Diffraction Lines Research Articles

Effects of Cold Rolling–Induced Defects on Proton Irradiation Response in Nb-1Zr-0.1C Alloy

This work highlights the effect of proton irradiation in the presence of preexisting defects in the Nb-1Zr-0.1C alloy. To introduce the initial defects, the Nb-1Zr-0.1C alloy was subjected to cold rolling (10% and 20%) prior to irradiation. Characterization of the irradiated material was performed using detailed X-ray diffraction line profile analyses. The results, in terms of various microstructural parameters, revealed that the preexisting defects in these materials act as effective sinks for irradiation-induced defects during the initial irradiation. Electron backscattered diffraction analyses suggested that the fraction of low-angle grain boundaries plays a crucial role during irradiation and determines the outcome of the competing process between defect annihilation and defect production. Transmission electron microscopy analyses revealed that the black dots were coexisting with carbide precipitate in the cold-rolled Nb alloy after irradiation. Mechanical properties were also assessed by measuring microhardness to correlate with the changes in microstructure after irradiation. The change in yield strength calculated from the change in the microhardness value as a function of dose indicated that the 20% cold-rolled Nb alloy was more radiation resistant than the 10% cold-rolled Nb alloy at ambient temperature and a low-dose regime. To see the effect of alloying elements, similar studies were also carried out on pure Nb, and the results were compared with that of the Nb-1Zr-0.1C alloy. All these findings help to develop a better understanding of the behavior of the proton-irradiated Nb-1Zr-0.1C alloy in the presence of preexisting defects introduced by means of cold rolling prior to irradiation.

Antibacterial and Cell-Viability of Hydroxyapatite Derived from Waste Marine Shell for Biomedical Applications

The present study discusses on the functional groups, structural characterization and thermal behaviour of Crassostrea angulata shell used for the synthesis of a biocompatible hydroxyapatite material. The hydroxyapatite was synthesized from C. angulata shell through precipitation method and characterized using XRD, FTIR, FE-SEM, EDX mapping, HR-TEM and SAED pattern. The formation of hydroxyapatite was confirmed from the high intense X-ray diffraction lines and by the presence of chemical groups such as PO43–, OH– and CO32–. The structural changes during the formation of hydroxyapatite from the thermal decomposition of C. angulata shell were studied through XRD and TG-DTA. The morphology study by FE-SEM indicates that the synthesized hydroxyapatite materials were in the form of clusters of rod-like particles. The SAED patterns and XRD spectral lines confirmed the crystalline nature of the synthesized hydroxyapatite. The antibacterial activity and cell viability assay of prepared hydroxyapatite were studied to assess its suitability in various biomedical applications. The antibacterial activity of hydroxyapatite was assessed against Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus saprophyticus) bacterial strains. The cytocompatibility of hydroxyapatite was assessed through an MTT assay using osteoblast cells (MG-63 cell). Thus, the prepared hydroxyapatite shows good antibacterial action and cell viability nature and it can be applied in various biomedical applications.

In-situ cryogenic X-ray diffraction analysis of Poly(dimethylsiloxane) oil and film

Understanding the phase transitions and crystallographic characteristics of polysiloxane materials poses a significant challenge. To address this issue, a custom cryogenic chamber has been developed and integrated with a laboratory X-ray diffraction apparatus, enabling the execution of in-situ temperature-dependent X-ray diffraction (XRD) analyses across the cooling and heating cycles. Through the utilization of diverse sample holders, the real-time monitoring of crystallization and melting phenomena in both linear poly(dimethylsiloxane) (PDMS) oil and crosslinked PDMS film has been made feasible. Notably, high-quality X-ray diffraction data, encompassing 13 diffraction lines, are successfully acquired for the first time for linear PDMS oil at 153K. Subsequent crystallographic examination has revealed a tetragonal unit cell characterized by lattice parameters a = b = 8.3379 Å, c = 11.9284 Å, and space group I 41, suggesting the adoption of a fourfold helical conformation by two polymer chains, each comprising four monomer units, within the lattice structure. This improved and versatile X-ray instrumentation presents clear advantages over conventional commercial powder X-ray diffractometers, which is anticipated to provide a promising in-situ characterization approach for investigating the low-temperature behaviors of liquid or oil materials.

Influence of hydrogen on deformation and embrittlement mechanisms in a high Mn austenitic steel: In-Situ neutron diffraction and diffraction line profile analysis

Austenitic steels have relatively high resistance to hydrogen embrittlement and play a critical role in hydrogen service applications. In particular, high Mn austenitic steels are considered economically viable alloy alternatives for these applications. The current study employed in-situ and ex-situ neutron diffraction techniques combined with diffraction line profile analysis (DLPA) to investigate the influence of hydrogen on deformation and embrittlement mechanisms in a high Mn (approximately 30 wt pct) austenitic steel. Investigation using both neutron diffraction and electron backscatter diffraction revealed the presence of extensive deformation twins and stacking faults within the steel microstructure after tensile deformation in the non-charged condition. These microstructural features suggest planar deformation behavior, which is expected from the relatively low stacking fault energy (SFE) of the alloy (approximately 29 mJ/m2). Hydrogen pre-charging resulted in apparent increases in both dislocations and stacking faults, contributing to macroscopic hardening and embrittlement mechanisms. Overall, numerical parameters obtained through neutron DLPA were used to elucidate the underlying mechanisms associated with hydrogen effects on the mechanical behavior, i.e. macroscopic strengthening, strain hardening rate, and embrittlement.

Highly saturated red-emitting novel europium doped yttrium calcium borate (Eu3+: Y2CaB10O19) phosphor materials for eco-friendly solid-state lighting applications

Optical parameters like low correlated color temperature (CCT), color rendering index (CRI), color purity, thermal stability and etc. are crucial parameters for the practical applications of white light emitting diode applications. High color purity around 100 % red emitting novel europium doped yttrium calcium borate (Eu3+: Y2CaB10O19) phosphors were harvested by conventional solid-state synthesis technique. The novel host material possesses monoclinic crystal structure with no observable shift in the diffraction lines with varying dopant concentrations. FTIR studies revealed the presence of BO3 and BO4 networks in the host lattice responsible for structural rigidity and good thermal stability. The phosphor materials synthesized xEu3+: Y2CaB10O19 (x = 0.01, 0.03, 0.05, 0.07 and 0.09), are sensitive to both 250 nm (UV) and 393 nm (Near UV/blue LED) for excitation that can produce deep orange (594 nm) emission along with red emission (612 nm). The optimum Eu3+ ion concentration was fixed at 5 mol% of dopant ions to prevent the concentration quenching. As prepared optimal phosphor material possesses high color purity around 100 %, CCT of 1214 K defines its applicability in WLED applications. The synthesized phosphor materials pertain excellent switching response, thermal stability and the fabricated P-i-G possesses desired photometric parameters for its practical applications.

Influence of a Constant Magnetic Field on the Parameters of the Magnetoplastic Effect in Aluminum Alloy B95pch

The present work is devoted to the comprehensive experimental study of the magnetoplastic effect found in the aluminum alloy B95pch aged in a weak constant magnetic field. The data on chemical composition of aluminum alloy B95pch, modes of thermal and thermomagnetic treatments and main experimentally observed regularities of changes in values of microhardness, modulus of elasticity of separate local areas and phase composition of aluminum alloy B95pch, aged at temperature 140°С, time from 2 to 8 h, in a constant magnetic field with intensity 557.0 kA/m and in its absence are presented. It was found that the constant magnetic field significantly affects the strength properties and structure of aluminum alloy B95pch. The negative magnetoplastic effect has been detected, the value of which is 21%. It is observed that the constant magnetic field does not significantly affect the average grain size, however, the size and number of observed foreign inclusions within the grain become significantly smaller compared to aging in the absence of magnetic field. In addition, the imposition of the constant magnetic field on the phase formation process leads to the formation of a more distorted structure: the half-width of diffraction lines becomes wider. The results of microhardness and modulus of elasticity measurements of aluminum alloy B95pc were found to be correlated.

Nanostructuring and Hardness Evolution in a Medium‐Mn Steel Processed by High‐Pressure Torsion Technique

Severe plastic deformation (SPD) is performed on a newly developed medium‐Mn steel with the composition of Fe–7.66Mn–2Ni–1Si–0.23C–0.05Nb (wt%) to achieve a nanocrystalline microstructure. The SPD process utilizes the high‐pressure torsion (HPT) technique, resulting in a nominal shear strain of approximately 36 000% after processing the disk for 10 turns. In X‐Ray diffraction line profile analysis, an increase in dislocation density to around 230 × 1014 m−2 is observed. In addition, under high strains, a face‐centered cubic (fcc) secondary phase emerges within the body‐centered cubic (bcc) matrix. In analytical transmission electron microscopy, using energy‐dispersive X‐Ray spectroscopy, it is indicated that the secondary‐phase particles are enriched in Al, Mn, and Si. As the strain imposed during HPT increases, the simultaneous rise in dislocation density and nanostructuring lead to material hardening. However, the partial phase transformation from bcc to fcc contributes to material softening. As a result of these two opposite effects, the hardness exhibits a non‐monotonic variation with the shear strain, displaying, for 10 turns of HPT, a lower hardness compared to fewer turns, despite the continuous increase in dislocation density and decrease in crystallite size.

Bobfinchite, Na[(UO2)8O3(OH)11]·10H2O, a new Na-bearing member of the schoepite family

Abstract The new mineral bobfinchite (IMA2020-082), Na[(UO2)8O3(OH)11]·10H2O, was found in the Burro mine, Slick Rock district, San Miguel County, Colorado, U.S.A., where it occurs as an oxidation product of uraninite on asphaltite matrix in intimate association with gypsum, natrozippeite, metaschoepite, and uranopilite. Bobfinchite crystals are transparent to translucent, yellow, lozenge-shaped disks up to 0.3 mm wide. Crystals are flattened on [100] and exhibit the forms {100}, {011}, {021}, {021}, and {011}. Bobfinchite has a pale-yellow streak and emits very dim yellow fluorescence under 365 nm ultraviolet illumination. The crystals are brittle with very good {100} cleavage and irregular, stepped fracture. The Mohs hardness is ca. 2 based on scratch tests. The calculated density is 5.044 g/cm3 based on the empirical formula and 5.036 g/cm3 for the ideal formula. Bobfinchite is optically biaxial (–), with α = 1.690(5), β = 1.7205(5), and γ = 1.730(5) (white light). The measured 2V, estimated from the interference figure, is 55(5)° and the calculated value is 59.1°. Dispersion is moderate, r > v; orientation: X = a, Y = b, Z = c; pleochroism: X nearly colorless, Y yellow, Z yellow; X < Y ≈Z. Electron microprobe analysis provided the empirical formula (Na0.99Pb0.02)[(UO2)7.99O3(OH)11]·10H2O. The five strongest X-ray powder diffraction lines are [dobs in Å(I)(hkl)]: 7.34(100)(200), 3.59(50)(024), 3.23(60)(224), 3.18(36)(240), and 2.01(23)(624,551,208,640,346). Bobfinchite is orthorhombic, Pbcn, a = 14.6249(9), b = 14.0389(10), c = 16.6923(10) Å, V = 3427.2(4) Å3, and Z = 4. The structure of bobfinchite (R1 = 0.0330 for 3770 I > 4σI) is built from uranyl oxide-hydroxide sheets that adopt the fourmarierite topology, with interlayer Na+ and H2O groups. Both the sheet and interlayer topology mimic those observed in natural and synthetic Na-metaschoepites studied previously, and as seen in other uranyl oxide hydrate minerals, charge balance is achieved at specific sites in the sheet through the substitution O2– ↔ (OH)–.

Analysis of the Structural, Morphological, and Elastic Properties of Nanosized CuFe2O4 Spinel Synthesized via Sol-Gel Self-Combustion Method

Nanosized CuFe2O4 ferrite was synthesized through the sol-gel self-combustion technique, using iron and copper nitrates with citric acid as fuel. The synthesized ferrite was subsequently analyzed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Scanning Electron Microscopy (SEM). X-ray diffraction studies validated the crystalline nature of the CuFe2O4, identifying it as having a mixed spinel structure within the Fd3m space group. Particle sizes were quantified using several methods including Debye-Scherrer, Williamson-Hall, Halder-Wagner, modified Debye-Scherrer, and size-strain plot (SSP), with all methods indicating a consistent average particle size of 28 nm. The elastic properties of the nanoparticles were extensively characterized, utilizing both diffraction line broadening (via the Williamson-Hall method) and Fourier-transform infrared spectroscopy (FTIR) to evaluate the materials' structural dynamics. Additionally, microstrain within the crystal lattice and various elastic constants, such as Young's modulus, Shear modulus, Debye temperature, and the velocities of longitudinal and transverse wave propagation were calculated. An electron density distribution was also constructed from the X-ray diffraction data, providing insight into the electronic environment and bonding characteristics of the material.

Microstructural Evolution of Tantalum During Deformation and Subsequent Annealing

Microstructure-aware models are necessary to predict the behavior of material based on process knowledge or to extrapolate mechanical properties of materials to environmental conditions which are not easily reproduced in the laboratory, e.g., nuclear reactor environments. Elemental Ta provides a relatively simple BCC system in which to develop a microstructural understanding of deformation processes which can then be applied to more complicated BCC alloys. In situ neutron diffraction during compressive deformation and subsequent heat treatment have been used to monitor the evolution of microstructural features in Ta throughout simulated processing steps. Crystallographic texture and dislocation density are determined as a function of first plastic strain, then temperature. Lattice strains are determined and attributed to stresses at macroscopic, grain and dislocation length scales. The increase of the dislocation density through deformation and subsequent recovery during heat treatment is monitored through the changing diffraction line profile. Also, randomization of the texture is used as a signature of recrystallization. The recovery of dislocations through annihilation is not observed to depend on the initial dislocation density in the range studied here. In contrast, recrystallization is observed to depend strongly on the initially dislocation density.

Mapping the microstructure and the mechanical performance of a combinatorial Co–Cr–Cu–Fe–Ni–Zn high-entropy alloy thin film processed by magnetron sputtering technique

The Co–Cr–Cu–Fe–Ni–Zn compositional library was studied on a combinatorial high-entropy alloy thin film processed on a silicon substrate by magnetron sputtering technique. The thickness of the coating was between 2 and 3 μm while the lateral dimension was 10 cm. The chemical composition in the layer depended on the location and for each constituent element the concentration varied between 5 and 42 at.%. The phase composition and the microstructure were mapped using synchrotron X-ray diffraction, and the crystallite size as well as the density of lattice defects (dislocations and twin faults) were determined by diffraction line profile profile analysis. In addition, selected locations were studied by transmission electron microscopy. The influence of the chemical composition on the microstructure and the mechanical behavior was revealed. The mechanical performance was characterized by nanoindentation mapping which determined the hardness and the elastic modulus versus the element concentrations. It was found that the coating contains single phase face-centered cubic (FCC) and body-centered cubic (BCC) regions as well as an intermediate two-phase area. In the whole combinatorial sample, the microstructure consisted of nanocrystalline columns growing perpendicular to the coating surface and having pores between them. Due to the porosity, the hardness and the elastic modulus were relatively low despite the nanostructure and the very high defect density. The highest hardness (3.4 GPa) and elastic modulus (119 GPa) were measured in the BCC region with the chemical composition of 10%Co–38%Cr–13%Cu–27%Fe–5%Ni–7%Zn (at.%).

Theuerdankite, Ag3AsO4, a new mineral from the Alter Theuerdank Mine, St. Andreasberg, Germany

Abstract The new mineral theuerdankite, ideally Ag3AsO4, was found in the Alter Theuerdank Mine, Beerberg, St. Andreasberg, Goslar District, Lower Saxony, Germany. Theuerdankite occurs as aggregates of anhedral grains up to 3 mm in size, growing in cavities of strongly supergene-weathered material consisting of native silver and chlorargyrite (but with calcite present). It is dark violet, changing to reddish and black when exposed to the air and light. It has a grey to violet grey streak; when readily fresh, its streak is brownish-red. The Mohs hardness is ~2. It is brittle with no observable cleavage or parting and with a conchoidal fracture. The calculated density is 6.620 g⋅cm–3. In reflected light, theuerdankite is dark grey with a pinkish tint, with no observable bireflectance, pleochroism, or anisotropy. It shows dark red internal reflections. The reflectance values for wavelengths recommended by the Commission on Ore Mineralogy of the International Mineralogical Association are (R, %): 13.3 (470 nm), 12.8 (546 nm), 12.7 (589 nm) and 12.5 (650 nm). The empirical formula (based on 4 apfu) is Ag3.00As1.00O4. Theuerdankite is cubic, space group P $\bar{4}$ 3n, a = 6.144(2) Å, V = 231.93(13) Å3 and Z = 2. The six strongest powder X-ray diffraction lines are [dobs in Å, (I) hkl]: 3.0736, (22) 200; 2.7502, (100) 210; 2.5106, (55) 211; 1.7050, (36) 320; 1.6249, (44) 321; and 1.3412, (17) 421. The crystal structure of theuerdankite (R1 = 1.69% for 519 reflections having I > 3σ(I)), is isotypic to those of synthetic Ag3AsO4 and Ag3PO4. The Gram–Charlier development describing the higher-order tensors representing the atomic displacement parameters of the silver atom was implemented, documenting that silver tends to behave anharmonically in the theuerdankite structure at room temperature.

Exploring the spectroscopic and I‑V‑T characteristics advancements of cadmium zinc tungsten phosphate diode

This research accomplished the growth of cadmium zinc tungsten phosphate (CZWP) thin films on both glass and p-Si substrates, employing the sol–gel spin coating method. The sol–gel technique offers a versatile and controlled approach for fabricating nanomaterials with tailored properties. The structural and morphological analyses, conducted through XRD and FE-SEM, provided comprehensive insights into the nature of the films. The optical properties, absorbance behavior, energy gap, refractive indices, dielectric, conductivity, and electronegativity, underwent meticulous examination through UV–Vis spectroscopy. The X-ray diffraction analysis of the zinc cadmium tungsten phosphate diode reveals diffraction lines indicative of a nanostructure featuring a monoclinic-phase Zn2P2O7 and Cd3P6O28. Furthermore, SEM analysis confirms a nanoporous morphology with a nanograpes-like structure in the successful crystalline structure of the cadmium zinc tungsten phosphate nanostructure. The optical absorption studies, covering a wavelength range from 190 to 1500 nm, unveiled both direct and indirect energy band gaps, measuring 4.14 and 3.77 eV, respectively. A rigorous analysis of the I-V-T characteristics for the CZNP/p-Si junction in dark mode led to the identification of key parameters, including the transport ideality factor, barrier height, and series resistance.

Construction of unary and ternary ZnO–CuO–CdO composite thin films and comprehensive analysis of their optical, electrical, and photocatalytic performance

In this study, unary ZnO, CuO, CdO, and ternary ZnO–CuO–CdO metal oxide thin film materials were fabricated using the SILAR procedure. The XRD spectra of the synthesized films show sharp and dominant diffraction lines, indicating the high crystallinity of both the unary and ternary composite films. The crystallite size values of unary ZnO, CuO, CdO, and ZnO–CuO–CdO ternary films were found to be 18.71 nm, 12.86 nm, 15.88 nm, and 21.96 nm, respectively. FESEM pictures exhibited that nanocomposites have spherical and nanorod-like hybrid morphology, and EDX showed that Cd has a higher content than Zn and Cu. The prepared samples’ FT-IR spectra in the wavenumber range of 500–4000 cm−1 revealed the existence of numerous vibrational modes. The optical bandgap values were found to be 1.47, 3.20, 2.21, and 2.51 eV for the CuO, ZnO, CdO, and ternary ZnO-CuO-CdO films, respectively. The photocatalytic efficiency of the ternary composites is higher than that of the unary metal oxides. The specific contact resistivity values were 780.83 kΩcm2, 213.33 kΩcm2 347.33 Ωcm2, and 1.97 kΩcm2 for ZnO, CuO, CdO, and ternary ZnO–CuO–CdO thin films, respectively. Our inventions provide advanced prompting for constructing new types of catalysts. The characterization results imply that the ternary nanocomposite can be used as a cost-effective alternative material for optoelectronic and photocatalytic implementations.

Kenoargentotetrahedrite-(Zn), [Ag6]4+(Cu4Zn2)Sb4S12□, a new member of the tetrahedrite group from the Yindongpo Au deposit, China

Abstract. The new mineral kenoargentotetrahedrite-(Zn), [Ag6]4+(Cu4Zn2)Sb4S12□, was discovered at the Yindongpo Au deposit, Henan Province, China. It occurs as black metallic anhedral grains or equant crystals up to 40 µm in size. It is opaque in transmitted light and shows a greenish-grey colour in reflected light. Electron microprobe analysis for the studied material gave the empirical formula (on the basis of total cations being equal to 16 atoms per formula unit, apfu): M(2)(Ag3.75Cu2.25)Σ6M(1)[Cu3.90(Zn1.18Fe0.69Cd0.26)Σ2.13]Σ6.03X(3)(Sb3.69As0.27)Σ3.96S(1)S11.94 S(2)□. Kenoargentotetrahedrite-(Zn) is cubic, I4‾3m (no. 217), with a = 10.4624(4) Å, V= 1145.23(13) Å3, and Z= 2. The crystal structure has been refined to a final value of R1= 0.0247 on the basis of 274 independent reflections (Fo > 4σ (Fo)) by using single-crystal X-ray diffraction data. The seven strongest X-ray powder diffraction lines (d in Å (I) (hkl)) are the following: 3.010 (100) (222), 1.844 (30) (044), 2.606 (22) (004), 1.572 (15) (226), 2.046 (9) (134), 7.35 (6) (011), and 1.909 (5) (125). Kenoargentotetrahedrite-(Zn) is isostructural with other keno-member tetrahedrites with the [Ag6]4+ cluster. The structure refinement result confirms the coupling between the site occupancy factor of subvalent hexasilver clusters at the M(2) site and that of the vacancy at the S(2) site. This relationship further substantiates the charge balance substitution mechanism of S-deficiency tetrahedrites: 6M(2)Ag++S(2)S2-= M(2)[Ag6]4++S(2)□.

X-ray Diffraction Line Profile Analysis of Natural Calcite Minerals found in Southern Philippines by Williamson-Hall Method

This study employs the Williamson–Hall (W–H) models to examine the microstrains and crystallite sizes of CaCO3 occurring as calcite in limestone samples found in General Santos City and Sarangani Province, Southern Philippines. Using both the Uniform Deformation Model (UDM) and Uniform Stress Deformation (USDM) models, computations for average sizes were established to be identical, implying minimal strain influence. The consistency of resulting measurements extends to the microstrain, revealing uniform results for all samples. Correlation between crystallite sizes and microstrains in the calcite crystals was observed, where high-purity calcites exhibited larger crystallite sizes and microstrains. The crystallite sizes decrease with microstrains for calcites with higher Mg concentration, a finding that can be attributed to lattice distortion and the formation of defects. The release of stress forms these defects, thereby resulting in a reduction of microstrains. Moreover, the distinctly variable responses to strain exhibited by the samples could be influenced by either their anisotropic properties or other additional components. The W–H models, used jointly with UDM and USDM consistently predicted crystallite sizes, and thus offer valuable insights into the uniform stress responses of calcites. These promising results notwithstanding, USDM is shown to be especially relevant for anisotropic samples owing to the display deviations of crystallite sizes, a key feature of anisotropic natural calcites. The microscopic analysis is expected to provide additional understanding regarding the state of the limestone samples.

Degradation of phenol and sulfamethoxazole with persulfate and ozone with nano‐MnO2–biochar composites

AbstractBACKGROUNDIn this study, nano‐MnO2–biochar composites were synthesized as catalysts to promote the oxidation of recalcitrant organic contaminants. MnO2 nanoparticles coated on biochar were hypothesized to enhance the oxidation of phenol and sulfamethoxazole (SMX) using ozone and/or persulfate.RESULTSThe optimal percentage of MnO2 coating on the surface of biochar was determined, and the synthesis of nano‐MnO2‐coated biochar was confirmed via scanning electron microscopy–energy‐dispersive X‐ray spectroscopy (EDS), X‐ray diffraction and EDS line mapping analyses. Compared with oxidation using ozone or persulfate in the presence of either nano‐MnO2 or biochar, the synthesized nano‐MnO2–biochar composite markedly enhanced the oxidation of phenol and SMX. This was probably due to the spreading of MnO2 nanorods on the surface of biochar and the synergistic involvement of nano‐MnO2 and biochar as catalysts. X‐ray photoelectron spectroscopy analysis confirmed the involvement of Mn3+ in MnO2 to promote oxidation using ozone or persulfate. The coexistence of ozone and persulfate could also promote oxidation. Hydroxyl radicals (OH•) and persulfate radicals (SO4−•) were major reactive oxygen species for ozone and persulfate systems, respectively.CONCLUSIONResults suggest that the synthesized nano‐MnO2–biochar composites may be effective catalysts for various types of advanced oxidation processes in environmental remediation. © 2024 Society of Chemical Industry (SCI).

On some Features of the Grain and Subgrain Size in a Cu-Cr-Zr Alloy After ECAP Processing and Aging

A Cu-1Cr-0.1Zr alloy has been subjected to ECAP processing via route Bc and aging at 250-800°C. Electron BackScatter diffraction (EBSD), Transmission Electron Microscopy (TEM) and X-Ray Diffraction Line Profile Analysis (XRDLPA) techniques have been used to unveil some peculiarities of the grain and subgrain structure with a special emphasis on the comparison of the grain size estimated by the three techniques. For the alloy ECAP processed and aged up to 16 passes, the grain size (from EBSD, 0.2 < d < 5 μm), subgrain size (from TEM, d ~ 0.75 μm) and “apparent” average crystallite size (from XRDLPA, d < 0.25 μm) are manifestly different. The results were compared to the published data and analyzed based on the fundamental aspects of these techniques.

On the stable/metastable nature of the γ-hydride phase in Zircaloy-2: Microstructural characterization by electron diffraction, electron energy-loss spectroscopy, and diffraction line profile analysis

This work investigates the potential metastable versus stable nature of the γ-hydride in Zircaloy-2. Specimens were hydrided, and hydrides were precipitated through water-quenching. Synchrotron X-ray diffraction of the water-quenched sample revealed a diffraction peak with the d-spacing value of ∼2.70 Å. While this peak is conventionally attributed to {111}-γ planes, it could also stem from the (0004)-ζ plane. To clarify this ambiguity, the crystal structure of nano-hydrides was characterized by nano-beam electron diffraction (NBED) and electron energy-loss spectroscopy (EELS). While EELS detected nano-hydrides with plasmon energy (PE) values associated with the ζ-,γ-, and δ-phases, suggesting all three types of phases might be present, complementary NBED analysis revealed that regardless of the measured PE values, the examined nano-hydrides were of only γ- or δ-nature.Repeating the heating/quenching cycles reduced the γ-phase volume fraction until its (almost) complete disappearance after three cycles. δ-phase, however, was observed after each heating/quenching cycle. This observation, in accordance with previous reports, indicates that the γ-phase is metastable in Zircaloy-2, such that even during water-quenching (which is conventionally believed to facilitate the formation of γ-phase) only δ-hydrides form in cases where microstructural conditions are suitable.Diffraction line profile analysis and transmission electron microscopy revealed an increase in dislocation density during the first heating/quenching cycle, with no noticeable variations during subsequent cycles. A mechanism is proposed that links microstructure (i.e., dislocation structure) evolution during heating/quenching cycles to the suppression of the (metastable) γ-phase.

Effect of high-pressure torsion on the structure and microhardness of biodegradable Fe-30Mn-5Si (WT.%) alloy

The effect of high-pressure torsion (HPT), including a new method of accumulative HPT (AccHPT), on the microstructure and mechanical properties of Fe-30Mn-5Si alloy is studied. It is shown that during HPT and AccHPT, stress-induced ε-martensite is predominantly formed, and a mixture of nanograined structure, nanosubgrained structure and highly-dislocated substructure after HPT, while predominantly nanograined structure after AccHPT, are obtained. The increase in the number of HPT revolutions results in a broadening of the X-ray diffraction lines and higher microhardness values. The highest values were achieved on samples after AccHPT.