The structure and magnetic properties of composite powders prepared by ball milling a mixture of Fe2O3 ‧ (0.4-1.0)Fe were investigated. Hysteresis loops and differential scanning calorimetry (DSC) curves are used to characterize the materials and to examine the effect of the solid state reaction induced by ball milling. The results showed that a solid state reaction in Fe2O3 ‧ (0.4-1.0)Fe clearly proceeds after only 1 h of ball milling. The system is characterized by a positive reaction heat of +2.23 kcal/mole. The diffraction lines related to Fe2O3 and Fe disappeared after 1 h of ball milling and, instead, diffraction lines of the intermediate phase of Fe3O4 plus FeO formed. The magnetization and coercivity of the Fe2O3 ‧ 0.8Fe powders were changed by the solid state reaction process of Fe2O3 by Fe during ball milling. The coercivity of the Fe2O3 ‧ 0.8Fe powders increased with increasing milling time and reached a maximum value of 340 Oe after 5 h of ball milling. This indicates the grain size of Fe3O4 was clearly reduced during ball milling. The magnetic properties of the annealed powders depend on the amount of magnetic Fe and Fe3O4 phases.

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.

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.

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.

Aluminum based metal matrix composite reinforced with SiC particles was fabricated by the powder-in sheath rolling method. A stainless steel tube with outer diameter of 12 mm and wall thickness of 1mm was used as a sheath. Mixture of aluminum powder and SiC particles of which volume content was varied from 5 to 20vol.% was filled in the tube by tap filling and then rolled to 75% reduction at ambient temperature. The rolled specimen was sintered at 56 for 0.5hr. The tensile strength of the (SiC)/Al composite increased with the volume content of SiC particles, and at 20vol.% it reached a maximum of 100㎫ which is 1.6 times higher than unreinforced material. The elongation decreased with the volume content of O particles. The mechanical properties of the (SiC)/Al composite fabricated by the powder-in sheath rolling is compared with that of (AlO)/Al composite by the same process.ess.

Recently, it has been found that mechanical alloying (MA) facilitates the nanocomposites formation of metal-metal oxide systems through solid-state reduction during ball milling. In this work, we studied the MA effect of FeO-M (M = Al, Ti) systems, where pure metals are used as reducing agents. It is found that composite powders in which O and TiO are dispersed in -Fe matrix with nano-sized grains are obtained by mechanical alloying of FeO with Al and Ti for 25 and 75 hours, respectively. It is suggested that the large negative heat associated with the chemical reduction of magnetite by aluminum is responsible for the shorter MA time for composite powder formation in FeO-Al system. X-ray diffraction results show that the reduction of magnetite by Al and Ti if a relatively simple reaction, involving one intermediate phase of FeAlO or FeTiO. The average grain size of -Fe in Fe-TiO composite powders is in the range of 30 nm. From magnetic measurement, we can also obtain indirect information about the details of the solid-state reduction process during MA.

Two-component ceramic (alumina-zirconia) composites were fabricated by a soft-solution process in which polyethylene glycol (PEG) was used as a polymeric carrier. Metal salts and PEG were dissolved in ethyl alcohol without any precipitation in 1:1 volume ratio of alumina and zirconia. In the non-aqueous system, the flammable solvent made explosive, exothermic reaction during drying process. The reaction resulted in formation of volume expanded, porous precursor powders by a vigorous decomposition of organic components in the precursor sol. The PEG content affected the grain size of sintered composites as well as the morphology of precursor powders. The difference of microstructure in sintered composite was attribute to the solubility and homogeneity of metal cations in precursor sol. At the optimum amount of the PEG polymer, the metal ions were dispersed effectively in solution and a homogeneous polymeric network was formed. It made less agglomerated particles in the precursor sol and affected on uniform grain size in sintered composite.

Mechanical alloying (MA) by high energy ball mill of Pure chromium Powders was carried out under the nitrogen gas atmosphere. Cr-N amorphous alloy powders have been produced through the solid-gas reaction subjected to MA. The atomic structure during amorphization process was observed by X-ray and neutron diffractions. An advantage of the neutron diffraction technique allows us to observe the local atomic structure surrounding a nitrogen atom. The coordination number of metal atoms around a N atom turns out to be 5.5 atoms. This implies that a nitrogen atom is located at both of centers of the tetrahedron and octahedron formed by metal atoms to stabilize an amorphous Cr-N structure. Also, we have revealed that a Cr-N amorphous alloy may produced from a mixture of pure Cr and Cr nitrides powders by solid-solid reaction during mechanical alloying.

The composites fabricated by powder in sheath rolling method were cold-rolled by 50% reduction and annealed for 1.8 ks at various temperatures ranging from 200 to 50, for improvement of the mechanical properties. The mechanical properties and texture of the composites after rolling and annealing were investigated. The tensile strength of the composites increased significantly due to work hardening after cold rolling, however it decreased due to restoration after annealing. The strength of the composites was improved by thermo mechanical treatment. On the other hand, the texture evolution with annealing temperatures wa,i different between the unreinforced material and the composites. The unreinforced material showed a deformation (rolling) texture of which main component is ｛112｝<111> at annealing temperatures up to 30. However, the composites have already exhibited a recrystallization texture of which main component is ｛001｝<100> after annealing at 20. This proves that the critical temperature for recrystailization is lower in the composites than in the unreinforced ones.

Aluminum-based composites were fabricated by a powder-in sheath rolling method. A stainless steel tube with outer diameter of 12 mm and wall thickness of 1 mm was used as a sheath. A mixture of aluminum powder and particles of which volume content was varied from 5 to 20%, was filled in the tube by tap filling and then rolled by 75% reduction in thickness at ambient temperature. The rolled specimen was then sintered at 56 for 0.5 h. The mixture of Al powders and particles was successfully consolidated by the sheath rolling. The composite fabricated by the sheath rolling showed a recrystallized structure, while unreinforced Al powder compact fabricated by the same procedure showed a deformed structure. The unreinforced Al powder compact was characterized by a deformation (rolling) texture of which main component is {112}<111>, while the composite showed a mixed texture oi deformation and recrystallization. The sintering resulted in recrystallization in Al powder compact and grain growth in the composite.

The powder-in sheath rolling was applied to the fabrication of composite. A stainless steel tube with outer diameter of 12 mm and wall thickness of 1 mm was used as a sheath. Mixture of aluminum powder and particles of which volume content was varied from 5 to 20 vol.% was filled in the tube by tap filling and then rolled to 75% reduction at ambient temperature. The re]]ed specimen was sintered at 56 for 0.5 hr. The composite fabricated by the sheath rolling and subsequent sintering showed the relative density higher than 0.96. The tensile strength of the composite increased with the volume content of particles, and it reached a maximum of 90 MPa which is 1.5 times higher than unreinforced material. The elongation decreased with the volume content of particles. It is concluded that the powder-in sheath rolling is an effective method for fabrication of composite.

Lee et al. reported that a mixture of Cu and Ta, the combination of which is characterized by a positive heat of mixing, of +2 kJ/㏖, can be amorphized by mechanical alloying(MA). It is our aim to investigate to what extent the MA is capable of producing a non-equilibrium phase with increasing the heat of mixing. The system chosen is the binary with =+19 kJ/㏖. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The vial and balls are made of Cu containing 1.8-2.0 wt.%Be to avoid contaminations arising mainly from Fe when steel balls and vial are used. The MA powders were characterized by the X-ray diffraction, EXAFS and thermal analysis. We conclude that two phase mixture of nanocrystalline fcc-Cu and bcc-Mo with grain size of 10 nm is formed by the ball-milling for a 3:7 mixture of pure Cu and Mo, the evidence for which has been deduced from the thermodynamic and structural analysis based on the DSC, X-ray diffraction and EXAFS spectra.

현재 기계적 합금화법에서는 주로 합금을 구성하는 성분원소 분말을 불활성분위기에서 볼밀처리 함으로써 함금화를 시키거나 모합금에 산화물을 분산시켜 복합화시키는 공정을 통하여 각종 화합물, 비정질상 및 과포화고용체등의 준안정상의 합성 뿐만이 아니라 초미세조직의 생성에 관한 폭 넓은 분야의 연구가 행하여지고 있다. 한편 MA에서는 볼멀처리중 기계적 에너지의 투여에 의하여 실제 반응온도보다 낮은 온도에서 발생하는 특이한 화학반응 즉 Mechanochemical