constituent redistribution in neutron irradiated U-10wt.%Zr fuel

Uranium-10 wt.% zirconium (U-10 wt.%Zr) is a primary candidate for fast reactor nuclear fuels. However, there is a lack of data characterizing the crystallographic phases and chemistry of the neutron irradiated fuel. In the current study, the microstructural evolution of a U-10 wt.%Zr fuel neutron irradiated to a burnup of 5.7 at.% was investigated using scanning transmission electron microscopy, energy dispersive X-ray spectroscopy, and selected area electron diffraction to determine the major phases, alterations in microstructure, and variations in local chemical composition at different localities of a fuel cross-section. The current study revealed that the irradiated U-10 wt.%Zr fuel was comprised of various major phases, including α-U, β-U, and δ-UZr2, as well as amorphous and crystalline solid fission product (FP) precipitates within different regions of the fuel cross-section. Regions A and A/B in the center of the fuel were comprised of U-rich, U-intermediate, and U-lean localities with α-U and δ-UZr2 composing the major phases. Regions B and C in the intermediate and peripheral fuel localities, respectively, were comprised of α-U grains, U-rich (β-U) grains with Zr-rich precipitates, U-intermediate grains (δ-UZr2), and solid FP precipitates. The major phases identified were associated with the nanoscopic chemical concentrations, the phase diagram, and the as-characterized specimen temperature, with the exception of the non-equilibrium β-U phase identified in Region B. The U-lean localities in Regions A, A/B, B, and C were Zr-enriched pathways along subgrain/grain boundaries, suggesting that Zr is susceptible to radiation-induced segregation in U-Zr fuels and indicating a new mechanism for constituent redistribution.

Comparison of the Late Miocene Sediments and Early Quaternary Red Paleosols in the Penghu Islands, Taiwan and Zhangpu, Fujian

This study aims to compare the clay mineralogy and whole-soil major chemistry of elements in late Miocene soil sediments and early Quaternary red paleosols in the Penghu Islands, (Pescadores), Taiwan, and Zhangpu Volcanic Park, Fujian. There were the late Miocene Chu Wan (CWI and CWII), Shiao Men Yu (SMY) and two intergrade red soils, Chu Wan (CW(irs)) and Shiao Men Yu (SMY(irs)), with three distinctive zones of different dominating kaolins in the profiles of the Penghu Islands. A Tong Wei (TW) paleosol of early Quaternary basaltic eruptions in the Penghu Islands was collected. The Anzei (AZ), Si Yu (HY) and Chianmei (CM) paleosols were sampled from the Penghu Islands and Yulinshi (YLS) paleosols near the Zhangpu Volcanic Park for this study. The CW and SMY paleosols erupted in the late Miocene, and the other paleosols erupted on the Penghu Islands. These paleosols were fractionated into clay fractions and subjected to soil physical and chemical analyses. Kaolin minerals were dominant in the CW(irs) and SMY(irs) paleosols. The top layer (layer one) in the CW(irs) was 7 Å-halloysite, and order/disordered kaolinites were present in layers two and three. The CW(irs) and SMY(irs) hexagonal-like, platy kaolinites (0.1–0.2 µm in diameter), spheroidal and hollow 7 Å-halloysite (layer 1) was determined with transmission electron microscopic (TEM) investigations. The early Quaternary red soil of TW consisted of kaolinite, illite, vermiculite and smectite clay assemblages. Late Miocene paleosols were classified as fine, kaolinite, hyperthermic and Typic Rhodic Paleudults, and the early Quaternary red paleosols were classified as fine, mixed, hyperthermic and Typic Rodistalf, respectively. Late Miocene paleosols contained more clays, lower SiO2/Al2O3 and higher chemical index of weathering (CIW) than early Quaternary paleosols. The kaolin, illite, smectite and vermiculite mineralogy, physical and chemical properties of paleosols and landscapes in the Zhangpu YLS, Fujian, were similar to those of late Miocene sediments and early Quaternary red paleosols in the Penghu Islands.

Influence of phase morphology, static recrystallization, and crystallographic texture on room temperature tensile properties of Ti–6Al–4V alloy: Comparison between post-tested equiaxed, bimodal, and lamellar microstructures

The influence of phase fractions, morphology, recrystallization, and crystallographic texture on the room temperature uniaxial tensile properties were investigated in a Ti–6Al–4V (Ti-64) alloy. The hot rolled and annealed Ti-64 alloy was heat treated to generate three different microstructures (equiaxed, bimodal, and lamellar) with varying volume fractions and dimensions of constituent phases (equiaxed primary α, transformed α laths, and β laths). The tested tensile specimens were characterized using techniques such as electron backscattered diffraction (EBSD), transmission electron microscopy (TEM), and X-Ray diffraction-based bulk texture analysis to determine the deformation mechanism of the alloy. Among three different microstructures, the equiaxed microstructure (α/β-900/950-FC) exhibited a superior strength-toughness combination, while the lamellar microstructure (β-1050-AC) displayed poor tensile properties. The bimodal microstructure (α/β-900/950-AC) showed intermediate tensile properties. Recrystallized α grains and their connectivity promoted an extended steady-state flow during deformation and ductile fracture. The bimodal microstructure work hardened faster as compared to the other two microstructures. TEM investigation on the post-tested microstructures showed that events such as dislocation multiplication and dislocation-dislocation interactions, formation of slip bands across the α grains, multiple slip and dislocation pile-ups contribute to hardening mechanisms during deformation. Whereas, slip transfer across α/α boundary and breaking of β laths are the events of softening mechanisms. The slip transfer across two adjacent α grains happens when the misalignment between grains is less than 10°. Equiaxed microstructures exhibited maximum slip transfer due to interconnected primary α grains. Bimodal microstructures (α/β-900/950-AC) exhibited slip transfer when a higher fraction of interconnected primary α is present in the microstructure. In contrast, the lamellar microstructure showed no evidence of slip transfer. The prism slip is the dominant active slip system in the equiaxed and bimodal microstructures. However, the lamellar microstructure with no primary α showed only the prismatic <c+a> and pyramidal <a> slip activities.

Role of grain boundary character on Bi segregation-induced embrittlement in ultrahigh-purity copper

Bismuth (Bi), as an impurity element in copper and copper-based alloys, usually has a strong tendency of grain boundary (GB) segregation, which depends on the GB characters. However, the influence of such a segregation on the properties of ultrahigh-purity copper has been rarely reported and the exact structural arrangements of Bi atoms at different GBs remain largely unclear. In this study, we investigated the influence of trace amounts of Bi (50-300 wt ppm) on the ductility of an ultrahigh-purity copper (99.99999%) in the range of room temperature to 900 °C. The tensile results show that the addition of Bi seriously damages the ductility of the ultrahigh-purity copper at temperatures of 450–900 °C, which is due to the GB segregation of Bi. On this basis, such a segregation behavior at different types of GBs, including high and low angle GBs (HAGBs/LAGBs), and twin boundaries (TBs), via the scanning electron microscope-electron backscattered diffraction (SEM-EBSD) and aberration-corrected scanning transmission electron microscope (AC-STEM) investigations, combined with the first-principles calculations were systematically studied. The atomistic characterizations demonstrate an anisotropic Bi segregation, where severe enrichment of Bi atoms typically occurs at the HAGBs, while the absence of Bi adsorption prevails at LAGBs or TBs. In particular, the segregated Bi at random HAGBs exhibited the directional bilayer adsorption, while the special symmetrical Σ7 HAGB presented a unique Bi-rich cluster superstructure. Our findings provide a comprehensive experimental and computational understanding on the atomic-scale segregation of impurities in metallic materials.

Wide-gamut structural colours on oakblue butterflies by naturally tuned photonic nanoarchitectures.

The iridescent structural colours of butterflies, generated by photonic nanoarchitectures, often function as species-specific sexual signals; therefore, they are reproduced precisely from generation to generation. The wing scales of oakblue hairstreak butterflies (genus Arhopala, Theclinae, Lycaenidae, Lepidoptera) contain multi-layer photonic nanoarchitectures, which can generate a wide range of structural colours, from violet to green. By scanning (SEM) and cross-sectional transmission electron microscopy (TEM) investigation, the colour tuning mechanism of the cover scales was explored. We revealed that the characteristic size change of structural elements in similar photonic nanoarchitectures led to different structural colours that were examined by various reflectance spectrophotometry techniques. The measured structural properties of the naturally tuned photonic nanoarchitectures were used to calculate wing reflectances, which were compared with the measurement results. We found that the simulated structural colours were systematically redshifted by 95-126 nm as compared with the measured normal-incidence reflectance results. This is attributed to the swelling of the chitinous multi-layer structures during the standard TEM sample preparation and the tilt of the cover scales, which both affect the apparent layer thicknesses in the TEM cross-sections. We proposed a simulation correction and compared the results with the layer thicknesses measured on cryogenically prepared non-embedded SEM cross-sections.

Diffusion of the hydrogen in nanocrystalline vanadium films

The β → α phase transition and diffusion of the hydrogen in nanocrystalline vanadium films were investigated. Films were deposited onto the glass substrate at the temperature 673 K and at room temperature. Transmission electron microscopy investigations of the structure of films showed that the averaged sizes of vanadium crystallites were 7 and 4 nm, respectively. The derivative of the electrical resistance of the saturated film revealed the broad β → α phase transition about 390 K. The diffusion coefficient of the hydrogen was obtained from the approximation of the time dependence of the increase of the electrical resistance of the non-saturated part of the film by an analytical expression. Values of the diffusion coefficient revealed the strong dependence on the concentration of the hydrogen. At small concentration of the hydrogen, the diffusion coefficient was equal to that in the bulk vanadium. At large concentrations of the hydrogen (above 20 at. %), the diffusion coefficient decreases by a thousand times. The activation energy of diffusion, calculated for samples with the large concentration of the hydrogen, is equal to (44.8 ± 0.8) kJ/mol [(0.464 ± 0.008) eV].

Innovative methodology for green synthesis of iridium nanoparticles of rod shapes by reduction of iridium (IV) using sustainable pectin with formation of keto-pectin derivatives

A prospective novel technique has been developed for green synthesis of iridium nanoparticles of rod shapes for the first time with simultaneous formation of keto-derivative oxidation product with a yield of 98.3 %. This takes place by reduction of hexacholoroiridate (IV) by using sustainable pectin as a powerful reducing agent biomacromolecule in acidic media. The formation of nanoparticles (IrNPS) was identified by Fourier transform infrared (FTIR), Transmission electron microscope (TEM), X-ray diffraction (XRD), and Scanning electron microscope (SEM) investigations. The TEM morphology showed that the iridium nanoparticles were of crystalline rod shapes on contrary to the spherical shapes reported on all synthesized IrNPS earlier. The rates of nanoparticles growth were followed kinetically using a conventional spectrophotometer. The kinetic measurements revealed a unity order reaction in [IrCl6]2− as oxidant and fractional first-order in [PEC] as a reducing agent, respectively. A decrease in the reaction rates was noticed with increasing the acid concentration. Kinetic evidence reveals the creation of intermediate complex as transient species prior to the slow step. Such complex formation may be facilitated by the participation of one chloride ligand from [IrCl6]2− oxidant forming a bridge between the oxidant and reductant in such formed intermediate complex. Plausible reaction mechanisms for electron transfer pathway routes consistent with the kinetics observations were discussed.