Search Results (40)

This study reports the synthesis of aluminum-doped ZnO nanoparticles (Al-ZnO NPs) via a top-down mechanochemical solid-state reaction (SSR) approach using high-energy ball milling (HEBM) as a rapid, controllable, and efficient method. Al-ZnO samples were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and UV-Vis diffuse reflectance spectroscopy. Significantly, the band gap decreased by 0.215 eV when transitioning from pure ZnO to 9 wt.% Al-doped ZnO (Al-ZnO9). TEM analysis showed that after 4 h of milling at 1000 rpm, the particle size was reduced to 59 nm, exhibiting a spherical morphology crucial for enhanced bioactivity. The antimicrobial properties of the Al-ZnO NPs were evaluated using the well diffusion method against various pathogenic microorganisms, with a particular focus on Staph. aureus ATCC 29213 and Staph. epidermidis ATCC 12228, given their clinical significance as common pathogens in infections related to medical implants and prosthetics. Al-ZnO9 demonstrated superior antibacterial performance, producing inhibition zones of 13 mm and 15 mm against Staph. aureus and Staph. epidermidis, respectively. Moreover, exposure to visible light further amplified the antimicrobial activity. This research underscores the potential for the scalable production of Al-ZnO NPs, presenting a promising solution for addressing infections linked to implanted medical devices. Full article

The tetragonal R_1−xZr_x(FeCo)₁₁Ti alloys, where R is a rare earth and Ti a transition metal, are promising candidates for permanent magnets. Sm_1−xZr_x(Fe_0.8Co_0.2)_12−yTi_y (x = 0 and 0.25; y = 1 and 0.7) master alloys were prepared by arc melting under argon atmosphere. Some of the samples were almost single-phase compounds at 1:12, with a very small amount of a-Fe(Co). Partially replacing Sm with Zr produced alloys with small amounts of Sm(FeCo)₂ Laves-type phases. The as-cast ingots were milled using high-energy ball milling (HEBM) for different times in an argon atmosphere and then annealed at 973 K–1173 K at different interval times (15–90 min). After annealing, the sample milled for 4 h contained a large variation of grain size from 2–4 μm to 20 μm or larger, while, after annealing, the other sampled milled for 8 h exhibited grains size in the range of 2–6 μm; therefore, their coercivity was higher, reaching a maximum value of 5.5 kOe for SmFe₉Co₂Ti annealed at 1123 K for 60 min. Coercivity was strongly affected by the annealing temperature and time. The microstructure evolution with emphasis on the particles size during annealing and their correlation with coercivity are herein discussed. Full article

The synthesis of CaKFe₄As₄ superconducting compounds either requires the adoption of high-temperature synthesis or implies the intimate mixing of the precursors via mechanochemical routes before the thermal step in order to avoid chemical inhomogeneities that lead to thermodynamically stable unwanted phases. High Energy Ball Milling (HEBM) represents a useful tool to ensure the comminution of the elements and their dispersion to obtain the target phase. The adoption of mechanochemical treatments is, however, known to lead to the formation of aggregates of small crystals, leading to a powder morphology not optimal for practical applications. In this work, we report our findings in the synthesis of CaKFe₄As₄ polycrystalline compounds showing the effect of milling energy on the morphology and phase composition of the powders. To overcome the limits of conventional synthesis, we report the results of a novel synthesis approach for CaKFe₄As₄ materials, highlighting how the choice of the proper precursors and the adoption of milder treatments can represent the key to optimizing the powder morphology. Full article

This study is inspired by the importance of advanced composites, combining spontaneous magnetization with electrical charge storage properties. It is focused on the investigation of magnetically hard SrFe₁₂O₁₉ (SFO) material and its composites with polypyrrole (PPy). For the first time, an organic surfactant–charge transfer mediator and high-energy ball milling (HEBM) were applied to the preparation of high-active-mass SFO composite electrodes. An important finding was the ability to achieve enhanced capacitance of SFO and its composites in a negative range of electrode potentials in an electrolyte. The benefits of the sodium sulfate electrolyte and the charge storage mechanism are discussed. Another important finding was the synergy of the properties of SFO and PPy, which allowed the preparation of highly capacitive conductive composites. The effects of HEBM and the SFO content in the composites on the capacitive properties were studied. Magnetic measurements revealed the effect of HEBM on the magnetic properties and demonstrated good magnetic properties of the composites, which also exhibited advanced capacitive properties. The composites were utilized for the manufacturing of an asymmetric device, which exhibited high capacitive properties at an applied voltage of 1.5 V. Full article

Carbon fiber reinforced polymer (CFRP) composites have very high specific properties, which is why they are used in the aerospace, wind power, and sports sectors. However, the high consumption of CFRP compounds leads to a high volume of waste, and it is necessary to formulate mechanical recycling strategies for these materials at the end of their useful life. The recycling differences between cutting-end mills and high-energy ball milling (HEBM) were evaluated. HEBM recycling allowed us to obtain small recycled particles, but separating their components, carbon fiber, epoxy resin, and CFRP particles, was impossible. In the case of mill recycling, these were obtained directly from cutting a CFRP composite laminate. The recycled materials resulted in a combination of long fibers and micrometric particles—a sieving step allowed for more homogeneous residues. Although long, individual carbon fibers can pass through the sieve. Ultrasonication did not significantly affect HEBM recyclates because of the high energy they are subjected to during the grinding process, but it was influential on end mill recyclates. The ultrasonication amplitude notably impacted the separation of the epoxy resin from the carbon fiber. The end mill and HEBM waste production process promote the presence of trapped air and electrostatics, which allows recyclates to float in water and be hydrophobic. Full article

This investigation is motivated by an interest in multiferroic BaFe₁₂O₁₉ (BFO), which combines advanced ferrimagnetic and ferroelectric properties at room temperature and exhibits interesting magnetoelectric phenomena. The ferroelectric charge storage properties of BFO are limited due to high coercivity, low dielectric constant, and high dielectric losses. We report the pseudocapacitive behavior of BFO, which allows superior charge storage compared to the ferroelectric charge storage mechanism. The BFO electrodes show a remarkably high capacitance of 1.34 F cm⁻² in a neutral Na₂SO₄ electrolyte. The charging mechanism is discussed. The capacitive behavior is linked to the beneficial effect of high-energy ball milling (HEBM) and the use of an efficient dispersant, which facilitates charge transfer. Another approach is based on the use of conductive polypyrrole (PPy) for the fabrication of PPy-BFO composites. The choice of new polyaromatic dopants with a high charge-to-mass ratio plays a crucial role in achieving a high capacitance of 4.66 F cm⁻² for pure PPy electrodes. The composite PPy-BFO (50/50) electrodes show a capacitance of 3.39 F cm⁻², low impedance, reduced charge transfer resistance, enhanced capacitance retention at fast charging rates, and good cyclic stability due to the beneficial effect of advanced dopants, HEBM, and synergy of the contribution of PPy and BFO. Full article

The influence of milling time and volume fraction of reinforcement on the morphology, microstructure, and mechanical behaviors of SiC_p-reinforced AA2017 composite powder produced by high-energy ball milling (HEBM) was investigated. AA2017 + SiC_p composite powder with different amounts of SiC particles (5, 10, and 15 vol%) was successfully prepared from gas-atomized AA2017 aluminum alloy powder with a particle size of <100 μm and silicon carbide (SiC) powder particles with an average particle size of <1 μm. An optical microscope (OM), X-ray diffraction (XRD), and scanning electron microscope (SEM) were utilized to characterize the microstructure of the milled composite powder at different milling periods. The results indicated that the SiC particles were homogeneously distributed in the AA2017 matrix after 5 h of HEBM time. The morphology of the particles transformed from a laminar to a nearly spherical shape, and the size of the milled powder particles reduced with increasing the content of SiC particles. The XRD analysis was carried out to characterize the phase constituents, crystallite size, and lattice strain of the composite powders at different milling periods. It was found that with increasing milling time and SiC volume fraction, the crystallite size of the aluminum alloy matrix decreased while the lattice strain increased. The average crystallite sizes were reduced from >300 nm to 68 nm, 64 nm, and 64 nm after 5 h of milling, corresponding to SiC contents of 5, 10, and 15 vol%, respectively. As a result, the lattice strain increased from 0.15% to 0.5%, which is due to significant plastic deformation during the ball milling process. XRD results showed a rapid decrease in crystallite size during the early milling phase, and the minimum grain size was achieved at a higher volume fraction of SiC particles. Microhardness tests revealed that the milling time has a greater influence on the hardness than the amount of SiC reinforcements. Therefore, the composite powder milled for 5 h showed an average microhardness three times higher than that of the unmilled powder particles. Full article

Achieving a combination of high strength and ductility in metal-based composites is still a difficult task, and it is especially challenging in a wide temperature range. Here, nanoAl₂O₃/nanoAl composites with high tensile and compressive strength and excellent ductility at 25 and 500 °C were obtained using Al and Al₂O₃ nanopowders via a combination of high-energy ball milling (HEBM) and spark plasma sintering (SPS). Being about three times lighter than conventional high-strength steel (with a density of 2.7 g/cm³ vs. that of 7.8 g/cm³ for steel), the nanoAl₂O₃/nanoAl materials demonstrated tensile strength and elongation before failure comparable with those of steel. The nanoAl₂O₃/nanoAl composites were strengthened with two types of Al₂O₃ NPs, in situ formed, and introduced into the powder mixture. The resulting materials had a bimodal microstructure consisting of Al with micron and submicron grains surrounded by an Al/Al₂O₃ framework whose structural components were all in the size range of 20–50 nm. Among the studied compositions (0, 1, 2, 3, 4, 5, 10, and 20 wt.% of Al₂O₃), the Al-3%Al₂O₃ material showed the best thermomechanical properties, such as a tensile strength of 512 MPa and 280 MPa and a compressive strength of 489 MPa and 344 MPa at 25 and 500 °C, respectively, with an elongation to failure of 15–18%. These results show the promise of nanoAl₂O₃/nanoAl composites for use as small items in the automotive and aviation industries. Full article

The present work was aimed at the investigation of the effect of high-energy ball milling (HEBM) time on the sintering kinetics, structure, and properties of the heavy tungsten alloy (HTA) W-7%Ni-3%Fe. The HTA samples were obtained from nanopowders (20–80 nm) using conventional liquid-phase sintering (LPS) in hydrogen and using spark plasma sintering (SPS) in vacuum. The HTA density was shown to depend non-monotonously on the HEBM time that originates from the formation of nonequilibrium solid solutions in the W-Ni-Fe systems during HEBM. The SPS kinetics of the HTA nanopowders was shown to have a two-stage character, the intensity of which depends on the Coble diffusion creep rate and on the intensity of diffusion of the tungsten atoms in the crystal lattice of the γ-phase. The kinetics of sintering of the initial submicron powders has a single-stage character originating from the intensity of the grain boundary diffusion in the γ-phase. The dependencies of the hardness and of the yield strength on the grain sizes were found to obey the Hall–Petch relation. The hardness, strength, and dynamic strength in the compression tests of the fine-grained tungsten alloys obtained using SPS and LPS were studied. Full article

This investigation is motivated by interest in nanostructured FeOOH anodes for aqueous asymmetric supercapacitors operating in Na₂SO₄ electrolyte. The research goal is the fabrication of anodes with high active mass loading of 40 mg cm⁻², high capacitance and low resistance. The influence of high-energy ball milling (HEBM), capping agents and alkalizer on the nanostructure and capacitive properties is investigated. HEBM promotes the crystallization of FeOOH, which results in capacitance reduction. Capping agents from the catechol family, such as tetrahydroxy-1,4-benzoquinone (THB) and gallocyanine (GC), facilitate the fabrication of FeOOH nanoparticles, eliminate the formation of micron size particles and allow the fabrication of anodes with enhanced capacitance. The analysis of testing results provided insight into the influence of the chemical structure of the capping agents on nanoparticle synthesis and dispersion. The feasibility of a conceptually new strategy for the synthesis of FeOOH nanoparticles is demonstrated, which is based on the use of polyethylenimine as an organic alkalizer-dispersant. The capacitances of materials prepared using different nanotechnology strategies are compared. The highest capacitance of 6.54 F cm⁻² is obtained using GC as a capping agent. The obtained electrodes are promising for applications as anodes for asymmetric supercapacitors. Full article

In this study, CNTs-reinforced Al-Cu-Mg-Si nanocomposites were successfully fabricated by high-energy ball milling (HEBM) combined with semi-solid stir casting. Then, the composites were subjected to hot extrusion. The Microstructure and Phase analysis of the CNT/Al-Cu-Mg-Si composites were characterized by an Optical microscope, Scanning Electron Microscope (SEM), and XRD. Additionally, density, hardness, and wear were measured. The results revealed that the addition of CNTs effectively inhibited the growth of α-Al grains, and the grains were dramatically refined. Additionally, the dynamic recrystallization degree of the composite extruded rod gradually increased from 1.3% to 68.4%, with the content of CNTs from 0 wt% to 3.0 wt%. The hardness values of the composite increased with an increase in CNTs. Moreover, the friction factor and wear rate of the composites first decreased and then increased as the content of CNTs increased. When 1.5CNTs were added, the friction coefficient (COF) and wear rate of composites reached the minimum of 0.3577 and 3.42 mg/km, which were reduced by 30.09% and 73.03% compared with Al-Cu-Mg-Si alloy, respectively. Full article

The research and development of materials suitable for hydrogen storage has received a great deal of attention worldwide. Due to the safety risks involved in the conventional storage of hydrogen in its gaseous or liquid phase in containers and tanks, development has focused on solid-phase hydrogen storage, including metals. Light metal alloys and high-entropy alloys, which have a high potential for hydrogen absorption/desorption at near-standard ambient conditions, are receiving interest. For the development of these alloys, due to the complexity of their compositions, a computational approach using CALPHAD (Calculation of Phases Diagrams) and machine learning (ML) methods that exploit thermodynamic databases of already-known and experimentally verified systems are being increasingly applied. In order to increase the absorption capacity or to decrease the desorption temperature and to stabilize the phase composition, specific material preparation methods (HEBM—high-energy milling, HPT—high-pressure torsion) referred to as activation must be applied for some alloys. Full article

In our search for an optimum soft magnet with excellent mechanical properties which can be used in applications centered around “electro mobility”, nanocrystalline CoCrFeNiGa_x (x = 0.5, 1.0) bulk high entropy alloys (HEA) were successfully produced by spark plasma sintering (SPS) at 1073 K of HEA powders produced by high energy ball milling (HEBM). SPS of non-equiatomic CoCrFeNiGa_0.5 particles results in the formation of a single-phase fcc bulk HEA, while for the equiatomic CoCrFeNiGa composition a mixture of bcc and fcc phases was found. For both compositions SEM/EDX analysis showed a predominant uniform distribution of the elements with only a small number of Cr-rich precipitates. High pressure torsion (HPT) of the bulk samples led to an increased homogeneity and a grain refinement: i.e., the crystallite size of the single fcc phase of CoCrFeNiGa_0.5 decreased by a factor of 3; the crystallite size of the bcc and fcc phases of CoCrFeNiGa—by a factor of 4 and 10, respectively. The lattice strains substantially increased by nearly the same extent. After HPT the saturation magnetization (M_s) of the fcc phase of CoCrFeNiGa_0.5 and its Curie temperature increased by 17% (up to 35 Am²/kg) and 31.5% (from 95 K to 125 K), respectively, whereas the coercivity decreased by a factor of 6. The overall M_s of the equiatomic CoCrFeNiGa decreased by 34% and 55% at 10 K and 300 K, respectively. At the same time the coercivity of CoCrFeNiGa increased by 50%. The HPT treatment of SPS-consolidated HEAs increased the Vickers hardness (H_v) by a factor of two (up to 5.632 ± 0.188) only for the non-equiatomic CoCrFeNiGa_0.5, while for the equiatomic composition, the H_v remained unchanged (6.343–6.425 GPa). Full article

Activated carbon (AC) from sugarcane bagasse was prepared using dry chemical activation with KOH. It was then subjected to a high-energy ball milling (HEBM) treatment under various milling speeds (600, 1200 and 1800 rpm) to produce AC nanoparticles from micro-size particles. The AC samples after the HEBM treatment exhibited reduced particle sizes, increased mesopore volume and a rich surface oxygen content, which contribute to higher pseudocapacitance. Notably, different HEBM speeds were used to find a good electrochemical performance. As a result, the AC/BM12 material, subjected to HEBM at 1200 rpm for 30 min, exhibited the highest specific capacitance, 257 F g⁻¹, at a current density 0.5 A g⁻¹. This is about 2.4 times higher than that of the AC sample. Moreover, the excellence capacitance retention of this sample was 93.5% after a 3000-cycle test at a current density of 5 A g⁻¹. Remarkably, a coin cell electrode assembly was fabricated using the AC/BM12 material in a 1 M LiPF₆ electrolyte. It exhibited a specific capacitance of 110 F g⁻¹ with a high energy density of 27.9 W h kg⁻¹. Full article

High-energy ball milling (HEBM) of powders is a complex process involving mixing, morphology changes, generation and evolution of defects of the crystalline lattice, and formation of new phases. This review is dedicated to the memory of our colleague, Prof. Michail A. Korchagin (1946–2021), and aims to highlight his works on the synthesis of materials by self-propagating high-temperature synthesis (SHS) and thermal explosion (TE) in HEBM mixtures as important contributions to the development of powder technology. We review results obtained by our group, including those obtained in collaboration with other researchers. We show the applicability of the HEBM mixtures for the synthesis of powder products and the fabrication of bulk materials and coatings. HEBM influences the parameters of synthesis as well as the structure, phase composition, phase distribution (in composites), and grain size of the products. The microstructural features of the products of synthesis conducted using the HEBM precursors are dramatically different from those of the products formed from non-milled mixtures. HEBM powders are also suitable as feedstock materials for depositing coatings by thermal spraying. The emerging applications of HEBM powders and future research directions in this area are discussed. Full article