High-energy Ball Milling Research Articles

Realizing synergistic optimization of electrical and thermal transport properties in BiCuSeO ceramics via multi-element doping

In this study, the design of high-entropy alloys (multi-element substitution, Al3+/La3+/Sb3+/Y3+) was used to increase material entropy and improve heat scattering to further reduce thermal conductivity. Concurrently, Ca2+ ion hole doping was used to improve its electrical conductivity. Therefore, a series of Bi0.92−xAl0.02La0.02Sb0.02Y0.02CaxCuSeO (x = 0, 0.02, 0.06, 0.10, and 0.14) ceramics was prepared using a combination of high-energy ball milling and cold isostatic pressing. The multi-element substitution of Al0.02La0.02Sb0.02Y0.02Ca0.02 in the Bi site resulted in a minimum thermal conductivity of 0.35 Wm−1K−1, which is one-third of that of intrinsic BiCuSeO. Simultaneously, the conductivity increased up to 10–20 times that of intrinsic BiCuSeO, proportional to the amount of Ca2+ doping. Furthermore, the optimum component Bi0.82Al0.02La0.02Sb0.02Y0.02Ca0.10CuSeO exhibited an extremely high power factor of 568.55 μWm−1K−2 at 773 K, significantly higher than that of pure BiCuSeO (148.7 μWm−1K−2). Consequently, a peak ZT value of approximately 1.12 was achieved at 773 K, which was 4.48 times higher than that of the pristine BiCuSeO specimen (approximately 0.25). Our findings provide a novel strategy to optimize the thermoelectric properties of BiCuSeO and other materials.

Exploring the potential of induced dipole-dominated electrorheological effect: advancing ER elastomers

Abstract Prior research has predominantly focused on traditional electrorheological (ER) effects while overlooking the transformative potential of induced dipoles in enhancing the overall performance of ER materials. In this study, we introduced a novel type of ER elastomer called induced dipole-dominated ER elastomer (ID-ERE). Through high-energy ball milling (HEBM) of the filler particles, the oxygen vacancies were produced within the particles that acted as local charge centers. In the presence of an external electric field (E), these oxygen vacancies induced the dipoles with significant dipole moments, thus amplifying the local electric field EL within the particle gaps. The powerful interactions of these dipoles significantly improved the overall performance of elastomer; the phenomenon referred to as the ID-ER effect. The viscoelastic results showed that ID-EREs have high field-induced storage modulus (G’ = 395.7 kPa), a significant increment in storage modulus (ΔG’ = 270.5 kPa) and high relative ER effect (ΔG’/G0 = 217.2%) at 3 kV mm−1. Additionally, after testing ID-EREs viscoelastic properties, it was discovered that excessive powder content leads to a decline in the elastomer’s performance. The results showed that ID-ERE’s viscoelastic, mechanical, dielectric, and overall efficiency is finer than the control ER elastomer (C-ERE) having unmilled TiO2 particles. Besides, the preparation method is straightforward, easily replicated, scalable, and cost effective. Thus, these ID-EREs should be a new generation of elastomer with the potential to be used in various automotive, robotics, construction, and electroactive actuators industries.

Synergistic Suppression of Bipolar Effect and Lattice Thermal Conductivity Leading to High Average Figure of Merit in Bi0.4Sb1.6Te3 Materials through Alloying with AgSbTe2.

Bismuth telluride-based materials have been widely used in commercial thermoelectric applications due to their excellent thermoelectric performance in the near-room-temperature range, yet further improvement of their thermoelectric properties is still necessary. Moreover, the narrow band gap of these materials results in a bipolar effect at elevated temperatures, which causes severe degradation of the thermoelectric performance. In this work, the commercial Bi0.4Sb1.6Te3 was alloyed with AgSbTe2 by using high-energy ball milling method combined with spark plasma sintering. It was found that ball milling can effectively reduce the lattice thermal conductivity of the samples. The alloying of AgSbTe2 leads to a gradual increase in hole carrier concentration, resulting in an enhanced electrical conductivity and optimized power factor. Additionally, the bipolar effect is also weakened due to the increased hole carrier concentration. Furthermore, the substitution of Ag in the Bi/Sb sublattice causes further reduction in the lattice thermal conductivity. Ultimately, the sample alloyed with 0.15 wt % AgSbTe2 demonstrates its best thermoelectric performance with a maximum zT of 1.35 at 393 K, showing a 20.5% improvement compared to the commercial sample. Besides, its average zT reaches a high value of 1.25 between 303 and 483 K, with a 27.6% improvement compared to that of the commercial sample.

Terraced (K, Na)NbO3 piezocatalysts with superior H2O2 production

Piezocatalytic hydrogen peroxide (H2O2) production is an emerging and green technology, but complex preparation process of piezocatalyst and low production rate limit its practical application. Herein, we propose a straightforward and efficient strategy, that is, fabricating a novel terraced potassium sodium niobate (KNN-H) by integrating high-energy pendulum ball-milling into the conventional solid-state method, to control the morphology of piezocatalyst and boost its piezocatalytic activities. By exposing a large number of edge sites with higher piezoelectric response and more active sites, KNN-H sample exhibits an extremely high H2O2 production rate of 47 μmol/h, about 35 times higher than that of previously reported potassium niobate piezocatalyst. Besides, KNN-H sample also has good effects on dye degradation and bacterial inhibition. Therefore, our strategy provides a paradigm for large-scale fabrication of high-performance perovskite piezocatalysts.

Effect of high energy ball milling, heat treatment and spark plasma sintering on structure, composition, thermal stability and magnetism in CoCrFeNiGax (x = 0.5; 1) high entropy alloys

Effect of high energy ball milling, heat treatment and spark plasma sintering on structure, composition, thermal stability and magnetism in CoCrFeNiGax (x = 0.5; 1) high entropy alloys

Microstructure and Corrosion Resistance of 7075 Aluminium Alloy Composite Material Obtained from Chips in the High-Energy Ball Milling Process.

The high-energy ball milling process was applied to fabricate a composite material from 7075 aluminium alloy milling chips, silicon carbide, and titanium dioxide powders. Raw materials were ground, and the obtained powders were cold pressed and sintered. It was demonstrated that this method can be used in the recycling of aluminium alloy scrap characterised by a high surface-to-volume ratio, and also that chemical removal of the oxide layer from chips is not necessary. The finest particles, with 50 vol.% of their population below 36 μm, were obtained after grinding for 60 min at a 1000 rpm rotational speed. Such an intensive grinding was necessary to fabricate the compact composite material with a homogeneous microstructure and a low porosity of 0.7%. The corrosion resistance of the composites was studied in 3.5 wt.% NaCl solution using cyclic voltammetry and electrochemical impedance spectroscopy, and corrosion rates in the range of ca. 342 and 3 μA∙cm-2 were obtained. The corrosion mechanism includes aluminium alloy dissolution at the matrix/reinforcement interphase and around intermetallic particles localised within the matrix grains.

Aluminum matrix composites reinforced with high-entropy oxides and in situ formed Al2O3 and intermetallic compounds through aluminothermic reactions during spark plasma sintering

This work proposes a new strategy for producing aluminum matrix composites with strong interfaces by forming additional reinforcing particles in situ through an aluminothermic reaction between the system components. Sol-gel synthesized high-entropy spinel-type (Cr0.23Mn0.22Fe0.22Co0.19Ni0.13)3O4 oxides (HEO) were added to Al nanopowder and the resulting mixture was subjected to high-energy ball milling (HEBM) and then spark plasma sintering (SPS). As a result of the aluminothermic reaction during SPS, HEO are partially reduced, providing excess oxygen for the formation of reinforcing Al2O3 nanoparticles, and the reduced metals react with Al with the formation of various intermetallic compounds (Al9Me2, Al5Me2, and Al2Me), which, in addition to HEO, serve as secondary strengthening phases. A new hexagonal AlMex phase with lattice parameters of approximately a = c = 1.76 nm has been well documented. HEBM has been shown to be an important step not only for uniform HEO distribution, but also for the aluminothermic reaction to occur at a relatively low temperature by improving the interaction between activated Al and HEO nanopowders. The maximum increase in hardness with the addition of HEO is 198 %, tensile strength 90 % (25°C) and 97 % (500°C), and compressive strength 220 % (25°C) and 250 % (500°C). Excellent mechanical properties are achieved at 500°C: the ultimate tensile and compressive strength are 258 MPa and 410 MPa, respectively. The introduction of HEO also leads to a significant reduction in the coefficient of friction (from 0.7 (0 %) to 0.2 (3 %HEO)) and a noticeable reduction in dynamic wear (5.9–6.3 (3 %HEO) and 10.6–14.3 (5 %HEO) times depending on applied load). Thus, our research opens up exciting new possibilities for creating lightweight and high strength composites for use in the mid-temperature range.

Synthesis, structural and spectroscopic characterization of defect-rich forsterite as a representative phase of Martian regolith.

Regolith draws intensive research attention because of its importance as the basis for fabricating materials for future human space exploration. Martian regolith is predicted to consist of defect-rich crystal structures due to long-term space weathering. The present report focuses on the structural differences between defect-rich and defect-poor forsterite (Mg2SiO4) - one of the major phases in Martian regolith. In this work, forsterites were synthesized using reverse strike co-precipitation and high-energy ball milling (BM). Subsequent post-processing was also carried out using BM to enhance the defects. The crystal structures of the samples were characterized by X-ray powder diffraction and total scattering using Cu and synchrotron radiation followed by Rietveld refinement and pair distribution function (PDF) analysis, respectively. The structural models were deduced by density functional theory assisted PDF refinements, describing both long-range and short-range order caused by defects. The Raman spectral features of the synthetic forsterites complement the ab initio simulation for an in-depth understanding of the associated structural defects.

Phase Regulation Promotes High Rate‐Long Term Na4Fe3(PO4)2P2O7 Cathode for Sodium‐Ion Batteries

AbstractSodium‐ion batteries (SIBs) have evoked much attention, benefiting from the advantages of low cost, high safety and excellent performance at low temperature. Especially, Na4Fe3(PO4)2P2O7 (NFPP) cathode is considered to be one of the best candidates for SIBs cathode with abundant resources and long‐term cycling stability. However, the impurities of NaFePO4 (NFP) and Na2FeP2O7 (NFPO) formed synchronously with NFPP which restrict the further application of NFPP. It is meaningful to clear the formation process and regulate the contents of NFP and NFPO. Therefore, NFPP cathodes with different contents of NFP and NFPO were prepared through high energy ball milling cooperated with post‐heat treatment by controlling the Fe concentration in reactants. The NFPP‐2.85 showed the best electrochemical performance because of the high content of NFPP and transition zone between NFPP and NFPO which fasts the Na+ transport kinetics. When employed as cathode for SIBs, the as‐prepared NFPP‐2.85 showed a specific capacity of 111.8 mAh g−1 at 0.1 C and maintained at 68.9 mAh g−1 even at 100 C. The retention ratio was as high as 93.6 % after 1500 cycles at 20 C, implying superior high rate‐long term cycling stability. This work provides a new way for impurities regulation and the improvement of NFPP electrochemical performance.

High-Energy Ball Milling Enables an Ultra-Fast Wittig Olefination Under Ambient and Solvent-free Conditions.

30 Seconds to success!-The Wittig reaction, a fundamental and extensively utilized reaction in organic chemistry, enables the efficient conversion of carbonyl compounds to olefins using phosphonium salts. Traditionally, meticulous reaction setup, including the pre-formation of a reactive ylide species via deprotonation of a phosphonium salt, is crucial for achieving high-yielding reactions under classical solution-based conditions. In this report, we present an unprecedented protocol for an ultra-fast mechanically induced Wittig reaction under solvent-free and ambient conditions, often eliminating the need for tedious ylide pre-formation under strict air and moisture exclusion. A range of aldehydes and ketones were reacted with diverse phosphonium salts under high-energy ball milling conditions, frequently giving access to the respective olefins in only 30 seconds.

Exceptional strength-toughness-hardness integrated B4C ceramics with synergistic reinforcement of nano-BN and in-situ ceramic phases

Boron carbide (B4C) ceramics with enhanced mechanical properties were fabricated by incorporating nano boron nitride (nano-BN), obtained through high-energy ball milling (HEBM) using ZrO2 balls as the medium, and utilizing the spark plasma sintering (SPS) technique. During the densification process of B4C/nano-BN composite powders, an in-situ reaction between the B4C matrix and ZrO2 resulted in the formation of ZrB2 ceramic phases at 1200–1300 °C. Additionally, the rapid sintering densification temperature of composites is reduced to 1500–1700 °C, approximately 80 °C lower than that required for pure B4C ceramics. Notably, while maintaining a high relative density (99.5 %), the Vickers hardness, flexural strength, and fracture toughness of B4C ceramics reinforced with synergistic effects of nano-BN and ZrB2 fabricated at 1750 °C are significantly improved to reach values of 36.8 ± 0.15 GPa, 701 ± 12 MPa, and 5.01 ± 0.13 MPa m1/2 respectively; representing an increase of 3.5 GPa (10.5 %), 225 MPa (47.3 %), and 1.72 MPa m1/2 (52.3 %) compared to pure B4C ceramics alone. The multiple reinforcement mechanisms including pinning effects provided by nano-BN and in-situ formed ZrB2 ceramic phases, B4C/ZrB2 grain boundary pressure and intracrystalline pressure within B4C, interlayer dislocations of nano-BN and turbulent layer of B4C/BN boundaries contribute to energy dissipation during fracture processes, such as crack deflection, bridging, propagation hindrance and branching effect; ultimately resulting in exceptional strength-toughness-hardness integrated B4C-based ceramics.

A Comparative Study of the Impact of La2O3 and La2Zr2O7 Dispersions on Molybdenum Microstructure, Mechanical Properties, and Fracture

AbstractWe report, for the first time, the effect of lanthanum zirconate (La2Zr2O7) particles on the microstructure and mechanical behavior of an experimental molybdenum oxide dispersion-strengthened alloy. The focus was on the preparation of the novel Mo–La2Zr2O7 composite using high-energy ball milling and spark plasma sintering and on the comparison of its microstructural and mechanical properties with pure Mo and Mo–La2O3 ODS alloy counterparts. Mechanical properties were assessed using a Vickers hardness test at room temperature and a three-point flexural test in the temperature range from − 150 to 150 °C. The microstructure of the studied materials and their fracture behavior were evaluated using x-ray diffraction, energy-dispersive x-ray spectroscopy, and scanning electron and transmission electron microscopy. The strengthening effect of La2Zr2O7 particles was found to be lower than that of La2O3 particles, resulting in a 30-35% lower yield stress and flexural strength of the Mo–La2Zr2O7 alloy compared to the Mo–La2O3 alloy. The experimental Mo–La2Zr2O7 alloy exhibited low plasticity and no distinct ductile-to-brittle transition temperature (DBTT) in the tested temperature range, unlike pure Mo and the Mo–La2O3 alloy, which had the DBTT of 63 and 1 °C, respectively. Fracture occurred mainly in a brittle intergranular manner in the entire testing temperature range, while the counterpart materials showed localized plastic stretching at grain boundaries and within grains at and above the transition region. The observed behavior was primarily related to lower strengthening and brittleness as well as less effective grain boundary purification.

Low Sintering Temperature Effect on Crystal Structure and Dielectric Properties of Lead-Free Piezoelectric Bi0.5Na0.5TiO3-NaFeTiO4

Bi0.5Na0.5TiO3 (BNT) emerges as a promising ferroelectric and piezoelectric lead-free candidate to substitute the contaminant Pb[TixZr1−x]O3 (PZT). However, to obtain optimal ferroelectric and piezoelectric properties, BNT must be sintered at high temperatures. In this work, the reduction of sintering temperature by using iron added to BNT is demonstrated, without significant detriment to the dielectric properties. BNT-xFe with iron from x = 0 to 0.1 mol (∆x = 0.025) were synthesized using high-energy ball milling followed by sintering at 900 °C. XRD analysis confirmed the presence of rhombohedral BNT together with a new phase of NaFeTiO4 (NFT), which was also corroborated using optical and electronic microscopy. The relative permittivity, in the range of 400 to 500 across all the frequencies, demonstrated the stabilization effect of the iron in BNT. Additionally, the presence of iron elevates the transition from ferroelectric to paraelectric structure, increasing it from 330 °C in the iron-free sample to 370 °C in the sample with the maximum iron concentration (0.1 mol). The dielectric losses maintain constant values lower than 0.1. In this case, low dielectric loss values are ideal for ferroelectric and piezoelectric materials, as they ensure minimal energy dissipation. Likewise, the electrical conductivity maintains a semiconductor behavior across a range of 50 Hz to 1 × 106 Hz, indicating the potential of these materials for applications at different frequencies. Additionally, the piezoelectric constant (d33) values decrease slightly when low concentrations of iron are added, maintaining values between 30 and 48 pC/N for BNT-0.025Fe and BNT-0.05Fe, respectively.

Synthesis of Mo-Cu nanocomposite powder by hydrogen reduction of copper nitrate coated MoO3 powder mixture

The fabrication of Mo-based nanocomposite powder with homogeneous dispersion of Cu was investigated. The fine MoO3 powders were prepared by high energy ball milling, and Cu particles on the ball-milled powder surfaces were formed by calcination of a precursor solution copper nitrate. In the powder mixture calcined at 300 °C, MoO3 and CuO appeared in the form of aggregates with fine particles. Microstructural analysis showed that the oxide powders were changed to Mo-Cu nanocomposite powders with an average particle size of about 150 nm and had microstructural homogeneity by hydrogen reduction at 800 °C for 1 h. These results are help to optimize the synthesis process of homogeneous Mo-Co nanocomposite powders.

Effect of milling time on structural and electrical properties of thermomechanically synthesized of Ba0.1 (Bi0.45Na0.45)TiO3 nanoceramics for ferroelectric random-access memory device

Lead-free Ba0.1(Bi0.45Na0.45)TiO3 (BBNTO) nanoceramics were synthesized using high-energy ball milling, followed by a solid-state reaction method. XRD analysis of the microstructure indicated the formation of tetragonal symmetry. The crystallite size of the nanoceramic powder decreased from ∼ 28 nm to 10 nm after milling for 0, 30, 60, and 90 hours. The dielectric properties of the nanoceramics showed significant improvement, with a diffuse phase transition occurring around 80 °C). The dielectric constant increased with temperature across various frequencies, reached a maximum value at approximately at temperature ∼ 380 °C. At lower temperatures and higher frequencies, the relative permittivity and tangent loss depend on the crystallite size and milling duration. Impedance spectroscopy data analysis revealed size-dependent impedance characteristics and dielectric relaxation. The ac conductivity plot adhered to the Arrhenius relation, and the calculated activation energy confirmed the negative temperature coefficient of resistance (NTCR) behavior. P-E loops confirmed ferroelectric properties, indicating potential for use in future ferroelectric-based storage devices.

Enhancing photovoltaic performance through high-energy ball milling of Nb-doped TiO2 nanoparticles

Enhancing photovoltaic performance through high-energy ball milling of Nb-doped TiO2 nanoparticles

Structure and mechanical properties of consolidated billets from recycled chip wastes of cast metal matrix composites of the Al-Si-SiC system

This study examines the structure and mechanical properties of billets produced via hot pressing from ball-milled chips of Al-Si-SiC metal matrix composites. The chips, derived from cast composites, were subjected to high-energy ball milling to obtain powder, which was then consolidated by hot pressing at 450 °C. The findings reveal that machining reduces the average size of SiC particles from 41.9 to 12.9 µm, and ball milling further reduces it to 5.9 µm. Powder-pressed billets exhibited a more homogeneous SiC distribution and showed ∼1.9 times higher hardness than the cast material, while chip-pressed billets showed only a ∼13 % increase. Compression tests indicated the highest yield strength of 333 ± 7 MPa in powder-pressed samples, compared to 225 ± 6 MPa in the cast state and 143 ± 26 MPa in chip-pressed samples. However, powder-pressed samples had lower ductility (∼3 %) than cast and chip-pressed samples. The influence of hot pressing temperature (350–500 °C) on the structure and mechanical properties was also explored, showing that higher temperatures improve silicon distribution but slightly reduce hardness and yield strength. Recycled composite materials from chip waste are promising for producing consolidated billets, especially for small-sized components in machinery and instrument engineering.

Interface-driven microwave absorption enhancement in Mn-optimized Co2FeAl1-xMnx Heusler alloys

To address the urgent need for efficient and stable electromagnetic wave absorbing materials for electromagnetic interference (EMI) protection, we synthesized Co2FeAl1−xMnx Heusler soft magnetic alloys using a high-energy planetary ball milling method. We comprehensively analyzed their structural characteristics, surface morphology, magnetic properties, and electromagnetic parameters to explore their potential in electromagnetic wave absorption. The results show that incorporating manganese (Mn) significantly changes the alloys' crystal structure, surface morphology, and magnetic properties, greatly enhancing their wave absorption performance. The Mn doping specifically alters the surface morphology, which plays a crucial role in influencing the wave absorption characteristics of the Heusler alloys. When the Mn content increased to 25 %, the sample exhibits superior wave absorption, achieving the maximum reflection loss of −44.83 dB at 13.68 GHz with a thickness of 1.5 mm and an effective absorption bandwidth of 5.52 GHz. With a significant increase in the aspect ratio and noticeable changes in surface morphology, the sample with 75 % Mn content shows exceptional performance with an effective absorption bandwidth of 5.68 GHz, representing the highest effective absorption bandwidth in single-phase Heusler alloys. The Mn doping strategy effectively improves the material's impedance matching by adjusting its permittivity and permeability, facilitating multiple polarization relaxation mechanisms and significantly enhancing the alloys' electromagnetic wave absorption efficiency. Our study provides detailed experimental data for optimizing the electromagnetic wave absorption characteristics of Heusler alloys, verifies their practical application potential, and paves the way for developing new high-performance electromagnetic wave absorbing materials.

Enhancing Long Stability of Solid-State Batteries Through High-Energy Ball Milling-Induced Decomposition of Sulfide-Based Electrolyte to Sulfur.

Metal sulfides are increasingly favored as cathode materials in all-solid-state batteries (ASSBs) due to their high energy density, stability, affordability, and conductivity. Metal sulfides often exhibit capacities exceeding their theoretical limits, a phenomenon that remains not fully understood. In this study, it reveals that this phenomenon is primarily due to the sulfur decomposition from sulfide-based electrolyte. By employing the high-energy ball milling (HEBM) technique, the deposition of sulfide-based electrolyte onto sulfur is intentionally promoted, resulting in higher charge capacities compared to the discharge capacities and surpass theoretical limits of metal sulfides. Using chromium sulfide (Cr2S3) as the active material, the sulfur decomposed from sulfide-based electrolyte transforms into lithium sulfide (Li2S) after discharge, resulting in an increased capacity by ≈439.6 mAhg-1 and improved cycling stability. Consequently, it demonstrates a specific capacity surpassing 1200 mAh g-1 with a capacity retention of over 80% after 650 cycles, maintaining cycling stability for more than 1900 cycles and achieving a Coulombic efficiency exceeding 99.9%. This versatile HEBM approach enables the fabrication of ASSBs utilizing various transition metal sulfides, such as molybdenum disulfide (MoS2), niobium disulfide (NbS2), and iron disulfide (FeS2), all exhibiting over theoretical limited capacities and prolonged cycling capabilities.

Innovation in sustainable composite research: Investigating graphene-reinforced MMCs for liquid hydrogen storage tanks in aerospace and space exploration

The demand for lightweight materials in space exploration applications has seen a significant rise. This study presents a novel approach by integrating graphene with Aluminium alloy (AA) 2900 powder, synthesized through High energy ball milling technique. The resulting powder was used to reinforce Aluminium alloy 2195, creating metal matrix composites (MMCs) via squeeze casting. The findings demonstrate that incorporating 0.5 wt % 2D graphene nanoplatelets (2D-Grnp) in AA 2195 achieved density match, enabling homogeneous dispersion, addressing composite casting challenges. Consequently, the AA 2900 alloy embedded with 2D-Grnp facilitated the homogeneous dispersion of reinforcements during the squeeze casting process, yielding MMCs Ideal for potential use in lightweight liquid hydrogen fuel tank structures for launch vehicles. Following T8 heat treatment, the final casted composite plate exhibited significant enhancements in ultimate tensile strength, with a 4.5% increase over monolithic Al 2195-T8, exhibiting nominal reduction in elongation behavior and higher hardness. Additionally, scanning and transmission electron microscopy (SEM, TEM), Small Angle Neutron Scattering (SANS) and Electron Backscatter Diffraction (EBSD) revealed the squeeze casting technique's effectiveness by exhibiting enhanced bonding among homogeneously reinforced 2D-Grnp, T1/θ’ precipitates, and AA 2195.