Toll-like receptor (TLR)-mediated inflammatory processes play a critical role in the innate immune response during the initial interaction between the infecting microorganism and immune cells. This study aimed to investigate the possible microanatomical and histological differences in mandibular and bronchial lymph nodes in Akkaraman and Romanov lambs induced by lipopolysaccharide (LPS) and lipoteichoic acid (LTA) and study the gene, protein, and immunoexpression levels of TLR4, myeloid differentiation factor 88 (MyD88), and tumor necrosis factor-α (TNF-α) that are involved in the immune system. Microanatomical examinations demonstrated more intense lymphocyte infiltration in the bronchial lymph nodes of Akkaraman lambs in the LPS and LTA groups compared to Romanov lambs. TLR4, MyD88, and TNF-α immunoreactivities were more intense in the experimental groups of both breeds. Expression levels of MyD88 and TNF-α genes in the bronchial lymph node of Akkaraman lambs were found to increase statistically significantly in the LTA group. TLR4 gene expression level in the mandibular lymph node was found to be statistically significantly higher in the LTA + LPS group. In conclusion, dynamic changes in the immune cell populations involved in response to antigens such as LTA and LPS in the lymph nodes of both breeds can be associated with the difference in the expression level of the TLR4/MyD88/TNF-α genes.

Grain refinement has been applied to enhance the materials strength for miniaturization and lightweight design of nuclear equipment. It is critically important to investigate the low-cycle fatigue (LCF) properties of grain refined 316LN austenitic stainless steels for structural design and safety assessment. In the present work, a series of fine-grained (FG) 316LN steels were produced by thermo-mechanical processes. The LCF properties were studied under a fully reversed strain-controlled mode at room temperature. Results show that FG 316LN steels demonstrate good balance of high strength and high ductility. However, a slight loss of ductility in FG 316LN steel induces a significant deterioration of LCF life. The rapid energy dissipation in FG 316LN steels leads to the reduction of their LCF life. Dislocations develop rapidly in the first stage of cycles, which induces the initial cyclic hardening. The dislocations rearrange to form dislocations cell structure resulting in cyclic softening in the subsequent cyclic deformation. Strain-induced martensite transformation appears in FG 316LN stainless steels at high strain amplitude (Δε/2 = 0.8%), which leads to the secondary cyclic hardening. Moreover, a modified LCF life prediction model for grain refined metals predicts the LCF life of FG 316LN steels well.

Fe–Al–O ODS alloy prepared via mechanical alloying was subjected to three different heat treatments. Material basic state exhibited a fine-grained (300–500 nm) microstructure with fine dispersion of aluminum oxide particles (60% up to 20 nm). Heat treatment at 1100 °C for 3 h resulted in local grain and particles coarsening. Prolongation of the heat treatment to 24 h resulted in further grain (50 % up to 5 μm) and particle (25 % with size 25–40 nm) coarsening. Annealing at 1200 °C for 24 h led to a bimodal microstructure (35 % of grains with size 100–250 μm and 45 % of particles with size 30–60 nm) and substantial oxide particle coarsening. Microstructural changes resulted in tensile strength decrease and ductility increase. Tensile tests at 800 °C revealed a 90% decrease of tensile strength while ductility increased 4–6 times when compared to the room temperature tests. The hardening ratio was below 10 % for all the alloys and both test temperatures.

An electrochemical cell was designed to enable in situ atomic force microscopy (AFM) measurements. The finite-element method was implemented using COMSOL Multiphysics to simulate the electrical field within the cell and to find the current and potential distribution. A comparative three-dimensional simulation study was made to compare two different designs and to elucidate the importance of the geometry on the electrical field distribution. The design was optimized to reduce the uncertainty in the measurement of the electrochemical impedance. Then, an in situ, simultaneous electrochemical and time-resolved AFM experiments were conducted to study the surface evolution of the aluminum alloy AA2024-T3 exposed to 0.5 M NaCl. The temporal change of the surface topography was recorded during the application of chrono-amperometric pulses using a newly designed electrochemical cell. Electrochemical impedance spectroscopy was conducted on the sample to confirm the recorded topographical change. The newly developed cell made it possible to monitor the surface change and the growth of the oxyhydroxide layer on the AA2024-T3 with the simultaneous application of electrochemical methods.

Hot deformation and softening response for the titanium aluminide Ti–48Al–2V–0.2B has been investigated. The deformation response to softening mechanisms has been examined. Deformation experiments were carried out in the strain rate range 0.01–10 s−1 keeping the temperature constant at 1200 °C and in the temperature range 1000–1200 °C at the strain rate 1 s−1. With an increase in strain rate, the microstructural changes associated with the softening mechanism include breaking of the lamellae, spheroidization of the broken laths and dynamic recrystallization. For the strain rate 1 s−1, deformation in the (α2 +γ) phase field leads to fine recrystallized grains, remnant lamellae and cavitation along the grain boundaries (for temperatures 1000 and 1100 °C). Deformation in the (α +γ) phase field leads to dynamic recrystallization at the shear bands, within the lamellae, breaking and rotation of the α phase during the continuous increase in the deformation strain.

Silicon electrodes with the columnar macroporous structure were investigated to determine the effect of variations in the columnar pore morphology on lithiation and energy storage capacity in Li-ion cells. Several variants of macroporous Si columnar electrodes were electrochemically cycled against the Li reference electrode. The changes in macro-pore size and Si wall thickness of the columnar architecture greatly affected the cyclic Li storage and discharge capacities. A strong correlation of the Li-storage capacity with the ratio of Si wall thickness to pore diameter is found to exist. Specifically, one columnar Si electrode with an optimum macroporous structure exhibited a very high reversible specific capacity of ~1250 mAh/g (total capacity 1.2 mAh/cm2) for over 200 cycles. Electron microscopy revealed that the high reversible Li-storage capacity is due to the macropores accommodating the change in volume of lithiation and providing nearly complete reconstruction of Si walls upon delithiation. The present observations can lead to practical, high-capacity, and damage-resistant Si electrodes for Li-ion batteries.

Meteorites have one of the most unique and beautiful microstructures, the Widmanstätten structure. This consists of large, elongated bands which form an intricate octahedral lace of crystalline metal. This structure makes meteorites an ideal case to demonstrate the capabilities of mechanical phase mapping using high-speed nanoindentation. In this work, the mechanical properties and composition of the Taza meteorite were mapped using ~100,000 indentations to statistically determine the properties of the individual phases. Five microstructural phases were characterized in this meteorite: Kamacite, Plessite, Tetrataenite, Cloudy Zone, and Schreibersite. Mechanical phase identification was confirmed using EDX measurements, and the first direct, point-to-point correlation of EDX and large-scale indentation maps was achieved. Mechanical phase maps showed superior phase contrast to EDX in two phases. An indentation property map or a mechanical phase map using a 2D histogram was used to visualize and statistically characterize the phases and identify trends in their relationships.

We describe experimental approaches to real time examination of the microstructural evolution of Ti 6%Al 4%V upon cooling from above the beta transus (~995 °C) while imaging in the scanning electron microscope. Ti 6%Al 4%V is a two phase, α+β titanium alloy with high strength and corrosion resistance. The β →α transformation on cooling can give rise to different microstructures and properties through various thermal treatments. Fully lamellar microstructures, bi-modal microstructures, and equiaxed microstructures can each be obtained by accessing different cooling rates upon the final treatment above the beta temperature, each resulting in uniquely enhanced material properties.

Utilizing the capabilities of a heating/ tensile stage developed by Kammrath & Weiss Inc., are able to apply real-time imaging techniques in the scanning electron microscope to monitor the development of the microstructure. Annealing temperatures up to 1100 °C are attainable, with cooling rates ranging from 0.1 ° C per second to 3.3 °C per second. This has allowed us to directly observe the formation of lamellae at different annealing temperature/ cooling rate combinations to determine the lamellar microstructure width, separation, and colony size.

The binary metal oxides are increasingly used as supercapacitor electrode materials in energy storing devices. Particularly NiCo2O4 has shown promising electrocapacitive performance with high specific capacitance and energy density. The electrocapacitive performance of these oxides largely depends on their morphology and electrical properties governed by their energy band-gaps and defects. The morphological structure of NiCo2O4 can be altered via the synthesis route, while the energy band-gap could be altered by doping. Also, doping can enhance crystal stability and bring in grain refinement, which can further improve the much-needed surface area for high specific capacitance. Given the above, this study evaluates the electrochemical performance of Ca-doped Ni1-xCaxCo2O4 (0 ≤ x ≤ 0.8) compounds. This stipulates promising applications for electrodes in future supercapacitors.

Investigations of the crystallization of aluminosilicate phases within Hanford nuclear waste glasses typically involve subjecting samples to the canister centerline cooling (CCC) schedule. This cooling schedule is representative of the slowest cooling thermal profile which these glasses will experience after the glass is poured into the high level waste (HLW) container. However, few investigations have observed how the crystallization behavior changes by varying the heat treatment schedule. In the present study, three Hanford HLW glasses are subjected to CCC and isothermal heat treatments (IHT) to better understand the evolution of phases and the chemical partitioning due to temperature schedule. Samples were characterized using electron probe microanalysis, X-ray diffraction, micro X-ray fluorescence, and micro X-ray absorption spectroscopy. From IHT, eucryptite and apatite phases were observed which were not observed during CCC. Spatially-resolved measurements demonstrated that the oxidation state of the iron was similar among glass and crystal, and we suggest a mechanism to describe the compositional fluctuations near the crystal-glass interface which influence crystallization.

In this study, biological hydroxyapatite (HAp) was synthesized from catfish (Pangasius hypophthalmus) bones. First, the as-received catfish bones were de-proteinized in open air, and then converted to HAp by a solid state heat treatment method at a temperature of 900 °C for a holding time of 2 h in a muffle furnace. X-ray diffraction (XRD) analysis confirmed that HAp with high crystallinity of 99.9% was formed matching the structural properties of flouro-apatite with crystallite sizes of approximately 37.1 nm. The morphology of the HAp prepared showed irregularly shaped particles and revealed the appearance of open pores with a less agglomerated structure and a Ca/P ratio of about 1.58. The specific mechanical properties: hardness, compressive strength and fracture toughness of the catfish derived scaffolds were recorded as 480 MPa, 1.92 MPa, and 5.72 Mpa.m1/2, respectively. The fracture toughness of the HAp derived scaffolds suggests that the produced biomaterial is promising for biomedical applications. These findings are useful for the production and application of the HAp powders prepared from catfish bones, and further suggests a possible low-cost route for producing inexpensive ceramics using natural catfish bones.

We report a simple and feasible technique for the formation of well-distributed nickel nanodot arrays on both oxidized and unoxidized silicon substrate by a conventional annealing process. The shape and distribution of nickel nanodots were maintained by adjusting annealing temperature, time and the SiO2 buffer layer thickness in between nickel film and the silicon substrate. The diffusion of nickel into the silicon is significantly reduced when the nickel film on the oxidized silicon substrate is annealed at high temperature. From this conventional annealing technique, we achieve a maximum nickel nanodots density up to (7.94±1.92) nanodot counts/µm2 on the oxidized silicon substrate with a well-defined spherical shape by adjusting the thickness of nickel film as well as buffer SiO2 layer. In the next experiment, the surface charge distribution on the nickel nanodot arrays were characterized through the Kelvin probe force microscope (KPFM) on tapping mode. It is found that the nickel nanodots can store and release the electric charges under an applied bias voltage.

LiNi0.5Mn1.5O4 cathode material, which has a higher working voltage (4.7 v) than NCM and a moderate specific capacity (148 mAh/g theoretical), has been studied to understand the source of capacity fade during the first 100 cycles in a half cell. The work mainly consisted of high resolution TEM observations and analysis of the surface microstructural properties, before and after cycling. We found that the pristine material consisted almost entirely of large FCC spinal domains but with cycling appears small simple cubic spinel domains at the surface. It is proposed that these small changes of the surface microstructure leads to impedance rise that results in the premature arrival to the upper cutoff voltage of 4.85V during charging and the subsequent loss of capacity with cycling.

P-type NiO powders with an average crystallite size of 16 nm as shown by x-ray diffraction analysis were produced via biosynthesis using cactus plant extract. SEM showed that the NiO powders consisted of particles with sizes in the 20-35 nm range. A cyclic voltammetric study of the NiO nanopowders showed a quasi-reversible redox processes with the NiO powder showing potential for pseudo capacitance. Through these findings the use of natural Cactus extracts is hereby shown to be a cost-effective and environmentally friendly alternative for preparing Nickel oxide nanosized powders that can be of use in a variety of energy storage applications.

Functional polymers were previously employed to minimize the susceptibility of metallic nanoparticles (MNPs) for aggregation. Herein, we intended to conjugate catechol moiety into the polymer chain end considering its anchoring ability to virtually most surfaces. Accordingly, catechol end-functionalized polysarcosine (cat-PSar) was successfully prepared from the ring-opening polymerization (ROP) of sarcosine N-carboxyanhydrides (Sar-NCA) using dopamine hydrochloride initiator. ROP of Sar-NCA was carried out at different monomer to initiator feed ratios. The molecular structure of cat-PSar was confirmed by 1H NMR and MALDITOF. Afterward, the obtained catechol functionalized polymer was used for in-situ synthesis and stabilization of silver nanoparticles (Ag-NPs) in aqueous solution. The observed characteristic absorption peak at λmax of 415 nm indicates the formation of Ag-NPs. Scanning electron microscope (SEM) images also elucidate the formation of Ag-NPs with the relatively small sizes of the nanocomposite at a high concentration of silver nitrate. Hence, biomimetic polymers could play a dual role as reducing and stabilizing agents in the preparation of monodispersed MNPs.

This overview is meant to help newer microscopists decide on an appropriate high-resolution method for nanoscale and microscale materials characterization. The operating principles, capabilities, and resolution of scanning electron microscopy (SEM) and atomic force microscopy (AFM), as well as the needs for sample preparation and the constraints imposed on the sample environment within the microscope, are compared and contrasted. This is followed by a similar assessment of the merits and challenges of transmission electron microscopy (TEM).

A major limitation in nanoindentation analysis techniques is the inability to accurately quantify pile-up/sink-in around indentations. In this work, the contact area during indentation is determined simultaneously using both contact mechanical models and direct in situ observation in the scanning electron microscope. The pile-up around indentations in materials with low H/E ratios (nanocrystalline nickel and ultrafine-grained aluminum) and the sink-in around a material with a high H/E ratio (fused silica) were quantified and compared to existing indentation analyses. The in situ projected contact area measured by Scanning Electron Microscopy using a cube-corner tip differs significantly from the classical models for materials with low H/E modulus ratio. Using a Berkovich tip, the in situ contact area is in good agreement with the contact model suggested by Loubet et al. for materials with low H/E ratio and in good agreement with the Oliver and Pharr model for materials with high H/E ratio.

Nowadays, hierarchical materials have received tremendous interests because of their unique physical and chemical properties. In this article, a novel and facile particle aggregation method was used to fabricate vertically aligned diamondoid nanowires and hierarchical branched nanowire cluster array by using an electrophoresis template method. Triamantane, a three-cage diamondoid, was applied as raw material in current research. Diamondoids are nanometer-sized, hydrogen-terminated diamond-like, saturated hydrocarbons, which process great potential in nanotechnology due to biocompatibility and ultrahard nature. By electrophoresis template method, triamantane molecules dissolved in toluene were transferred into a porous alumina template by electric field and form the one-dimensional (1D) nanostructure with high aspect ratio. After that, a two-step thermal treatment was applied to the nanowires to achieve hierarchical branched nanowires. The surface morphologies of triamantane nanowire array with different treatments were characterized by scanning electron microscopy. This approach opens a new avenue for mass production of the vertically aligned diamondoid nanowires and hierarchical branched nanowire cluster arrays.