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At least 577 records · Page 32

Physics Discovery in Nanoplasmonic Systems via Autonomous Experiments in Scanning Transmission Electron Microscopy

Abstract Physics‐driven discovery in an autonomous experiment has emerged as a dream application of machine learning in physical sciences. Here, this work develops and experimentally implements a deep kernel learning (DKL) workflow combining the correlative prediction of the target functional response and its uncertainty from the structure, and physics‐based selection of acquisition function, which autonomously guides the navigation of the image space. Compared to classical Bayesian optimization (BO) methods, this approach allows to capture the complex spatial features present in the images of realistic materials, and dynamically learn structure–property relationships. In combination with the flexible scalarizer function that allows to ascribe the degree of physical interest to predicted spectra, this enables physical discovery in automated experiment. Here, this approach is illustrated for nanoplasmonic studies of nanoparticles and experimentally implemented in a truly autonomous fashion for bulk‐ and edge plasmon discovery in MnPS 3 , a lesser‐known beam‐sensitive layered 2D material. This approach is universal, can be directly used as‐is with any specimen, and is expected to be applicable to any probe‐based microscopic techniques including other STEM modalities, scanning probe microscopies, chemical, and optical imaging.

42 ENGINEERING↗

Atomic layer deposition of cerium oxide for potential use in diesel soot combustion

The particulate soot emission from diesel motors has a severe impact on the environment and people's health. The use of catalytic convertors is one of the ways to minimize the emission and decrease the hazard level. In this paper, the activity of cerium oxide for catalytic combustion of diesel soot was studied. Thin films of cerium dioxide were synthesized by atomic layer deposition using tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)cerium [Ce(thd){sub 4}] and ozone as precursors. The characteristics of the films were studied as a function of deposition conditions within the reaction temperature range of 180–350 °C. Thickness, crystallinity, elemental composition, and morphology of the CeO{sub 2} films deposited on Si (100) were characterized by ellipsometry, x-ray diffraction, x-ray photoelectron spectroscopy, atomic force microscopy, and field emission scanning electron microscopy, respectively. The growth rate of CeO{sub 2} was observed to be 0.30 Å/cycle at temperatures up to 250 °C with a slight increase to 0.37 Å/cycle at 300 °C. The effect of CeO{sub 2} films grown on stainless steel foil supports on soot combustion was measured with annealing tests. Based on the analysis of these, in catalytic applications, CeO{sub 2} has been shown to be effective in lowering the soot combustion temperature from 600 °C for the uncoated substrates to 370 °C for the CeO{sub 2} coated ones. It was found that the higher deposition temperatures had a positive effect on the catalyst performance.

36 MATERIALS SCIENCE↗

Examination of Lunar Regolith Simulants By SEM-EDS and Imaging Raman Spectroscopy

The Artemis series lunar missions will include sample returns from the lunar south pole. Lunar regolith simulants (RS) generated in the lab provide opportunities to compare two surface science techniques: scanning electron microscopy (SEM-EDS) and Raman induced surface spectroscopy. The results will also be applicable for supporting future commercial lunar payload services (CLPS) and Artemis surface. Surface characterization contributes to continued development of lunar regolith studies and adds to various regolith databases. In characterizing various lunar regolith simulants, part of the aim should be to standardize techniques and utilize anticipated methods available for astromaterials studied during, or returned from, upcoming missions, particularly samples collected from the Moon’s south pole and permanently shadowed regions (PSRs).. An initial survey of available simulants has been started with Raman scanning process for particle counting the results of which will enrich the NASA-JSC Simulant Development Lab (SDL) simulant properties database and the Colorado School of Mines Planetary Simulant Data Base. An SEM-EDS dataset of raw regolith simulant materials are collected.

Raman Microscopy↗

The role of Sr doping on structure and microstructural properties of LaFeO{sub 3}

The doping of Strontium in LaFeO{sub 3} and its influence on the structural and microstructure properties were studied thoroughly. A few sets of Sr doping in La{sub (1-x)}Fe{sub x}O{sub 3}, where x=0.00, 0.02, and 0.06 were made through the solution combustion synthesis method using urea as fuel. X-ray diffraction was applied to get information about the structure and purity. The Rietveld refinement on X-ray diffraction peaks have been done, in order to calculate various structural parameters. The morphology of La{sub (1-x)}Sr{sub x}FeO{sub 3} nanoscale particles has been confirmed by field emission scanning electron microscopy (FESEM) technique. Differential scanning calorimetry (DSC) signals demonstrated the antiferromagnetic to paramagnetic transition (T{sub N}). The FTIR spectra was provided the information about various vibration modes in samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Acid resistance and corrosion protection potential of concrete prepared with alkali aluminosilicate cement

An experimental investigation was conducted on two key aspects of the durability characteristics of concrete materials prepared with an alkali aluminosilicate hydraulic cement and with Portland cement, both cured at room temperature. The durability characteristics evaluated concerned the acid resistance of concrete, and its ability to protect the embedded reinforcing steel against corrosion under wet-dry cycles. Acid resistance was evaluated through monitoring of mass and strength change over time under acid attack, visual observations, and scanning electron microscopy (SEM). Corrosion resistance was evaluated through measurement of the corrosion potential, visual observations and scanning electron microscopy. The acid resistance and corrosion protection potential of the concrete prepared with the alkali aluminosilicate cement were found to be superior to those of Portland cement concrete.

42 ENGINEERING↗

Mechanism of action and in vitro activity of short hybrid antimicrobial peptide PV3 against Pseudomonas aeruginosa

Antimicrobial peptides are attractive candidates for developing novel therapeutic agents, since they are lethal to a broad spectrum of pathogens and have a unique low tendency for resistance development. In this study, mechanism of action and in vitro anti-pseudomonal activity of previously designed short hybrid antimicrobial peptide PV3 were investigated. Compared to ceftazidime, PV3 had not only higher antibacterial activity but also faster bactericidal activity. PV3 reduced biofilm biomass and viability of biofilm embedded bacteria in a concentration-dependent manner. Although the antimicrobial activity of PV3 was reduced in Mueller-Hinton broth (MHB) containing human serum, it was still active enough to eradication of bacteria at low concentrations. Compared with standard condition (MHB only), there was no significant decrease in antibacterial activity of PV3 against P. aeruginosa strains under 150 mM NaCl (p = 0.615) and 1 mM MgCl{sub 2} (p = 0.3466). Fluorescence microscopy and field emission scanning electron microscopy further indicated that PV3 killed bacteria by disrupting the cell membrane. Since PV3 has potent anti-pseudomonal activity and has little cytotoxicity in vitro, it seems plausible that the peptide should be further investigated with animal studies to support future pharmacological formulations and potential topical applications. - Highlights: • PV3 killed Pseudomonas aeruginosa by membrane-disrupting mechanism. • PV3 reduced biofilm biomass and viability of biofilm embedded bacteria in a concentration-dependent manner. • Short hybrid antimicrobial peptide PV3 exhibited higher and faster bactericidal activity comparing to ceftazidime.

60 APPLIED LIFE SCIENCES↗

Reinforcing blade-cast photocatalytic-titania thin film by titanate nanotubes

Highlights: • Suspension-based photocatalysts are inferior to thin-films due to separation issues. • Hydrothermal TiO{sub 2} nanotubes and sol-gel Ti(n-OBu){sub 4} blends were tape casted on glass. • Optimum blend composition yields mechanical stability due to the tubes reinforcing effect. • At optimum gel content the nanotube bundles are smoothed without stabilizers added. • Surface accessibility and mass transfer dominate the photocatalytic dye degradation. - Abstract: Titanate nanotubes/titania gel blends were prepared as composite sol-gel material, deposited on a glass substrate using a doctor blade and calcined in order to create thin films. In order to get an insight in titania nanotubes’ ability to reinforce thin films, drying control chemical agents were not used. The effects of titanate nanotubes to titanium n-butoxide ratio on surface morphology, phase composition, mechanical stability and photocatalytic activity were studied. Characterization of the thin films was carried out by means of optical and scanning electron microscopy, powder X-ray diffraction, synchrotron radiation grazing incidence X-ray diffraction and mechanical stability testing. Photocatalytic properties of the obtained thin films were evaluated on the basis of methylene blue degradation. Moderate blends exhibit favourable microstructural features while the dye degradation rate was greater for films with a greater amount of titanate nanotubes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Quantitative phase retrieval and characterization of magnetic nanostructures via Lorentz (scanning) transmission electron microscopy

Magnetic materials phase reconstruction using Lorentz transmission electron microscopy (LTEM) measurements have traditionally been achieved using longstanding methods such as off-axis holography (OAH) fast-Fourier transform technique and the transport-of-intensity equation (TIE). The increase in access to processing power alongside the development of advanced algorithms have allowed for phase retrieval of nanoscale magnetic materials with greater efficacy and resolution. Specifically, reverse-mode automatic differentiation (RMAD) and the extended electron ptychography iterative engine (ePIE) are two recent developments of phase retrieval that can be applied to analyzing micro-to-nano- scale magnetic materials. This work evaluates phase retrieval using TIE, RMAD, and ePIE in simulations of Permalloy (Ni 80 Fe 20 ) nanoscale islands, or nanomagnets. Extending beyond simulations, we demonstrate total phase retrieval and image reconstructions of a NiFe nanowire using OAH and RMAD in LTEM and ePIE in Lorentz-mode-4D scanning transmission electron microscopy experiments and determine the saturation magnetization through corroborations with micromagnetic modeling. Finally, we demonstrate the efficacy of these methods in retrieving the total phase and highlight its use in characterizing and analyzing the proximity effect of the magnetic nanostructures.

Lorentz transmission electron microscopy↗

Tribological Behavior of Electrochemically Etched AISI 316 Stainless Steel with a Textured Surface

In this work, AISI 316 stainless steel (316 SS) was electrochemically etched in four NaCl solutions (10, 15, 20, and 25 wt.%) to form textured surfaces. Surface morphologies, three-dimensional surface topographies, and surface profiles of the textured 316 SS samples were obtained by scanning electron microscopy (SEM) and laser scanning confocal microscope (LSCM). Sliding friction tests of the textured 316 SS samples were conducted in air and under grease lubrication. The results suggested that the variable degrees of microtextured surfaces after electrochemical etching in 10, 15, and 20 wt.% NaCl solutions. The 316 SS samples etched in 15 and 20 wt.% NaCl solutions showed more promising tribological performance than other samples, as reflected by their friction coefficients, mass loss per unit distance traveled (mg/m), and wear morphologies.

36 MATERIALS SCIENCE↗

Characterization of Micro-arc Oxidation Coatings on 6N01 Aluminum Alloy Under Different Electrolyte Temperature Control Modes

The micro-arc oxidation coatings of 6N01 aluminum alloy produced under different control modes of the electrolyte temperature are discussed in detail. Compared to those coated by a thermostatically controlled treatment, the coatings had different surface characterizations when they were coated without controlling the electrolyte temperature, particularly after treatment involving boiling electrolytes. Scanning electron microscopy and confocal laser scanning microscopy were used to observe the morphology of the coatings. Energy-dispersive spectrometry and x-ray diffractometer were used to characterize their elemental and crystalline phase compositions. The results indicate that the treatment without a controlled electrolyte temperature ultimately led to a thicker and rougher film with a respectably thick inner barrier film, a lower content of γ-Al{sub 2}O{sub 3} and better corrosion resistance.

36 MATERIALS SCIENCE↗

Effect of Friction Stir Processing on the Microhardness, Wear and Corrosion Behavior of Al6061 and Al6061/SiO{sub 2} Nanocomposites

An effect of the friction stir processing (FSP), its pass numbers and addition of the SiO{sub 2} nanoparticles on microhardness, wear behavior and corrosion performance of the Al6061 aluminum alloy was investigated. Scanning electron microscopy (SEM) and optical microscopy were utilized to characterize the microstructure of the alloy, FSPed and composite samples. SEM observations revealed that the SiO{sub 2} particles were not uniformly dispersed in the matrix after two passes of FSP. However, increasing the pass number more than two passes resulted in a great improvement in the distribution of the SiO{sub 2} particles. The application of FSP led to overall softening compared to the base metal. Softening of the Al6061 alloy was probably attributed to the coarsening of Mg{sub 2}Si. Corrosion resistance of the FSPed samples found a significant reduction compared to the base metal. Applying higher pass number of the process and also addition of the SiO{sub 2} nanoparticles improved the wear behavior of the samples.

36 MATERIALS SCIENCE↗

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe{sub 3}O{sub 4} particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO{sub 2} at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

36 MATERIALS SCIENCE↗

Synthesis of CS/PVA Biodegradable Composite Nanofibers as a Microporous Material with Well Controllable Procedure Through Electrospinning

In this study, we have showed a facile route for fabrication of a novel microporous material based on chitosan (CS) and poly(vinyl alcohol) (PVA) biodegradable nanofibers that have high specific surface area, considerable porosity, and small diameter. Scanning electron microscopy, thermogravimetric analysis, differential scanning calorimetry, fourier transform infrared spectroscopy, Brunauer–Emmett–Teller surface area analysis, and CHNS/O elemental analyser were applied to characterize the fabricated CS/PVA composite nanofibers. Moreover, the influences of spinning conditions including concentration, voltage, electrospinning distance, and flow rate, on size distribution and pore diameter of the final product were systematically studied using 2{sup k−1} factorial design experiments, and the response surface optimization was used for determining the best synthesis parameter. The results obtained from 2{sup K−1} factorial design experiments showed that electrospinning parameters influenced the size distribution and pore diameter of the CS/PVA microporous material. Based on the response surface methodology, the CS/PVA product could be obtained with a high microporous diameter of 1.8 nm and a small diameter distribution of 15.0 nm under optimized conditions. The obtained results showed that the fabricated samples could be utilized in different applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microstructure Stability During Creep of Friction Stir Welded AA2024-T3 Alloy

The poor weldability of the AA2024 aluminum alloy limits its use in industrial applications. Because friction stir welding (FSW) is a non-fusion welding process, it seems to be a promising solution for welding this alloy. In the current study, FSW was applied to butt weld AA2024-T3 aluminum alloy plates. Creep tests were conducted at 250 and at 315 °C on both the parent material and the friction stir welded specimens. The microstructures of the welded and non-welded AA2024-T3 specimens before and after the creep tests were studied and compared. A comprehensive transmission electron microscopy study together with a high-resolution scanning electron microscopy study and energy-dispersive x-ray spectroscopy analysis was conducted to investigate the microstructure stability. The parent material seems to contain two kinds of Cu-rich precipitates—coarse precipitates of a few microns each and uniformly dispersed fine nanosized precipitates. Unlike the parent material, the crept specimens were found to contain the two kinds of precipitates mentioned above together with platelet-like precipitates. In addition, extensive decoration of the grain boundaries with precipitates was clearly observed in the crept specimens. Controlled aging experiments for up to 280 h at the relevant temperatures were conducted on both the parent material and the welded specimens in order to isolate the contribution of exposure to high temperatures to the microstructure changes. TEM study showed the development of dislocation networks into a cellular dislocation structure in the case of the parent metal. Changes in the dislocation structure as a function of the creep strain and the FSW process were recorded. A detailed creep data analysis was conducted, taking into account the instability of the microstructure.

36 MATERIALS SCIENCE↗

The modification of BaCe{sub 0.5}Zr{sub 0.3}Y{sub 0.2}O{sub 3–δ} with copper oxide: Effect on the structural and transport properties

The effect of the content of CuO additive on the sinterability, phase composition, microstructure, and electrical properties of BaCe{sub 0.5}Zr{sub 0.3}Y{sub 0.2}O{sub 3–δ} proton-conducting material is studied. Ceramic samples were produced by the citrate–nitrate synthesis method with the addition of 0, 0.25, 0.5, and 1% CuO. It is shown that the relative density of the samples containing 0.5 and 1% CuO is higher than 94% at a sintering temperature of 1450°C, whereas the relative density of the material is no higher than 85% at a lower content of the sintering additive. From the data of X-ray diffraction analysis and scanning electron microscopy, it is established that the introduction of a small CuO content (0.25%) is inadequate for single-phase and high-dense ceramics to be formed. The conductivity and scanning electron microscopy data show that the sample with BaCe{sub 0.5}Zr{sub 0.3}Y{sub 0.2}O{sub 3–δ} + 0.5% CuO composition possesses high total and ionic conductivities as well as a high degree of microstructural stability after hydrogen reduction of the ceramics. The citrate–nitrate method modified by the introduction of a small CuO content can be recommended for the production of single-phase, gas-tight, and high-conductivity electrolytes based on both BaCeO{sub 3} and BaZrO{sub 3}.

36 MATERIALS SCIENCE↗

Effects of Solution Treatment on Microstructure Transformation, Tensile and Exfoliation Corrosion Properties of 7136 Aluminum Alloy

The effects of solution treatment on microstructure transformation and tensile properties of 7136 aluminum alloys were investigated by means of scanning electron microscopy, electron backscatter diffraction, differential scanning calorimeter, x-ray diffraction and tensile test, electrochemical evaluations, exfoliation corrosion tests, respectively. The results indicate that solution treatment had a significant effect on the microstructure transformation and tensile properties. Soluble constituents of 7136 aluminum alloys were more likely to form the η(MgZn{sub 2}) phase rather than the S(Al{sub 2}CuMg) phase. With increasing the solution temperature, the η phase was re-dissolved into the α(Al) matrix gradually. After solution treatment of 475 °C/1 h, the η phase was completely dissolved into the matrix, with insoluble Fe-rich phases remained. The dissolution of η phase would increase the strength and the corrosion resistance of the alloys. When continuing to increase the solution temperature, the recrystallized fraction increased obviously, resulting in the decrease in the strength and the corrosion resistance. Consequently, the strength and the corrosion resistance of the alloys increased firstly and then decreased with the increase in solution temperature. After solution treatment of 475 °C/1 h, the tensile strength and yield strength of the aged alloy reached their peaks, 738 and 715 MPa, respectively. The elongation of the alloy solution treated at 475 °C/1 h reached 11.2%, and its exfoliation corrosion rating got EB level. Furthermore, after the double-stage solution treatment of 450 °C/1 h + 475 °C/1 h, the recrystallized fraction decreased, resulting in a slight increase to 12.6% of the elongation, a slight increase in the corrosion resistance and a slight decrease in the strength.

36 MATERIALS SCIENCE↗

Characterization of stress corrosion cracks in Ni-based weld alloys 52, 52M and 152 grown in high-temperature water

Ni-based weld alloys 52, 52M and 152 are extensively used in repair and mitigation of primary water stress corrosion cracking (SCC) in nuclear power plants. In the present study, a series of microstructure and microchemistry at the SCC tips of these alloys were examined with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), scanning transmission electron microscopy (STEM) and energy filtered transmission electron microscopy (EFTEM). The specimens have similar chemical compositions and testing conditions. Intergranular (IG) and transgranular (TG) SCC was observed in all of them. The cracks were filled with nickel-oxides and partial precipitations of chrome carbides (CrCs), niobium carbides (NbCs), titanium nitrides (TiNs) and silicon carbides (SiCs), while iron (Fe) was largely dissolved into the solution. However, the crack densities, lengths and distributions were different for all three specimens. - Highlights: • Microstructure and microchemistry at the SCC tips of Ni-based weld alloys 52, 52M and 152 were examined. • The crack densities, lengths and distributions were found to be different for different alloys. • IGSCC and TGSCC were observed on alloy 52, only TGSCC was observed on alloy 52M and 152. • The cracks were filled by Ni-oxides and precipitated CrCs, NbCs, TiNs and SiCs.

36 MATERIALS SCIENCE↗