Transmission Electron Microscopy Observations Research Articles

Multi-Technique Characterization of 3.45 Ga Microfossils on Earth: A Key Approach to Detect Possible Traces of Life in Returned Samples from Mars.

The NASA Mars 2020 Perseverance rover is actively exploring Jezero crater to conduct analyses on igneous and sedimentary rock targets from outcrops located on the crater floor (Máaz and Séítah formations) and from the delta deposits, respectively. The rock samples collected during this mission will be recovered during the Mars Sample Return mission, which plans to bring samples back to Earth in the 2030s to conduct in-depth studies using sophisticated laboratory instrumentation. Some of these samples may contain traces of ancient martian life that may be particularly difficult to detect and characterize because of their morphological simplicity and subtle biogeochemical expressions. Using the volcanic sediments of the 3.45 Ga Kitty's Gap Chert (Pilbara, Australia), containing putative early life forms (chemolithotrophs) and considered as astrobiological analogues for potential early Mars organisms, we document the steps required to demonstrate the syngenicity and biogenicity of such biosignatures using multiple complementary analytical techniques to provide information at different scales of observation. These include sedimentological, petrological, mineralogical, and geochemical analyses to demonstrate macro- to microscale habitability. New approaches, some unavailable at the time of the original description of these features, are used to verify the syngenicity and biogenicity of the purported fossil chemolithotrophs. The combination of elemental (proton-induced X-ray emission spectrometry) and molecular (deep-ultraviolet and Fourier transform infrared) analyses of rock slabs, thin sections, and focused ion beam sections reveals that the carbonaceous matter present in the samples is enriched in trace metals (e.g., V, Cr, Fe, Co) and is associated with aromatic and aliphatic molecules, which strongly support its biological origin. Transmission electron microscopy observations of the carbonaceous matter documented an amorphous nanostructure interpreted to correspond to the degraded remains of microorganisms and their by-products (extracellular polymeric substances, filaments…). Nevertheless, a small fraction of carbonaceous particles has signatures that are more metamorphosed. They probably represent either reworked detrital biological or abiotic fragments of mantle origin. This study serves as an example of the analytical protocol that would be needed to optimize the detection of fossil traces of life in martian rocks.

Dislocation avalanches in nanostructured molybdenum nanopillars

We investigate intermittent plasticity in nanopillars of nanocrystalline molybdenum based on in situ transmission electron microscopy observations. By correlating electron imaging results with the measured nanopillar mechanical response, we demonstrate that the intermittent plasticity in nanocrystalline molybdenum is largely caused by dislocation avalanches. Electron imaging further reveals three types of dislocation avalanches, from intragranular to transgranular to cross-granular avalanches. The measured strain bursts resulted from avalanches have similar magnitudes to those reported for the molybdenum single-crystal pillars, while the corresponding flow stress in nanocrystalline molybdenum is greatly enhanced by the small grain size. Statistical analysis also shows that the avalanches behavior has similar characteristic as single crystals in the mean field theory model. Together, our findings here provide critical insights into the deformation mechanisms in a nanostructured body-centered-cubic metal.

Zebrafish prss59.1 is involved in chorion development

The prss59.1 gene was identified as one of 11 genes that were highly upregulated during the induction of ovulation in zebrafish by using an in vivo ovulation assay. Previously, we conducted biochemical characterization of Prss59.1 and revealed it to be a trypsin-like proteolytic enzyme. In this study, we established a prss59.1 gene knockout strain using the CRISPR/Cas9 system. Phenotypic analysis of prss59.1 knockout fish showed that prss59.1 is associated with chorion elevation, a prominent event in egg activation during fertilization. The chorions of heterozygous and homozygous prss59.1 mutant zebrafish were smaller than those of the wild type. The results suggested that Prss59.1 is necessary for chorion expansion. The homozygous prss59.1 mutant strain, with a small chorion, showed an extremely low survival rate. Fiber-supported knob-like structures (KS) on the chorion showed an abnormal structure in prss59.1 mutants. Prss59.1 was detected in the KS on the chorion. The pores on the chorion were smaller in the prss59.1 mutants than in the wild type. Transmission electron microscopy (TEM) observations of the cross sections of the chorions showed abnormalities in the chorion structure in prss59.1 mutants. These results demonstrated that Prss59.1 is involved in chorion elevation and in proper formation of the chorion, which is necessary for embryo development.

Rapid Plasma Electrolytic Oxidation Synthesis of Intermetallic PtBi/MgO/Mg Monolithic Catalyst for Efficient Removal of Organic Pollutants.

The intermetallic PtBi/MgO/Mg monolithic catalyst was first prepared using non-equilibrium plasma electrolytic oxidation (PEO) technology. Spherical aberration-corrected transmission electron microscope (ACTEM) observation confirms the successful synthesis of the PtBi intermetallic structure. The efficiency of PtBi/Mg/MgO catalysts in catalyzing the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the presence of NaBH4 was demonstrated. The activity factor for the catalyst is 31.8 s-1 g-1, which is much higher than reported values. In addition, the resultant catalyst also exhibits excellent catalytic activity in the organic pollutant reaction of p-nitrobenzoic acid (p-NBA) and methyl orange (MO). Moreover, benefiting from ordered atomic structures and the half-embedded PtBi nanoparticles (NPs), the catalyst demonstrates excellent stability and reproducibility in the degradation of 4-NP. This study provides an example of a simple method for the preparation of intermetallic structures as catalysts for organic pollutant degradation.

Oxide characteristics of 90Nb-10Zr alloy corroded under different water chemistry conditions

In water-cooled nuclear power reactors, zirconium alloys as fuel cladding are important structural materials. Many factors will lead to the failure of the zirconium alloy cladding, and the corrosion resistance is the most important factor that affects the service life of the fuel element. E110 (Zr-1Nb, wt.%) and M5 (Zr-1Nb-0.16O) alloys are typical Zr-Nb series zirconium alloys used in commercial reactors. It is well-known that most of second phase particles are β-Nb in Zr-Nb series alloys, and many researchers believe that the corrosion resistance of Zr-Nb alloy is related to the oxidation process of β-Nb precipitates. Due to its size limitations, it is difficult to conduct in-depth and systematic research on the oxidation process of β-Nb precipitates. Therefore, we prepared the 90Nb-10Zr binary alloy with the same microstructure and composition of β-Nb and investigated its oxide characteristics in different water chemical environments. The corrosion products of 90Nb-10Zr alloy vary with the corrosion environments. Based on the transmission electron microscopy observation results of corrosion products formed on the 90Nb-10Zr alloy, a hypothesis of corrosion acceleration of Zr-1Nb alloy in lithiated water is proposed from the perspective of β-Nb SPPs oxidation.

Local strain distribution analysis in strained SiGe spintronics devices

This paper reports nanobeam X-ray diffraction (nanoXRD) measurement results for strained SiGe spintronics devices grown by MBE. A quantitative nanoXRD analysis verifies that in-plane strain is properly exerted on the SiGe spin channel layer in the device showing enhanced spin diffusion length, whereas overall strain relaxation and local change in crystallinity occur in the sample with unclear spin signals. Crystal defects such as dislocations and stacking faults found in cross-sectional transmission electron microscopy observations are correlated with the results of nanoXRD analysis and their influence on spin transport properties are discussed. The present results demonstrate the capability of the nanoXRD based method for quantitative nondestructive analysis of strain distribution and crystallinity in real device structures.

Chitosan surface-modified bovine serum albumin-oleic acid self-assembled complexes: Improving the thermal stability, controlled release and bioaccessibility of fucoxanthin

Fucoxanthin (FUCO) is a marine xanthophyll carotenoid with widespread potential physiological functions. However, poor water solubility and chemical instability limit FUCO's processing adaptability and bioavailability. In this study, chitosan surface-modified bovine serum albumin (BSA)-oleic acid (OA) self-assembled complexes were fabricated to improve the thermal stability as well as the controlled release and bioaccessibility of FUCO during gastrointestinal digestion. The results showed that glucose-grafted chitosan (GGC) could surface modify BSA-OA complexes by non-covalent affinity adhesion, resulting in a stable hydrophilic dispersion system with a polydispersity index <0.25 and a Zeta potential > −20 mV. Fourier transform infrared spectroscopy and transmission electron microscope observations revealed that GGC covered the surface of BSA-OA particles through hydrogen bonding, hydrophobic and electrostatic interactions. The GGC-BSA-OA delivery system captured FUCO with >88.00% encapsulation efficiency. Additionally, embedding FUCO in the GGC-modified BSA-OA complex improved its thermal stability. In vitro, gastrointestinal digestion simulations showed that the GGC-modified protein shell had a controlled-release effect on FUCO, which prevented acidic pH from destroying FUCO due to premature release during gastric digestion and released it during intestinal digestion. As expected, GGC-BSA-OA, an encapsulated carrier, dramatically improved the FUCO's digestive stability (retention rate >74.00%), bioaccessibility (>54.42%), and micellization rate (>70.00%) in simulated gastrointestinal digestion. These findings suggested that GGC-BSA-OA as a delivery vehicle could effectively improve FUCO's thermal processing stability and absorbability.

Structural and mechanical responses of (ZrTiNbTa)C4 and ZrC ceramics under energetic He-ions irradiation

High entropy ceramics are potential structural materials for advanced reactor concepts where numerous helium atoms would be produced due to the (n, α) nuclear transmutation reaction. However, the irradiation behaviors of high entropy ceramics are not well understood until now. In present work, the responses of high entropy (ZrTiNbTa)C4 and its binary constituent ZrC ceramics to energetic He-ions irradiation have been studied. X-ray diffraction analysis showed that He-ions irradiation resulted in peak shift and broadening of diffraction peaks in both (ZrTiNbTa)C4 and ZrC, which denotes lattice expansion and structural damages induced by the irradiation. Transmission electron microscope observation revealed that spherical helium bubbles distribute uniformly in the grain interiors of (ZrTiNbTa)C4 while “string-like” bubbles with a preferred orientation are observed in ZrC grains. Nanoindentation characterization gives that the irradiation induced hardening of (ZrTiNbTa)C4 is less definite than that of ZrC. The irradiation mechanisms of high entropy ceramics have been discussed.

Stromal Cell-Derived Factor 1α Inhibits Chondrocyte Apoptosis and Promotes Autophagy Through the Akt Signaling Pathway

To investigate the effects of stromal cell-derived factor 1α (SDF-1α) on the apoptosis and autophagy of chondrocytes and the underlying mechanisms. Chondrocytes were isolated from the knee joints of neonatal mice. The chondrocytes were then stimulated with 0 (the control group), 50, 100, and 200 ng/mL of SDF-1α. CCK-8 assay was performed to determine the effects of SDF-1α stimulation for 24 h, 48 h, and 72 h on the viability of the chondrocytes. Wound healing assay was conducted to determine the effects of SDF-1α stimulation for 12 h and 24 h on chondrocyte migration. The changes in the expression of Akt signaling pathway proteins in chondrocytes were determined by Western blot assay. Chondrocytes were stimulated with 0 (the control group) and 200 ng/mL of SDF-1α. Flow cytometry was performed to determine the effect of SDF-1α on the apoptosis of chondrocytes. Transmission electron microscope was used to examine the effect of SDF-1α on chondrocyte autophagy. Immunofluorescence staining assays were performed to visualize the differences in p-Akt expression and distribution in chondrocytes treated with SDF-1α. Compared with the control group, findings for the experimental groups showed that SDF-1α at the concentrations of 50, 100, and 200 ng/mL did not decrease chondrocyte activity at any time point (P<0.01) and it consistently promoted chondrocyte migration at 24 h (P<0.05). Western blot results revealed that, in comparison to the control group, SDF-1α at concentrations of 50, 100, and 200 ng/mL significantly up-regulated the protein expression of p-Akt in chondrocytes, while no significant difference in Akt expression was observed. Flow cytometry demonstrated that SDF-1α could inhibit chondrocyte apoptosis (P<0.05) and transmission electron microscopic observation showed that SDF-1α promoted chondrocyte autophagy (P<0.05). Immunofluorescence staining showed that the expression of p-Akt in chondrocytes was concentrated in the perinuclear area of the cells and this expression was further enhanced in the perinuclear area of the chondrocytes after treatment with SDF-1α. SDF-1α inhibits chondrocyte apoptosis and promotes chondrocyte migration and autophagy through activating the Akt signaling pathway.

Amorphous shear band formation in elemental β-boron

We report the formation of shear-induced amorphization in elemental β‑boron (β-B) using transmission electron microscopy (TEM) and density function theory (DFT) simulations. TEM observations beneath the residual indentation of β-B revealed intragranular nanoscale shear bands along 1¯11¯ and 111 crystallographic planes, which are preceded by nucleation of dislocations. Strain map analyses of the shear band indicated that compressive strain assists in the process of bond breaking and shear strain is involved in the disassembly of icosahedral clusters by forming amorphization within a unit cell of β-B. Further DFT simulations confirmed that the deconstruction of triply fused icosahedral (B28) along 11¯0111slip system in β-B106 has the lowest shear strength leading to the formation of a kink followed by amorphization, which is in line with our experimental observations. This study illustrates the structural evolution of shear amorphization in β-B and provides the basis to improve their mechanical properties through modification of internal structure.

Nano-captured water affects the wettability of cellulose nanofiber films

In this study, we report that the wettability of cellulose nanofiber films varies with their thickness, and this variation is attributed to the amount of water captured within the hydrogel-like film. To investigate this, we conducted water contact angle measurements on cellulose nanofiber films with different thicknesses. The wettability of the films was found to change from hydrophilic (approximately 20°) to that of the underlying silicon substrate (approximately 80°) by decreasing the mean film thickness within a range of 150 nm or less. Transmission electron microscope observations revealed that even under high-vacuum conditions (< 10−5 Pa), water was captured in regions where the film was thick enough to form a dense, three-dimensional network. However, in regions where the film was thin, the network structure became sparse and two-dimensional, and no water was observed. We propose that the wettability of cellulose nanofiber films changes based on the area ratio of water captured in thick 3D network regions, the underlying substrate, and the cellulose nanofibers. Furthermore, we quantitatively evaluated the relationship between the area ratio and the wetting state of the composite surface based on the Cassie-Baxter equation, then determined the minimum thickness at which water is retained within the cellulose fiber network.

Nanoscrolls of Janus Monolayer Transition Metal Dichalcogenides.

Tubular structures of transition metal dichalcogenides (TMDCs) have attracted attention in recent years due to their emergent physical properties, such as the giant bulk photovoltaic effect and chirality-dependent superconductivity. To understand and control these properties, it is highly desirable to develop a sophisticated method to fabricate TMDC tubular structures with smaller diameters and a more uniform crystalline orientation. For this purpose, the rolling up of TMDC monolayers into nanoscrolls is an attractive approach to fabricating such a tubular structure. However, the symmetric atomic arrangement of a monolayer TMDC generally makes its tubular structure energetically unstable due to considerable lattice strain in curved monolayers. Here, we report the fabrication of narrow nanoscrolls by using Janus TMDC monolayers, which have an out-of-plane asymmetric structure. Janus WSSe and MoSSe monolayers were prepared by the plasma-assisted surface atom substitution of WSe2 and MoSe2 monolayers, respectively, and then were rolled by solution treatment. The multilayer tubular structures of Janus nanoscrolls were revealed by scanning transmission electron microscopy observations. Atomic resolution elemental analysis confirmed that the Janus monolayers were rolled up with the Se-side surface on the outside. We found that the present nanoscrolls have the smallest diameter of about 5 nm, which is almost the same as the value predicted by the DFT calculation. The difference in work functions between the S- and Se-side surfaces was measured by Kelvin probe force microscopy, which is in good agreement with the theoretical prediction. Strong interlayer interactions and anisotropic optical responses of the Janus nanoscrolls were also revealed by Raman and photoluminescence spectroscopy.

Quantitative study on dynamic instantaneous dissolution of precipitated phases in 2195-T6 Al-Li alloy based on characterizations with SANS and TEM

The kinetics of the dynamic instantaneous dissolution of the precipitated phases in 2195-T6 Al-Li alloy under high strain rate loading was firstly studied quantitatively by means of the small angle neutron scattering (SANS) and transmission electron microscopy (TEM) techniques, and the thermodynamics and transformation mechanism were also illustrated in this paper. The high strain rate loadings were performed by the split Hopkinson pressure bar. The maximum flow stresses increased but the pulse durations decreased with increasing strain rates. TEM observations indicated that the size and volume fraction of the T1 phases decreased. The SANS fitting results showed that the radius and volume fraction of the T1 phase decreased after loading. The dissolution activation energy (Qd) was calculated to be 28.4 kJ/mol by combining the Johnsone-Mehl-Avrami-Kolmogorov (JMAK) equation and the Arrhenius equation, indicating that the instantaneous dissolution of T1 phase was kinetically feasible. The T1 phase generated a larger distortion energy, and the surface energy as well as the internal pressure of T1 phase increased in dissolving during dynamic loading to increase the free energy difference (driving force for dissolving) between T1 phase and matrix, making the instantaneous dissolution of the T1 phases be thermodynamically feasible. The diffusion rates of Cu and Li atoms were significantly accelerated to promote the instantaneous dissolution of T1 phase particles. The results of the Vickers hardness values showed that the hardness increased after loadings, due to the high density of dislocations and only partial dissolution of the T1 phase particles.

Bidirectional phase transformation facilitated by ε-martensite bands interaction in metastable Fe50Mn30Co10Cr10 dual-phase high entropy alloys

The phase transformation-induced plasticity (TRIP) metastable Fe50Mn30Co10Cr10 dual-phase high entropy alloys exhibit an excellent combination of strength and ductility. The interaction between ε-martensite (HCP phase) bands plays a fundamental role in determining the mechanical properties of Fe50Mn30Cr10Co10 alloys. In this work, the phase transition mechanism of Fe50Mn30Co10Cr10 dual-phase high entropy alloy was studied by using electron backscatter diffraction (EBSD), transmission electron microscope (TEM) observation and molecular dynamic (MD) simulations. The results indicated that the orientation relationship and character of the ε-martensite band play a crucial role in the phase transition and growth of ε-martensite bands. As an expanding ε-martensite band is obstructed by another ε-martensite band, the cross slip or dissociation of the Shockley partial dislocations at the ε-martensite junction lead to the growth of the ε-martensite bands. When two ε-martensite bands form a cross structure and the phase transition partial dislocations of the incident ε-martensite band are edge type, a new FCC-structured grain will be formed in the domain where the ε-martensite bands intersect. While the dissociation and gliding of Shockley partial dislocations at the phase boundaries will lead to the growth of the ε-martensite bands when the phase transition dislocations of the incident ε-martensite band are mixed type.

Isolation, identification, and monoclonal antibody development of largemouth bass virus

Largemouth bass virus (LMBV) poses a significant threat to largemouth bass farming, leading to substantial economic losses. In December 2022, massive largemouth bass juveniles died at a fish farm in the city of Xinxiang, China. Through a series of experiments, we conclusively identified LMBV as the causative pathogen. The affected fish displayed anorexia, lethargy, and hemorrhage at the pectoral and caudal fin base. No parasites or pathogenic bacteria were detected on the body surface or gills, or isolated from the diseased fish. Severe hemorrhage, lymphocyte infiltration, and extensive necrosis were observed in the liver, spleen, intestine, and stomach of the moribund fish. The tissue homogenate from the diseased fish induced epithelioma papulosum cyprini cells (EPC) cell death, while no such effects were observed in grouper spleen (GS) cells. Sequence similarity analysis of the major capsid protein (MCP) indicated the virus shared 100% similarity with the LMBV-FS2021 strain, placing it within the Ranavirus genus. Transmission electron microscopy (TEM) observations revealed plenty of hexagonal virions accumulated in the cytoplasm of infected EPC cells. Artificial infection demonstrated that LMBV-XX01 was highly fatal to Micropterus salmoides juveniles, with an LD50 of 103.081 TCID50/fish. RT-qPCR detection confirmed that LMBV appeared in all sampled tissues of the challenged largemouth bass, with significantly higher viral loads detected in the liver and heart compared to other tissues. Additionally, we successfully obtained a highly purified recombinant MCP of LMBV and developed two strains of monoclonal antibodies targeting MCP of LMBV-XX01. Overall, our findings provide valuable materials and insights for the design of prevention strategies and the development of detection methods for LMBV.

Perfluorooctane sulfonate (PFOS) induces apoptosis and autophagy by inhibition of PI3K/AKT/mTOR pathway in human granulosa cell line KGN

Perfluorooctane sulfonate (PFOS) is recognized as an environmental endocrine disruptor with widespread use in industrial manufacturing and daily life, contributing to various public health concerns. However, the precise impacts of PFOS on the ovary and its regulatory mechanisms remain unclear. This study aims to delineate the ovarian toxicity of PFOS and scrutinize its effects on apoptosis and autophagy through modulation of the PI3K/AKT/mTOR pathway in the human granulosa cell line (KGN). Cell viability, assessed via the Cell Counting Kit-8 (CCK8), revealed a dose-dependent reduction in cell viability upon PFOS exposure. Flow cytometry analysis demonstrated an elevated proportion of apoptotic cells following PFOS treatment. Western blot analyses unveiled increased expression of Bax, Cyt c, cleaved caspase-9, and LC3-II/I, coupled with decreased expression of Bcl-2 and p62. Transmission electron microscopy (TEM) observations illustrated a heightened number of autophagosomes induced by PFOS. Molecular docking investigations, in conjunction with Western blot experiments, substantiated PFOS's significant inhibition of the PI3K/AKT/mTOR signaling pathway. These findings collectively underscore that PFOS induces apoptosis and autophagy in KGN cells through modulation of the PI3K/AKT/mTOR pathway, providing experimental evidence for PFOS-induced ovarian toxicity and elucidating the underlying regulatory mechanisms in KGN cells.

Solution-Plasma Synthesis and Characterization of Transition Metals and N-Containing Carbon-Carbon Nanotube Composites.

Lithium-air batteries (LABs) have a theoretically high energy density. However, LABs have some issues, such as low energy efficiency, short life cycle, and high overpotential in charge-discharge cycles. To solve these issues electrocatalytic materials were developed for oxygen reduction reaction (ORR) and oxygen evolution reaction (OER), which significantly affect battery performance. In this study, we aimed to synthesize electrocatalytic N-doped carbon-based composite materials with solution plasma (SP) using Co or Ni as electrodes from organic solvents containing cup-stacked carbon nanotubes (CSCNTs), iron (II) phthalocyanine (FePc), and N-nethyl-2-pyrrolidinone (NMP). The synthesized N-doped carbon-based composite materials were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). TEM observation and XPS measurements revealed that the synthesized carbon materials contained elemental N, Fe, and electrode-derived Co or Ni, leading to the successful synthesis of N-doped carbon-based composite materials. The electrocatalytic activity for ORR of the synthesized carbon-based composite materials was also evaluated using electrochemical measurements. The electrochemical measurements demonstrated that the electrocatalytic performance for ORR of N-doped carbon-based composite material including Fe and Co showed superiority to that of N-doped carbon-based composite material including Fe and Ni. The difference in the electrocatalytic performance for ORR is discussed regarding the difference in the specific surface area and the presence ratio of chemical bonding species.

In Situ Transmission Electron Microscopy Observation of Electrochemical Process Between Li–C Nanocomposites and Multilayer Graphene

AbstractPortable power supplies, particularly lithium‐ion batteries (LIBs), will play a key role in achieving sustainable development goals, and electrode active materials for the next generation of LIBs with higher energy density and longer life time is highly demanded. For this, in situ visualization of Li behavior during the charge/discharge process is essential, and transmission electron microscopy (TEM) will be promising for this purpose. Here, a quite simple experimental setup consisting of a newly developed Li–C nanocomposite film sputter‐deposited onto Au nanoprotrusions at room temperature and graphene synthesized on a W probe at 500 °C for the in situ TEM observation of the battery reaction is proposed. The preservation of the metallic Li in the Li–C film that is transferred to TEM without using any transfer vessels under atmospheric conditions is confirmed by high resolution TEM before the in situ electrochemical process in TEM. After the one cycle of the in situ electrochemical process, the intercalation of Li ions into graphene (lithiation) is clearly observed. Thus, it is concluded that the metallic Li stored in the Li–C film works well as the anode active material in the electrochemical process for solid state LIBs, implying the developed in situ experimental system is promising.

Influence of dynamic strain aging on low-cycle fatigue behavior in nano-sized κ-carbide strengthened FeMnAlC lightweight steel

The effects of dynamic strain aging (DSA) on the cyclic response and deformation behavior of a hot rolled Fe–22Mn–8Al–0.9C–0.02Nb (wt.%) lightweight steel have been investigated during strain-controlled low-cycle fatigue (LCF) tests at the temperature range of 25–400 °C. The initial microstructure consisted of a complete γ-matrix with nano-sized κ-carbides. During LCF testing, the cyclic stress amplitude displayed a monotonous softening until fracture at 25 °C, 100 °C, and 400 °C in all the investigated strain ranges (Δεt) of 0.8–2.2 %. However, at 200 °C and 300 °C, cyclic softening was followed by pronounced cyclic hardening. Notably, hysteresis loops at the cycle of half-life exhibited serrations in the flow stress at 200 °C and 300 °C. This indicated that cyclic hardening was attributed to the DSA phenomenon, which was confirmed by a negative strain rate sensitivity at 200 °C and 300 °C. A significant reduction in LCF life was observed under the DSA regime. During LCF testing, sequential transmission electron microscopic (TEM) observation indicated that deformation led to the formation of shear bands in multiple directions. Gliding of wavy dislocations was frequently observed at 200 °C compared to that at 25 °C, which resulted from the dragging effect by carbon solute atoms.

Enhanced photocatalytic antibacterial activity of Au-coated Ni–Ti–O nanotubes for biomedical applications

Nickel-titanium (NiTi) alloy is a smart material exhibiting superelasticity, contributing to low stiffness and facilitating integration with bone structures. However, NiTi alloy's bioactivity and antibacterial activity limit its dental applications. In this study, we fabricated nickel titanium oxide (Ni–Ti–O) nanotubes with the potential for bioactivity and photocatalytic properties on the surface of NiTi alloy. Specifically, we applied a coating of gold (Au) nanoparticles to the surface of Ni–Ti–O nanotubes, in order to leverage the antibacterial activity through the photocatalytic effect under 470 nm visible light. Field-emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HR-TEM) observations revealed that Au was deposited mainly at the top surface of Ni–Ti–O nanotubes (diameter: 12.76 ± 2.91 nm, height: 721.12 ± 50.25 nm). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and diffuse reflectance spectroscopy (DRS) analyses revealed that the Ni–Ti–O nanotubes were NiTiO3 crystalline phases with low crystallinity. Therefore, based on the methylene blue (MB) degradation test, the photocatalytic effect was only achieved under visible light at 470 nm, facilitated by the presence of Au. The antibacterial colony forming unit test and enzymatic activity tests demonstrated that Au-coated Ni–Ti–O nanotubes displayed excellent antibacterial activity under 470 nm visible light irradiation, which was also attributed to photocatalytic effect. Consequently, the combination of Au-coated Ni–Ti–O nanotubes and visible light-based photofunctionalization holds promise for expressing antibacterial properties in dental applications.