Materials Science Forum Vols. 534-536

Abstract: Lithium is one of the active metals and reacts with nitrogen even at room temperature. In this study, in order to grind and activate Li, the mechanical milling of Li with stable metal oxide, namely, Al2O3 and MgO, using a high energy vibrating ball mill was performed. In the case of Li- MgO system, it reacts with N2, but hardly reacts with O2. The reaction with N2 generally produces Li3N, while for some vigorous reactions the Mg3N2 and Li2O are produced as the major phases. In the case of Li-Al2O3 system, however, reactivities with both N2 and O2 are high. The difference will be explained in terms of the reaction mechanism and the Li state.

Abstract: Mechanochemical synthesis of zinc ferrite, ZnFe2O4, was attempted from a powder mixture of iron (III) oxide, alpha-Fe2O3 and zinc (II) oxide, ZnO. Nanocrystalline zinc ferrite, ZnFe2O4 powders were successfully synthesized only by milling for 30 hours. The X-ray diffraction spectrum of the as-milled powders (without heating) showed twelve ZnFe2O4 peaks and four weak peaks of coexisting unreacted Fe2O3. The crystallite size of the mechanochemicallysynthesized ZnFe2O4 was 26.3 nm. Evidence of the ZnFe2O4 formation was absent for the powders milled for 10 and 20 hours; milling lowered the crystallinity of the starting materials. Heating after milling enhanced the formation of ZnFe2O4, the crystal growth of ZnFe2O4 and the unreacted starting materials. The unreacted starting materials decreased their amounts by heating at higher temperatures.

Abstract: Mg55Y15Cu30 metallic glass powders were prepared by the mechanical alloying of pure Mg, Y, and Cu after 10 h of milling. The thermal stability of these Mg55Y15Cu30 amorphous powders was investigated using the differential scanning calorimeter (DSC). Tg ,Tx , and Δ Tx are 442 K, 478 K, and 36 K, respectively. The as-milled Mg55Y15Cu30 powders were then consolidated by vacuum hot pressing into disk compacts with a diameter and thickness of 10 mm and 1 mm, respectively. This yielded bulk Mg55Y15Cu30 metallic glass with nanocrystalline precipitates homogeneously embedded in a highly dense glassy matrix. The pressure applied during consolidation can enhance thermal stability and prolong the existence of amorphous phase within Mg55Y15Cu30 powders.

Abstract: Recent research at Harbin Institute of Technology on the synthesis of nanocrystalline and untrafine grained materials by mechanical alloying is reviewed. Examples of the materials include aluminum alloy, copper alloy, Ti/Al composite, magnesium-based hydrogen storage material, and Nd2Fe14B/α-Fe magnetic nanocomposite. Details of the processes of mechanical alloying and consolidation of the mechanically alloyed nanocrystalline powder materials are presented. The microstructure characteristics and properties of the synthesized materials are addressed.

Abstract: The precipitation behaviors of γ″(Ni3Nb) in four Ni-base alloys were investigated. The four alloys were forged Ni20Cr20Fe5Nb alloy, mechanically alloyed Ni20Cr20Fe5Nb alloy, IN 718 alloy and ECAPed(equal channel angular pressing) IN 718 alloy. Aging treatment was employed at either 600°C or 720°C for 20 hrs. The TEM observation and hardness test were performed to identify the formation of γ″. The precipitation of γ″ was noticed after aging at 600°C for 20 hrs in the mechanically alloyed Ni20Cr20Fe5Nb alloy and ECAPed IN 718 alloy, while it was observed after aging at 720°C for 20 hrs in the forged Ni20Cr20Fe5Nb alloy and IN 718 alloy before ECAP. It seemed that the lower aging temperature for γ″ precipitation in the mechanically alloyed Ni20Cr20Fe5Nb alloy and ECAPed IN 718 alloy than in the forged Ni20Cr20Fe5Nb alloy and IN 718 alloy before ECAP appeared to be due to the severe plastic deformation which occurred during mechanical alloying or ECAP.

Abstract: TiC particulate reinforced Fe matrix composite compacts with controlled interfacial reaction was processed by spark plasma sintering after mechanical alloying. Milled powders were fabricated for 1-5 hours by spex shaker mill with the ball to powder ratio of 25:2. Metal matrix composites (MMCs) based on the Fe-40%TiC system can be synthesized by spark plasma sintering of the D’AE powders with TiH2-graphite powders under vacuum in the temperature range 1273-1473K for 5-20 min. TiC phase was formed by self combustion reaction with temperature increase. The specimen that was formed by sintering Fe-TiC powders displayed a microstructure of uniformly dispersed TiC grain in a continuous metal matrix. The densifications of the TiC-Fe materials were increased as the heat-treatment holding time increasing. In the same time, relative density and hardness of TiC-Fe sintering materials was increased.

Abstract: Magnesium base alloys
and compounds are attractive
for various applications as a functional material. In particular, a series of binary system by Mg2X (X = Si, Ge, Sn and Pb) has fascinated many researchers and engineers by its thermoelectric properties and semi-conductive performance. Many barriers in its processing rejects precise investigation of these types of semiconductive compounds: high vaporizing pressure and mechanical adhesion of magnesium, reaction of germanium and tin with crucibles, and, difference of melting point among elements, X. Solidstate processing via the bulk mechanical alloying enables us to directly fabricate these Mg2X semiconductive materials in high density performs. The precise control of chemical composition leads to an investigation on the dilution and enrichment of X in Mg2X. Two types of solid-state reactivity are introduced: e.g. synthesis of Mg2Si from an elemental mixture Mg – Si, which is a nucleationcontrolled process, while synthesis of Mg2Sn from Mg – Sn is a diffusion-controlled process. The thermoelectricity of these Mg2X is evaluated for discussion on the validity and effectiveness of this new PM route as a reliable tool for fabrication of thermoelectric compounds.

Abstract: TiC cermet is widely used for working dies with a high hardness and tool materials. In this research, we attempted to produce submicron sized TiC powders from the ball milled TiH2 and carbon black mixture by thermal treatment. The titanium hydride and carbon composite powders were milled under argon atmosphere for 7 hours at various ball to powder ratios. At the initial stage, an increase in particle size was observed, and graphite phase disappered. The TiC phase of 300nm mean particle size was obtained by milling for 5 hours. As a result, its morphologies were excessively agglomerated. At the heat treating temperature of 500°C, TiH2 phase transformed to Ti completely and the complete TiC of lattice parameter 0.431 nm was formed when the temperature reached 1000°C. Metal matrix composites(MMCs) based on the Fe-TiC system can be synthesized by spark plasma sintering. Specimen formed sintering Fe-TiC powders display a microstructure of uniformly dispersed TiC grain in a continuous metal matrix.

Abstract: Fe-doped TiO2 nanocrystalline powders were prepared by mechanical alloying (MA) by varying Fe contents up to 8.0 wt.%. The TEM analyses were carried out to clarify morphologies and position of Fe within the mechanically alloyed powders. The Fe-doped powder consisted of spherical particles, and the average grain size was less than 10 nm. For the Fe-doped TiO2, the color of the powders changed from white to bright yellow with increasing concentration of Fe. The UVvis absorption showed that the UV absorption for the Fe-doped powder shifted to a longer wavelength (red shift) and the photo-efficiency was enhanced. The absorption threshold depends on the concentration of nano-sized Fe dopant. Mössbauer spectrum for 4 wt.% Fe showed the ferromagnetic phase (sextet) and paramagnetic phase (doublet). However, the only paramagnetic phase (doublet) was seen for 8 wt.% Fe. As the Fe concentration increased up to 4 wt.%, the UV-vis absorption and the magnetization were increased. The beneficial effect of Fe doping for photocatalysis and ferromagnetism was observed at the critical dopant concentration of 4 wt.%. Based on the UV absorption and magnetization, the dopant level was localized to the valence band of TiO2.

Abstract: Ti-Cu-Ni-Sn quaternary amorphous alloys of Ti50Cu32Ni15Sn3, Ti50Cu25Ni20Sn5, and Ti50Cu23Ni20Sn7 composition were prepared by mechanical alloying in a planetary high-energy ballmill (AGO-2). The amorphization of all three alloys was found to set in after milling at 300rpm speed for 2h. A complete amorphization was observed for Ti50Cu32Ni15Sn3 and Ti50Cu25Ni20Sn5 after 30h and 20h of milling, respectively. Differential scanning calorimetry analyses revealed that the thermal stability increased in the order of Ti50Cu32Ni15Sn3, Ti50Cu25Ni20Sn5, and Ti50Cu23Ni20Sn7.