The effects of annealing on the microstructure and mechanical properties of Al–Zn–Mg–Cu–Si alloys fabricated by high-energy ball milling (HEBM) and spark plasma sintering (SPS) were investigated. The HEBM-free sintered alloy primarily contained Mg2Si, Q-AlCuMgSi, and Si phases. Meanwhile, the HEBM-sintered alloy contains Mg-free Si and θ-Al2Cu phases due to the formation of MgO, which causes Mg depletion in the Al matrix. Annealing without and with HEBM at 500oC causes partial dissolution and coarsening of the Q-AlCuMgSi and Mg2Si phases in the alloy and dissolution of the θ-Al2Cu phase in the alloy, respectively. In both alloys, a thermally stable α-AlFeSi phase was formed after long-term heat treatment. The grain size of the sintered alloys with and without HEBM increased from 0.5 to 1.0 μm and from 2.9 to 6.3 μm, respectively. The hardness of the sintered alloy increases after annealing for 1 h but decreases significantly after 24 h of annealing. Extending the annealing time to 168 h improved the hardness of the alloy without HEBM but had little effect on the alloy with HEBM. The relationship between the microstructural factors and the hardness of the sintered and annealed alloys is discussed.

Recently, high-entropy carbides have attracted considerable attention owing to their excellent physical and chemical properties such as high hardness, fracture toughness, and conductivity. However, as an emerging class of novel materials, the synthesis methods, performance, and applications of high-entropy carbides have ample scope for further development. In this study, equiatomic (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide powders have been prepared by an ultrahigh- energy ball-milling (UHEBM) process with different milling times (1, 5, 15, 30, and 60 min). Further, their refinement behavior and high-entropy synthesis potential have been investigated. With an increase in the milling time, the particle size rapidly reduces (under sub-micrometer size) and homogeneous mixing of the prepared powder is observed. The distortions in the crystal lattice, which occur as a result of the refinement process and the multicomponent effect, are found to improve the sintering, thereby notably enhancing the formation of a single-phase solid solution (high-entropy). Herein, we present a procedure for the bulk synthesis of highly pure, dense, and uniform FCC single-phase (Fm3m crystal structure) (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide using a milling time of 60 min and a sintering temperature of 1,600oC.

The activation energy to create a phase transformation or for the reaction to move to the next stage in the milling process can be calculated from the slop of the DSC plot, obtained at the various heating rates for mechanically activated Al-Ni alloy systems by using Kissinger's equation. The mechanically activated material has been called “the driven material” as it creates new phases or intermetallic compounds of AlNi in Al-Ni alloy systems. The reaction time for phase transformation by milling can be calculated using the activation energy obtained from the above mentioned method and from the real required energy. The real required energy (activation energy) could be calculated by subtracting the loss energy from the total input energy (calculated input energy from electric motor). The loss energy and real required energy divided by the reaction time are considered the “metabolic energy” and “the effective input energy”, respectively. The milling time for phase transformation at other Al-Co alloy systems from the calculated data of Al-Ni systems can be predicted accordingly.

Aluminum nitride (AlN) powder specimens are treated by high-energy bead milling and then sintered at various temperatures. Depending on the solvent and milling time, the oxygen content in the AlN powder varies significantly. When isopropyl alcohol is used, the oxygen content increases with the milling time. In contrast, hexane is very effective at suppressing the oxygen content increase in the AlN powder, although severe particle sedimentation after the milling process is observed in the AlN slurry. With an increase in the milling time, the primary particle size remains nearly constant, but the particle agglomeration is reduced. After spark plasma sintering at 1400℃, the second crystalline phase changes to compounds containing more Al2O3 when the AlN raw material with an increased milling time is used. When the sintering temperature is decreased from 1750℃ to 1400℃, the DC resistivity increases by approximately two orders of magnitude, which implies that controlling the sintering temperature is a very effective way to improve the DC resistivity of AlN ceramics.

A Nanosized WO3 and CuO powder mixture is prepared using novel high-energy ball milling in a bead mill to obtain a W-Cu nanocomposite powder, and the effect of milling time on the structural characteristics of WO3-CuO powder mixtures is investigated. The results show that the ball-milled WO3-CuO powder mixture reaches at steady state after 10 h milling, characterized by the uniform and narrow particle size distribution with primary crystalline sizes below 50 nm, a specific surface area of 37 m2/g, and powder mean particle size (D50) of 0.57 μm. The WO3-CuO powder mixtures milled for 10 h are heat-treated at different temperatures in H2 atmosphere to produce W-Cu powder. The XRD results shows that both the WO3 and CuO phases can be reduced to W and Cu phases at temperatures over 700oC. The reduced W-Cu nanocomposite powder exhibits excellent sinterability, and the ultrafine W-Cu composite can be obtained by the Cu liquid phase sintering process.

Carbonyl iron (CI) is successfully incorporated as an additive into a polystyrene (PS) matrix via a highenergy ball milling method, under an n-hexane medium with volume fractions between 1% and 5% for electromagnetic interference shielding applications by the combination of magnetic CI and an insulating PS matrix. The morphology and the dispersion of CI are investigated by field emission scanning electron microscopy, which indicates a uniform distribution of CI in the PS matrix after 2 h of milling. The thermal behavior results indicate no significant degradation of the PS when there is a slight increase in the onset temperature with the addition of CI powder, when compared to the as-received PS pellet. After milling, there are no interactions between the CI and the PS matrix, as confirmed by Fourier transformed infrared spectroscopy. In this study, the milled CI-PS powder is extruded to make filaments, and can have potential applications in the 3-D printing industry.

In this study, 5 um sized ZrSiO4 was ground to 1.9 um, 0.3 um, and 0.1 um sized powders by wet high energy milling process, and the sintering characteristics were observed. Pure ZrSiO4 itself can-not be sintered to these levels of theoretical density, but it was possible to sinter ZrSiO4 powder of nano-scale size of, −0.1 um to the theoretical density and to lower the sintering temperature for full density. Also, the decomposition of ZrSiO4 with a size in the micron range resulted in the formation of monoclinic ZrO2; however, in the nano sized range, the decomposition resulted in the tetragonal phase of ZrO2. So, it was possible to improve the sintering characteristics of nano-sized ZrSiO4 powders.

Fe-base superalloy powders with Y2O3 dispersion were prepared by high energy ball milling, followed by sparkplasma sintering for consolidation. High-purity elemental powders with different Fe powder sizes of 24 and 50mm were usedfor the preparation of Fe-20Cr-4.5Al-0.5Ti-O.5Y2O3 powder mixtures (wt%). The milling process of the powders was carriedout in a horizontal rotary ball mill using a stainless steel vial and balls. The milling times of 1 to 5 h by constant operation(350 rpm, ball-to-powder ratio of 30:1 in weight) or cycle operation (1300 rpm for 4 min and 900 rpm for 1 min, 15:1) wereapplied. Microstructural observation revealed that the crystalline size of Fe decreased with an increase in milling time by cyclicoperation and was about 15nm after 3 h, forming a FeCr alloy phase. The cyclic operation had an advantage over constantmilling in that a smaller-agglomerated structure was obtained. The milled powders were sintered at 1100oC for 30 min invacuum. With an increase in milling time, the sintered specimen showed a more homogeneous microstructure. In addition, ahomogenous distribution of Y-compound particles in the grain boundary was confirmed by EDX analysis.

The 304 stainless steel powders were prepared by high energy ball milling and subsequently sintered byspark plasma sintering, and the microstructural characteristics and micro-hardness were investigated. The initial size ofthe irregular shaped 304 stainless steel powders was approximately 42 µm. After high energy ball milling at 800 rpmfor 5h, the powders became spherical with a size of approximately 2 µm, and without formation of reaction compounds.From TEM analysis, it was confirmed that the as-milled powders consisted of the aggregates of the nano-sized particles.As the sintering temperature increased from 1073K to 1573K, the relative density and micro-hardness of sintered sampleincreased. The sample sintered at 1573K showed the highest relative density of approximately 95% and a micro-hard-ness of 550 Hv.

Fe-TiC composite was fabricated from Fe and TiC powders by high-energy milling and subsequent spark- plasma sintering. The microstructure, particle size and phase of Fe-TiC composite powders were investigated by field emission scanning electron microscopy and X-ray diffraction to evaluate the effect of milling conditions on the size and distribution of TiC particles in Fe matrix. TiC particle size decreased with milling time. The average TiC particle size of 38 nm was obtained after 60 minutes of milling at 1000 rpm. Prepared Fe-TiC powder mixture was densified by spark- plasma sintering. Sintered Fe-TiC compacts showed a relative density of 91.7~96.2%. The average TiC particle size of 150 nm was observed from the FE-SEM image. The microstructure, densification behavior, Vickers hardness, and frac- ture toughness of Fe-TiC sintered compact were investigated.

Fe-based oxide dispersion strengthened (ODS) powders were produced by high energy ball milling, fol- lowed by spark plasma sintering (SPS) for consolidation. The mixed powders of 84Fe-14Cr-2Y2O3 (wt%) were mechanically milled for 10 and 90 mins, and then consolidated at different temperatures (900~1100o C). Mechani- cally-Alloyed (MAed) particles were examined by means of cross-sectional images using scanning electron micros- copy (SEM). Both mechanical alloying and sintering behavior was investigated by X-ray diffraction (XRD) and high resolution transmission electron microscopy (HR-TEM). To confirm the thermal behavior of Y2O3, a replica method was applied after the SPS process. From the SEM observation, MAed powders milled for 10 min showed a lamella structure consisting of rich regions of Fe and Cr, while both regions were fully alloyed after 90 min. The results of sintering behavior clearly indicate that as the SPS temperature increased, micro-sized defects decreased and the den- sity of consolidated ODS alloys increased. TEM images revealed that precipitates smaller than 50 nm consisted of YCrO3.

TiB2-reinforced iron matrix composite (Fe-TiB2) powder was in-situ fabricated from titanium hydride (TiH2) and iron boride (FeB) powders by the mechanical activation and a subsequent reaction. Phase formation of the composite powder was identified by X-ray diffraction (XRD). The morphology and phase composition were observed and measured by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The results showed that TiB2 particles formed in nanoscale were uniformly distributed in Fe matrix. Fe2B phase existed due to an incomplete reaction of Ti and FeB. Effect of milling process and synthesis temperature on the formation of composite were discussed.

Fe-TiC composite powder was fabricated via two steps. The first step was a high-energy milling of FeO and carbon powders followed by heat treatment for reduction to obtain a (Fe+C) powder mixture. The optimal condition for high-energy milling was 500 rpm for 1h, which had been determined by a series of preliminary experiment. Reduction heat-treatment was carried out at for 1h in flowing argon gas atmosphere. Reduced powder mixture was investigated by X-ray Diffraction (XRD), Field Emission-Scanning Electron Microscopy (FE-SEM) and Laser Particle Size Analyser (LPSA). The second step was a high-energy milling of (Fe+C) powder mixture and additional powder, and subsequent in-situ synthesis of TiC particulate in Fe matrix through a reaction of carbon and Ti. High-energy milling was carried out at 500 rpm for 1 h. Heat treatment for reaction synthesis was carried out at for 1 h in flowing argon gas atmosphere. X-ray diffraction (XRD) results of the fabricated Fe-TiC composite powder showed that only TiC and Fe phases exist. Results from FE-SEM observation and Energy-Dispersive X-ray Spectros-copy (EDS) revealed that TiC phase exists uniformly dispersed in the Fe matrix in a form of particulate with a size of submicron.

Nanocrystalline powder could be synthesized by solid-state reaction using the mixture which was prepared by a high energy milling process in a bead mill for and nanocrystalline powders mixture. Effect of the milling time on the powder characteristic of the synthesized powder was investigated. Nanocrystalline with a particle size of 50 nm was obtained at . High tetragonal powder with a tetragonality(=c/a) of 1.009 and a specific surface area of was acquired after heat-treatment at for 2 h. High energy ball milling was effective in decreasing the reaction temperature and increasing the tetragonality.

The Fe-based self-fluxing alloy powders and TiC particles were ball-milled and subsequently compacted and sintered at various temperatures, resulting in the TiC particle-reinforced Fe self-fluxing alloy hybrid composite, and the microstructure and micro-hardness were investigated. The initial Fe-based self-fluxing alloy powders and TiC particles showed the spherical shape with a mean size of approximately 80 and the irregular shape of less than 5 , respectively. After ball-milling at 800 rpm for 5 h, the powder mixture of Fe-based self-fluxing alloy powders and TiC particles formed into the agglomerated powders with the size of approximately 10 that was composed of the nanosized TiC particles and nano-sized alloy particles. The TiC particle-reinforced Fe-based self-fluxing alloy hybrid composite sintered at 1173 K revealed a much denser microstructure and higher micro-hardness than that sintered at 1073 K and 1273 K.

In this study, a high energy ball milling process was employed in order to improve the densification of direct nitrided AlN powder. The densification behavior and the sintered microstructure of the milled AlN powder were investigated. Mixture of AlN powder doped with 5 wt.% as a sintering additive was pulverized and dispersed up to 50 min in a bead mill with very small beads. Ultrafine AlN powder with a particle size of 600 nm and a specific surface area of 9.54 was prepared after milling for 50 min. The milled powders were pressureless-sintered at for 4 h under atmosphere. This powder showed excellent sinterability leading to full densification after sintering at for 4 h. However, the sintered microstructure revealed that the fraction of yitttium aluminate increased with milling time and sintering temperature and the newly-secondary phase of ZrN was observed due to the reaction of AlN with the impurity.

In this research, the indium dissolution properties of the waste LCD panel powders were investigated as a function of milling time fabricated by high-energy ball milling (HEBM) process. The particle morphology of waste LCD panel powders changed from sharp and irregular shape of initial cullet to spherical shape with an increase in milling time. The particle size quickly decreased to 15 until the first minute, then decreased gradually about 6 with presence of agglomerated particles after 5 minutes, which increased gradually reaching a uniform size of 13 consist of agglomerated particles after 30 minutes. The glass recovery, after dissolution, was over 99% at initial cullet, which decreased to 90.1 and 78.6% with increasing milling time of 1 and 30 minute respectively, due to a loss in remaining powder of the surface ball and jar, as well as the filter paper. The dissolution amount of indium out of the initial cullet was 208 ppm before milling, turning into 223 ppm for the mechanically milled powder after 1 minute, and nearly 146~125 ppm with further increase in milling time because of the reaction surface decrease of powders due to agglomeration. With this process, maximum dissolving indium amount (223 ppm) could be achieved at a particle size of 15 with 1 minute of milling.

The effects of high energy ball-milling (HEBM) on the sintering behavior and piezoelectric properties of 0.1 wt% doped 0.8Pb()-0.2Pb() (PMN-PZT) ceramics were investigated. It was found that HEBM treatment was quite effective to reduce the average particle size down to 300 nm, leading to increased density as well as enhanced piezoelectric properties of a sintered specimen even though prolonged HEBM resulted in unwanted secondary phases that caused a degradation of piezoelectric properties. The dielectric constant (), piezoelectric coupling factor () and piezoelectric constant of 0.1 wt% doped PMN-PZT ceramics prepared via HEBM for 10 h reached 2040, 0.68 and 554 pC/N, respectively.

In this research, the refinement behavior of the coarse magnesium powders fabricated by gas atomization was investigated as a function of milling time using a short duration high-energy ball milling equipment, which produces fine powders by means of an ultra high-energy within a short duration. The microstructure, hardness, and formability of the powders were investigated as a function of milling time using X-ray diffraction, scanning electron microscopy, Vickers micro-hardness tester and magnetic pulsed compaction. The particle morphology of Mg powders changed from spherical particles of feed metals to irregular oval particles, then platetype particles, with increasing milling time. Due to having HCP structure, deformation occurs due to the existence of the easily breakable C-axis perpendicular to the base, resulting in producing plate-type powders. With increasing milling time, the particle size increased until 5 minutes, then decreased gradually reaching a uniform size of about 50 micrometer after 20 minutes. The relative density of the initial power was 98% before milling, and mechanically milled powder was 92~94% with increase milling time (1~5 min) then it increased to 99% after milling for 20 minutes because of the change in particle shapes.

In this research, the optimal manufacturing conditions of fine Si powders from Si scrap were investigated as a function of different initial powder size using the high-energy ball milling equipment, which produces the fine powder by means of an ultra high-energy within a short duration. The morphological change of the powders according to the milling time was observed by Scanning electron microscopy (SEM). With the increasing milling time, the size of Si powder was decreased. In addition, more energy and stress for milling were required with the decreasing initial powder size. The refinement of Si scrap was rapidly carried out at 10min ball milling time. However, the refined powder started to agglomerate at 30 min milling time, while the powder size became uniform at 60 min milling time.