Transmission Electron Microscopy Investigations Research Articles

Comparative study between oxide/soft ferrite, oxide/hard ferrite, and soft/hard ferrite nanocomposites: structural, electrical, and magnetic properties

Three binary nanocomposites (NCs): (0.5NiO/0.5Ni0.5Zn0.5Fe2O4), (0.5NiO/0.5BaFe12O19), and (0.5Ni0.5Zn0.5Fe2O4/0.5BaFe12O19) were prepared using the co-precipitation method followed by the wet ball-milling technique. X-ray diffraction analysis showed the production of NiO and Ni0.5Zn0.5Fe2O4 single phases, while the α-Fe2O3 secondary phase appeared in the BaFe12O19 and the 0.5Ni0.5Zn0.5Fe2O4/0.5BaFe12O19 nanocomposite. The transmission electron microscopy investigation and the selected area electron diffraction demonstrated the presence of the nanocomposites’ constituent phases. x-ray photoelectron spectroscopy identified the oxidation states found in the prepared samples (Ba2+, Ni2+, Ni3+, Zn2+, Fe3+, and O2−). The bandgap values (Eg) of the nanocomposites are in the range between 2.79 and 3.66 eV, which indicates their semiconductor nature. The DC conductivity experiment confirmed the semiconducting nature of all samples, and the activation energies ( EaH ) and ( EaL ) at high and low-temperature regions, respectively, were calculated from the Arrhenius equation. According to the vibrating sample magnetometer, the NCs exhibited ferromagnetic (FM) as showed by the M-H loops. In the oxide/soft ferrite NC, the dM/dH curve indicated strong exchange coupling interactions, while the hard and the soft magnetic phases in the oxide/hard ferrite and the soft/hard ferrite NCs were weakly exchanged coupled. Significant uses had been found for each of the three nanocomposites according to their constituent phases and properties.

Creep anisotropy of additively manufactured Inconel-738LC: Combined experiments and microstructure-based modeling

The current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis.

Interplay of Heat Treatment and Deformation Temperature on the Microstructural Evolution and Mechanical Behavior of SLM AlSi10Mg Alloy

This study conducts a comprehensive examination of the microstructural and dislocation dynamics of AlSi10Mg alloys under various thermal conditions, utilizing quasi in-situ Electron Backscatter Diffraction (EBSD) and Transmission Electron Microscopy (TEM) analyses. The research focuses on comparing the microstructural response of as-built and T6 heat-treated samples to mechanical stress at both ambient (298K) and cryogenic (77K) temperatures. EBSD analysis underscores the grain stability under applied strain, while TEM investigations expose notable variations in dislocation mobility influenced by temperature, with a particular emphasis on the interaction between dislocations and silicon particles at cryogenic temperatures. An observed increase in Geometrically Necessary Dislocation (GND) density at 77K points to enhanced resistance to plastic deformation, suggesting mechanisms of cryogenic strengthening. The findings illuminate the impact of heat treatment in augmenting the mechanical properties of the alloy, shedding light on its potential applications in aerospace and cryogenic environments.

In situ high-temperature transmission electron microscopy investigation of dynamic element migration for Sm-Co-Fe-Cu-Zr sintered magnets

The investigation delved into the dynamic migration of elements and the evolution of interface structures within the Sm(CobalFe0.09Cu0.09Zr0.03)7.2 magnet as temperature increased, employing high-temperature transmission electron microscopy. Notably, the Cu distribution exhibited temperature susceptibility. Elevating the temperature from room temperature (RT) to 400 °C led to a notable expansion in the distribution width of Cu, ranging from 28.5 to 50.8 nm. Simultaneously, the average Cu content at the cell boundaries decreased from 14.4 to 11.6 at.%. According to the high-temperature in-situ experimental results of the transmission electron microscopy thin-film samples, the derived diffusion coefficients, D300°Cand D400°C, were determined as 0.0525 nm2/s and 1.414 nm2/s, respectively. The significantly higher D400°C compared to D300°C underscores the considerable influence of temperature on Cu element diffusion behavior. The simulation results demonstrate that the trend of magnetic properties variation at different temperatures closely aligns with the observed trend. Subsequent calculation of the temperature coefficient of intrinsic coercivity (β) reveals that |β300–400°C| is notably higher than |βRT-300°C|. This suggests a substantial impact of Cu diffusion-induced deterioration on the β. Moreover, micromagnetic simulation results delineated the reverse magnetization process for magnets at varying temperatures, revealing that the presence of the Cu diffusion region diminished the pinning effect of the cell boundary phase. Furthermore, a wider Cu diffusion region facilitated easier magnetic moment reversal at the cell boundary phase, resulting in a marked deterioration of intrinsic coercivity. This elucidates that the formation of the Cu diffusion region stands as one of the primary reasons for the sharp decline in magnetic properties of Sm2Co17-type magnets under high-temperature conditions.

Stacking fault energy, thermal expansion behavior, and elastic coefficients of a single-crystalline CrFeNi medium-entropy alloy

The equiatomic CrFeNi alloy is considered to be a model single-phase face-centered cubic medium-entropy alloy. The Bridgman technique was employed to grow a single crystal of this alloy and its dilatation behavior and elastic properties were measured in the temperature range: 100 K–673 K. Based on transmission electron microscopy investigations, plastic deformation is initially caused by the glide of dissociated dislocations (Shockley pairs bounded by a stacking fault ribbon). From their dissociated widths, a stacking fault energy of 36 mJ∙m-2 was determined.

Structural Evolution of GaOx-Shell and Intermetallic Phases in Ga-Pt Supported Catalytically Active Liquid Metal Solutions.

We present a comprehensive scale-bridging characterization approach for supported catalytically active liquid metal solutions (SCALMS) which combines lab-based X-ray microscopy, nano X-ray computed tomography (nano-CT), and correlative analytical transmission electron microscopy. SCALMS catalysts consist of low-melting alloy particles and have demonstrated high catalytic activity, selectivity, and long-term stability in propane dehydrogenation (PDH). We established an identical-location nano-CT workflow which allows us to reveal site-specific changes of Ga-Pt SCALMS before and after PDH. These observations are complemented by analytical transmission electron microscopy investigations providing information on the structure, chemical composition, and phase distribution of individual SCALMS particles. Key findings of this combined microscopic approach include (i) structural evolution of the SCALMS particles' GaOx shell, (ii) Pt segregation toward the oxide shell leading to the formation of Ga-Pt intermetallic phases, and (iii) cracking of the oxide shell accompanied by the release of liquid Ga-Pt toward the porous support.

Impact of Sample Preparation Approach on Transmission Electron Microscopy Investigation of Sputtered AlNi Multilayers Used for Reactive Soldering

This work presents studies of sputtered Al/Ni reactive multilayers by transmission electron microscopy. They are prepared for these analyses by three methods (both Ga‐ and Xe‐based focused ion beam, FIB, and tripod polishing plus Ar+ ion milling in precision ion polishing system, PIPS) to check their impact on these materials. Every sample shows polycrystalline and mostly chemically pure Al/Ni layers. They also hint existence of intermetallic compounds, especially the tripod‐prepared sample. These intermetallics first originate from the sputtering process. The layers are increasingly rough along the growth direction. Other remarkable findings can be highlighted. First, the heating operations applied during the tripod polishing preparation lead to recrystallization and blurred Al/Ni interfaces due to increased metals reactions, although additional contributions by roughness and preparation thickness to the current compositional uncertainties must be distinguished by optimizing future sample fabrications and preparations. Second, Xe‐based FIB leads to lamellae with seemingly low contamination, although Ga‐FIB is a potentially good alternative. Finally, FIB is better to study cross‐section preparations of pristine Al/Ni multilayers, whereas the present tripod polishing procedures are unsuitable for this purpose but allow to observe the beginning of Al/Ni transformations upon heating, which is interesting for the technological optimization of these materials.

Sustainable and cost-effective edge oxidized graphite/PEDOT:PSS nanocomposites with improved electrical conductivity

Poly(3,4-ethylenedioxythiophene): polystyrene sulfonate (PEDOT:PSS) is a soft and conjugated polymer whose conductive properties can be properly tuned through doping with various additives or solvents, preserving its excellent processability. In this work PEDOT:PSS was combined with a cost-effective graphite derivative named Edge Oxidized Graphite (EOG) for developing a nanocomposite with improved electrical conductivity, with respect to the pristine PEDOT:PSS, through an easy and environmentally friendly doping process. Firstly, the EOG powders, produced by a green oxidation process of graphite, were deeply characterized through Fourier transform infrared (FT-IR), Thermogravimetric (TGA), and Wide-angle X-ray scattering (WAXD) analysis, showing that this nanofiller has oxygenated functional groups on the sheet edges. The quality and the stability of the EOG dispersions within PEDOT:PSS were investigated at different carbon-filler concentrations, up to high loading of 25 %wt/V of EOG through rheological analyses, demonstrating pseudo-plastic behavior and excellent long-term stability of the inks due to the absence of inhomogeneities and aggregates over time; in fact, the same inks were tested under the same rheological conditions after 21 days, showing the same viscosity trend for all EOG concentrations (%wt/V). Transmission electron microscopy (TEM) and (Scanning Electron microscopy) SEM investigation of spin-coated samples onto glass substrates were performed to morphologically evaluate the nanocomposites and estimate the average size of the sheets, particularly the mean length of 1.2 μm and an approximated thickness of 26 nm of the EOG sheets dispersed into the polymer matrix (PEDOT:PSS) was determined, while WAXD analysis allowed to identify the average layer number of the EOG sheets, obtaining thus, a direct measurement of the EOG sheets aspect ratio equal to 45. Finally, sheet resistance tests showed that the increasing concentration of EOG leads to a significant improvement in the electrical conductivity of the nanocomposites, from 1.1 S/cm for pristine PEDOT:PSS to 21.9 S/cm for nanocomposites with the highest EOG content (25 %wt/V). This work demonstrates the successful development of nanocomposite based on PEDOT:PSS doped with carbon-based filler synthesized through a green and cost-effective process, promoting their use in the production of bio/electrochemical sensors or optoelectronic devices.

Deformation behavior of the hybrid S-phase layer formed on a stainless-steel substrate by thermochemical heat treatment under mechanical loading

The hybrid S-phase layer was formed on the surface of an austenitic stainless steel by the thermomechanical heat treatment, which was carried out at a low temperature (475 °C). The thickness of the layer depends on the methane (CH4) gas content in the heat treatment chamber. The microstructure of the layer contains plenty of microstructural defects, such as slip bands, twins, stacking faults, and entangle dislocations, as confirmed by detail electron microscopy investigations. The S-phase layers were subjected to nanoindentation and nanoscratching to investigate their micro-mechanical properties and deformation aspects; and compared against the substrate (bulk austenitic) material. This layer exhibit about 6 folds increase in hardness (11.65–14.65 GPa) to that of bulk austenitic (2.33 GPa), whereas the Young's modulus increased by 1.70 times (124.84–142.34 GPa for the S phase layers and 83.25 GPa for bulk material). This increase in hardness caused relatively less plastic deformation in the layer, compared to bulk austenitic under identical loading conditions. This induced different sub-surface deformation aspects, not only in terms of deformation depth, but also in microstructural aspects, as reviled through a transmission electron microscopy investigation on the residual nanoindentation imprint and scratch tracks.

Achieving ultra-strong and ductile CoNi-based FCC multi-principal element alloys via alloying with refractory Mo and W

FCC single-phase multi-principal element alloys (MPEAs) often suffer from insufficient strength, which limits their wide applications. Here a CoNi-based FCC MPEA (Co44Ni44Mo9W3, at. %) was designed by alloying with refractory Mo and W. The Co44Ni44Mo9W3 alloy possesses an ultrahigh yield strength of ∼1050 MPa and good ductility of ∼30 % at ambient temperature. The excellent mechanical properties were correlated to its superior lattice friction stress and grain boundary strengthening compared to most reported FCC MPEAs and conventional alloys. By density-functional theory calculations, such extraordinary mechanical properties were further attributed to its high lattice distortion, low intrinsic stacking fault energy and high unstable stacking fault energy due to the addition of Mo and W. Transmission electron microscopy investigations revealed that the high strength-ductility combination arises from the synergistic effect of planar slip bands, stacking faults and deformation nano-twins.

Switching Behavior of the Composite Low Dimensional Structural Hybrids of Carbon After UV Exposure

Low dimensional multi structural components of carbon are of great interest currently owing to their applications in developing flexible plastic electronics. In this work, we discuss emergence of different structural hybrids of carbon from as-prepared HiPCO SWCNTs subjecting them to oxidative acid purification and covalent functionalization process. Transmission electron microscopy (TEM) investigations reveal single wall carbon nanotubes (SWCNTs) serve as a building block to obtain multi wall carbon nanotubes (MWCNTs), graphene sheets (GS), carbon nano scrolls (CNS) structures which coexist in the sample. These structures when grafted with polymer binder and spray coated on Si substrate provide highly sustainable thin film coatings that are stable even in adverse space conditions [1]. These CNT and CNS based composite coatings are promising candidates for stray light control space applications exhibiting a low reflectance of the order of 2-3% in the visible spectral range [1]. Electrical switching behaviour of these films were investigated by capturing current(time) (I(t)) response, displaying promising switching character with distinct ON-OFF cycle. These coatings offer opportunities for the development of facile, cost-effective carbon-based devices without going into the nontrivial task of separating different the structures.

Microstructural evolution and its influence on the wear resistance of a laser directed energy deposited Ni-based single crystal superalloy

The wear behavior of Ni-based single crystal (NBSC) superalloy SRR99 fabricated by laser-directed energy deposition (LDED) is investigated and compared with that of its cast counterpart. While γ’ precipitate size in the latter is > 400 nm, that in the former is an order of magnitude lower. Dry sliding wear tests reveal that the wear rate and coefficient of friction of the LDED alloy are 75% and 20% lower than that of its cast counterpart, respectively. Detailed transmission electron microscopy investigation of the wear-tested cast alloy indicates that there is orientation change and formation of nanoscale grains only at the top layer of the worn surface, whereas regions below undergo moderate plastic deformation via dislocation slip. In contrast, the sub-surface of the worn LDED alloy has a graded microstructure, with a composite of NiO/γ-Ni on the top, γ’ free nano-grains in the middle, and a highly deformed nanoscale layer at the bottom. The improved wear behavior of the LDED alloy is attributed to its higher dislocation density, finer γ’ precipitates, and the formation of this graded microstructure. Finally, a detailed description of mechanisms that lead to the formation of this unique graded microstructure is provided.

Green Synthesis of Metal-Doped ZnO Nanoparticles Using Bauhinia racemosa Lam. Extract and Evaluation of Their Photocatalysis and Biomedical Applications.

A fascinating problem in the fields of nanoscience and nanobiotechnology has recently emerged, and to tackle this, the production of metal oxide nanoparticles using plant extracts offers numerous benefits over traditional physicochemical methods. In the present investigation, ZnO nanoparticles were fabricated from Bauhinia racemosa Lam. (BR) leaves extract with various transition metal (TM) dopants (Ni, Mn, and Co). Plant leaves extract containing metal nitrate solutions were utilized as a precursor to synthesize the pristine and TM-doped ZnO nanoparticles. Structural, functional, optical, and surface properties of the fabricated samples were studied by using physicochemical and photoelectrochemical measurements. The organic pollutants tetracycline (TC), ampicillin (AMP), and amoxicillin (AMX) were used in the photocatalytic degradation assessment of the fabricated samples. Through X-ray diffraction (XRD) and transmission electron microscopy (TEM) investigation, the fabricated nanoparticles wurtzite crystal structure was verified. Moreover, Fourier transform infrared (FT-IR) analysis verified the existence of functional groups in the fabricated nanoparticles. The migration of electrons from the deep donor level and zinc interstitial to the Zn-defect and O-defect is related to the emission peaks seen at 468, 480, 534, and 450 nm in photoluminescence (PL) spectra. Co-ZnO nanoparticles demonstrated potent and excellent photocatalytic degradation performance for TC (91.09%), AMP (87.97%), and AMX (92.42%) antibiotics within 210, 180, and 150 min of visible light irradiation. Co-ZnO nanoparticles also demonstrated strong antimicrobial performance against Escherichia coli, Staphylococcus aureus, Klebsiella pneumoniae, Aspergillus flavus, Aspergillus niger, and Bacillus subtilis. Further investigation of in vitro cytotoxic potential against the A549 cell line (IC50 = 24 ± 0.5 μg/mL) utilizing MTT assay and the free radical scavenging performance of Co-ZnO nanoparticles estimated by DPPH assay utilizing l-ascorbic acid as a reference was also performed. Anti-inflammatory potential is also reviewed by comparing it with the standard drug Diclofenac, and the maximum activity was obtained for Ni-ZnO nanoparticles (IC50 = 72.4 μg/mL).

Multiscale Regulation of Ordered PtCu Intermetallic Electrocatalyst for Highly Durable Oxygen Reduction Reaction.

Transforming the Pt-M alloy into an ordered intermetallic is an effective strategy to improve the electrocatalytic activity and stability toward the oxygen reduction reaction (ORR). However, the synthesis of nanosized intermetallics remains challenging. Herein, we report an efficient ORR electrocatalyst, consisting of a monodisperse nanosized PtCu intermetallic on hollow mesoporous carbon spheres (HMCS). As predicted by theoretical calculations, PtCu intermetallics exhibit beneficial electronic structure, with a low theoretical overpotential of 0.33 V and enhanced Cu stability. Resulting from the multiscale modulation of catalyst structure, the O-PtCu/HMCS catalyst delivers a high mass activity of 2.73 A cm-2Pt at 0.9 V and remarkable stability. Identical location transmission electron microscopy (IL-TEM) investigations demonstrate that the rate of carbon corrosion is alleviated on HMCS, which contributes to the long-term durability. This work provides a promising design strategy for an ORR electrocatalyst, and the IL-TEM investigations offer new perspectives for the performance enhancement mechanism.

Ultra-high dilutions analysis: Exploring the effects of potentization by electron microscopy, Raman spectroscopy and deep learning

The subject of ultrahigh dilutions has been under continuous debate over the years, mainly because the possibilities to analyze such diluted solutions are limited. In this context, transmission electron microscopy (TEM) investigations were conducted to evaluate the morphological characteristics of ethanol- and water-based highly diluted solutions of gold; three levels of potentization (6C, 30C, and 200C) were examined for each type of solution. Moreover, Raman spectroscopy and deep learning (DL) algorithms were employed for the analysis of the three potentization levels of purified water, unpurified water, and purified water-based gold solutions. Three batches were assessed for each considered category, and the ability to discriminate between all investigated classes, between the potencies within each group or between the classes within the same level of potentization were presented and discussed in correlation with the TEM findings. Distinct forms of organization were revealed by TEM for the three levels of potentization, while the gated recurrent unit (GRU) model showed great accuracy (88 %) for discriminating all classes, over 90 % accuracy for distinguishing the samples within each group and over 95 % accuracy for classification within the same level of potentization if unpretreated Raman spectra were used. Thus, this suite of methods (TEM-EDX and Raman spectroscopy in combination with DL) can be successfully used for the characterization and differentiation of highly diluted solutions resulting after potentization treatment. Furthermore, considering the results obtained from the discrimination study involving all 11 classes and a data augmentation approach, the spectral segmentation method can be seen as a valuable strategy for increasing the model prediction accuracy.

Complementary metalloporphyrin-based nanostructure decorated with silver nanoparticles for photocatalytic degradation of organic dyes

A hybrid composite photocatalyst, SA-T@Ag, was fabricated by the photoreduction of silver salts in the presence of nanomaterials composed of self-assembled complementary porphyrin triad SA-T. We confirmed the formation of SA-T@Ag from SA-T using various spectroscopic techniques, including X-ray diffraction (XRD), infrared (IR) spectroscopy, UV–visible spectroscopy, and fluorescence spectroscopy. Field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) investigations revealed that a substantial amount of silver nanoparticles (AgNPs) were deposited on the surface of SA-T and that the microstructure of SA-T was intact during photoreduction. The formation of AgNPs on the surface of SA-T reduced the band gap energy (Eg) of SA-T@Ag compared to that of SA-T. This not only improves its light-harvesting properties but also delays the recombination of photogenerated electron-hole pairs, which promotes more reactivity under visible light irradiation and improves the efficiency of polluted dye degradation. These photophysical properties are reflected in the degradation of methylene blue (MB) dye under visible light irradiation. The first-order degradation rate constant of MB dye within 45 min of visible light irradiation is much higher for SA-T@Ag (0.081 min−1) than SA-T (0.028 min−1). This report is of great importance in the field of environmental remediation and provides new opportunities for designing porphyrin-based photocatalytic systems as alternatives to conventional photocatalysts.

A transmission electron microscopy investigation suggests that telocytes, skeletal muscles, myoblasts, and stem cells in common carp (Cyprinus carpio) respond to salinity challenges

BackgroundTelocytes are modified interstitial cells that communicate with other types of cells, including stem cells. Stemness properties render them more susceptible to environmental conditions. The current morphological investigation examined the reactions of telocytes to salt stress in relation to stem cells and myoblasts. The common carp are subjected to salinity levels of 0.2, 6, and 10 ppt. The gill samples were preserved and prepared for TEM.ResultsThe present study observed that telocytes undergo morphological change and exhibit enhanced secretory activities in response to changes in salinity. TEM can identify typical telocytes. This research gives evidence for the communication of telocytes with stem cells, myoblasts, and skeletal muscles. Telocytes surround stem cells. Telopodes made planar contact with the cell membrane of the stem cell. Telocytes and their telopodes surrounded the skeletal myoblast. These findings show that telocytes may act as nurse cells for skeletal stem cells and myoblasts, which undergo fibrillogenesis. Not only telocytes undergo morphological alternations, but also skeletal muscles become hypertrophied, which receive telocyte secretory vesicles in intercellular compartments.ConclusionIn conclusion, the activation of telocytes is what causes stress adaptation. They might act as important players in intercellular communication between cells. It is also possible that reciprocal interaction occurs between telocytes and other cells to adapt to changing environmental conditions.

Nanostructured Coatings Based on Graphene Oxide for the Management of Periprosthetic Infections.

To modulate the bioactivity and boost the therapeutic outcome of implantable metallic devices, biodegradable coatings based on polylactide (PLA) and graphene oxide nanosheets (nGOs) loaded with Zinforo™ (Zin) have been proposed in this study as innovative alternatives for the local management of biofilm-associated periprosthetic infections. Using a modified Hummers protocol, high-purity and ultra-thin nGOs have been obtained, as evidenced by X-ray diffraction (XRD) and transmission electron microscopy (TEM) investigations. The matrix-assisted pulsed laser evaporation (MAPLE) technique has been successfully employed to obtain the PLA-nGO-Zin coatings. The stoichiometric and uniform transfer was revealed by infrared microscopy (IRM) and scanning electron microscopy (SEM) studies. In vitro evaluation, performed on fresh blood samples, has shown the excellent hemocompatibility of PLA-nGO-Zin-coated samples (with a hemolytic index of 1.15%), together with their anti-inflammatory ability. Moreover, the PLA-nGO-Zin coatings significantly inhibited the development of mature bacterial biofilms, inducing important anti-biofilm efficiency in the as-coated samples. The herein-reported results evidence the promising potential of PLA-nGO-Zin coatings to be used for the biocompatible and antimicrobial surface modification of metallic implants.

Dislocation structure evolution during room temperature dwell loading of a Ti-6Al-4 V alloy

The current work examines the evolution of the dislocation structure, within both the α and β phases, of a Ti-6Al-4 V alloy subjected to room temperature dwell loading performed at about 96% of the macroscopic yield stress level for several durations, as part of a synchrotron in-situ deformation experiment. The obtained findings represent a vital contribution to creating a scientific basis for improving lifing predictions for aero-propulsion components. The dislocation configuration, type and density were examined post-mortem using transmission electron microscopy (TEM). Despite the relatively low applied stress level, well-developed dislocation structures were already formed within the α phase at a dwell duration of 10 min and changed only modestly up to 60 min. The plastic deformation of the above phase took place solely via dislocation slip. To facilitate a comparison between different dwell durations, the TEM investigation focused on the regions oriented for the prismatic glide that represented the main deformation mode due to the starting crystallographic texture. After deformation, the regions oriented for the prismatic slip contained planar slip bands largely consisting of dislocations of a screw type. There was rather limited interaction between different bands, as the dislocation arrays passed through the slip band intersections with only minor difficulty. The screw-type dislocations seemed to preferentially form during straining. Dislocation Burgers vectors experimentally determined within the β phase occasionally departed from the Schmid rule and such dislocations typically showed a prevalent screw component. Some deformation banding and {112} 〈111〉 − type mechanical twin formation were locally detected within the β phase.

High-Resolution Characterization of Enamel Remineralization Using Time-of-Flight Secondary Ion Mass Spectrometry and Electron Microscopy

Introduction: The aim of this in vitro study was to assess the suitability of high-resolution time-of-flight secondary ion mass spectrometry (ToF-SIMS) for visualizing cross-sectional changes in human enamel microstructure and chemical composition during treatment and remineralization cycling of artificially generated caries lesions underneath an artificial plaque. Methods: Treatments consisted of exposure to twice daily toothpaste/water slurries prepared from 0, 1,100, and 5,000 μg/g fluoride (F) NaF/silica toothpastes. In addition, treatments with slurries prepared from 1,100 μg/g F SnF2/silica toothpastes were done using 44Ca in the remineralization solution to allow for differentiation of newly formed mineral and exploration of incorporated metal dopants using ToF-SIMS. Complementary microhardness, scanning electron microscopy, and high-resolution transmission electron microscopy (HR-TEM) investigations were performed on enamel cross sections. Results: HR-TEM was used for the first time to determine the change in crystallinity during remineralization revealing distinct microstructural zones within one lesion. Chemical mapping using ToF-SIMS demonstrated that the distribution of F, while observed primarily in the new mineral phase, was widespread throughout the lesion with 44Ca substantially limited to the remineralizing mineral. Both penetrated the inter-rod spaces of the sound enamel illustrating how acid damage propagates into the native mineral as the caries lesion deepens. HR-TEM examination revealed different regions within the lesion characterized by distinct micro- and ultrastructures. Importantly, HR-TEM revealed a return of crystallinity following remineralization. F dose-response observations verified the ability of these high-resolution techniques to differentiate remineralization efficacy. Conclusion: The collective results provided new insights such as the visualization of F or calcium penetration pathways, as well as new tools to study the caries process.