The aerospace and power generation industries have an increasing demand for high-temperature, highstrength materials. However, conventional materials typically lack sufficient fracture toughness and oxidation resistance at high temperatures. This study aims to enhance the high-temperature properties of Nb-Si-Ti alloys through ball milling. To analyze the effects of milling time, the progression of alloying is evaluated on the basis of XRD patterns and the microstructure of alloy powders. Spark plasma sintering (SPS) is employed to produce compacts, with thermodynamic modeling assisting in predicting phase fractions and sintering temperature ranges. The changes in the microstructure and variation in the mechanical properties due to the adjustment of the sintering temperature provide insights into the influence of Nb solid solution, Nb5Si3, and crystallite size within the compacts. By investigating the changes in the mechanical properties through strengthening mechanisms, such as precipitation strengthening, solid solution strengthening, and crystallite refinement, this study aims to verify the applicability of Nb-Si-Ti alloys in advanced material systems.

High-entropy alloys (HEAs) are characterized by having five or more main elements and forming simple solids without forming intermetallic compounds, owing to the high entropy effect. HEAs with these characteristics are being researched as structural materials for extreme environments. Conventional refractory alloys have excellent hightemperature strength and stability; however, problems occur when they are used extensively in a high-temperature environment, leading to reduced fatigue properties due to oxidation or a limited service life. In contrast, refractory entropy alloys, which provide refractory properties to entropy alloys, can address these issues and improve the hightemperature stability of the alloy through phase control when designed based on existing refractory alloy elements. Refractory high-entropy alloys require sufficient milling time while in the process of mechanical alloying because of the brittleness of the added elements. Consequently, the high-energy milling process must be optimized because of the possibility of contamination of the alloyed powder during prolonged milling. In this study, we investigated the hightemperature oxidation behavior of refractory high-entropy alloys while optimizing the milling time.

High-strength low-alloy steel is one of the widely used materials in onshore and offshore plant engineering. We investigated the alloying effect of solute atoms in α-Fe based alloy using ab initio calculations. Empirical equations were used to establish the effect of alloying on the Vicker’s hardness, screw energy coefficient, and edge dislocation energy coefficient of the steel. Screw and edge energy coefficients were improved by the addition of V and Cr solute atoms. In addition, the addition of trace quantities of V, Cr, and Mn enhanced abrasion resistance. Solute atoms and contents with excellent mechanical properties were selected and their thermal conductivity and thermal expansion behavior were investigated. The addition of Cr atom is expected to form alloys with low thermal conductivity and thermal expansion coefficient. This study provides a better understanding of the state-of-the-art research in low-alloy steel and can be used to guide researchers to explore and develop α-Fe based alloys with improved properties, that can be fabricated in smart and cost-effective manners.

A mixture of elemental Co50Si50 powders was subjected to mechanical alloying (MA) at room temperature to prepare a CoSi thermoelectric compound. Consolidation of the Co50Si50 mechanically alloyed powders was performed in a spark plasma sintering (SPS) machine using graphite dies up to 800 °C and 1,000 °C under 50 MPa. We have revealed that a nanocrystalline CoSi thermoelectric compound can be produced from a mixture of elemental Co50Si50 powders by mechanical alloying after 20 hours. The average grain size estimated from a Hall plot of the CoSi intermetallic compound prepared after 40 hours of MA was 65 nm. The degree of shrinkage of the consolidated samples during SPS became significant at about 450 °C. All of the compact bodies had a high relative density of more than 94 % with a metallic glare on the surface. X-ray diffraction data showed that the SPS compact produced by sintering mechanically alloyed powders for 40-hours up to 800 °C consisted of only nanocrystalline CoSi with a grain size of 110 nm.

In this study, we investigate the effect of the duration of mechanical alloying on the microstructures and mechanical properties of ODS ferritic/martensitic steel. The Fe(bal.)-10Cr-1Mo pre-alloyed powder and Y2O3 powder are mechanically alloyed for the different mechanical alloying duration (0 to 40 h) and then constantly fabricated using a uniaxial hot pressing process. Upon increasing the mechanical alloying time, the average powder diameter and crystallite size increased dramatically. In the initial stages within 5 h of mechanical alloying, inhomogeneous grain morphology is observed along with coarsened carbide and oxide distributions; thus, precipitate phases are temporarily observed between the two powders because of insufficient collision energy to get fragmented. After 40 h of the MA process, however, fine martensitic grains and uniformly distributed oxide particles are observed. This led to a favorable tensile strength and elongation at room temperature and 650oC.

Fabrication of a ferromagnetic composite powder for the magnesium and BaFe12O19 system by mechanical alloying (MA) is investigated at room temperature. Mixtures of Mg and BaFe12O19 powders with a weight ratio of Mg:BaFe12O19 = 4:1, 3:2, 2:3 and 1:4 are used. Optimal MA conditions to obtain a ferromagnetic composite with fine microstructure are investigated by X-ray diffraction, differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM) measurement. It is found that Mg-BaFe12O19 composite powders in which BaFe12O19 is dispersed in Mg matrix are successfully produced by MA of BaFe12O19 with Mg for 80 min. for all compositions. Magnetization of Mg- BaFe12O19 composite powders gradually increases with increasing the amounts of BaFe12O19, whereas coercive force of MA powders gradually decreases due to the refinement of BaFe12O19 powders with MA time for all compositions. However, it can be seen that the coercivity of Mg-BaFe12O19 MA composite powders with a weight ratio of Mg:BaFe12O19=4:1 and 3:2 for MA 80 min. are still high, with values of 1260 Oe and 1320 Oe compared to that of Mg:BaFe12O19=1:4. This clearly suggests that the refinement of BaFe12O19 powders during MA process for Mg:BaFe12O19=4:1 and 3:2 tends to be suppressed due to ductile Mg powders.

Titanium aluminides have attracted special interest as light-weight/high-temperature materials for structural applications. The major problem limiting practical use of these compounds is their poor ductility and formability. The powder metallurgy processing route has been an attractive alternative for such materials. A mixture of Ti and Al elemental powders was fabricated to a mechanical alloying process. The processed powder was hot pressed in a vacuum, and a fully densified compact with ultra-fine grain structure consisting of Ti3Al intermetallic compound was obtained. During the compressive deformation of the compact at 1173 K, typical dynamic recrystallization (DR), which introduces a certain extent of grain refinement, was observed. The compact had high density and consisted of an ultra-fine equiaxial grain structure. Average grain diameter was 1.5 μm. Typical TEM micrographs depicting the internal structure of the specimen deformed to 0.09 true strain are provided, in which it can be seen that many small recrystallized grains having no apparent dislocation structure are generated at grain boundaries where well-developed dislocations with high density are observed in the neighboring grains. The compact showed a large m-value such as 0.44 at 1173 K. Moreover, the grain structure remained equiaxed during deformation at this temperature. Therefore, the compressive deformation of the compact was presumed to progress by superplastic flow, primarily controlled by DR.

In this research, a new medium-entropy alloy with an equiatomic composition of FeCuNi was designed using a phase diagram (CALPHAD) technique. The FeCuNi MEA was produced from pure iron, copper, and nickel powders through mechanical alloying. The alloy powders were consolidated via a high-pressure torsion process to obtain a rigid bulk specimen. Subsequently, annealing treatment at different conditions was conducted on the four turn HPT-processed specimen. The microstructural analysis indicates that an ultrafine-grained microstructure is achieved after post-HPT annealing, and microstructural evolutions at various stages of processing were consistent with the thermodynamic calculations. The results indicate that the post-HPT-annealed microstructure consists of a dual-phase structure with two FCC phases: one rich in Cu and the other rich in Fe and Ni. The kernel average misorientation value decreases with the increase in the annealing time and temperature, indicating the recovery of HPT-induced dislocations.

Synthesis of composite powders for the Fe2O3-Zn system by mechanical alloying (MA) has been investigated at room temperature. Optimal milling and heat treatment conditions to obtain soft magnetic composite with fine microstructure were investigated by X-ray diffraction, differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM) measurement. It is found that α-Fe/ZnO composite powders in which ZnO is dispersed in α-Fe matrix can be obtained by MA of Fe2O3 with Zn for 4 hours. The change in magnetization and coercivity also reflects the details of the solid-state reduction process of hematite by pure metal of Zn during MA. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine at 900 ~ 1,000 ℃ under 60 MPa. Shrinkage change after SPS of sample MA'ed for 5 hrs was significant above 300 ℃ and gradually increased with increasing temperature up to 800 ℃. X-ray diffraction results show that the average grain size of α-Fe in the α-Fe/ZnO composite sintered at 900 ℃ is in the range of 110 nm.

The Fe-22wt.%Cr-6wt.%Al foams were fabricated via the powder alloying process in this study. The structural characteristics, microstructure, and mechanical properties of Fe-Cr-Al foams with different average pore sizes were investigated. Result of the structural analysis shows that the average pore sizes were measured as 474 μm (450 foam) and 1220 μm (1200 foam). Regardless of the pore size, Fe-Cr-Al foams had a Weaire-Phelan bubble structure, and α-ferrite was the major constituent phase. Tensile and compressive tests were conducted with an initial strain rate of 10−3 /s. Tensile yield strengths were 3.4 MPa (450 foam) and 1.4 MPa (1200 foam). Note that the total elongation of 1200 foam was higher than that of 450 foam. Furthermore, their compressive yield strengths were 2.5 MPa (450 foam) and 1.1 MPa (1200 foam), respectively. Different compressive deformation behaviors according to the pore sizes of the Fe-Cr-Al foams were characterized: strain hardening for the 450 foam and constant flow stress after a slight stress drop for the 1200 foam. The effect of structural characteristics on the mechanical properties was also discussed.

Fabrication of soft magnetic composite powders for the Fe2O3-Ca system by mechanical alloying(MA) has been investigated at room temperature. It is found that soft magnetic composite powders in which CaO is dispersed in α-Fe matrix are obtained by MA of Fe2O3 with Ca for 5 hours. Changes in magnetization and coercivity also reflect the details of the solidstate reduction process of hematite by pure metal of Ca during MA. The saturation magnetization of MA powders increases with increasing MA time and reaches a maximum value of 65 emu/g after 7 hours of MA. The average grain size of α-Fe in MA powders, estimated by diffraction line-width, gradually decreases with increasing MA time and reaches 52 nm after 5 hours of MA. It can also be seen that the coercivity of the 5-hour MA sample is fairly high at 190 Oe, suggesting that the grain refinement of already-produced α-Fe tends to clearly occur during MA.

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.

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.

This study investigates the oxidation properties of Fe-14Cr ferritic oxide-dispersion-strengthened (ODS) steel at various high temperatures (900, 1000, and 1100°C for 24 h). The initial microstructure shows that no clear structural change occurs even under high-temperature heat treatment, and the average measured grain size is 0.4 and 1.1 μm for the as-fabricated and heat-treated specimens, respectively. Y–Ti–O nanoclusters 10–50 nm in size are observed. High-temperature oxidation results show that the weight increases by 0.27 and 0.29 mg/cm2 for the asfabricated and heat-treated (900°C) specimens, and by 0.47 and 0.50 mg/cm2 for the as-fabricated and heat-treated (1000°C) specimens, respectively. Further, after 24 h oxidation tests, the weight increases by 56.50 and 100.60 mg/cm2 for the as-fabricated and heat-treated (1100°C) specimens, respectively; the latter increase is approximately 100 times higher than that at 1000°C. Observation of the surface after the oxidation test shows that Cr2O3 is the main oxide on a specimen tested at 1000°C, whereas Fe2O3 and Fe3O4 phases also form on a specimen tested at 1100°C, where the weight increases rapidly. The high-temperature oxidation behavior of Fe-14Cr ODS steel is confirmed to be dominated by changes in the Cr2O3 layer and generation of Fe-based oxides through evaporation.

Tensile tests and creep tests were carried out at high temperatures on an Al-Al4C3 alloy prepared by mechanical alloying technique. The material contains about 2.0 % carbon and 0.9 % oxygen in mass percent, and the volume fractions of Al4C3 and Al2O3 particles are estimated at 7.4 and 1.4 %, respectively, from the chemical composition. Minimum creep rate decreased steeply near two critical stresses, σcl (the lower critical stress) and σcu (the upper critical stress), with decreasing applied stress at temperatures below 723 K. Instantaneous plastic strain was observed in creep tests above a critical stress, σci, at each test temperature. σcu and σci were fairly close to the 0.2% proof stress obtained by tensile tests at each test temperature. It is thought that σcl and σcu correspond to the microscopic yield stress and the macroscopic yield stress, respectively. The lower critical stress corresponds to the local yield stress needed for dislocations to move in the soft region within subgrains. The creep strain in the low stress range below 723 K arises mainly from the local deformation of the soft region. The upper critical stress is equivalent to the macroscopic yield stress necessary for dislocations within subgrains or in subboundaries; this stress can extensively move beyond subboundaries under a stress above the critical point to yield a macroscopic deformation. At higher temperatures above 773 K, the influence of the diffusional creep increases and the stress exponent of the creep rate decreases.

A Ni-Ti-B alloy powder prepared by mechanical alloying (MA) of individual Ni, Ti, and B components is examined with the aim of elucidating the phase transitions and crystallization during heat treatment. Ti and B atoms penetrating into the Ni lattice result in a Ni (Ti, B) solid solution and an amorphous phase. Differential thermal analysis (DTA) reveals peaks related to the decomposition of the metastable Ni (Ti, B) solid solution and the separation of equilibrium Ni3Ti, TiB2, and τ-Ni20Ti3B6 phases. The exothermal effects in the DTA curves move to lower temperatures with increasing milling time. The formation of a TiB2 phase by annealing indicates that the mechanochemical reaction of the Ni-Ti-B alloy does not comply with the alloy composition in the ternary phase diagram, and Ti-B bonds are found to be more preferable than Ni-B bonds.

P-type ternary Bi0.5Sb1.5Te3 alloys are fabricated via mechanical alloying (MA) and spark plasma sintering (SPS). Different ball sizes are used in the MA process, and their effect on the microstructure; hardness, and thermoelectric properties of the p-type BiSbTe alloys are investigated. The phases of milled powders and bulks are identified using an X-ray diffraction technique. The morphology of milled powders and fracture surface of compacted samples are examined using scanning electron microscopy. The morphology, phase, and grain structures of the samples are not altered by the use of different ball sizes in the MA process. Measurements of the thermoelectric (TE) transport properties including the electrical conductivity, Seebeck coefficient, and power factor are measured at temperatures of 300- 400 K for samples treated by SPS. The TE properties do not depend on the ball size used in the MA process.

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.

In the present work, we investigated the mechanical alloying of binary Ga-Se(1:1) and Ga-Te(1;1) sysyems. The high-energy ball-milling was performed at 40℃ where one of constituents (Ga) is molten state. The purpose of the work was to see whether reactions between constituent elements are accelerated by the presence of a liquid phase. During the ball-milling, the liquid Ga phase completely disappeared and the resulting powders consist of nanocrystalline grain of ~20 nm with partly amorphized phases. However, no intermetallic compounds formed in spite of the presence of the liquid phases which has much higher diffusivity than solid constituents. By subsequent heat-treatments, the intermetallic compounds such as GaSe and GaTe formed at relatively low temperatures. The formation temperature of theses compound was much lower than those predicted by equilibrium phase diagram. The comparison of the ball-milled powders with un-milled ones indicated that the easy formation of intermetallic compound or allying occurs at low temperatures.

Mg3-xZnxSb2 powders with x = 0-1.2 were fabricated by mechanical alloying in a planetary ball mill with a speed of 350 rpm for 24 hrs and then hot pressed under a pressure of 70 MPa at 773 K for 2 hrs. It was found that there were systematic shifts in the X-ray diffraction peaks of Mg3Sb2 (x = 0) toward a higher angle with increasing Zn for both the powder and the bulk sample and finally the phase of Mg1.86Zn1.14Sb2 was formed at the Zn content of x = 1.2. The Mg3-xZnxSb2 compounds had nano-sized grains of 21-30 nm for the powder and 28-66 nm for the hot pressed specimens. The electrical conductivity of hot pressed Mg3-xZnxSb2 increased with increasing Zn content and temperature from 33 Sm-1 for x = 0 to 13,026 Sm-1 for x = 1.2 at 323 K. The samples for all the compositions from x = 0 to x = 1.2 had positive Seebeck coefficients, which decreased with increasing Zn content and temperature, which resulted from the increased charge carrier concentration. Most of the samples had relatively low thermal conductivities comparable to the high performance thermoelectric materials. The dimensionless figure of merit of Mg3-xZnxSb2 was directly proportional to the Zn content except for the compound with Zn = 1.2 at high temperature. The Mg3-xZnxSb2 compound with Zn = 0.8 had the largest value of ZT, 0.33 at 723 K.