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Structure-property relationships and mobility optimization in sputtered La-doped BaSn O 3 films: Toward 100cm 2 V -1 s -1

he wide band gap semiconducting perovskite BaSnO 3 is of high current interest due to outstanding room temperature mobility at high electron density, fueled by potential applications in oxide, transparent, and power electronics. Due in part to a lack of lattice-matched substrates, BaSnO 3 thin films suffer from high defect densities, however, limiting electron mobility. Additionally, the vast majority of BaSnO 3 thin film research has focused on pulsed laser deposition or molecular beam epitaxy. In this work, we present an exhaustive optimization of the mobility of Ba 0.98 La 0.02 SnO 3 films grown by a scalable, high-throughput method: high-pressure-oxygen sputter deposition. Considering target synthesis conditions, substrate selection, buffer layer structure, deposition temperature, deposition rate, thickness, and postdeposition annealing conditions, and by combining high-resolution x-ray diffraction, reciprocal space mapping, rocking curve analysis, scanning transmission electron microscopy, atomic force microscopy, and temperature-dependent electronic transport measurements, detailed understanding of synthesis-structure-property relationships is attained. Optimized room temperature mobility of 96 cm 2 V –1 s –1 is achieved in vacuum-annealed GdScO 3 (110)/BaSnO 3 (120 nm)/Ba 0.98 La 0.02 SnO 3 (200 nm) heterostructures, as well as 92 cm 2 V –1 s –1 on unbuffered substrates and 87 2 V –1 s –1 without postdeposition annealing. These results, including important trends in defect densities and a surprising dependence of mobility on lattice mismatch, substantially expand the understanding of the interplay between deposition conditions, microstructure, and transport in doped BaSnO 3 films, establishing competitive mobilities in films fabricated via a scalable, high-throughput, industry-standard technique.

36 MATERIALS SCIENCE↗

Microstructural, nanomechanical, and microtribological properties of Pb thin films prepared by pulsed laser deposition and thermal evaporation techniques

In this work, the authors compare the morphological, structural, nanomechanical, and microtribological properties of Pb films deposited by thermal evaporation (TE) and pulsed laser deposition (PLD) techniques onto Si (111) substrates. Films were investigated by scanning electron microscopy, surface probe microscopy, and x-ray diffraction in θ-2θ geometry to determine their morphology, root-mean-square (RMS) roughness, and microstructure, respectively. TE films showed a percolated morphology with densely packed fibrous grains while PLD films had a granular morphology with a columnar and tightly packed structure in accordance with the zone growth model of Thornton. Moreover, PLD films presented a more polycrystalline structure with respect to TE films, with RMS roughness of 14 and 10 nm, respectively. Hardness and elastic modulus vary from 2.1 to 0.8 GPa and from 14 to 10 GPa for PLD and TE films, respectively. A reciprocal friction test has shown that PLD films have lower friction coefficient and wear rate than TE films. Our study has demonstrated for first time that, at the microscale, Pb films do not show the same simple lubricious properties measured at the macroscale.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of Si on the Formation and Growth of Intermetallic Compounds at Roll-Bonded Aluminum–Steel (Al-St) Interface

The formation and growth of intermetallic compounds (IMC) were investigated using the Al-St clad materials with additional different Si content to aluminum and steel substrate by differential scanning calorimetry, scanning electron microscopy and energy-dispersive x-ray spectroscopy, x-ray diffraction and transmission electron microscopy. The addition of Si to Al (Al-0.8Si/St) can drastically delay the formation of IMC and accelerate the growth of IMC layer. The Si (Al-0.8Si/St) segregates at the interface and inhibits the diffusion of Al atom to steel before the IMC forms, which further decreases the diffusion depth of Al in the steel layer. By contrast, the addition of Si to St (Al/St-0.8Si) has limited impact on delaying the formation and decelerating the growth of IMC layer. The Si (Al/St-0.8Si) hardly affects the diffusion of Fe atom to the aluminum layer. Among the four clad materials, the major IMC layer (η-Fe{sub 2}Al{sub 5}) always exhibits the parabolic growth phenomenon. The addition of Si cannot influence the phase compositions of IMC at the interface between the η-Fe{sub 2}Al{sub 5} layer and the aluminum. However, we observe an extra Fe-rich phase β{sub 1}-Fe{sub 3}Al at the interface between the Fe{sub 2}Al{sub 5} layer and steel substrate in the Al-0.8Si/St clad material.

36 MATERIALS SCIENCE↗

Retaining Geochemical Signatures during Aragonite-Calcite Transformation at Hydrothermal Conditions

Transformation of aragonite, a mineral phase metastable at Earth’s surface, to calcite widely occurs in both sedimentary and metamorphic systems with the presence of an aqueous phase. The transformation process can affect geochemical signatures of aragonite (a protolith). This study focused on quantification of the retention of Mg/Ca and Sr/Ca ratios, and δ18O during the transformation process as well as evaluation of the transformation rate. To investigate the effect of transformation from aragonite to calcite on elemental and stable isotope ratios, we conducted a series of experiments in NaCl solutions at temperatures between 120 and 184 °C. Two additional experiments at 250 °C were conducted to estimate the transformation rate of aragonite to calcite. Protolith materials consist of (1) synthetic (Mg; Sr-bearing or non-Mg; Sr bearing) needle-shaped microcrystals of aragonite (<5 µm in size) and (2) larger chips (>100 µm in size) of natural aragonite. X-ray diffraction (XRD) showed that microcrystals successfully transformed to calcite within 30 h and scanning electron microscopy (SEM) yielded a change in the crystal size to >10 µm in rhombohedral shape. Electron backscatter diffraction (EBSD) of the larger aragonite chips showed that transformation to randomly oriented calcite occurred at the rims and along the cracks while the core retained an aragonite crystal structure. Isotope-ratio mass spectrometry (IRMS) analyses showed that calcite δ18O was controlled by temperature and δ18O of the solution. The obtained calibration curve of isotope fractionation factor versus temperature is consistent with other studies. Inductively coupled plasma optical emission spectroscopy (ICP-OES) analyses showed that calcite partially or completely retained Mg/Ca and Sr/Ca ratios through the transformation.

58 GEOSCIENCES↗

Investigations of γ′, γ″ and δ precipitates in heat-treated Inconel 718 alloy fabricated by selective laser melting

Highlights: • The γ austenite matrix shows a fine cellular substructure. • γ′ and three variants of γ″ precipitates around 10–50 nm develop within cellular γ. • Coarser acicular γ″ and plate-like δ occur at grain boundaries and intragranular γ. • The orientation relationships of γ″ with γ, and of δ with γ are observed. - Abstract: Inconel 718 alloy samples were fabricated by selective laser melting (SLM). Microstructure and precipitation in solution-heat-treated- and double-aging-SLM-made Inconel 718 were studied by scanning and transmission electron microscopy. Electron microscope observations showed that disc-shaped and cuboidal γ″, and circular γ′ precipitates with an average size of 10–50 nm developed within cellular γ austenite matrix. The simulated, experimentally observed electron diffraction patterns, and dark-field imaging further revealed that the precipitation of three variants of γ″ in the γ matrix occurred. The coarser acicular γ″, and globular as well as plate-like δ phases precipitated at grain boundaries and also within the interior of austenite matrix. The morphology, distribution and crystallography of these precipitates and their formation mechanisms were analyzed and discussed.

36 MATERIALS SCIENCE↗

Role of bromine doping on the photovoltaic properties and microstructures of CH{sub 3}NH{sub 3}PbI{sub 3} perovskite solar cells

Organic-inorganic hybrid heterojunction solar cells containing CH{sub 3}NH{sub 3}PbI{sub 3} perovskite compound were fabricated using mesoporous TiO{sub 2} as the electronic transporting layer and spirobifluorence as the hole-transporting layer. The purpose of the present study is to investigate role of bromine (Br) doping on the photovoltaic properties and microstructure of CH{sub 3}NH{sub 3}PbI{sub 3} perovskite solar cells. Photovoltaic, optical properties and microstructures of perovskite-based solar cells were investigated. The X-ray diffraction identified crystal structure of the perovskite layer doped with Br in the solar cell. Scanning electron microscopy observation showed a different behavior of surface morphology and the perovskite crystal structure on the TiO{sub 2} mesoporous structure depending on extent amount of hydrogen doping of Br. The role of bromide halogen doping on the perovskite crystal structure and photovoltaic properties was due to improvement of carrier mobility, optimization of electron structure, band gap related with the photovoltaic parameters of V{sub oc}, J{sub sc} and η. Energy diagram and photovoltaic mechanism of the perovskite solar cells varied with halogen doping was discussed by experimental results.

36 MATERIALS SCIENCE↗

Effect of Melt Temperature on Surface Films Formed on Molten AZ91D Alloy Protected by Graphite Powder

Graphite powder was adopted to prevent AZ91D alloy from oxidizing during melting and casting. The microstructure of the resultant surface films, formed at 933 K, 973 K, 1013 K, and 1053 K (660 °C, 700 °C, 740 °C, and 780 °C) for 30 minutes, was investigated by scanning electron microscopy, energy dispersive spectrometer, and X-ray diffraction, and the phase composition of the surface films was analyzed by the standard Gibbs free energy change of the reactions between the graphite powder, the alloy melt, and the ambient atmosphere. The effect and mechanism of melt temperature on the resultant surface films were also discussed. The results indicated that the surface films, of which the surface morphology comprised folds and wrinkles, were composed of a protective layer and MgF{sub 2} particles. The protective layer was contributive to the prevention of the molten alloy from oxidizing, and consisted of magnesium, oxygen, fluorine, carbon, and a small amount of aluminium existing in the form of MgO, MgF{sub 2}, C, and MgAl{sub 2}O{sub 4}. The layer thickness was 200 to 900 nm. The melt temperature may affect the surface films through the increased interaction between the graphite powder, the melt, and the ambient atmosphere. The oxygen content and thickness of the protective layer decreased and then increased, while the height of the folds increased with melt temperature.

36 MATERIALS SCIENCE↗

A facile and scalable route to nano-crystallized kesterite Cu{sub 2}ZnSnS{sub 4} fibers via electrospinning/sulfurization

Detailed characterization of the microstructure and its properties have been done on the nanocrystallized CZTS nanofibers fabricated via electrospinning following sulfurization. The fiber growth mechanism is proposed to explain the spontaneous reaction and crystallization of CZTS, as confirmed by the thermodynamic calculations. - Abstract: In this work, we report facile route to quaternary kesterite Cu{sub 2}ZnSnS{sub 4} (CZTS) microfibers through electrospinning method. Precursor fibers are electrospun from the solution composed of Cu(CH{sub 3}COO){sub 2}, Zn(CH{sub 3}COO){sub 2{sup ,}} and SnCl{sub 4} as the solutes, ethylene glycol methyl ether as the solvent, and polyvinylpyrrolidone (PVP) as the plasticizer. CZTS fibers are obtained after annealing at 773 K for 40 min in a sulfur ambient. Characterization including scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Raman spectra, confirm the formation of single-phased, well-crystallized CZTS fibers, with a band gap of about 1.48 eV estimated from the optical absorption curve. In addition, the fiber growth mechanism is proposed to explain the spontaneous reaction and crystallization of CZTS, as confirmed by the thermodynamic calculations.

36 MATERIALS SCIENCE↗

Mössbauer Studies and Magnetic Properties of Cubic CuFe{sub 2}O{sub 4} Nanoparticles

This study reports the preparation and characterization of nanocrystalline spinel powder of cubic copper ferrite nanoparticles (NPs) which have been fabricated via a cost-effective citrate sol–gel approach. The structural and morphological properties of the nanoparticles are analyzed by X-ray diffraction (XRD), Fourier transform spectroscopy (FT-IR), and scanning electron microscopy (SEM) whereas magnetic properties and Mössbauer analysis were performed using vibrating sample magnetometer (VSM) and Mössbauer spectra, respectively, and were characterized in detail. The empirical aim of this study is to perceive the transition phase of CuFe{sub 2}O{sub 4} as cubic symmetry which was confirmed by SEM images, and a couple of studies reported on the cubic structure of copper ferrite and discussed the magnetic properties. However, the present study gives the detailed information of the formation of cubic structure and magnetic behavior of the CuFe{sub 2}O{sub 4} cubic structure. X-ray diffraction measurements of resulting NPs show that the grain size of the particles is about 42.08 nm while SEM analysis showed that the particles have cubic nanostructured shapes with non-homogeneous sizes in around 80–100 nm. From {sup 57}Fe, Mössbauer parameters consist of one superparamagnetic doublet and superposition of four sextets. VSM result shows the enhanced superparamagnetic nature of the CuFe{sub 2}O{sub 4} NPs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Local ordering in Ge/Ge–Sn semiconductor alloy core/shell nanowires revealed by extended x-ray absorption fine structure (EXAFS)

Short-range atomic order in semiconductor alloys is a relatively unexplored topic that may promote design of new materials with unexpected properties. Here, local atomic ordering is investigated in Ge–Sn alloys, a group-IV system that is attractive for its enhanced optoelectronic properties achievable via a direct gap for Sn concentrations exceeding ≈10 at. %. The substantial misfit strain imposed on Ge–Sn thin films during growth on bulk Si or Ge substrates can induce defect formation; however, misfit strain can be accommodated by growing Ge–Sn alloy films on Ge nanowires, which effectively act as elastically compliant substrates. In this work, Ge core/Ge 1–x Sn x (x ≈ 0.1) shell nanowires were characterized with extended x-ray absorption fine structure (EXAFS) to elucidate their local atomic environment. Simultaneous fitting of high-quality EXAFS data collected at both the Ge K-edge and the Sn K-edge reveals a large (≈ 40%) deficiency of Sn in the first coordination shell around a Sn atom relative to a random alloy, thereby providing the first direct experimental evidence of significant short-range order in this semiconductor alloy system. Furthermore, comparison of path length data from the EXAFS measurements with density functional theory simulations provides alloy atomic structures consistent with this conclusion.

36 MATERIALS SCIENCE↗

Reduction of hexavalent chromium by the thermophilic methanogen Methanothermobacter thermautotrophicus

Despite the significant progress on iron reduction by thermophilic microorganisms, studies on their ability to reduce toxic metals are still limited, despite their common co-existence in high temperature environments (up to 70°C). In this study, Methanothermobacter thermautotrophicus, an obligate thermophilic methanogen, was used to reduce hexavalent chromium. Experiments were conducted in a growth medium with H 2 /CO 2 as substrate with various Cr 6+ concentrations (0.2, 0.4, 1, 3, and 5 mM) in the form of potassium dichromate (K 2 Cr 2 O 7 ). Time-course measurements of aqueous Cr 6+ concentrations with the 1, 5-diphenylcarbazide colorimetric method showed complete reduction of the 0.2 and 0.4 mM Cr 6+ solutions by this methanogen. However, much lower reduction extents of 43.6%, 13.0%, and 3.7% were observed at higher Cr 6+ concentrations of 1, 3 and 5 mM, respectively. These lower extents of bioreduction suggest a toxic effect of aqueous Cr 6+ to cells at this concentration range. At these higher Cr 6+ concentrations, methanogenesis was inhibited and cell growth was impaired as evidenced by decreased total cellular protein production and live/dead cell ratio. Likewise, Cr 6+ bioreduction rates decreased with increased initial concentrations of Cr 6+ from 13.3 to1.9 μM h ₋1 . X-ray absorption near-edge structure (XANES) spectroscopy revealed a progressive reduction of soluble Cr 6+ to insoluble Cr 3+ precipitates, which was confirmed as amorphous chromium hydroxide by X-ray diffraction and selected area electron diffraction pattern. However, a small fraction of reduced Cr occurred as aqueous Cr 3+ . Scanning and transmission electron microscope observations of M. thermautotrophicus cells after Cr 6+ exposure suggest both extra- and intracellular chromium reduction mechanisms. Results of this study demonstrate the ability of M. thermautotrophicus cells to reduce toxic Cr 6+ to less toxic Cr 3+ and its potential application in metal bioremediation, especially at high temperature subsurface radioactive waste disposal sites, where the temperature may reach ~70°C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of graphene oxide produced by Hummers method and its supercapacitor applications

In this study, Graphene Oxide (GO) is produced using Hummers method. The produced GO were investigated by x-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), UV-Vis spectrum, Raman spectroscopy and scanning electron microscopy (SEM). GO films on Ni foam were prepared by doctor-blading technique. The electrochemical performances of the as-synthesized GO electrode was evaluated using cyclic voltammetry (CV) in 6 M KOH aqueous solution. Capacitances of GO electrode was measured as 0.76 F/g.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterisation of silica derived from rice husk (Muar, Johor, Malaysia) decomposition at different temperatures

Rice husk was thermally decomposed to yield powder composed of silica (SiO{sub 2}). Temperatures of 700°C and 1000°C were chosen as the decomposition temperatures. X-Ray Diffraction (XRD), X-Ray Florescence (XRF), Fourier Transform Infrared (FTIR), and Field Emission Scanning Electron Microscope (FESEM) analyses were conducted on a synthetic silica powder (SS-SiO{sub 2}) and the rice husk ash as for the comparative characterisation study. XRD analyses clearly indicated that the decomposed rice husk yielded silica of different nature which are Crystalline Rice Husk Silica (C-RHSiO{sub 2}) and Amorphous Rice Husk Silica (A-RHSiO{sub 2}). Moreover, it was found that SS-SiO{sub 2} was of Quartz phase, C-RHSiO{sub 2} was of Trydimite and Cristobalite. Through XRF detection, the highest SiO{sub 2} purity was detected in SS-SiO{sub 2} followed by C-RHSiO{sub 2} and A-RHSiO{sub 2} with purity percentages of 99.60%, 82.30% and 86.30% respectively. FTIR results clearly indicated silica (SiO{sub 2}) bonding 1056, 1064, 1047, 777, 790 and 798 cm{sup −1}) increased as the crystallinity silica increased. The Cristobalite phase was detected in C-RH SiO{sub 2} at the wavelength of 620 cm{sup −1}. Morphological features as observed by FESEM analyses confirmed that, SS-SiO{sub 2} and C-RH SiO{sub 2} showed prominent coarse granular morphology.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

An assessment of spall failure modes in laser powder bed fusion fabricated stainless steel 316L with low-volume intentional porosity

Here, this paper reports on spall failure and damage modes in Laser Powder Bed Fusion fabricated Stainless Steel 316L (SS316L) with intentional levels of low-volume (1–5 vol. %) porosity and pore sizes of 200, 350, and 500 μm. The fabricated specimens were subjected to uniaxial-strain plate-impact loading at ~4.5 GPa, to initiate incipient spall failure. Analysis of velocimetry profiles measured using multi-probe photon-Doppler velocimetry coupled with post-mortem analysis of soft-recovered samples reveals local suppression of spall failure (termed as spall-dominated) as a function of porosity, as the failure mechanism transitions from spall-centered tensile stress dominated to a pore-centered microstructure-dominated damage mode involving void/crack nucleation and growth at pre-existing pores. The critical porosity level where the suppression of spall failure is first observed, as well as the spall location, is dependent on both the volume fraction and the size of the initially fabricated pores. In samples of 500 μm pore size, the suppression of spall failure is observed with as little as 1 vol. % porosity, while samples with smaller pores (200 μm) still experience spall-centered tensile stress dominated failure with higher levels (5 vol. %) of porosity. In the case of pore-centered microstructure-dominated failure, spall damage can occur but the spall plane is shifted toward the rear free surface, or more generally in areas further away from the region with pores. Highly heterogeneous deformation twinning, shear banding, grain rotation, and cracking are observed in the vicinity of pre-existing pores and expected spall failure sites.

36 MATERIALS SCIENCE↗

Microstructure and Properties of AlCoCrFeNiTi High-Entropy Alloy Coating on AISI1045 Steel Fabricated by Laser Cladding

AISI1045 steel is widely used in mechanical engineering. In spite of the favorable toughness and strength, the surface properties of AISI1045 steel, such as hardness, wear resistance and corrosion resistance, are not ideal. Therefore, surface modification of AISI1045 is necessary, especially for the parts suffering severe work condition. Laser cladding is a promising surface modification technology. In this work, the AlCoCrFeNiTi high-entropy alloy (HEA) coatings were prepared on the AISI1045 steel to improve its surface properties. Metallurgical bonding is obtained between the coating and the substrate. The microstructure and surface properties of the coating were characterized by scanning electron microscope, energy-dispersive spectrometry, x-ray diffraction, electrochemical workstation, microhardness tester and pin-on-ring wear tester. The microstructure of the coating produced by laser cladding is dendritic. The AlCoCrFeNiTi HEA coating is mainly composed of disordered body-centered cubic phase (Fe-Cr), ordered B2 phase (AlNi) and intermetallic phase (Ti-rich). The coating shows excellent abrasion resistance and corrosion resistance in comparison with the substrate. The maximum microhardness of the coating reaches approximately 865 HV, which is 4.5 times of AISI1045 steel.

36 MATERIALS SCIENCE↗

Solute Redistribution During Aging in a Laser-Based Powder Bed Fusion-Produced Fe-18Ni-9Co-5Mo-Ti Maraging Steel

Solute distribution during the laser-based powder bed fusion of metals process is highly complex because of solidification. This study builds on a previous investigation of how solute heterogeneities across different scales influence phase distribution and aging physical phenomena in a Fe-18Ni-9Co-5Mo-Ti maraging steel (Santana et al. in Addit Manuf 104494, 2024). Previous work using energy-dispersive X-ray spectroscopy revealed heterogeneous Ni and Mo enrichment at intercellular regions. Using X-ray diffraction, 8 ± 3% retained austenite was quantified in as-built samples. Additionally, electron backscatter diffraction analysis exposed the location of retained austenite along cell boundaries. In this work, scanning transmission electron microscopy results revealed the presence of non-enriched retained austenite in the as-built condition. With increased aging temperature, Ni and Mo enrichment in austenite increased, especially at the austenite/martensite boundary. Solute diffusion was simulated in DICTRA Thermo-Calc® software to assess solute redistribution between the matrix and second phases and to comprehend whether elemental diffusion processes are interconnected. Three different scenarios were considered: (1) solute diffusion in the matrix; (2) diffusion with enriched austenite in the intercellular region; (3) diffusion with non-enriched austenite in the intercellular region. Results showed that Ni partitioning controls austenite growth and that boundary regions exhibit higher element enrichment than the core.

42 ENGINEERING↗

Structural and morphological characterization of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} hydrotalcite produced by mechanochemistry method

Chlorine intercalated Mg–Al layered double hydroxides (Mg–Al–Cl–LDH) with a chemical formula Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} were successfully produced by the one-step mechanochemistry method and subsequent water washing followed by drying in oven for 1 h at 80 °C. The samples were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FT–IR), field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), elemental mapping analysis, transmission electron microscopy (TEM), X-ray fluorescence (XRF), and the differential thermogravimetric analysis (DTGA). Results revealed that the structural characteristics of Mg–Al–Cl–LDH were affected strongly by milling time. At the beginning of milling (up to 1 h), Hydrotalcite (HT) and Brucite were the dominant phases, while the progressive mechanical activation was completed as milling time increased, which resulted in the formation of nanostructured Mg–Al–Cl–LDH. Based on XRD and FTIR data, Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} with high purity was obtained at 5 h milling. The interlayer spacing of LDH is also strongly influenced by milling time so that it escalated from 7.737±0.001 to 8.005±0.002 (1–15 h) and then decreased to 7.937±0.001 for 20 h milled sample. Electron microscopic observation displayed that the final product had hexagonal platelet structure with lateral dimension of 20–100 nm. Therefore, the synthesis of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} via mechanochemistry owing to simplicity and versatility can be a promising candidate for use in catalyst carriers, drug delivery, and gene delivery. - Graphical Abstract: TEM image of milled sample (Mg–Al–Cl–LDH). - Highlights: • Chlorine intercalated LDH was synthesized by a facile solid-state process. • Structural features of products were influenced strongly by the milling time. • XRD and FTIR spectra suggested predominant Mg–Al–Cl–LDH after 5 h milling. • Products showed hexagonal platelet structure with lateral dimension of 20–100 nm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structure of the Fe-Mn-Si alloys submitted to γ ↔ ε thermocycling

Highlights: • The effect of thermal cycling Fe–Mn–Si alloys is studied. • In situ neutron diffraction, internal friction, DSC and TEM results are analysed. • Lattice defects accumulation both in martensitic and austenitic phases. • Microstrains in the γ and ε phases are estimated. - Abstract: The accumulation of defects and internal stresses and related changes of the direct and reverse martensitic transition (MT) on thermocycling over the phase transition in different Fe–Mn–Si alloys are investigated by in situ neutron diffraction, TEM, SEM-EBSD, DSC and mechanical spectroscopy. The temperature of direct MT in Fe-22Mn-3Si, Fe-26Mn-4Si and Fe-26Mn-7Si alloys decreases during thermal cycling, while that of the inverse MT increases, which causes a widening of the transformation hysteresis. Transmission electron microscopy shows that a large number of dislocations and stacking faults are formed in both martensitic and austenitic phases in the Fe-22Mn-3Si annealed alloy submitted to γ ↔ ε thermocycling. From in situ neutron diffraction tests on Fe-22Mn-3Si annealed alloy and classical Williamson-Hall analysis, we found that the microstrains in the ε-martensite after 1 and 12 thermocycles are roughly twice higher as compared with the austenite phase.

36 MATERIALS SCIENCE↗

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