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 Mn-Zn ferrite powders were prepared by high energy ball milling, then compacted and sintered at various temperatures to assess their sintering behavior and magnetic properties. The initial ferrite powders were spherical in shape with the size of approximately 70 m. After 3 h of ball milling at 300 rpm, aggregated powders ~230 nm in size and composed of ~15 nm nanoparticles were formed. The milled powders had a density of ~70 % when compacted at 490 MPa for 3 min. In the samples subsequently sintered at 1,273 K ~ 1,673 K for 3 h, the MnZnFe2O4 phase was detected. The density of the sintered samples had a tendency to increase with increasing sintering temperature up to 1,473 K, which produced the highest density of 98 %. On the other hand, the sample sintered at 1,373 K had the highest micro-hardness of approximately 610 Hv, which is due to much finer grains.

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.

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-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.

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.

Sm-16.7wt%Co alloy powders were prepared by high energy ball milling under the conditions of various milling time and the content of process control agent (PCA), and their microstructure and magnetic properties were investigated to establish optimum processing conditions. The initial powders employed showed irregular shape and had a size ranging from 5 to . After milling for 5 h, the shape of powders changed to round shape and their mean powder size was approximately , which consisted of the agglomerated nano-sized particles with 15 nm in diameter. The coercivity was reduced with increasing the milling time, whereas the saturation magnetization increased. As the content of PCA increased, the powder size minutely decreased to approximately at the PCA content of 10 wt%. The XRD patterns showed that the main diffraction peaks disappeared apparently after milling, indicating the formation of amorphous structure. The measured values of coercivity were almost unchanged with increasing the content of PCA.

TiCuNiAl quaternary amorphous alloy was prepared by high-energy ball milling process. A complete amorphization was confirmed for the composition of TiCuNiAl after milling for 30hrs. Differential scanning calorimetry showed a large super-cooled liquid region (T = T T, T and T: glass transition and crystallization onset temperatures, respectively) of 80 K. Prepared amorphous powders of TiCuNiAl were consolidated by spark-plasma sintering. Densification behavior and microstructure changes were investigated. Samples sintered at higher temperature of 713 K had a nearly full density. With increasing the sintering temperature, the compressive strength increased to fracture strength of 756 MPa in the case of sintering at 733 K, which showed a 'transparticle' fracture. The samples sintered at above 693 K showed the elongation maximum above 2%.

doped (GDC) solid solutions have been considered as a promising materials for electrolytes in intermediate-temperature solid oxide fuel cells. In this study, the nano-sized GDC powder with average panicle size of 69nm was prepared by a high energy ball milling process and its sintering behavior was investigated. Heat-treatment at of nano-sized GDC powder mixture led to GDC solid-solution. The enhanced densification over 96% of relative density was obtained after sintering at for 2h. It was found that the sinterability of GDC powder could be significantly improved by the introduction of a high energy ball milling process

Study about the feasibility and effect of high-energy ball milling on a specific Mg alloy under protection medium of alcohol was presented via comparing with conventional vacuum milling. More fine particles with wider powder size distribution but more irregular shape were shown of the powder milled under alcohol. No obvious oxide was revealed from the two kinds of Mg alloy powders with limited milling time. And since slip induced in a preferential direction, the (002) texture was formed in the Mg alloy powders at the initial stage of alcohol milling. More O and Fe contaminants were introduced into the powders milled under alcohol according to the EDS analysis.