Fabrication of Fe-Si-B Based Amorphous Powder Cores by Spark Plasma Sintered and Their Magnetic Properties

Mechanical ball milling was used to coat SiO₂ nanopowder on a Fe-Si-B amorphous powder in this study. The Fe-Si-B/SiO₂ core–shell amorphous composite powder was obtained after 6h of ball milling. At 490 °C, the amorphous powder is thermally stable. Discharge plasma sintering was used to create a Fe-Si-B/SiO₂ magnetic powder core (SPS). At a sintering temperature of 420 to 540 °C, the phase composition and magnetic characteristics of the magnetic particle core were investigated. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to examine the structural features of the magnetic particle core. A precision resistance tester and a vibrating sample magnetometer were used to assess the resistivity and magnetic characteristics of the magnetic particle core. The findings showed that Fe₃Si and Fe₂B are the phases generated during spark plasma sintering. High-frequency power loss increases as density rises. However, at the measured frequency, the magnetic permeability of the magnetic particle core changes slightly and has excellent frequency characteristics, making it appropriate for use in high-frequency components.     

Corrosion Behavior of Candidate Functional Materials for Molten Salts Reactors in LiF–NaF–KF Containing Actinide Fluoride Imitators

Molten fluorides of alkali metals are considered a technological medium for molten salt reactors (MSRs). However, these media are known to be extremely corrosive. The successful implementation of high-temperature technological devices using molten alkali metal fluorides requires the selection of such structural materials that have high corrosion resistance in melts with compositional characteristic of MSRs. In this research, the corrosion behavior of 12Cr18Ni10Ti steel, the alloy Ni60Cr20Mo15, and the alloy Monel 404 (Ni50Cu50) was investigated in the LiF–NaF–KF eutectic melt, containing additions of CeF₃ and NdF₃ from 0 to 5 wt.% as imitator fluorides of actinides in an inert argon atmosphere at 550 °C for 100 h. Gravimetry, energy-dispersive X-ray (EDX) microanalysis of surfaces and cross-section of samples, and ICP-MS were used to establish the corrosion behavior of the investigated alloys. Corrosion resistance of the studied materials was found to decrease in a row from Monel 404 > Hastelloy C2000 > 12Cr18Ni10Ti. The addition of cerium fluoride into the melt resulted in the additional etching of the alloy surface. The addition of neodymium fluoride resulted in the formation of the point/inter-crystalline corrosion damages in the sample bulk. The samples of steel 12Cr18Ni10Ti were subjected to local cracking corrosion. The austenitic nickel-based alloys suffered specific local corrosion with formation of subsurface voids. Excellent corrosion resistance of the Monel alloy under the test conditions was found.     

Controllable Preparation of Spherical Molybdenum Nano-Powders by One-Step Reduction of APM in Radio Frequency Hydrogen Plasma

Spherical molybdenum nano-powders were in-situ ultrafast synthesized from ammonium paramolybdate (APM) raw materials in a one-step reduction method by radio frequency (RF) hydrogen plasma. Due to the extreme conditions of the RF plasma torch such as its high temperature and large temperature gradient, the injected raw APM powder was quickly gasified and then reduced into nano-sized metal molybdenum (Mo) powder. The influences of APM powder delivery rate and H₂ concentration on the properties of the obtained powders were investigated. Field-emission scanning electron microscope (FESEM), transmission electron microscope (TEM), X-ray diffraction (XRD), nanolaser particle analyzer, and specific surface area method were used to characterize the morphology, phase, and particle size distribution of the powders. The results showed that the nano-sized Mo powder obtained by hydrogen plasma treatment had a quasi-spherical morphology and an average particle size of about 30 nm. The particle size could be successfully adjusted by varying H₂ concentrations. In addition, spherical nano-sized MoO₃ powder could be obtained when no H₂ was added into the RF plasma.     

Cast Microstructure of a Complex Concentrated Noble Alloy Ag20Pd20Pt20Cu20Ni20

A complex concentrated noble alloy (CCNA) of equiatomic composition (Ag₂₀Pd₂₀Pt₂₀Cu₂₀Ni₂₀–20 at. %) was studied as a potential high—performance material. The equiatomic composition was used so that this alloy could be classified in the subgroup of high—entropy alloys (HEA). The alloy was prepared by induction melting at atmospheric pressure, using high purity elements. The degree of metastability of the cast state was estimated on the basis of changes in the microstructure during annealing at high temperatures in a protective atmosphere of argon. Characterisation of the metallographically prepared samples was performed using a scanning electron microscope (SEM) equipped with an energy dispersive spectrometer (EDS), differential scanning calorimetry (DSC), and X–ray diffraction (XRD). Observation shows that the microstructure of the CCNA is in a very metastable state and multiphase, consisting of a continuous base of dendritic solidification—a matrix with an interdendritic region without other microstructural components and complex spheres. A model of the probable flow of metastable solidification of the studied alloy was proposed, based on the separation of L—melts into L₁ (rich in Ni) and L₂ (rich in Ag). The phenomenon of liquid phase separation in the considered CCNA is based on the monotectic reaction in the Ag−Ni system.     

Preparation and Chromaticity Control of CoTiO3/NiTiO3 Co-Coated TiO2 Composite Pigments

In this study, home-made amorphous TiO₂ microspheres with good mono-dispersity and large numbers of mesopores on the surface were used as substrates. The intermediate microspheres were obtained by adding Co/Ni sources with different Co/Ni molar ratios in a water bath and making them react by water bath heating. By calcining the intermediate microspheres deposited on the TiO₂ ones, a core–shell structured spherical CoTiO₃/NiTiO₃ inorganic composite pigment was prepared. The synthesized pigments were characterized by X-ray diffraction (XRD), Raman spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDS), laser particle size (LPS) analysis and colorimetry. The results show that when the calcination temperature is 800 °C and the Co/Ni molar ratio is 0.5:0.5, the pigments consist of a TiO₂ core and outer ilmenite CoTiO₃/NiTiO₃ shell. Moreover, the surface of the product microspheres is smooth, and the particles are of regular sphericity with a uniform particle size of about 1.8 μm. The colorimetric analysis from the samples calcined at 800 °C shows color changes from yellow-green to dark green as the Co/Ni molar ratio increases (0.1:0.9 to 0.9:0.1). A Co/Ni molar ratio that is too high or too low results in the formation of by-products such as Co₃O₄ or NiO, respectively, which adhere to the product surface and affect the chromaticity of the product. This work has enabled the chromatic modulation of yellow-green inorganic pigments, providing a solution for the preparation of spherical inorganic pigments that are more suitable for industrial inkjet printing.     

Searching New Solutions for NiTi Sensors through Indirect Additive Manufacturing

Shape Memory Alloys (SMAs) can play an essential role in developing novel active sensors for self-healing, including aeronautical systems. However, the NiTi SMAs available in the market are almost limited to wires, small sheets, and coatings. This restriction is mainly due to the difficulty in processing NiTi through conventional processes. Thus, the objective of this study is to evaluate the potential of one of the most promising routes for NiTi additive manufacturing—material extrusion (MEX). Optimizing the different steps during processing is mandatory to avoid brittle secondary phases formation, such as Ni₃Ti. The prime NiTi powder is prealloyed, but it also contains NiTi₂ and Ni as secondary phases. The present study highlights the role of Ni and NiTi₂, with the later having a melting temperature (Tm = 984 °C) lower than the NiTi sintering temperature, thus allowing a welcome liquid phase sintering (LPS). Nevertheless, the reaction of the liquid phase with the Ni phase could contribute to the formation of brittle intermetallic compounds, particularly around NiTi and NiTi₂ phases, affecting the final structural properties of the 3D object. The addition of TiH₂ to the virgin prealloyed NiTi powder was also studied and revealed the non-formation of Ni₃Ti for a specific composition. The balancing addition of extra Ni revealed priority in the Ni₃Ti appearance, emphasizing the role of Ni. Feedstocks extruded (filaments) and green strands (layers), before and after debinding & sintering, were used as homothetic of 3D objects for evaluation of defects (microtomography), microstructures, and mechanical properties. The composition of prealloyed powder with 5 wt.% TiH₂ addition after sintering showed a homogeneous matrix with the NiTi₂ second phase uniformly dispersed.     

Impact of Particle Size on Performance of Selective Laser Sintering Walnut Shell/Co-PES Powder

The agricultural and forestry waste walnut shell and copolyester hot-melt adhesives (Co-PES) powder were selected as feedstock. A kind of low-cost, low-power consumption, and environmentally friendly walnut shell/Co-PES powder composites (WSPC) was used for selective laser sintering (SLS). Though analyzing the size and morphology of walnut shell particle (≤550 μm) as well as performing an analysis of surface roughness, density, and mechanical test of WSPC parts with different particle sizes, results showed that the optimal mechanical performance (tensile strength of 2.011 MPa, bending strength of 3.5 MPa, impact strength of 0.718 KJ/m²) as walnut shell powder particle size was 80 to 120 μm. When walnut shell powder particle diameter was 120 to 180 μm, the minimum value of surface roughness of WSPC parts was 15.711 μm and density was approximately the maximum (0.926 g/cm³).     

High-Temperature Corrosion of APS- and HVOF-Coated Nickel-Based Super Alloy under Air Oxidation and Melted Salt Domains

Various thermal spraying approaches, such as air/atmospheric plasma spraying (APS) and high-velocity oxy-fuel (HVOF) spraying, are widely employed by plants owing to their flexibility, low costs and the high surface quality of the manufactured product. This study focuses on the corrosion behavior of a Ni superalloy coated with powder Cr₃C₂-25NiCr through APS and HVOF at 950 °C under air oxidation and Na₂SO₄ + 0.6V₂O₅ molten salt environments (MSE). The results show that HVOF-deposited Ni superalloys have higher hardness and bond strength than the respective APS coating. The thermo-gravimetric probe reveals that the Ni superalloys exposed to an oxidizing air environment has a minor mass gain compared to those under the MSE domain for both non-coated and coated samples, in line with the parabola curvature rate oxidizing law. The Ni superalloys show good corrosion resistance but poor oxidation resistance in APS-deposited Ni superalloys under the MSE. HVOF-coated Ni superalloys in both environments exhibit better corrosion resistance and lower mass gain than APS-coated superalloys. The excellent coating characteristics of HVOF-coated Ni superalloys lead to their better high-temperature corrosion performance than APS.     

Ultrafine-Grained Zn–Mg–Sr Alloy Synthesized by Mechanical Alloying and Spark Plasma Sintering

Zinc materials are considered promising candidates for bioabsorbable medical devices used for the fixation of broken bones or stents. Materials for these applications must meet high mechanical property requirements. One of the ways to fulfil these demands is related to microstructure refinement, particularly the decrease in grain size. In the present work, we combine two powder metallurgy techniques (mechanical alloying—MA, and spark plasma sintering—SPS) to prepare Zn–1Mg–0.5Sr nanograin material. The microstructure of compacted material consisted of Zn grains and particles of Mg₂Zn₁₁ intermetallic phases from 100 to 500 nm in size, which resulted in high values of hardness and a compressive strength equal to 86 HV1 and 327 MPa, respectively. In this relation, the combination of the suggested techniques provides an innovative way to form extremely fine microstructures without significant coarsening during powder compaction at increased temperatures.     

Sulfidized Nanoscale Zerovalent Iron Supported by Oyster Powder for Efficient Removal of Cr (VI): Characterization,Performance, and Mechanisms

In this study, sulfidized nanoscale zerovalent iron (S-nZVI) supported by oyster shell (OS) powder (S-nZVI@OS) was synthesized by controlling the initial S/Fe ratios (0.1–0.5) to explore the potential synergistic effects during the adsorption and reduction of Cr (VI). X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analyses showed that Fe (0) and FeS were well dispersed on the OS surface. Furthermore, the stability of S-nZVI@OS composite was higher than that of nZVI, which was proved by the material ageing experiment. The effects of different S/Fe molar ratios, time, temperature, the initial concentration of Cr (VI), and initial pH on the removal efficiency were also studied. The results indicated that with the increase of the S/Fe molar ratio, the removal capacity of Cr (VI) first increased rapidly and then decreased slowly. Batch experiments showed that an optimal S/Fe molar ratio of 0.2 offered a Cr (VI) removal capacity of about 164.7 mg/g at pH 3.5. The introduction of S can not only promote Cr (VI) reduction but also combine with Cr (III) by forming precipitate on S-nZVI@OS mainly as Cr_xFe_(1−x) OOH and Cr₂S₃. The adsorption thermodynamics and kinetics demonstrated that the Langmuir model and pseudo-second-order kinetics model can describe the adsorption isotherms and kinetics. These results suggest that S-nZVI@OS is an effective and safe material for removing Cr (VI) from aqueous solutions.     

Granulation of Silicon Nitride Powders by Spray Drying: A Review

Spray drying is a widely used method of converting liquid material (aqueous or organic solutions, emulsions and suspensions) into a dry powder. Good flowability, narrow size distribution, and controllable morphology are inherent in powders produced by spray drying. This review considers the granulation factors that influence the final properties of the silicon nitride dried powders. The first group includes the types of atomizers, manifolds, and drying chamber configurations. The process parameters fall into the second group and include the following: inlet temperature, atomizing air flow, feed flow rate, drying gas flow rate, outlet temperature, and drying time. Finally, the last group, feedstock parameters, includes many factors such as feed surface tension, feed viscosity, solvent type, solid particle concentration, and additives. Given the large number of factors affecting morphology, particle size and moisture, optimizing the spray drying process is usually achieved by the “trial and error” approach. Nevertheless, some factors such as the effect of a solvent, dispersant, binder, and sintering additives considered in the literature that affect the Si₃N₄ granulation process were reviewed in the work. By summarizing the data available on silicon nitride powder production, the authors attempt to tackle the problem of its emerging demand in science and industry.     

Reactive Flash Sintering of High-Entropy Oxide (Mg,Co, Ni,Cu, Zn)1−xLixO at Room Temperature

(Mg, Co, Ni, Cu, Zn)_1−xLi_xO is a type of high-entropy oxide that has high ionic conductivity at room temperature and is used as a solid electrolyte. (Mg, Co, Ni, Cu, Zn)_1−xLi_xO was successfully synthesized from precursor powder by applying reactive flash sintering for less than 4 min at room temperature (25 °C). AC and DC electric fields were independently applied to sinter ceramic samples; consequently, AC and DC electric field application resulted in relative densities that exceeded 90% and 80%, respectively. X-ray diffraction spectra of samples revealed the existence of a clear halite structure with an insignificant impurity phase, proving that (Mg, Co, Ni, Cu, Zn)_1−xLi_xO crystals were successfully produced.     

Facilitated Synthesis of Mg2Ni Based Composites with Attractive Hydrogen Sorption Properties

Composites based on Mg₂Ni with 5% activated carbon from apricot stones (ACAP) have been prepared by ball milling and subsequent annealing in hydrogen atmosphere. The purpose of the primary metal (Mg, Ni, and V) milling was to reduce the particle size and achieve a good contact between them, without forming intermetallic compounds. During hydriding/dehydriding at 300 °C the amount of the Mg₂Ni phase progressively increased, and after 10 cycles about 50% Mg₂(Ni,V) was achieved. The hydrogenation produced mainly Mg₂NiH₄, but small amounts of MgH₂ and VH_x were also detected in the powder mixture. Relatively high hydrogen storage capacity and fast hydriding/dehydriding kinetics of the Mg_2.1Ni_0.7V_0.3—5 wt.% ACAP composite were determined both from hydrogen gas phase and electrochemically.     

Molten Salt Synthesis of Intermetallic Compound TiNi Nanopowder Passivated by TiOx Shell Prepared from NiTiO3 for Catalytic Hydrogenation

Titanium-nickel alloy is an attractive material due to its unique properties of shape memory effect, superior elasticity, and biocompatibility. Generally, Ti-Ni alloy powders are prepared from pure elemental powders of Ti and Ni as starting materials, but it is an energy-intensive process to obtain pure titanium. In this study, intermetallic compound TiNi powder passivated by TiO_x shell was prepared by directly reducing a commercial NiTiO₃ using CaH₂ reducing agent in a molten LiCl at 650 °C. Analyses by X-ray diffraction, scanning electron microscopy/transmission electron microscopy with energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy revealed that the powder had a core–shell structure, with the core of TiNi and the shell of TiO_x-rich composition with scarce metallic Ni nicely catalyzing hydrogenation reactions with good recyclability and stability.     

One-Pot Synthesis of Nanostructured Ni@Ni(OH)2 and Co-Doped Ni@Ni(OH)2 via Chemical Reduction Method for Supercapacitor Applications

Crystalline Ni@Ni(OH)₂ (cNNH) and Co-doped cNNH were obtained via a simple one-pot hydrothermal synthesis using a modified chemical reduction method. The effect of each reagent on the synthesis of the nanostructures was investigated concerning the presence or absence of each reagent. The detailed morphology shows that both nanostructures consist of a Ni core and Ni(OH)₂ shell layer (~5 nm). Co-doping influences the morphology and suppresses the particle agglomeration of cNNH. Co-doped cNNH showed a specific capacitance of 1238 F g⁻¹ at 1 A g⁻¹ and a capacitance retention of 76%, which are significantly higher than those of cNNH. The enhanced performance of the co-doped cNNH is attributed to the reduced path length of the electrons caused by the decrease in the size of the nanostructure and the increased conductivity due to Co ions substituting Ni ions. The reported synthesis method and electrochemical behaviors of cNNH and Co-doped cNNH affirm their potential as electrochemically active materials for supercapacitor applications.     

Phase Transformation after Heat Treatment of Cr-Ni Stainless Steel Powder for 3D Printing

Today, Ni-Cr steel is used for advanced applications in the high-temperature and electrical industries, medical equipment, food industry, agriculture and is applied in food and beverage packaging and kitchenware, automotive or mesh. A study of input steel powder from various stages of the recycling process intended for 3D printing was conducted. In addition to the precise evaluation of the morphology, particle size and composition of the powders used for laser 3D printing, special testing and evaluation of the heat-treated powders were carried out. Heat treatment up to 950 °C in an air atmosphere revealed the properties of powders that can appear during laser sintering. The powders in the oxidizing atmosphere change the phase composition and the original FeNiCr stainless steel changes to a two-phase system of Fe₃Ni and Cr₂O₃, as evaluated by X-ray diffraction analysis. Observation of the morphology showed the separation of the oxidic phase in the sense of a brittle shell. The inner part of the powder particle is a porous compact core. The particle size is generally reduced due to the peeling of the oxide shell. This effect can be critical to 3D printing processing, causing defects on the printed parts, as well as reducing the usability of the precursor powder and can also change the properties of the printed part.     

Comparative Study on the Thermal Performance of Cr-CrxOy and YSZ-CoNiCrAlY Coatings Exposed at 900 °C

Yttria stabilized zirconia (YSZ) thermal barrier coatings (TBCs) deposited on CoNiCrAlY oxidation protective bond coats are commonly required in temperature regimes up to 1200 °C (e.g., hot gas turbine regions) due to their superior thermal behavior and mechanical properties. For temperatures up to around 900 °C, oxidation protection can be alternatively provided by metallic-ceramic Cr-Cr_xO_y coatings. For the present research, Cr-Cr_xO_y atmospheric plasma sprayed (APS) and YSZ-CoNiCrAlY APS-high velocity oxy-fuel TBC coatings were deposited on a NiCr20Co18Ti substrate. The samples were isothermally heat treated at 900 °C for 10 h in an environmental atmosphere and subsequently isothermally oxidized at the same temperature for 1200 h. Investigations of the physical, chemical, and mechanical properties were performed on the as-sprayed, heat-treated, and oxidized samples. The oxidation behavior, microhardness, cohesion, and adhesion of the samples were correlated with the microstructural investigations and compared to the conventional TBC system. It could be shown that heat treating decreased the Cr-Cr_xO_y coatings crack susceptibility and led to the formation of a protective thermally grown Cr oxide layer. The experimental work on the YSZ-CoNiCrAlY system revealed that the phase composition of the bond coat has a direct influence on the oxidation protection of the coating system.     

Corrosion Behavior of Detonation Gun Sprayed Fe-Al Type Intermetallic Coating

The detonation gun sprayed Fe-Al type coatings as an alternative for austenitic valve steel, were investigated using two different methods of testing corrosion resistance. High temperature, 10-hour isothermal oxidation experiments at 550, 750, 950 and 1100 °C show differences in the oxidation behavior of Fe-Al type coatings under air atmosphere. The oxide layer ensures satisfying oxidation resistance, even at 950 and 1100 °C. Hematite, α-Al₂O₃ and metastable alumina phases were noticed on the coatings top surface, which preserves its initial thickness providing protection to the underlying substrate. In general, only negligible changes of the phase composition of the coatings were noticed with simultaneous strengthening controlled in the micro-hardness measurements, even after 10-hours of heating at 1100 °C. On the other hand, the electrochemical corrosion tests, which were carried out in 200 ppm Cl⁻ (NaCl) and pH ~4 (H₂SO₄) solution to simulate the acid-rain environment, reveal higher values of the breakdown potential for D-gun sprayed Fe-Al type coatings than the ones for the bulk Fe-Al type alloy and Cr21Mn9Ni4 austenitic valve steel. This enables these materials to be used in structural and multifunctional applications in aggressive environments, including acidic ones.     

Plasma-Induced Catalyst Support Defects for the Photothermal Methanation of Carbon Dioxide

The presence of defects in a catalyst support is known to benefit catalytic activity. In this work, a He-plasma treatment-based strategy for introducing and stabilising defects on a Ni/TiO₂ catalyst for photothermal CO₂ hydrogenation was established. The impact of pretreatment step sequence—which comprised He-plasma treatment and reduction/passivation—on defect generation and stabilisation within the support was evaluated. Characterisation of the Ni/TiO₂ catalysts indicated that defects created in the TiO₂ support during the initial plasma treatment stage were then stabilised by the reduction/passivation process, (P-R)Ni/TiO₂. Conversely, performing reduction/passivation first, (R-P)Ni/TiO₂, invoked a resistance to subsequent defect formation upon plasma treatment and consequently, poorer photothermal catalytic activity. The plasma treatment altered the metal-support interaction and ease of catalyst reduction. Under photothermal conditions, (P-R)Ni/TiO₂ reached the highest methane production in 75 min, while (R-P)Ni/TiO₂ required 165 min. Decoupling the impacts of light and heat indicated thermal dominance of the reaction with CO₂ conversion observed from 200 °C onwards. Methane was the primary product with carbon monoxide detected at 350 °C (~2%) and 400 °C (~5%). Overall, the findings demonstrate the importance of pretreatment step sequence when utilising plasma treatment to generate active defect sites in a catalyst support.     

Phase Changes in the Surface Layer of Stainless Steel Annealed at a Temperature of 550 °C

Stainless steels have the advantage of forming a protective surface layer to prevent corrosion. This layer results from phase and structural changes on the steel surface. Stainless steel samples (1.4404, 316L), whose alloying elements include Cr, Ni, Mo, and Mn, were subjected to the study of the surface layer. Prism-shaped samples (25 × 25 × 3) mm³ were made from CL20ES stainless steel powder, using selective laser melting. After sandblasting with corundum powder and annealing at 550 °C for different periods of time (2, 4, 8, 16, 32, 64, 128 h), samples were studied by conversion X-ray Mössbauer spectroscopy (CXMS), conversion electron Mössbauer spectroscopy (CEMS), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). The main topics of the research were surface morphology and elemental and phase composition. The annealing of stainless steel samples resulted in a new surface layer comprising leaf-shaped crystals made of chromium oxide. The crystals grew, and their number increased as annealing time was extended. The amount of chromium increased in the surface layer at the expense of iron and nickel, and the longer the annealing time was set, the more chromium was observed in the surface layer. Iron compounds (BCC iron, mixed Fe–Cr oxide) were found in the surface layer, in addition to chromium oxide. BCC iron appeared only after annealing for at least 4 h, which is the initial time of austenitic–ferritic transformation. Mixed Fe–Cr oxide was observed in all annealed samples. All phase changes were observed in the surface layer at approximately 0.6 µm depth.