In this study, freeze drying of a porous Ni with unidirectionally aligned pore channels is accomplished by using a NiO powder and camphene. Camphene slurries with NiO content of 5 and 10 vol% are prepared by mixing them with a small amount of dispersant at 50℃. Freezing of a slurry is performed at -25℃ while the growth direction of the camphene is unidirectionally controlled. Pores are generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies are hydrogen-reduced at 400℃ and then sintered at 800℃ and 900℃ for 1 h. X-ray diffraction analysis reveals that the NiO powder is completely converted to the Ni phase without any reaction phases. The sintered samples show large pores that align parallel pores in the camphene growth direction as well as small pores in the internal walls of large pores. The size of large and small pores decreases with increasing powder content from 5 to 10 vol%. The influence of powder content on the pore structure is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.
The present study demonstrates the effect of freezing conditions on the pore structure of porous Cu-10 wt.% Sn prepared by freeze drying of CuO-SnO2/camphene slurry. Mixtures of CuO and SnO2 powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of CuO-SnO2 are unidirectionally frozen in a mold maintained at a temperature of -30oC for 1 and 24 h, respectively. Pores are generated by the sublimation of camphene at room temperature. After hydrogen reduction and sintering at 650oC for 2 h, the green body of the CuO-SnO2 is completely converted into porous Cu-Sn alloy. Microstructural observation reveals that the sintered samples have large pores which are aligned parallel to the camphene growth direction. The size of the large pores increases from 150 to 300 μm with an increase in the holding time. Also, the internal walls of the large pores contain relatively small pores whose size increases with the holding time. The change in pore structure is explained by the growth behavior of the camphene crystals and rearrangement of the solid particles during the freezing process.
In order to fabricate the porous Al₂O₃ with dispersion of nano-sized Cu particles, freeze-drying of cam-phene/Al₂O₃ slurry and solution chemistry process using Cu-nitrate are introduced. Camphene slurries with 10vol% Al₂O₃ was frozen at -25˚C. Pores were generated by sublimation of the camphene during drying in air. The sinteredsamples at 1400 and 1500oC showed the same size of large pores which were aligned parallel to the sublimable vehiclesgrowth direction. However, the size of fine pores in the internal walls of large pores decreased with increase in sinteringtemperature. It was shown that Cu particles with the size of 100 nm were homogeneously dispersed on the surfaces ofthe large pores. Antibacterial test using fungus revealed that the porous Al₂O₃/1vol% Cu composite showed antifungalproperty due to the dispersion of Cu particles. The results are suggested that the porous composites with required porecharacteristics and functional property can be fabricated by freeze-drying process and addition of functional nano par-ticles by chemical method.
Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-SnO2 and camphene. Camphene slurries with CuO-SnO2 content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at 50˚C. Freezing of a slurry was done at -25˚C while the growth direction of the camphene was unidirectionally controlled. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies were hydrogen-reduced at 650˚C and then were sintered at 650˚C and 750˚C for 1 h. XRD analysis revealed that the CuO-SnO2 powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above 100μm which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-SnO2 content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from 650˚C to 750˚C, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.
In the DBC (direct bonding of copper) process the oxygen partial pressure surrounding the AlN/Cu bonding pairs has been controlled by Ar gas mixed with oxygen. However, the direct bonding of Cu with sound interface and good adhesion strength is complicated process due to the difficulty in the exact control of oxygen partial pressure by using Ar gas. In this study, we have utilized the in-situ equilibrium established during the reaction of + 1/2 by placing powder bed of CuO or around the Cu/AlN bonding pair at . The adhesion strength was relatively better in case of using CuO powder than when powder was used. Microstructural analysis by optical microscopy and XRD revealed that the interface of bonding pair was composed of , Cu and small amount of CuO phase. Thus, it is explained that the good adhesion between Cu and AlN is attributed to the wetting of eutectic liquid formed by reaction of Cu and .
Porous Al2O3 dispersed with nano-sized Cu was fabricated by freeze-drying process and solution chemistry method using Cu-nitrate. To prepare porous Al2O3, camphene was used as the sublimable vehicle. Camphene slurries with Al2O3 content of 10 vol% were prepared by milling at 50˚C with a small amount of oligomeric polyester dispersant. Freezing of the slurry was done in a Teflon cylinder attached to a copper bottom plate cooled to -25˚C while unidirectionally controlling the growth direction of the camphene. Pores were subsequently generated by sublimation of the camphene during drying in air for 48 h. The green body was sintered in a furnace at 1400˚C for 1 h. Cu particles were dispersed in porous Al2O3 by calcination and hydrogen reduction of Cu-nitrate. The sintered samples showed large pores with sizes of about 150μm; these pores were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores due to the traces of camphene left between the concentrated Al2O3 particles on the internal wall. EDS analysis revealed that the Cu particles were mainly dispersed on the surfaces of the large pores. These results strongly suggest that porous Al2O3 with Cu dispersion can be successfully fabricated by freeze-drying and solution chemistry routes.
An attempt was made to evaluate creep reliability of two commercial Ni-based superalloys by using ultrasonic wave. The materials include fine-grained PM alloy fabricated by mechanical alloying and subsequent hot isostatic pressing, and IN738LC cast alloy with a grain size of a few cm. Microstructural parameters (fraction of creep cavity and size of precipitates) and ultrasonic parameters (velocity, attenuation) were measured to try to find relationships between them. Ultrasonic velocity decreased with creep cavity formation in PM alloy. On the other hand, no distinct changing trend of ultrasonic velocity was observed for IN738LC alloy. Ultrasonic attenuation was found to have a linear correlation with the size of precipitates and was suggested as a potential parameter for monitoring creep reliability of IN738LC alloy.
To increase pot life in the formulation mixed with bisphenol F epoxy resin, anhydride-based curing agent, and imidazole-based curing accelerator powders as a paste material for high-speed RFID chip bonding, size variation of the imidazole-based powders and a coating method of the powders were adopted in this study. In experiment with regard to the size variation, the pot life was not outstandingly increased. Through the idea using the coating method, however, the pot life was increased up to 4.25 times in comparison with the addition of initial imidazole-based powders. Consequently, successive bonding of RFID chip could be performed with very short time of 5sec using the suggested formulation having improved pot life.
Characteristics of Al-based composites with waste stainless steel short fiber, fabricated by magnetic pulsed compaction and sintering were investigated. The compacts prepared by magnetic pulsed compaction showed high relative density and homogeneous microstructure compared with that by conventional press compaction. The relative density of sintered composites at for 1 h exhibited the same value with compacts and decreased with increase in STS short fiber content. The reaction between Al and STS phase was confirmed by the microstructural analysis using EDS. The sintered composites, prepared by magnetic pulsed compaction, showed increased hardness value with increasing STS fiber content. Maximum yield strength of 100 MPa and tensile strength of 232 MPa were registered in the AI-based composite with 30 vol% STS short fiber.
Porous and porous surfaced Ti-6Al-4V implant compacts were fabricated by electro-discharge-sintering (EDS) of atomized spherical Ti-6Al-4V powders with a diameter of , The solid core formed in the center of the compact after discharge was composed of acicular Widmanstatten grains, The hardness value at the solid core was much higher than that at the particle interface or particles in the porous layer, which can be attributed to both heat treatment and work hardening effects induced from EDS, The compressive yield strength was in a range of 19 to 436 MPa which significantly depends on both input energy and capacitance, Selected porous-surfaced Ti-6Al-4V implant compacts with a solid core have much higher compressive strengths compared to the human teeth and sintered Ti dental implants.
Implant prototypes with various porosities were fabricated by electro-discharge-sintering of atomized spherical Ti-6Al-4V powders. Single pulse of 0.75 to 2.0 kJ/0.7 g-powder, using 150, 300, and capacitors was applied to produce a fully porous and porous surfaced implant compact. The solid core formed in the center of the compact after discharge was composed of acicular grains and porous layer consisted of particles connected in three dimensions by necks. The solid core and neck sizes increased with an increase in input energy and capacitance. On the other hand, pore volume decreased with increased capacitance and input energy due to the formation of solid core. Capacitance and input energy are the only controllable discharge parameters even though the heat generated during a discharge is the unique parameter that determines the porosity of compact. It is known that electro-discharge-sintering of spherical Ti-6Al-4V powders can efficiently produce fully-porous and porous surfaced Ti-6Al-4V implants with various porosities in a short time less then 400 isec by manipulating the discharging condition such as input energy and capacitance including powder size.