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.

Titanium, which has excellent strength and toughness characteristics, is increasingly used in the aerospace field. Among the titanium alloys used for body parts, more than 80 % are Ti-6Al-4V alloys with a tensile strength of 931 MPa. The spark plasma sintering (SPS) method is used for solidification molding of powder manufactured by the mechanical milling (MM) method, by sintering at low temperature for a short time. This sintering method avoids coarsening of the fine crystal grains or dispersed particles of the MM powder. To improve the mechanical properties of pure titanium without adding alloying elements, stearic acid was added to pure titanium powder as a process control agent (PCA), and MM treatment was performed. The properties of the MM powder and SPS material produced by solidifying the powder were investigated by hardness measurement, X-ray diffraction, density measurement and structure observation. The processing deformation of the pure titanium powder depends on the amount of stearic acid added and the MM treatment time. TiN was also generated in powder treated by MM 8 h with 0.50 g of added stearic acid, and the hardness of the powder was higher than that of Ti-6Al-4V alloy when treated with MM for 8 h. When the MM-treated powder was solidified in the SPS equipment, TiC was formed by the solid phase reaction. The SPS material prepared as a powder treated with MM 8 h by adding 0.50 g of stearic acid also formed TiN and exhibited the highest hardness of Hv1253.

Oxide dispersion-strengthened (ODS) steel has excellent high-temperature properties, corrosion resistance, and oxidation resistance, and is expected to be applicable in various fields. Recently, various studies on mechanical alloying (MA) have been conducted for the dispersion of oxide particles in ODS steel with a high number density. In this study, ODS steel is manufactured by introducing a complex milling process in which planetary ball milling, cryogenic ball milling, and drum ball milling are sequentially performed, and the microstructure and high-temperature mechanical properties of the ODS steel are investigated. The microstructure observation revealed that the structure is stretched in the extrusion direction, even after the heat treatment. In addition, transmission electron microscopy (TEM) analysis confirmed the presence of oxide particles in the range of 5 to 10 nm. As a result of the room-temperature and high-temperature compression tests, the yield strengths were measured as 1430, 1388, 418, and 163 MPa at 25, 500, 700, and 900oC, respectively. Based on these results, the correlation between the microstructure and mechanical properties of ODS steel manufactured using the composite milling process is also discussed.

High-entropy alloys have excellent mechanical properties under extreme environments, rendering them promising candidates for next-generation structural materials. It is desirable to develop non-equiatomic high-entropy alloys that do not require many expensive or heavy elements, contrary to the requirements of typical high-entropy alloys. In this study, a non-equiatomic high-entropy alloy powder Fe49.5Mn30Co10Cr10C0.5 (at.%) is prepared by high energy ball milling and fabricated by spark plasma sintering. By combining different ball milling times and ball-topowder ratios, we attempt to find a proper mechanical alloying condition to achieve improved mechanical properties. The milled powder and sintered specimens are examined using X-ray diffraction to investigate the progress of mechanical alloying and microstructural changes. A miniature tensile specimen after sintering is used to investigate the mechanical properties. Furthermore, quantitative analysis of the microstructure is performed using electron backscatter diffraction.

In this study, we report the microstructure and characterization of Ta20Nb20V20W20Ti20 high-entropy alloy powders and sintered samples. The effects of milling time on the microstructure and mechanical properties were investigated in detail. Microstructure and structural characterization were performed by scanning electron microscopy and X-ray diffraction. The mechanical properties of the sintered samples were analyzed through a compressive test at room temperature with a strain rate of 1 × 10−4 s−1. The microstructure of sintered Ta20Nb20V20W20Ti20 high-entropy alloy is composed of a BCC phase and a TiO phase. A better combination of compressive strength and strain was achieved by using prealloyed Ta20Nb20V20W20Ti20 powder with low oxygen content. The results suggest that the oxide formed during the sintering process affects the mechanical properties of Ta20Nb20V20W20Ti20 high-entropy alloys, which are related to the interfacial stability between the BCC matrix and TiO phase.

In this study, we investigate the deformation behavior of Hf44.5Cu27Ni13.5Nb5Al10 metallic glass powder under repeated compressive strain during mechanical milling. High-density (11.0 g/cc) Hf-based metallic glass powders are prepared using a gas atomization process. The relationship between the mechanical alloying time and microstructural change under phase transformation is evaluated for crystallization of the amorphous phase. Planetary mechanical milling is performed for 0, 40, or 90 h at 100 rpm. The amorphous structure of the Hf-based metallic glass powders during mechanical milling is analyzed using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Microstructural analysis of the Hf-based metallic glass powder deformed using mechanical milling reveals a layered structure with vein patterns at the fracture surface, which is observed in the fracture of bulk metallic glasses. We also study the crystallization behavior and the phase and microstructure transformations under isothermal heat treatment of the Hf-based metallic glass.

In this study, Bi-Sb-Te thermoelectric materials are produced by mechanical alloying (MA) and spark plasma sintering (SPS). To examine the influence of the milling atmosphere on the microstructure and thermo-electric (TE) properties, a p-type Bi-Sb-Te composite powder is mechanically alloyed in the presence of argon and air atmospheres. The oxygen content increases to 55% when the powder is milled in the air atmosphere, compared with argon. All grains are similar in size and uniformly, distributed in both atmospheric sintered samples. The Seebeck coefficient is higher, while the electrical conductivity is lower in the MA (Air) sample due to a low carrier concentration compared to the MA (Ar) sintered sample. The maximum figure of merit (ZT) is 0.91 and 0.82 at 350 K for the MA (Ar) and MA (Air) sintered samples, respectively. The slight enhancement in the ZT value is due to the decrease in the oxygen content during the MA (Ar) process. Moreover, the combination of mechanical alloying and SPS process shows a higher hardness and density values for the sintered samples.

Y2O3–H3BO3:Eu3+ powders are synthesized using a mechanical alloying method, and their photoluminescence (PL) properties are investigated through luminescence spectrophotometry. For samples milled for 300 min, some Y2O3 peaks ([222], [440], and [622]) and amorphous formations are observed. The 300-min-milled mixture annealed at 800°C for 1 h with Eu = 8 mol% has the strongest PL intensity at every temperature increase of 100°C (increasing from 700 to 1200°C in 100°C increments). PL peaks of the powder mixture, as excited by a xenon discharge lamp (20 kW) at 240 nm, are detected at approximately 592 nm (orange light, 5Do → 7F1), 613 nm, 628 nm (red light, 5Do → 7F2), and 650 nm. The PL intensity of powder mixtures milled for 120 min is generally lower than that of powder mixtures milled for 300 min under the same conditions. PL peaks due to YBO3 and Y2O3 are observed for 300-min-milled Y2O3–H3BO3 with Eu = 8 mol% after annealing at 800°C for 1 h.

This study focuses on fabricating silver flake powder by a mechanical milling process and investigating the formation of flake-shaped particles during milling. The silver flake powder is fabricated by varying the mechanical milling parameters such as the amount of powder, ball size, impeller rotation speed, and milling time of the attrition ballmill. The particle size of the silver flake powder decreases with increasing amount of powder; however, it increases with increasing impeller rotation speed. The change in the particle size of the silver flake powder is analyzed based on elastic collision between the balls, taking energy loss of the balls due to the powder into consideration. The change in the particle size of the silver flake powder with mechanical milling parameters is consistent with the change in the diameter of the elastic deformation contact area of the ball, due to the collision between the balls, with milling parameters. The flake-shaped silver particles are formed at the elastic deformation contact area of the ball due to the collision. Keywords: Flake powder, Milling, Ball collision, Elastic deformation

This study is focused on investigating the relation between the particle size of silver flake powder and mechanical milling parameters. Mechanical milling parameters such as ball size, impeller rotation speed and milling time of the attrition ball-mill were controlled to produce silver flake powder. The particle size of the silver flake powder increased with increasing ball size and impeller rotation speed. The change of the particle size of the silver flake powder with mechanical milling parameters was analyzed based on balls motion in the mill container of the attrition ball-mill. The silver flake particles were formed at the elastic deformation area of the ball due to the collision between balls. The change of the particle size of the silver flake powder with mechanical milling parameters well consists with the change of the collision energy of ball with parameters mentioned above.

A 90 wt% Mg-10 wt% NbF5 sample was prepared by mechanical milling under H2 (reactive mechanical grinding). Its hydriding and dehydriding properties were then examined. Activation of the 90 wt% Mg-10 wt% NbF5 sample was not required. At n=1, the sample absorbed 3.11 wt% H for 2.5 min, 3.55 wt% H for 5 min, 3.86 wt% H for 10 min, and 4.23 wt% H for 30 min at 593K under 12 bar H2. At n=1, the sample desorbed 0.17 wt% H for 5 min, 0.74 wt% H for 10 min, 2.03 wt% H for 30 min, and 2.81 wt% H for 60 min at 593K under 1.0 bar H2. The XRD pattern of the 90 wt% Mg-10 wt% NbF5 after reactive mechanical grinding showed Mg, β-MgH2 and small amounts of γ-MgH2, NbH2, MgF2 and NbF3. The XRD pattern of the 90 wt% Mg-10 wt% NbF5 dehydrided at n=3 revealed Mg, β-MgH2, a small amount of MgO and very small amounts of MgH2 and NbH2. The 90 wt% Mg-10 wt% NbF5 had a higher initial hydriding rate and a larger quantity of hydrogen absorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% Fe2O3, which were reported to have quite high hydriding rates and/or dehydriding rates. The 90 wt% Mg-10 wt% NbF5 had a higher initial dehydriding rate (after an incubation period) and a larger quantity of hydrogen desorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% Fe2O3.

In the present work, Al- composite powders were fabricated using a mechanical milling process and its milling behaviors and mechanical properties as functions of sizes ( , 500 nm and 50 nm) and concentrations (1, 3 and 10 wt.%) were investigated. For achieving it, composite powders and their compacts were fabricated using a planetary ball mill machine and magnetic pulse compaction technology. Al- composite powders represent the most uniform dispersion at a milling speed of 200 rpm and a milling time of 240 minutes. Also, the smaller particles were presented, the more excellent compositing characteristics are exhibited. In particular, in the case of the 50 nm added compact, it showed the highest values of compaction density and hardness compared with the conditions of and 500 nm additions, leading to the enhancement its mechanical properties.

This study investigated refinement behaviors of TiC powders produced under different impact energy conditions using a mechanical milling process. The initial coarse TiC powders with an average diameter of 9.3 were milled for 5, 20, 60 and 120 mins through the conventional low energy mechanical milling (LEMM, 22G) and specially designed high energy mechanical milling (HEMM, 65G). TiC powders with angular shape became spherical one and their sizes decreased as the milling time increased, irrespective of milling energy. Based upon the FE-SEM and BET results of milled powders, it was found initial coarse TiC powders readily became much finer near 100 nm within 60 min under HEMM, while their sizes were over 200 nm under LEMM, despite the long milling time of up to 120 min. Particularly, ultra-fine TiC powders with an average diameter of 77 nm were fabricated within 60 min in the presence of toluene under HEMM.

In this study, the effect of milling time on the microstructure and phase transformation behaviors of Ni-12 wt.%B powders was investigated using vibratory ball milling process. X-ray diffraction patterns showed that the phase transformation of mixed Ni-B elemental powder occurred after 50 hours of milling, with a formation of nickel boride phases. Through the study of microstructures in mechanical alloying process, it was considered that ball milling strongly accelerates solid-state diffusions of the Ni and B atoms during mechanical alloying process. The results of X-ray photoelectron spectroscopy showed that most of B atoms in the powder were linked to Ni with a formation of nickel boride phases after 200 hours of milling. It was finally concluded that mechanical alloying using ball milling process is feasible to synthesize fine and uniform nickel boride powders.

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%.

A composite of rapidly solidified Al-6061 alloy powder with graphite particle reinforcements was prepared by ball milling and subsequent hot extrusion. The microstructure and mechanical properties of these composites were investigated as a function of milling time. With increasing milling time, the gas atomized initially and spherical powders became elongated with a maximum aspect ratio after milling for 30 h. Then, refinement and spheroidization were achieved by further milling to 70 h with a homogeneous and fine dispersion of graphite particles forming between the matrix alloy layers. The best compression and wear properties were obtained in the powder milled for 70 h, associated with the increased fine and homogeneous distribution of graphite particles in the aluminum alloy matrix.

Al2O3 sol with long-term stability was prepared by mechanical milling. Thin films were evaluated and created for use as coating materials. The particle size of the manufactured sol was 98 nm when 2 wt% of nitric acid was added. This indicates that the viscosity of the sol is 12 cps and that it has long-term stability. The thickness of the thin films, which varied from 100 nm to 500 nm, could be managed by adjusting the draw rate and the amount of an organic additive. A thin film heated to 500˚C indicated a hydrophilic property against water and excellent permeability against a visible ray.

The present study was focused on the synthesis of a dispersed copper matrix composite material by the combination of the mechanical milling and plasma activated sintering processes. The mixed powder was prepared by the combination of the mechanical milling and reduction processes using the copper oxide and titanium diboride powder as the raw material. The synthesized mixed powder was sintered by the plasma activated sintering process. The hardness and electric conductivity of the sintered bodies were measured using micro vickers hardness and four probe method, respectively. The relative density of composite material sintered at showed about 98% of theoretical density. The composite material has a hardness of about 130Hv and an electric conductivity of about 85% IACS. The hardness and electric conductivity of composite material were about 140 Hv and about 45% IACS, respectively.

Bulk metallic glass (BMG) composite was fabricated by consolidation of milled metallic glass composite powders. The metallic glass composite powder was synthesized by a controlled milling process using the Cu-based metallic glass powder blended with 30 vol% Zr-based metallic glass powders. The milled composite powders showed a layered structure with three metallic phases, which is formed as a result of mechanical milling. By spark plasma sintering of milled metallic glass powders in the supercooled liquid region, a fully dense BMG composite was successfully synthesized.