High-energy Milling Research Articles

Formulation, Characterization, and Evaluation of Wound Healing Potency of a Novel Mattan tailam Nanogel Based on a Famous Traditional Siddha Formula.

The Mattan tailam mixture has been extensively used to heal ulcerous wounds in traditional Siddha practice. The present study aimed to synthesize a Mattan tailam nanogel and evaluate the enhancement of wound healing potential in an experimental wound model. Mattan tailam nanogel was synthesized using the high-energy milling approach, and characterization of nanogel and potency of wound healing was investigated. The novelty of this study was the nanogel preparation of Mattan tailam. As expected, a synthesized novel nanogel of Mattan tailam has a distinct, prominent peak with a spherical form, is negatively charged and has an average particle size of 20-30 nm. Mattan tailam nanogel treated rats showed a remarkable reduction (p<0.001) in the wound area. On the 16th day, 10% Mattan tailam nanogel treatment resulted in a higher percentage of wound contraction. The 10% Mattan tailam nanogel group exhibited a faster epithelialization time (14.33 days) and a greater hydroxyproline concentration than the others. The topical application of 10% Mattan tailam nanogel increased tensile strength, signifying a better therapeutic indication. The present findings prove that polyherbal Mattan tailam nanogel formulation significantly improves collagen production, wound contraction, and tensile strength.

Ultralight Functionally Graded Hybrid Nanocomposites Based on Yttrium and Silica-Reinforced Mg10Li5Al Alloy: Thermal and Tribomechanical Properties.

Despite the amazing properties of lightweight Mg10Li5Al alloy, its use in industrial applications is highly limited due to its low mechanical properties, wear resistance, and coefficient of thermal expansion (CTE). In this context, this work aimed to improve the above properties without sacrificing the important benefit of this alloy being lightweight. Therefore, function grade composites (FGCs) were prepared based on the Mg10Li5Al alloy reinforced by yttrium (Y) and silica fume using the powder metallurgy technique. Then, the nanocomposite's microstructure, mechanical properties, artificial aging, wear resistance, and thermal expansion were examined. The results indicated that the precipitation (MgAlLi2), softening (AlLi2), and Mg24Y5 phases were formed in high-reinforced samples during high-energy milling. Furthermore, the addition of reinforcements accelerated the decomposition from the MgAlLi2 phase to the Al-Li phase (softening point). For the layer containing the highest reinforcement content, microhardness, strength, and Young's modulus improved up to 40, 22.8, and 41%, respectively, due to the combined effect of the high strength of silica fume and the dispersion strengthening Mg24Y5 phase. Meanwhile, the same sample exhibited a remarkable improvement in wear rate and the CTE value to about 43 and 16.5%, respectively, compared to the non-reinforced alloy.

Acute toxicity test nanoherbal mahkota dewa fruit (Phaleria macrocarpa)

A common plant from Papua, Indonesia, called Phaleria macrocarpa (mahkota dewa), has potent therapeutic components. The aim of this study was to evaluate the toxicity level of nanoherbal mahkota dewa and its effect on the changes in hematology, biochemistry, electrolytes, and histopathology of the organ. High Energy Milling (HEM) was used to produce nanoherbal mahkota dewa. LD50 was determined in three stages: dose orientation test (12 mice), preliminary test (20 mice), and LD50 determination (30 mice) for 14 days using the Thomson Weil formula. LC50 was determined using the Brine Shrimp Lethality Test method with concentrations of 1, 10, 100, 1000, and 10,000 ppm. This study revealed that the LD50 value was 1g/kg BW 0,075 and the LC50 value was 2145,0407 ppm. The nanoherbal mahkota dewa affected the histological organs, hematological, biochemical, and electrolyte parameters but did not affect the weight of the organ significantly. From this study, it can be concluded that nanoherbal mahkota dewa belongs to the category of moderate toxicity. In a proper dose, it could be processed as an herbal medicine in the future.

Microchemical homogeneity and quenching-induced property enhancement in BiFeO3–BaTiO3 ceramics

BiFeO3–BaTiO3 (BF-BT) solid solutions are promising as the basis for high temperature dielectric and piezoelectric materials, but their microstructural aspects have received relatively little attention. This study evaluates the influence of different processing procedures on the micro-chemical heterogeneity and functional properties of 0.67BF-0.33BT ceramics prepared by solid state reaction. It is shown that the use of high energy planetary ball milling after calcination is an effective method to improve chemical homogeneity and circumvent the core-shell type features found in conventional vibration-milled materials. BF-BT ceramics prepared by high energy milling exhibit enhanced remnant polarization, piezoelectric charge coefficient and coupling factor values of 0.34C m−2, 105 pC/N and 0.24, in comparison with those of vibration milled materials (0.30 C m−2, 73 pC/N and 0.19 respectively). Further improvements in functional properties were achieved by application of an air quenching process, which also led to an increase of 50 °C in both the Curie point and depolarization temperature; these modifications were correlated with increased structural distortion and volume fraction of the rhombohedral phase. Quenched BF-BT ceramics also exhibited mixed inter- and trans-granular fracture modes, whereas that of the as-sintered materials was predominantly inter-granular.

Anion exchanged NiP2-xSx solid solution as an anode for sodium ion battery

Anion exchanged NiP2-xSx solid solution series were synthesized by high-energy mechanical milling, and their electrochemical properties as an anode for sodium-ion batteries were investigated. A complete solid solution was achieved between two end members (NiP2 and NiS2). The as-synthesized NiP2-xSx solid solutions were a few hundred nanometer-sized nanopowders composed of ∼20 nm sized nanocrystallites. The solid solution affected the redox reactions of each end member and shifted the sodiation/desodiation potentials, which activated the reaction between P and Na ions and increased the discharge capacity. The NiP2-xSx solid solutions exhibited sequential conversion reactions with Na ions, resulting in a nanocomposite of sodiation products (Na3P, Na2S, and Ni), which effectively reduced the volume change, prevented the agglomeration of active materials, and ensured the electron and ion transport. Consequently, the NiP1.5S0.5 solid solution electrode exhibited excellent cycle stability, delivering a reversible capacity of 299 mA h g−1 after 200 cycles at a high current density of 500 mA g−1.

Synthesis and characterization of amorphous alloy Co69Nb25b6

. In this paper, amorphous alloy composition Co69Nb25B6 was prepared by high-energy ball milling which allows the formation of phases through solid state reaction. In addition, the effects of a 21:1 powder to ball mass ratio were used and the milling time during high energy milling was crucial for the formation of the amorphous and ferromagnetic phases. The characterization of the Co69Nb25B6 alloy was investigated by X-ray diffraction, scanning electron microscopy and hysteresis loops of alloy were measured with a VSM, and exhibited the typical soft magnetic character.

Co-synthesis of zirconium boride/silicide/oxide composite powders by magnesiothermic reduction

This study uses a magnesiothermic reduction method to investigate the co-synthesis of zirconium boride, silicides, and oxide powder composites using ZrO2, B2O3, Si, and Mg initial powders. The synthesis of high-temperature ceramic powders is examined through milling durations, reduction temperatures, and excess magnesium addition. Thermochemical analysis of probable reaction products was conducted by the Factsage software. According to the results, the thermochemical predictions and resultant powder phases showed good coherency. High-energy milling has a significant effect on the formation of the zirconium boride phase after annealing. However, extended milling time and higher annealing temperature have no significant effects on the composition of the constituted composite powders according to the X-ray diffraction results. An annealing temperature of 600 ºC was enough to obtain ZrB2-based ceramic composite powders. In the final powder phases, the excess magnesium addition to the stoichiometric displays an important feature. After the milling, annealing, and leaching procedure, the stoichiometric powder composition comprises ZrB2, ZrSi, ZrSi2, ZrO2, and MgSiO2, and excess Mg added powders have the ZrB2, ZrSi, ZrSi2, ZrO2 phases in their structure. Scanning electron microscopy analysis was utilized to observe the morphologies of the powders throughout each step of the synthesis procedure and revealed the finely structured morphology of synthesized powders.

The impact of outgassing on the nano-oxides kinetics of ferritic oxide dispersion strengthened steel

Oxide Dispersion Strengthened (ODS) steels are studied for their application in fission and fusion nuclear power plants. These steels are processed by powder metallurgy involving a high energy milling of Fe-Cr with oxides powders, followed by outgazing and hot consolidation. The temperature increase during these last two stages triggers the precipitation of a fine dispersion of nano-oxides. The outgazing stage is generally conducted at temperature between 300 and 800 °C for several hours, which can already trigger the formation of nano-oxides, and thus may have an influence on the final nano-oxide characteristics. In this work we assess the nano-oxides size by Small Angle X-Ray Scattering (SAXS) and get insight on the nano-oxides chemical and structural properties by comparison between SAXS and Atom Probe Tomography (APT) during a thermal treatment at 700 °C for 5 h, simulating the outgazing stage. We show that despite that the nano-oxides slightly grow during the 700 °C heating, the final properties of the nano-oxides in term of size and number density are extremely close to those where no 700 °C isothermal was applied. Moreover, the growth rate of the nano-oxides is surprisingly higher at 700 °C than 1100 °C. APT and SAXS comparison shows that the nano-oxides do not stabilize in terms of stoichiometry and structure in the studied conditions, and that a small quantity of Al remain in the precipitates during this 700 °C isothermal treatment. Both of these factors could influence the nano-oxides kinetics at low temperature. • The outgazing shows no influence on the final nano-oxides size and number density. • No stabilization of the nano-oxides is observed at 700 °C after 5 h isothermal. • The nano-oxides growth rate is surprisingly higher at 700 °C than at 1100 °C. • Nano-oxides contains Al on the 700 °C isothermal, which is removed after heating at 1100°C. • TiC or Ti(C,N) is likely to form after the outgazing, between 700 and 1100 °C.

Enabling Li3.75Si alloy coupled with Argyrodite Electrolyte with Desirable Performance for All-solid-state Batteries

With excellent safety and outstanding energy density, all-solid-state batteries is of a prospect for surpassing liquid Li+ batteries. Li6PS5Cl, exhibits desirable ductility and good Li+ conduction property, which is the most commonly used solid-state electrolyte. Herein, Li3.75Si alloys have been prepared by high energy milling technology as an anode to couple with NCM811 cathode and demonstrated an outstanding capacity. During the charging/discharging process, a microstructural defect surface was obtained, and a large impedance interface was verified by EIS tests.

Microscopic and structural study on the formation of mechanochemical synthesized BaTiO3 and ZnTiO3 perovskites

AbstractIn this work, the properties of mechanochemically produced (by using mills made from different materials) barium-titanate (BaTiO3) and zinc-titanate (ZnTiO3) perovskites are compared. Mechanochemistry is a process that can cover the energy demand of some reaction pathways between solid materials. This process is called “high-energy milling”, for which not all types of mills are suitable. In our case, a planetary ball mill provided the necessary energy. Using a model, the required energy is determinable; the energy released during an impact of a milling ball (Eb – ball-impact energy), as well as during the whole milling (Ecum – cumulative milling energy). Thus, a milling-energy map was created, with which the applied Eb and Ecum values were visualized depending on the different grinding parameters. The parameters changed were the material of the grinding vessels, the number of grinding balls, and the rotational speed. The transformation was tracked by X-ray diffraction (XRD) measurements, and electron microscopic images (TEM and SEM) of the perovskites produced were taken. This study aimed to draw conclusions that will help later in the synthesis of materials with other perovskite structures by choosing optimal milling parameters.

Properties and ballistic tests of strong B4C-TiB2 composites densified by gas pressure sintering

B4C-TiB2 composites with classical 75/25 vol ratio were sintered by pressureless sintering with and without gas pressure application in the final stage of densification, using a novel prototypal furnace. A small fraction of WC was introduced through high energy milling of the starting powders with WC-Co spheres. High energy milling facilitated the densification thanks to incorporation of WC impurities acting as sintering aid, and size reduction of the starting powders. Strength, stiffness and toughness of the ceramic densified at 2050 °C via gas pressure sintering were even better than hot pressed composites at 1900 °C. Depth of Penetration tests on plates with 3–5 mm thickness demonstrated that the gas pressure sintered material had a superior performance compared to the hot pressed one. This work also revealed that hardness was not the property spotting the best ballistic performance.

Phase Formation of Iron-Based Superconductors during Mechanical Alloying.

We successfully synthesized bulk Ba0.6Na0.4Fe2As2 and Sr0.5Na0.5Fe2As2 compounds by high-energy mechanical alloying (MA) technique. The MA process results in homogeneous amorphous phases of BaFe2As2 and SrFe2As2. It was found that the optimum time for high-energy milling in all cases is about 1.5-2 h, and the maximum amount of amorphous phase could be obtained when energy of 50-100 MJ/kg was absorbed by the powder. After a short-term heat treatment, we obtained nearly optimum sodium-doped Ba1-xNaxFe2As2 and Sr1-xNaxFe2As2 superconducting bulk samples. Therefore, MA is a potential scalable method to produce bulk superconducting material for industrial needs.

Metallic Materials for Hydrogen Storage—A Brief Overview

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.

Green Composites from Thiophene Chalcones and Rice Husk Lignin: An Alternative of Powder for Latent Fingermark

This study reports a route to obtaining a novel and cost-effective rice husk-derived lignin/thiophene chalcone green composite for application in forensic science as a fingermark developer through high energy milling. The material was properly characterized by UV-Vis, IR, fluorescence, X-ray diffraction and scanning electron microscopy. The product provided clear and sharp images of latent fingermarks with minimal background staining, revealing all ridge details. Thus, the composite presented good performance as a fingermark developer, becoming an interesting alternative to being applied as a technological, reproducible and renewable product.

Effect of the preparation technique and the H2 reduction temperature of AHM-15.34 wt%Cu powder on the characteristics of sintered Mo-25%Cu powders compacts

Mo-25wt%Cu composite powders were obtained by high energy milling and mechanical mixing of ammonium heptamolybdate (AHM)-15.34wt%Cu powders and reduction in an H 2 atmosphere. The AHM-Cu powders were reduced at three different temperatures to study the influence of the reduction temperature on the characteristics of the Mo-Cu powders. The raw materials AHM and Cu; the mixed powders AHM-15.34wt%Cu, the composite powders Mo-25wt%Cu and the sintered bodies were characterized. The particle size of Mo-Cu powders increases with increasing reduction temperature. Good sinterability was exhibited by Mo-Cu powders obtained after milled for 20 h and reduced by H 2 at 700 °C. However, sinterability decreases with increasing reduction temperature from 700 to 800 °C. The samples were sintered at 1150 °C for 1 h under H 2 gas. Relative densities of 95.57 ± 2.49% and 83.61 ± 2.67% were achieved by compacts of milled and mixed Mo-Cu powders, respectively. A maximum electrical conductivity of 38.50 and 30.30% IACS and Vickers microhardness of 302 and 274.14 Hv were obtained by the sintered compacts prepared with milled and mixed Mo-Cu powders, respectively. • Impact of the preparation technique on the characteristics of Mo-Cu composites. • Mo-Cu composites prepared by High Energy Milling. • High energy milling improves the bond between Mo and Cu. • Mo-Cu composites with a relative density of 95.57 ± 2.49%. • Electrical conductivity of 38.50% IACS and Vickers microhardness of 302 HV.

Synthesis, characterization and energy gap of silica quantum dots from rice husk

This study aimed to reveal roles of KOH and HCl in a synthesis process of Silica Quantum Dots (Si-QDs) from environmentally friendly rice husk waste, the morphological characteristics, size and crystal structure of particles as well as the energy gap of Si-QDs. The results showed that High Energy Milling (HEM) caused electron excitation, delocalized bonding, nanocrack and fracture. KOH played a role in producing Si-QDs sizes around 0.386–2.5 nm. The most efficient hexagonal crystal structure absorbed the peak wavelength of about 250–400 nm and glowed a purplish-blue color. The Si-QDs produced Si and O content was 97 % with 3 % of K, Fe, and Ca impurities. The obtained energy gap 1.59–2.36 eV and HOMO-LUMO 127 99.5 kcal/mol. The smaller size of Si QDs, the higher energy gap which was associated with the quantum confinement effect.

Development of a New Method for Synthesizing HITEC Salt-Based Alumina Nanofluids

This study presents a new two-step method to synthesize molten salt-based nanofluids by replacing water with butanol and using an Emax high-energy mill to ensure good stability and homogeneity. Commercial HITEC molten salt was selected as the base fluid, and alumina nanoparticles (nominal size of 5,1 nm) were used as an additive in three different proportions: 0,5, 1,0, and 1,5 wt.%. The specific heat capacity was evaluated through two different methods: differential scanning calorimetry (DSC) and modulated differential scanning calorimetry (MDSC). According to the evaluation by MDSC, an increment of up to 4,27% in the specific heat capacity was achieved with 1,0 wt.% of alumina nanoparticles in comparison with the raw salt, without affecting the melting point and thermal stability of the salt. This behavior may be related to the good distribution of the nanoparticles in the salt. However, no significant improvement in the specific heat capacity of the nanofluid was observed when the standard DSC method was applied. This behavior may be due to the different sensitivities of the two methods to small changes in the sample, with MDSC being the more sensitive technique, as it establishes the contribution of the two phases that make up the nanofluid: the molten salt as the base fluid and the solid nanoparticles. Similarly, the heating rate used in each of the techniques can influence the sensitivity with regard to determining changes in nanofluids.

Modeling of the mechanical treatment of a solid reactant under active gas in the high-energy mill on the example of the titanium-gaseous nitrogen system

A mathematical model for calculating the dynamics of product formation (titanium nitride) in the gas (nitrogen) medium during milling and activation of a solid reactant in the high-energy mill was built based on a new macrokinetic theory of mechanochemical synthesis. For the first time, the model uses an approach based on the theory of short-lived active sites to take into account the intensification of chemical processes in the volume of the solid and on the surface formed during destruction. The model can calculate the following macroscopic parameters: temperature, depth of chemical transformations, size of particles, gas pressure, structural defects of particles (excess energy). An analytical formula for determining the mechanochemical reaction on an active surface was derived. The modelling results were compared with the known experimental data.

Study of the Microstructural, Thermal, and Magnetic Properties of High-Energy Ball-Milled Nanocrystalline Fe(Al)

In this work, structural, microstructural, thermal, and magnetic properties of a Fe-25at%Al alloy produced by high-energy mechanical milling were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and vibrating sample magnetometry (VSM) techniques. At the early stage of the milling process, three phases, namely, Fe, Al, and Fe(Al), coexist in the milled powder. After 20 h of milling, the results of the refinement of the XRD pattern reveal the formation of the supersaturated bcc-Fe(Al) solid solution with a crystallite size of 10 nm. The DSC curves show several overlapped exothermic peaks associated with the relaxation of the deformed structure and various phase transitions, such as the formation of Al13Fe4 and Fe3Al intermetallic. During milling times, the alloyed samples have a hard-ferromagnetic behavior, where Hc varies from 628 Oe to 746 Oe when the milling time increases from 4 to 40 h. The magnetic properties were related to the microstructural changes.

(Invited) High Entropy Multication Oxide Battery Materials

High entropy oxides (HEOs), in which multication occupation of a single crystallographic site plays an important role in the properties, have become relevant in energy storage [1,2], catalysis [3.4], and many more areas. In a subset of these compounds the entropy, rather than enthalpy, plays a dominant role in stabilizing a single-phase structure at high temperatures. In other cases, the multication occupation merely contributes to stability and properties, but the entropy remains dominant in the stability. The field originated with high entropy metal alloys (HEAs)[5], and then expanded to oxides, borides, sulfides, and more. In the case of HEOs, the first example is the rock salt (Mg0.2Ni0.2Co0.2Cu0.2Zn0.2)O, which has generated a great deal of interest in this class of materials.[6,7] It has been shown that HEOs are of interest for high ionic conductivity and electrochemical energy storage. We have examined the electrochemical performance of new high entropy elecrolytes and found an effect of composition on the cycling performance. Samples were prepared through sol-gel routes and high energy milling of starting binary oxides. We have investigated the synthesis using high temperature in-situ X-ray diffraction on a Panalytical diffractometer equipped with an XRK900 stage. STEM/EDS studies on ex-situ samples will be presented that show elemental distribution, with Raman and EIS measurements providing information on ionic diffusion. The results of this study will be highly impactful for the growing community of researchers investigating the design and synthesis of the new class of materials, the high entropy oxides.[1] Q. Wang, et. al., Multi-anionic and -cationic compounds: new high entropy materials for advanced Li-ion batteries, Energy Environ. Sci., 2019, 12, 2433; [2] D. Berardan, et. al., Room temperature lithium superionic conductivity in high entropy oxides, J. Mater. Chem. A, 2016, 4, 9536.; [3] H. Chen, et al., Mechanochemical Synthesis of High Entropy Oxide Materials under Ambient Conditions: Dispersion of Catalysts via Entropy Maximization, ACS Materials Lett. 2019, 1, 1, 83–88; [4] H. Chen, et. al., Entropy-stabilized metal oxide solid solutions as CO oxidation catalysts with high-temperature stability, J. Mater. Chem. A 2018, 6, 11129-11133; [5] Y. Lu, et. al., Sci. Rep. 4, 6200 (2014); Y. F. Ye, et. al., Mater. Today 19 (6), 349 (2016); Zhang, Y., et. al., Nature Commun. 6, 8736 (2015); [6] C. M. Rost, et. al., Nature Commun. 6, 8485 (2015); [7] B. Jiang, et. al., Probing the Local Site Disorder and Distortion in Pyrochlore High-Entropy Oxides. Journal of the American Chemical Society 2021, 143, (11), 4193-4204