A sintered body of TiB2-reinforced iron matrix composite (Fe-TiB2) is fabricated by pressureless-sintering of a mixture of titanium hydride (TiH2) and iron boride (FeB) powders. The powder mixture is prepared in a planetary ball-mill at 700 rpm for 3 h and then pressurelessly sintered at 1300, 1350 and 1400°C for 0-2 h. The optimal sintering temperature for high densities (above 95% relative density) is between 1350 and 1400°C, where the holding time can be varied from 0.25 to 2 h. A maximum relative density of 96.0% is obtained from the (FeB+TiH2) powder compacts sintered at 1400°C for 2 h. Sintered compacts have two main phases of Fe and TiB2 along with traces of TiB, which seems to be formed through the reaction of TiB2 formed at lower temperatures during the heating stage with the excess Ti that is intentionally added to complete the reaction for TiB2 formation. Nearly fully densified sintered compacts show a homogeneous microstructure composed of fine TiB2 particulates with submicron sizes and an Fe-matrix. A maximum hardness of 71.2 HRC is obtained from the specimen sintered at 1400°C for 0.5 h, which is nearly equivalent to the HRC of conventional WC-Co hardmetals containing 20 wt% Co.
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Fe-30 wt% TiC composite powders are fabricated by in situ reaction synthesis after planetary ball milling of (Fe, TiH2, Carbon) powder mixture. Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-30 wt% TiC composite powder compacts. Pressureless sintering is performed at 1100, 1200 and 1300°C for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of 1050°C, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of 50°C/min, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts are not densified even after sintering at 1300°C for 3 h, which shows a relative denstiy of 66.9%. Spark-plasma sintering at 1050°C for 10 min exhibits nearly full densification of 99.6% relative density under the sintering pressure of 50 MPa.
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Effect of oxygen content in the ultrafine tungsten powder fabricated by electrical explosion of wire method on the behvior of spark plasma sintering was investigated. The initial oxygen content of 6.5 wt% of as-fabricated tungsten powder was reduced to 2.3 and 0.7 wt% for the powders which were reduction-treated at 400°C for 2 hour and at 500°C for 1h in hydrogen atmosphere, respectively. The reduction-treated tungsten powders were spark-plasma sintered at 1200-1600°C for 100-3600 sec. with applied pressure of 50 MPa under vacuum of 0.133 Pa. Maximun sindered density of 97% relative density was obtained under the condition of 1600°C for 1h from the tungsten powder with 0.7 wt% oxygen. Sintering activation energy of 95.85 kJ/mol−1 was obtained, which is remarkably smaller than the reported ones of 380~460 kJ/mol−1 for pressureless sintering of micron-scale tungsten powders.
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Fe-TiC composite powder was fabricated by high-energy milling of powder mixture of (Fe, TiC) and (FeO, TiH2, C) as starting materials, respectively. The latter one was heat-treated for reaction synthesis of TiC phase after milling. Both powders were spark-plasma sintered at various temperatures of 680-1070°C for 10 min. with sintering pressure of 70 MPa and the heating rate of 50°C/min. under vacuum of 0.133 Pa. Density and hardness of the sintered compact was investigated. Fe-TiC composite fabricated from (FeO, TiH2, C) as starting materials showed better sintered properties. It seems to be resulted from ultra-fine TiC particle size and its uniform distribution in Fe-matrix compared to the simply mixed (Fe, TiC) powder.
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The present study demonstrates the effect of solidification condition on the pore structure in freeze drying process using the slurries of CuO/sublimable vehicles. Camphene and Camphor-45 wt% naphthalene based slurries with 14 vol% CuO powder were frozen into a mold at -25°C, followed by sublimation at room temperature. The green bodies were hydrogen-reduced and sintered at 500°C for 1 h. The porous Cu specimen, frozen the CuO/camphene slurry into the heated mold of the upper part, showed large pores with unidirectional pore channels and small pores in their internal wall. Also, it was observed that the size of large pores was decreasing near the bottom part of specimen. The change of pore structure depending on the freezing condition was explained by the nucleation behavior of camphene crystals and rearrangement of solid powders during solidification. In case of porous Cu prepared from CuO/Camphornaphthalene system, the pore structure exhibited plate shape as a replica of the original structure of crystallized vehicles with hypereutectic composition.
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