To fabricate intermetallic nanoparticles with high oxygen reduction reaction activity, a high-temperature heat treatment of 700 to 1,000 °C is required. This heat treatment provides energy sufficient to induce an atomic rearrangement inside the alloy nanoparticles, increasing the mobility of particles, making them structurally unstable and causing a sintering phenomenon where they agglomerate together naturally. These problems cannot be avoided using a typical heat treatment process that only controls the gas atmosphere and temperature. In this study, as a strategy to overcome the limitations of the existing heat treatment process for the fabrication of intermetallic nanoparticles, we propose an interesting approach, to design a catalyst material structure for heat treatment rather than the process itself. In particular, we introduce a technology that first creates an intermetallic compound structure through a primary high-temperature heat treatment using random alloy particles coated with a carbon shell, and then establishes catalytic active sites by etching the carbon shell using a secondary heat treatment process. By using a carbon shell as a template, nanoparticles with an intermetallic structure can be kept very small while effectively controlling the catalytically active area, thereby creating an optimal alloy catalyst structure for fuel cells.
Ni-based oxide dispersion strengthened (ODS) alloys have a higher usable temperature and better hightemperature mechanical properties than conventional superalloys. They are therefore being explored for applications in various fields such as those of aerospace and gas turbines. In general, ODS alloys are manufactured from alloy powders by mechanical alloying of element powders. However, our research team produces alloy powders in which the Ni5Y intermetallic phase is formed by an atomizing process. In this study, mechanical alloying was performed using a planetary mill to analyze the milling behavior of Ni-based oxide dispersions strengthened alloy powder in which the Ni5Y is the intermetallic phase. As the milling time increased, the Ni5Y intermetallic phase was refined. These results are confirmed by SEM and EPMA analysis on microstructure. In addition, it is confirmed that as the milling increased, the mechanical properties of Ni-based ODS alloy powder improve due to grain refinement by plastic deformation.
Fundamental studies of microstructural changes and high temperature deformation of titanium aluminide (TiAl) were conducted from the view point of the effect of Al content in order to develop the manufacturing process of TiAl. Microstructures in an as cast state consisted mainly of lamellar structure irrespective of Al content. By homogenization at 1473 K, the microstructures of Ti-49Al and Ti-51Al were transformed into an equiaxial structure which was composed of γ-TiAl, while the lamellar structure that was observed in Ti-46Al and Ti-47Al was much more stable. We found that the reduction of Al content suppressed the formation of equiaxial grains and resulted in a microstructure of only a lamellar structure. On Ti-49Al and Ti-51Al, dynamic recrystallization occurred during high temperature deformation, and the microstructure was transformed into a fine equiaxial one, while the microstructures of Ti-46Al and Ti-47Al contained few recrystallized grains and consisted mainly of a deformed lamellar structure. We observed that on the low-Al alloys the lamellar structure under hard mode deformation conditions deformed as kink observed B2-NiAl. High temperature deformation characteristics of TiAl were strongly affected by Al content. An increase of Al content resulted in a decrease of peak stress and activation energy for plastic deformation and an increase of the recrystallization ratio in TiAl.
The mechanical behavior and microstructural evolution during high temperature tensile deformation of recrystallizedNi3Al polycrystals doped with boron were investigated as functions of initial grain size, tensile strain rate and temperature. Inorder to obtain more precise information on the deformation mechanism, tensile specimens were rapidly quenched immediatelyafter deformation at a cooling rate of more than 2000Ks−1, and were then observed by transmission electron microscopy (TEM).Mechanical tests in the range of 923K to 1012K were carried out in a vacuum of less than 3×10−4 Pa using an Instron-typemachine with various but constant cross head speeds corresponding to the initial strain rates from 1.0×10−4 to 3.1×10−5s−1.After heating to deformation temperature, the specimen was kept for more than 1.8ks before testing. The following results wereobtained: (1) Flow behavior was affected by initial strain size; with decreasing initial grain size, the level of a stress peak inthe true stress-true strain curve decreased, the steady state region was enlarged and elongation increased. (2) On the basis ofTEM observation of rapidly quenched specimens, it was confirmed that dynamic recrystallization certainly occurred ondeformation of fine-grained (3.3µm) and intermediate-grained (5.0µm) specimens at an initial strain rate of 3.1×10−5s−1 andat 973K. (3) There were some dislocation-free grains among the new recrystallized grains. The obtained results suggest thatboth dynamic recrystallization and grain boundary sliding are operative during high temperature deformation.
The objective of the present study is to investigate the increase in the functional characteristics of a substrate by the formation of a thin coating layer. Thin coating layers of have high potential because exhibits high hardness. Shock induced reaction synthesis is an attractive fabrication technique to synthesize uniform coating layer by controlling the shock wave. Ti and Si powders to form using shock induced reaction synthesis, were mixed using high-energy ball mill into small scale. The positive effect of this technique is highly functional coating layer on the substrate due to ultra fine substructure, which improves the bonding strength. These materials are in great demand as heat resisting, structural and corrosion resistant materials. Thin coating layer was successfully recovered and showed high Vickers' hardness (Hv=1183). Characterization studies on microstructure revealed a fairly uniform distribution of powders with good interfacial integrity between the powders and the substrate.
Microstructural evolution and the intermetallic compound (IMC) growth kinetics in an Au stud bump were studied via isothermal aging at 120, 150, and 180˚C for 300hrs. The AlAu4 phase was observed in an Al pad/Au stud interface, and its thickness was kept constant during the aging treatment. AuSn, AuSn2, and AuSn4 phases formed at interface between the Au stud and Sn. AuSn2, AuSn2/AuSn4, and AuSn phases dominantly grew as the aging time increased at 120˚C, 150˚C, and 180˚C, respectively, while (Au,Cu)6Sn5/Cu3Sn phases formed at Sn/Cu interface with a negligible growth rate. Kirkendall voids formed at AlAu4/Au, Au/Au-Sn IMC, and Cu3Sn/Cu interfaces and propagated continuously as the time increased. The apparent activation energy for the overall growth of the Au-Sn IMC was estimated to be 1.04 eV.
[ ] alloys with Al, B or Nb were prepared by an advanced consolidation process that combined mechanical alloying with pulse discharge sintering (complex forming) to improve the mechanical properties. Their microstructure and mechanical properties were investigated. The alloys fabricated by complex forming method showed very fine microstructure when compared with the sample sintered from commercial powders. Alloys made from powders milled in Ar gas had fewer silica or alumina phases as compared to their counterparts sintered from powders milled in air. In densification of the sintered body, addition of B was more effective than Al or Nb. Both Victors hardness and tensile test indicated that the alloy fabricated by the complex forming method showed better properties than the sample sintered from commercial powders. The Al added alloy sintered from the powders milled in air had the superior mechanical properties due to the suppression of and formation of fine particles.
A non-equilibrium powder metallurgy processing such as an MA/SPS (Mechanical Alloying / Spark Plasma Sintering) process is examined in a Ti-48moll%Al. TiAl intermetallic compound is a potential light-weight/high-temperature structural material. One of the major problems, however, limiting the practical use of the material is its poor workability. From this point, the powder metallurgy (PM) processing route has been attractive alternative of the conventional processing for such material The MA/SPS process is able to apply to a LIGA process. Optimization of the pseudo-superplasticity enables to fabricate micro-parts made of fine grained ceramics composites of TiAl by the LIGA process.
Metallic compound of ternary Al-B-C system was prepared by mechanical alloying (MA) using Al, boron and graphite powders as starting materials. MA was carried out using Spex 8000 mixer/mill for 50 hours in an argon atmosphere without process control reagent such as methyl alcohol. The MA powders obtained were heat-treated in vacuum at the temperature of 873 and 1273 K for 5 hour. Pure ternary Al-B-C compound was obtained in the chemical content of Al:B:C=55:27:18. The ternary compound obtained in this study has a new phase whose crystal structure is not identified yet.
Gas filtration at high temperature from industrial processes offers various advantages such as increasing process efficiency, improving heat recovery and materials resource recovery, etc. At the same time, it is an advanced environment protection technology. This paper describes a newly developed metallic filter element. The manufacturing process of sintered metallic powder and the mechanical and filtration characteristics of this filter element were investigated. In this work, the phase constituent changes of the powder during sintering were studied. The newly developed filter elements were found to have excellent corrosion resistance, good thermal resistance, high strength and high filtration efficiency.
고온구조용 재료로 사용이 기대되는 Al3Hf금속간 화합물의 단점인 낮은 연성을 개선하기 위하여 SPEX mill을 이용한 기계적 합금화 과정에서의 Ll2상 생성거동과 이에 미치는 제3원소의 영향, 그리고 이들 금속간 화합물의 진공열간 압축성형 거동을 조사하였다. Al과 Hf 혼합분말을 기계적 합금화한 결과에 따르면 6시간 milling후에 L2Hf 금속간 화합물이 생성되었으며, 이때 결정립 크기가 7~8nm 정도인 nanocrystalline이 형성되었다. Cu를 첨가한 경우에는 10시간 milling 후에 2원계와 동일한 Ll2구조의 금속간 화합물이 생성되었으며, 격자상수는 Cu의 함량이 증가함에 따라 감소하였다. 2원계 Al3Hf 금속간 화합물의 경우에 Ll2상에서 D023 상으로의 변태 시작온도는 380˚C 정도였으며, 변태 종료온도는 열처리시간에 따라 480˚C에서 550˚C 정도를 나타내었다. Cu 함량이 증가함에 따라 변태 시작온도는 상승하였으며 10at.%의 Cu 첨가는 변태 시작온도를 700˚C까지 상승시켰다. 2원계 Al-25at.%Hf 혼합분말의 VHP 성형시 750MPa, 400˚C, 3시간에서 약 89%의 비이론 밀도를 얻을 수 있었다. 같은 온도에서 Cu를 10at.% 첨가한 경우의 VHP 성형시 90%정도의 비이론 밀도를 보여 2원계 A13Hf보다 성형성이 약간 증가하는 것을 볼 수 있었으며, 성형온도를 500˚C로 증가시킨 경우에는 Ll2상에서 D023상으로의 상변화나 결정립의 증가없이 약 92.5%의 비이론 밀도를 얻을 수 있었다.