The hydrogen reduction behavior of the CuO-Co₃O₄ powder mixture for the synthesis of the homogeneous Cu-15at%Co composite powder has been investigated. The composite powder is prepared by ball milling the oxide powders, followed by a hydrogen reduction process. The reduction behavior of the ball-milled powder mixture is analyzed by X-ray diffraction (XRD) and temperature-programmed reduction at different heating rates in an Ar-10%H2 atmosphere. The scanning electron microscopy and XRD results reveal that the hydrogen-reduced powder mixture is composed of fine agglomerates of nanosized Cu and Co particles. The hydrogen reduction kinetics is studied by determining the degree of peak shift as a function of the heating rate. The activation energies for the reduction of the oxide powders estimated from the slopes of the Kissinger plots are 58.1 kJ/mol and 65.8 kJ/mol, depending on the reduction reaction: CuO to Cu and Co₃O₄ to Co, respectively. The measured temperature and activation energy for the reduction of Co₃O₄ are explained on the basis of the effect of pre-reduced Cu particles.

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• Synthesis of Porous Cu-Co using Freeze Drying Process of Camphene Slurry with Oxide Composite Powders
  Gyuhwi Lee, Ju-Yeon Han, Sung-Tag Oh
  Journal of Korean Powder Metallurgy Institute.2020; 27(3): 193.     CrossRef

In this study, porous Mo-5 wt% Cu with unidirectionally aligned pores is prepared by freeze drying of camphene slurry with MoO₃-CuO powders. Unidirectional freezing of camphene slurry with dispersion stability is conducted at -25°C, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The green bodies are hydrogen-reduced at 750°C and sintered at 1000°C for 1 h. X-ray diffraction analysis reveals that MoO₃-CuO composite powders are completely converted to a Mo-and-Cu phase without any reaction phases by hydrogen reduction. The sintered bodies with the Mo-Cu phase show large and aligned parallel pores to the camphene growth direction as well as small pores in the internal walls of large pores. The pore size and porosity decrease with increasing composite powder content from 5 to 10 vol%. The change of pore characteristics is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

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• Characteristic Evaluation of WC Hard Materials According to Ni Content Variation by a Pulsed Current Activated Sintering Process
  Hyun-Kuk Park
  Korean Journal of Materials Research.2020; 30(12): 672.     CrossRef
• Effect of α-lath size on the mechanical properties of Ti–6Al–4V using core time hydrogen heat treatment
  Gye-Hoon Cho, Jung-Min Oh, Hanjung Kwon, Jae-Won Lim
  Materials Science and Technology.2020; 36(7): 858.     CrossRef

The hydrogen reduction behavior of MoO₃-CuO powder mixture for the synthesis of homogeneous Mo-20 wt% Cu composite powder is investigated. The reduction behavior of ball-milled powder mixture is analyzed by XRD and temperature programmed reduction method at various heating rates in Ar-10% H₂ atmosphere. The XRD analysis of the heat-treated powder at 300°C shows Cu, MoO₃, and Cu₂MoO₅ phases. In contrast, the powder mixture heated at 400°C is composed of Cu and MoO₂ phases. The hydrogen reduction kinetic is evaluated by the amount of peak shift with heating rates. The activation energies for the reduction, estimated by the slope of the Kissinger plot, are measured as 112.2 kJ/mol and 65.2 kJ/mol, depending on the reduction steps from CuO to Cu and from MoO₃ to MoO₂, respectively. The measured activation energy for the reduction of MoO₃ is explained by the effect of pre-reduced Cu particles. The powder mixture, hydrogen-reduced at 700°C, shows the dispersion of nano-sized Cu agglomerates on the surface of Mo powders.

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• Fabrication of Porous Mo-Cu by Freeze Drying and Hydrogen Reduction of Metal Oxide Powders
  Hyunji Kang, Ju-Yeon Han, Sung-Tag Oh
  Journal of Korean Powder Metallurgy Institute.2019; 26(1): 1.     CrossRef
• Hydrogen Reduction Behavior and Microstructure Characteristics of Ball-milled CuO-Co₃O₄ Powder Mixtures
  Ju-Yeon Han, Gyuhwi Lee, Hyunji Kang, Sung-Tag Oh
  Journal of Korean Powder Metallurgy Institute.2019; 26(5): 410.     CrossRef

Porous Cu with a dispersion of nanoscale Al₂O₃ particles is fabricated by freeze-drying CuO-Al₂O₃/camphene slurry and sintering. Camphene slurries with CuO-Al₂O₃ contents of 5 and 10 vol% are unidirectionally frozen at -30°C, and pores are generated in the frozen specimens by camphene sublimation during air drying. The green bodies are sintered for 1 h at 700°C and 800°C in H₂ atmosphere. The sintered samples show large pores of 100 μm in average size aligned parallel to the camphene growth direction. The internal walls of the large pores feature relatively small pores of ~10 μm in size. The size of the large pores decreases with increasing CuO-Al₂O₃ content by the changing degree of powder rearrangement in the slurry. The size of the small pores decreases with increasing sintering temperature. Microstructural analysis reveals that 100-nm Al₂O₃ particles are homogeneously dispersed in the Cu matrix. These results suggest that a porous composite body with aligned large pores could be fabricated by a freeze-drying and H₂ reducing process.

Porous W-10 wt% Ti alloys are prepared by freeze-drying a WO₃-TiH₂/camphene slurry, using a sintering process. X-ray diffraction analysis of the heat-treated powder in an argon atmosphere shows the WO₃ peak of the starting powder and reaction-phase peaks such as WO_2.9, WO₂, and TiO₂ peaks. In contrast, a powder mixture heated in a hydrogen atmosphere is composed of the W and TiW phases. The formation of reaction phases that are dependent on the atmosphere is explained by a thermodynamic consideration of the reduction behavior of WO₃ and the dehydrogenation reaction of TiH₂. To fabricate a porous W-Ti alloy, the camphene slurry is frozen at -30°C, and pores are generated in the frozen specimens by the sublimation of camphene while drying in air. The green body is hydrogen-reduced and sintered at 1000°C for 1 h. The sintered sample prepared by freeze-drying the camphene slurry shows large and aligned parallel pores in the camphene growth direction, and small pores in the internal walls of the large pores. The strut between large pores consists of very fine particles with partial necking between them.