Milling Time Research Articles

The adsorption behavior and mechanism of antimony in water by jarosite ball milling mixed with nano zero-valent iron

In this study, the functional material (BMJR-nZVI) of jarosite (JR) mixed with nano-zero-valent iron (nZVI) was prepared by mixed ball milling. The surface morphology, elemental composition, specific surface area and functional groups of adsorbed materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier infrared light (FTIR), X-ray photoelectron spectroscopy (XPS), specific surface area analyzer (BET) and vibrating sample magnetometer (VSM). The influence of different mixing ratio, ball milling time and other process conditions on the antimony removal performance of BMJR-nZVI was studied, and the treatment conditions were optimized. Effects of combination method, milling ratio and milling time on the adsorption properties of BMJR-nZVI were investigated by single factor test. The results showed that the adsorbent had the best adsorption properties for Sb under the conditions of JR: nZVI 2:1 and milling time of 2 h. In antimony containing solution with pH 6 and initial concentration of 20 mg·L−1, the removal rate of Sb(III) and Sb(V) can reach up to 60.92 % and 99.82 % respectively, and BMJR-nZVI material is magnetic and can be recycled well. Main mechanism of adsorption, complexation and co-precipitation of antimony by BMJR-nZVI was confirmed.

Effect of Milling Time on the Structural and Magnetic Properties of Nanostructured Fe90Si10 Alloys

Effect of Milling Time on the Structural and Magnetic Properties of Nanostructured Fe90Si10 Alloys

Influence of processing methods on the strength activity index for sludge as a supplementary cementitious material

Utilizing activated sludge as a partial substitute for cement can both curb cement consumption and address sludge reuse in an economically and environmentally-friendly manner. This study delves into the pozzolanic activity of mechanically-thermal (MT) activated sludge and alkali-mechanical-thermal (AMT) activated sludge, employing the strength activity index (SAI) method. Microscopic insights provided by X-ray diffraction (XRD), scanning electron microscopy (SEM), and laser particle size analysis aid in the interpretation of observed phenomena. The findings underscore the superiority of MT activation over AMT activation, with an SAI of 97 %. Optimal pozzolanic activity is achieved through a 2-hours holding time, slow heating at 10 °C/min, and rapid cooling. A calcination temperature of 800 °C effectively promotes the decomposition of active minerals and enhances the sludge's pozzolanic activity. Additionally, a ball milling time of 2 minutes proves sufficient to meet practical demands, as prolonged ball milling has a limited impact on sludge pozzolanic activity.

Preparation of Humic Acid from Weathered Coal by Mechanical Energy Activation and Its Properties

Humic acid (HA) is rich in functional groups with high activity, which can effectively improve the soil environment. The large reserves of weathered coal in China provide sufficient raw material guarantee for HA extraction and utilization. At present, the activation side of weathered coal is still the main technical difficulty that restricts HA extraction. In this study, the weathered coal from Inner Mongolia was used as the raw material, and the mechanical energy was used to activate the weathered coal through a planetary ball mill, which improved the extraction rate of HA and optimized the molecular structure and composition of HA. The effects of four parameters, namely, ball material ratio, ball milling time, ball milling speed, and ball size, on the free HA content of weathered coal were investigated, the HA was extracted by alkaline extraction method, and the activated weathered coal and the extracted HA were characterized. The results showed that a ball material ratio of 9:1, a ball milling speed of 200 r/min, a ball milling time of 200 min, a milling ball size of Ф5:Ф10:Ф15 = 48:42:45 and 56:42:37 are the optimal parameters for the mechanical energy activation, and the HA extraction rate of activated weathered coal under these conditions reached 82.3%, which was 15% higher than that of the unactivated one. Moreover, the aroma of the ball-milled weathered coal increased, the content of oxygenated functional groups increased, and the molecular weight and aroma of HA increased. This provides scientific theoretical guidance for the preparation of HA with high aromaticity and large molecular weight from weathered coal.

Microstructural and photocatalytic properties of nanostructured near-β Ti-Nb-Zr alloy for total hip prosthesis use

With its unique corrosion resistance, light weight, mechanical strength, and biocompatibility, TNZ is a versatile metal alloy that is used in the aerospace and medical industries. The current study aims to investigate the effect of milling time (2, 12, 24, and 36 h) on the nanostructured ternary alloy Ti-25Nb-25Zr (TNZ) prepared by high energy ball milling, a process involving the use of a high-energy ball mill to mix and grind the alloy powders, on its structural, physical, and photocatalytic characterizations. The alloys' characteristics, such as morphology, structural properties, relative density/porosity, surface roughness, hardness, and Young's modulus, were evaluated using SEM, XRD, surface profilometer, and microdurometer, respectively. The photocatalytic characterization was conducted by measuring their absorbance as a function of time using a spectrophotometer of visible and ultraviolet light in the wavelength range of 250–650 nm. Results showed that the crystallite and mean pore size reduced with increasing milling time, with the smallest values of 25 nm and 34 μm, respectively, after 36 h. This indicates that longer milling times result in a more compact and uniform structure, which could enhance the mechanical properties of the alloy. Structural characterization shows that the amount of the β-Ti phase increased with increasing milling time, resulting in the spherical morphology and texturing of the synthesized alloys. The milled alloys' structural evolution and morphological changes were sensitive to their milling times. Also, the relative density, Young's modulus, and hardness increased, reaching values of 89 %, 105 GPa, and 352 HV, respectively, due to grain size decreasing with increasing milling time. This suggests that longer milling times lead to a denser and harder alloy, which could be beneficial for its use in total hip prostheses. The photocatalytical characterization demonstrated that the degradation of orange II (OII) increased with increasing milling time. The Ti-25Nb-25Zr catalyst gave the best degree of degradation, which meant that the decolorization process could be operated rapidly and at a relatively low cost without UV irradiation.

Exploring the relationship between bulk Young’s Modulus of materials and milling efficiency during wet bead milling of pharmaceutical compounds

Wet bead milling (WBM) is one of the main approaches for manufacturing long acting injectable (LAI) suspensions, wherein the particle size of an Active Pharmaceutical Ingredient (API) is reduced in a liquid vehicle via grinding. A common challenge observed during WBM is long milling time to achieve target particle size, resulting in poor milling efficiency. The objective of this work was to identify potential API attributes predictive of milling efficiency during WBM. In this study, physical and mechanical properties of nine APIs were characterized. Formulations with these APIs were manufactured using WBM. Bulk Young’s Modulus was identified to have a significant influence on the rate of particle attrition. The rank order of Young’s Moduli of the APIs was consistent with that of milling efficiency, estimated by an empirical function defined in this study called Milling Resistance (ϕ), representing the holistic impact of milling time, tip speed, bead loading, and batch to chamber volume ratio. The identification of such intrinsic material properties, which provide an early evaluation of potential manufacturing risks, is beneficial to product development, as these assessments can be performed with limited quantities of materials and help identify and design out scale-up challenges.

Effect of ball milling time on Sr0.7Sm0.3Fe0.4Co0.6O2.65 perovskites and their application as semiconductor layers in dye-sensitized solar cells

The practical utilization of TiO2 as a semiconductor in dye-sensitized solar cells (DSSCs) has been set back by poor visible light absorption, high charge carrier recombination, and low electrical conductivity, which reduce the power conversion efficiency (PCE) and sustainability of the device. In this respect, perovskites with excellent properties, such as large surface area, good optical properties, high electrical conductivity, and superior electrochemical stability, have recently emerged as promising alternatives capable of overcoming the drawbacks of TiO2. Herein, Sr0.7Sm0.3Fe0.4Co0.6O2.65 (SSFC) perovskites were prepared via the ball milling method at various milling times of 0, 5, and 10 h, and the obtained samples were denoted by SSFC-0, SSCF-5, and SSCF-10, respectively. Increasing the ball milling time led to a significant reduction in nanoparticle size and agglomeration, which, in turn, increased the surface area and electrical conductivity of the samples. As a consequence, the SSFC-10 perovskite exhibited the smallest average particle sizes (18.9 nm) with the largest surface area (61.8 m2 g−1) and minimum defects, which allowed for efficient electron transport, resulting in the best electrical conductivity of 49.8 S cm−1. Ultimately, DSSCs fabricated using SSFC-10 semiconductor layers achieved an optimum PCE of 6.01 %, which is an improvement of 8.67 %, 1.1 %, and 6.56 % for SSFC-0 (3.69 %), SSFC-5 (4.96 %), and TiO2 (5.64 %), respectively. Thus, varying the ball milling time can be used as an effective technique to tailor the physicochemical properties of SSFC to suit desired applications, particularly the fabrication of highly efficient and sustainable DSSC semiconductor layers.

Preparation and properties of porous rice husk ash for internal curing of high performance cement pastes

To address the challenges posed by significant autogenous shrinkage in high-performance concrete and mitigate the adverse effects of conventional internal curing materials on its mechanical properties, this study explored the potential use of rice husk ash (RHA) as internal curing materials. The research investigated the impact of combustion regime (combustion temperature and dwelling time) and the milling process on the microstructure and physical-chemical properties of RHA. Moreover, the effect of RHA on autogenous shrinkage, compressive strength, and microstructure in cement pastes were also reported. Experimental results demonstrated that the combustion regime and milling time could significantly affect the pore structure, particle size and pozzolanic activity of RHA. RHA had good potential for internal curing when it was burned at 600°C for 1 h and milled for 15–30 min. RHA released the entrained water after 12 h to slow down the depletion of free water, and thus inhibited the development of self-drying and autogenous shrinkage. The 168 h shrinkage was reduced by 56.8 %, 62 %, and 51.8 %, respectively when the milling time increased to 30 min. Moreover, the addition of RHA with a smaller particle size could refine the microstructure of matrix and enhance the compressive strength due to its higher pozzolanic activity. These findings suggest promising applications for RHA as an effective internal curing material in high-performance cementitious materials.

Wood waste ash as sole solid precursor in a novel alkali-activated material: Influence of the ash particle size

Wood waste ash (WWA) was utilized as sole solid precursor in alkali-activated material (AAM) with NaOH as alkaline activator. WWA was milled at different times (15–30-60–120-180–240-300–360-600 min) to obtain the optimum milling time. Characterization results showed that WWA was mainly composed of SiO2 (68.6 wt%); XRD identified amorphous phase, quartz, and calcite; and volume moment mean diameter (D[4,3]) was 9.97 µm after 240 milling minutes. XRD/FTIR of pastes showed that WWA reacted with NaOH, chemical shrinkage concluded that occurred formation of expansive reaction products, and SEM/EDS identified poorly compacted and layered Na-Si reaction products. Compressive strength of mortars reached 17.0 ± 0.8 MPa (3 days at 65 °C) and 5.0 ± 0.2 MPa (7 days at 25 °C). Highest reaction development and strength were obtained for AAM produced with WWA milled for 240 min.

Исследование железоматричных композитов с карбидным упрочнением, полученных спеканием механоактивированных смесей титанидов железа с углеродом

Introduction. The addition of dispersed solid particles of refractory compounds (carbides, borides, silicides) to the structure of alloy is a widely used effective way to increase the wear resistance of steels and alloys. Composites with a matrix of iron-based alloys (steel and cast iron) strengthened by titanium carbide particles are of great practical interest. The main structural characteristics, which define hardness and wear resistance of the composites, are volume fraction, dispersion and morphology of the particles of the strengthening carbide phase. The structure of composites depends on the method of its preparation. The methods of powder metallurgy combined with preliminary mechanical activation of powder mixtures have become widespread. It is previously established that in mechanically activated powder mixtures of FTi35S5 ferrotitanium, consisting of 82 % of (Fe,Al)2Ti phase, and P-803 carbon black, a reaction occurs with the formation of a composite consisting of a steel binder and titanium carbide. The synthesis reaction of carbides occurs in a solid-phase mode at combustion’s temperatures of 900–950 °C. Therefore, there is no coarsening of the structure due to the growth of carbide particles, which is typical for reactions in the presence of a liquid phase. FTi35S5 alloy contains a plenty of impurities (silicon, aluminum and etc). The purpose of the work is to investigate the phase composition and structure of the products of the interaction of Fe2Ti and FeTi iron titanides with carbon under the conditions of reaction sintering of mechanically activated powder mixtures and to determine the possibility of synthesizing iron-matrix composites strengthened with submicron titanium carbide particles. Research methods. The structure and phase composition of sintered compacts from mechanically activated powders were studied by optical metallography, X-ray diffraction (XRD) and scanning electron microscopy (SEM) using determination of the elemental composition by energy-dispersive X-ray spectroscopy (EDX). Experimental technique. The reaction mixtures were prepared using intermetallic powders obtained by vacuum sintering of compacts from iron and titanium powder mixtures of 2Fe+Ti and Fe+Ti compositions. Carbon black was added to the intermetallic powders to convert all the titanium containing in the intermetallic compounds into carbide. The titanides – carbon black mixtures were processed by an Activator 2S planetary ball mill for 10 min milling time at a rotation speed of 755 rpm (40g). The mechanically activated mixtures were cold compacted into cylindrical samples with a diameter of 20 mm, which were sintered in vacuum at а temperature of 1,200 °C and an isothermal holding time of 60 minutes. Results and discussion. According to the results of X-ray diffraction analysis, almost all titanium contained in iron titanides reacts with carbon to form carbide and reduced iron. The sintering products of compacts of both compositions contain target phases: titanium carbide with a slight shift from the equiatomic ratio and α-iron, which has the lattice parameters close to the reference data, and also a few of other phases. The titanium carbide particles in the iron binder were identified on the back-scattered electron (BSE) images due to the tonal contrast: the heavy iron appears darker against the carbide, which is composed of lighter elements. According to EDX analysis, the relative content of titanium and carbon in the carbide particles indeed corresponds to the composition of non-stoichiometric titanium carbide. Conclusion. The composites including titanium carbide and α-iron binder were obtained by sintering of iron titanides and carbon (carbon black) mechanically activated powder mixtures. The granules of composite powders obtained by crushing of sintered compacts are of interest as feedstocks for wear-resistant coatings and additive technologies, as well as for manufacturing of dense materials by other compaction methods: spark plasma sintering (SPS) or hot pressing (HP).

Quercetin nanocrystals for bioavailability enhancement: impact of different functional stabilizers on in vitro/in vivo drug performances

The purpose of this study was to investigate the impact of different functional stabilizers on in vitro/in vivo drug performances after oral administration of drug nanocrystals. Quercetin nanocrystals (QT-NCs) respectively stabilized by five types of functional stabilizers, including hydroxypropyl methyl cellulose E15 (HPMC E15), poloxamer 407 (P407), poloxamer 188 (P188), D-α-tocopherol polyethylene glycol succinate (TPGS), and glycyrrhizin acid (GL), were fabricated by wet media milling technique. The particle size, morphology, physical state, drug solubility, drug dissolution in vitro, and orally pharmacokinetic behaviors of all QT-NCs were investigated. All QT-NCs with similar particle size about 200 nm were obtained by controlling milling speed and milling time. No significant differences in particles shape and crystalline nature were found for QT-NCs stabilized by different functional stabilizers. But the solubility and dissolution of QT-NCs were significantly influenced by the different functional stabilizers. The AUC0∼ t of all QT-NCs after oral administration was in the following order: QT-NCs/P188 ≈ QT-NCs/HPMC E15 > QT-NCs/GL > QT-NCs/P407 ≈ QT-NCs/TPGS, and the C max showed an order of QT-NCs/P407 > QT-NCs/P188 ≈ QT-NCs/GL > QT-NCs/HPMC E15 > QT-NCs/TPGS. Both of QT-NCs/P407 and QT-NCs/TPGS exhibited faster oral absorption with T max at 0.5 h and 0.83 h, respectively, while the other three QT-NCs (QT-NCs/P188, QT-NCs/GL and QT-NCs/HPMC E15) showed a relatively slow absorption with same T max at 5.33 h. The longest MRT0∼ t (11.72 h) and t 1/2z (32.22 h) were observed for QT-NCs/HPMC E15. These results suggested that the different functional stabilizers could significantly influence on drug solubility, drug dissolution in vitro and orally pharmacokinetic behavior of QT-NCs, and it is possible to alter the drug dissolution in vitro, oral absorption and drug retention in vivo by changing the type of functional stabilizers in NCs preparation.

Effect of Angle of Incident on Taper Angle in Femtosecond Laser Machining for Fabrication of Cross Section Analysis Specimen

Focused ion beam (FIB) technology is one of the most widely used methods for fabricating crosssectional analysis specimens because of its high precision and characteristics that minimize the occurrence of defects. Demand for large cross-sectional area analysis is increasing to improve product reliability in various industries, but is limited by the low milling speed of FIB. Other potential techniques such as Ar ion milling and plasma FIB have been adopted, but low milling speed for large areas still remains a problem. A promising solution to this issue involves laser machining prior to FIB milling. In laser machining a laser beam is irradiated to remove materials from the target. This technique can provide several orders of magnitude higher material removal rate than FIB, however, tapering of the machined surface and laser induced damage can occur. Removing these defects leads to increased FIB milling time. In this study, the laser parameters including angle of incident (AOI) were optimized to achieve a vertical like sidewall and minimize laser induced defects. Before applying AOI, laser machining parameters were optimized to reduce the angle of the machined sidewall. The taper angle of 2.5° was fabricated using the optimized parameters and application of AOI. Raman spectroscopy, SEM, and EDS analysis were used to measure not only the geometry of the laser machined sidewalls, but laser induced residual stress and defects. These results were then used to calculate the volume of FIB milling required to remove the laser induced damages and achieve vertical sidewalls. The application of AOI can significantly reduce the processing time in the FIB milling compared to the processing time when AOI is not applied.

The mechanochemistry of lanthanum dihydride (LaH\(_{2}\)) with hydrogen (H\(_{2}\)) using the ball-mill process and the effect of oxidation on the resulting products

The complex behavior of LaH2 during ball milling was investigated in this study, with its mechanical, chemical, and morphological changes explored. The relationship between milling time and hydrogen pressure reduction was uncovered through detailed experiments, reflecting the dynamic nature of the process. A transient yet significant event was observed upon unsealing the milling jar post-milling: the emergence of a minor fire ember, indicative of the interplay between mechanical forces and chemical reactivity within the LaH2 powder. Profound changes in the structure, composition, and shape were unraveled using advanced techniques such as X-ray diffraction (XRD), scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM/EDX), and particle size distribution analysis. The resulting powder exhibited a dual-phase composition of lanthanum dihydride (LaH2, 68.1% to 71.5%) and lanthanum oxide (La2O3, 28.5% to 31.9%), reflecting a dynamic chemical equilibrium during milling. Particle size distribution analysis revealed a notable increase in average diameter to 6420 nm, accompanied by a polydispersity index (PDI) of 0.831, signifying a broadening compared to the initial LaH2 powder. The morphological evolution of the powder was elucidated through SEM imaging, showing predominantly spherical and rounded forms, indicating extensive particle agglomeration and plastic deformation during milling. Additionally, the formation of oxide layers on the powder surface, intertwined with pronounced particle agglomeration, was highlighted through EDX mapping, shedding light on the mechanical aspects of morphological evolution during milling. These findings contribute to our understanding of LaH2 behavior under extreme mechanical and chemical conditions and have implications for materials processing, hydrogen storage technologies, and broader applications in materials science and engineering.

Enhancing thermal properties and surface quality of lappato glazed porcelain tiles through milling time optimization

Increasing the surface quality of porcelain tiles, preferred in public, commercial, and living centers, where human density is high, is one of the crucial goals. Surface applications can be applied on the tiles produced as glazed and unglazed tiles in different versions. In lappato glazed tiles, staining-resistance is of great importance besides glossy-surface and wear-resistance. In this study, technical properties such as staining, chemical agent-resistance, color-parameters, thermal-behavior (heat microscopy), roughness, abrasion resistance, and microstructure of glazes (SEM/EDS) depending on the optimizing grinding time were examined with compared to standard lappato-glaze under the industrial conditions. It was observed that with the increase of the glaze grinding, the whiteness value and the increasing smoothness, and higher staining chemicals resistance and the glaze which has lower characteristic temperatures than the standard. As the surface roughness decreased due to grinding, the number and size of pores in the microstructure decreased. The glassy phase exhibited homogeneous distribution due to the dissolution of anorthite crystals.

Experimental conditions for room temperature ferromagnetism in Fe-doped SnO2 via mechanochemical milling and thermal treatment

Identifying optimal experimental conditions, preferably through a simple and cost-effective method, for the fabrication of oxide-diluted magnetic semiconductors, such as Fe-doped SnO2, holds great significance in the quest for spintronic materials operating at room temperature (RT). While mechanochemical milling is a well-established technique meeting these requirements, its numerous milling variables necessitate careful consideration of restricted experimental conditions. In this study, we present some experimental mechanochemical milling conditions to prepare impurity-free iron-doped tin dioxide nanoparticles exhibiting RT ferromagnetic signal. To achieve this, we investigated the effects of milling time, the choice of the starting Sn reactant, and iron concentration on the purity of Sn1−xFexO2 (x = 0, 0.03, and 0.05) nanopowders obtained through mechanochemical milling followed by thermal treatment. Characterization through XRD, XANES, and EXAFS at the Fe K-edge, RT Raman spectroscopy, 119Sn and 57Fe Mössbauer spectroscopies, and magnetic measurements was conducted. Among the experimental techniques, micro-Raman spectroscopy proved the most effective in detecting the formation of hematite as an impurity phase. Our results indicate that extending the milling time to 12 h, as opposed to 3 h, employing anhydrous SnCl2, instead of SnCl2·2H2O and using the low iron concentration of x = 0.03, results in proper conditions for producing impurity-free samples with a robust RT ferromagnetic signal. The oxidation states for iron and tin ions were determined to be 3+ and 4+, respectively, with both occupying octahedral sites, suggesting iron’s replacement of tin. Our findings propose that both the bound magnetic polaron and RKKY models offer potential explanations for the origin of the ferromagnetic signal observed at room temperature in Sn0.97Fe0.03O2 sample milled for 12 h.

Obtaining ultra-high hardness in spark plasma sintered Ge40As40Se20 bulk glass

In order to overcome the narrow glass-forming compositional range with traditional melt-quenching method, we here performed the mechanical milling and Spark Plasma Sintering technology to fabricate a high Ge content chalcogenide glass, the Ge40As40Se20 glass, which locates edge of the Ge-As-Se glass-forming domain. By using the optimal ball milling time of 50 h and sintering stress of 37.5 MPa, the large size Ge40As40Se20 bulk glasses were obtained, which possesses both a large Vickers hardness of 369 kgf/mm2 and a relative high infrared optical transmission of 43 % (@5 and 9 μm). Moreover, it was found there are pores in the sintered glasses more or less, and the pore size and number significantly affect the transmission, i.e., the optimal Ge40As40Se20 bulk glasses were demonstrated has the smallest and least pores via scanning electron microscope. The combination of mechanical milling and low-temperature sintering methods has been confirmed can be used to improve the glass formability and then obtain the high Ge content component with a potential high hardness glass to break through the limited mechanical property of chalcogenides.

Impacts of ball-milling on ZSM-5 zeolite properties and its catalytic activity in the two-phase glycerol ketalization with acetone

A series of acidic ZSM-5 zeolites were mechanically ball-milled for different periods and further applied as catalysts in the liquid-phase glycerol ketalization with acetone. Structural and textural characterizations showed that the samples had considerable crystallinity and micropore volume loss due to amorphization. On the other hand, due to a comminution effect, the external surface area increased and particle size reduced. TPD and FTIR analyses with probe molecules with different sizes, such as ammonia, pyridine (Py), and 2,6-di-tert-butylpyridine (DTBPy) chemisorbed on the catalyst acid sites, aided in quantifying the various levels of accessibility of chemicals. The treated materials lost acidity due to amorphization or blockage of pores, but the milling enabled higher accessibility of bulkier chemicals to acid sites, as revealed by the chemisorption of Py and DTBPy. A crucial balance of acidity, accessibility, and hydrophobicity was tailored by milling time. The one-hour grounded zeolite had a glycerol conversion 35 % greater than the pristine sample and 67 % greater than the eight-hour milled sample. The results showed that ball milling is a tool to improve the catalytic activity of zeolites with bulky chemicals by fine-tuning the milling time.

Formation of skyrmion phase in the Fe–Co–Si system by mechanochemical activation

Fe, Co and Si powders were exposed to mechanochemical activation by high-energy ball milling for 0, 2, 4, 8 and 12 h. The samples were subsequently characterized by Mössbauer spectroscopy, X-ray powder diffraction (XRPD), magnetic measurements and optical diffuse reflectance spectroscopy. The room temperature Mössbauer measurements were consistent with the occurrence of FeCo2Si and Fe0.5Co0.5Si crystalline phases. The low temperature Mössbauer spectra confirmed the absence of superparamagnetism up to 44 K in the milled system. XRPD patterns supported the phase sequence derived from Mössbauer spectroscopy. The coercive field was found to increase with the ball milling time (BMT). Zero-field-cooling-field-cooling (ZFC-FC) measurements performed at 200 Oe in the temperature range 5–300 K evidenced the transition to the skyrmion phase of the Fe0.5Co0.5Si material below the critical temperature of 44 K. The optical absorption in the UV–Vis–NIR region of the spectrum was found to increase with BMT.

Production of Mg thin flakes with enhanced hydrogen storage performance

Flake-like particles are interesting materials for the preparation of alloys and homogeneous nanocomposites, they also have potential use as hydrogen storage materials. However, limited information is available regarding the synthesis of pure magnesium with flake-like morphology. In this study, the successful production of Mg flakes was conducted using a cost-effective and simple method, such as high energy ball milling. Various milling parameters, including different milling times and process control agents, were tested. Optimal conditions led to the formation of coarse flakes with ∼1.72 μm thickness, while a two-step milling process produced thinner flakes with submicron thickness (∼242 nm). Ductilization of the material and a significant reduction in crystal size during the milling process were observed via X-ray diffraction. Isothermal kinetic tests at 350 °C and 20 bar revealed improved hydrogen storage performance for both coarse and thin flakes compared to pristine Mg. Coarse flakes achieved capacities of 4.1 wt% in 60 min while thin flakes reached 4.6 wt% in 6 min, compared to 3.4 wt% achieved in 100 min by pristine Mg. The improved behavior of thin flake-shaped Mg was maintained at 300 °C and 20 bar, with 4.5 wt% of hydrogen absorbed in 6 min. Even at lower testing pressures (10 bar) higher capacities were achieved at the expense of slower kinetics. These findings suggest that thin flake-shaped Mg is a suitable material with enhanced performance for hydrogen storage applications.

Effect of process parameter on the flowability of nanocrystalline CoNiCrAlY powder synthesized by mechanical milling

The present study concerns understanding the effect of process parameters on the characteristics and flowability of nanocrystalline CoNiCrAlY powder synthesized by mechanical milling. Mechanical milling has been conducted in a planetary ball mill with tungsten carbide (WC) ball, with ball to powder ratio of 10:1 at 300 rpm speed, using 1% stearic acid and toluene as process control agent (PCA) with time varying from 10 h to 36 h. The synthesized nanocrystalline powder were characterized by Scanning Electron Microscopy, X-ray Diffraction technique, X-ray Photoelectron Spectroscopy, and Differential Scanning Calorimetry. Subsequently, flowability in terms of Hausner ratio was assessed by Tap Density Tester. Average particle size of the powder was found to decrease from 33 μm to 22 μm after 10 h of milling and further increases to 43 μm and 38 μm after 25 and 36 h of milling, respectively, in stearic acid medium. However, in toluene medium particle size continuously decreases from 33 μm to 9.7 μm with increasing milling time. The particle morphology changes from spherical to platelet shape at low milling hours in both of the media. After 25 h of milling, the shape of the particles is nearly spherical for stearic acid and irregular for toluene used as a PCA. Crystallize size was found to decrease with increasing milling time from 147 nm to 7.7 nm and to 6.4 nm in stearic acid and toluene media, respectively. There was presence of γ, γʹ, β, hcp-Co, Al2O3 and AlOOH phases on the powder particles milled in both the medium. The measured Hausner ratio of the powders was found to vary from 1.18 to 1.32 in stearic acid medium, and was found to increase with increasing milling time. On the other hand, in toluene media flowability decreases (Hausner ratio increases from 1.33 to 1.44) with increasing milling time.