The synthesis of porous W by freeze-casting and vacuum drying is investigated. Ball-milled WO₃ powders and tert-butyl alcohol were used as the starting materials. The tert-butyl alcohol slurry is frozen at –25°C and dried under vacuum at –25 and –10°C. The dried bodies are hydrogen-reduced at 800°C and sintered at 1000°C. The XRD analysis shows that WO₃ is completely reduced to W without any reaction phases. SEM observations reveal that the struts and pores aligned in the tert-butyl alcohol growth direction, and the change in the powder content and drying temperature affects the pore structure. Furthermore, the struts of the porous body fabricated under vacuum are thinner than those fabricated under atmospheric pressure. This behavior is explained by the growth mechanism of tert-butyl alcohol and rearrangement of the powders during solidification. These results suggest that the pore structure of a porous body can be controlled by the powder content, drying temperature, and pressure.

The effects of drying temperature on the microstructure of porous W fabricated by the freeze-casting process of tert-butyl alcohol slurry with WO₃ powder was investigated. Green bodies were hydrogen-reduced at 800°C for 1 h and sintered at 1000°C for 6 h. X-ray diffraction analysis revealed that WO₃ powders were completely converted to W without any reaction phases by hydrogen reduction. The sintered body showed pores aligned in the direction of tertbutyl alcohol growth, and the porosity and pore size decreased as the amount of WO₃ increased from 5 to 10v ol%. As the drying temperature of the frozen body increased from -25°C to -10°C, the pore size and thickness of the struts increased. The change in microstructural characteristics based on the amount of powder added and the drying temperature was explained by the growth behavior of the freezing agent and the degree of rearrangement of the solid powder during the solidification of the slurry.

The effect of tert-butyl alcohol (TBA) as a freezing solvent on the pore structure of a porous tungsten body prepared by freeze-drying is analyzed. TBA slurries with a WO₃ content of 10 vol% are prepared by mixing with a small amount of dispersant and binder at 30°C. The slurries are frozen at -25°C, and pores are formed in the frozen specimens by the sublimation of TBA during drying in air. After hydrogen reduction at 800°C and sintering at 1000°C, the green body of WO₃ is completely converted to porous W with various pore structures. Directional pores from the center of the specimen to the outside are observed in the sintered bodies because of the columnar growth of TBA. A decrease in pore directionality and porosity is observed in the specimens prepared by long-duration drying and sintering. The change in pore structure is explained by the growth of the freezing solvent and densification.

In this study, the effects of kaolin addition on the properties of reticulated porous diatomite-kaolin composites are investigated. A reticulated porous diatomite-kaolin composite is prepared using the replica template method. The microstructure and pore characteristics of the reticulated porous diatomite-kaolin composites are analyzed by controlling the PPI value (45, 60, and 80 PPI) of the polyurethane foam (which are used as the polymer template), the ball-milling time (8 and 24 h), and the amount of kaolin (0–50 wt. %). The average pore size decreases as the amount of kaolin increases in the reticulated porous diatomite-kaolin composite. As the amount of kaolin increases, it can be determined that the amount of inter-connected pore channels is reduced because the plate-shaped kaolin particles connect the gaps between irregular diatomite particles. Consequently, a higher kaolin percentage affects the overall mechanical properties by improving the pore channel connectivity. The effect of kaolin addition on the basic properties of the reticulated porous diatomite-kaolin composite is further discussed with characterization data such as pore size distribution, scanning electron microscopy images, and compressive strength.

The effect of sublimable vehicles on the pore structure of Cu fabricated by freeze drying is investigated. The 5 vol% CuO-dispersed slurries with camphene and various camphor-naphthalene compositions are frozen in a Teflon mold at -25°C, followed by sublimation at room temperature. After hydrogen reduction at 300°C and sintering at 600 °C, the green bodies of CuO are completely converted to Cu with various pore structures. The sintered samples prepared using CuO/camphene slurries show large pores that are aligned parallel to the sublimable vehicle growth direction. In addition, a dense microstructure is observed in the bottom section of the specimen where the solidification heat was released, owing to the difference in the solidification behavior of the camphene crystals. The porous Cu shows different pore structures, such as dendritic, rod-like, and plate shaped, depending on the composition of the camphornaphthalene system. The change in pore structure is explained by the crystal growth behavior of primary camphor and eutectic and primary naphthalene.

Porous Cu-14 wt% Co with aligned pores is produced by a freeze drying and sintering process. Unidirectional freezing of camphene slurry with CuO-Co₃O₄ powders is conducted, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The dried bodies are hydrogen-reduced at 500°C and sintered at 800°C for 1 h. The reduction behavior of the CuO-Co₃O₄ powder mixture is analyzed using a temperature-programmed reduction method in an Ar-10% H₂ atmosphere. The sintered bodies show large and aligned parallel pores in the camphene growth direction. In addition, small pores are distributed around the internal walls of the large pores. The size and fraction of the pores decrease as the amount of solid powder added to the slurry increases. The change in pore characteristics according to the amount of the mixed powder is interpreted to be due to the rearrangement and accumulation behavior of the solid particles in the freezing process of the slurry.

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°C. Freezing of a slurry is performed at -25°C 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°C and then sintered at 800°C and 900°C 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.

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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

Porous metals demonstrate not only excessively low densities, but also novel physical, thermal, mechanical, electrical, and acoustic properties. Thus, porous metals exhibit exceptional performance, which are useful for diesel particulate filters, heat exchangers, and noise absorbers. In this study, SUS316L foam with 90% porosity and 3,000 μm pore size is successfully manufactured using the electrostatic powder coating (ESPC) process. The mean size of SUS316L powders is approximately 12.33 μm. The pore properties are evaluated using SEM and Archimedes. As the quantity of powder coating increases, pore size decreases from 2,881 to 1,356 μm. Moreover, the strut thickness and apparent density increase from 423.7 to 898.3 μm and from 0.278 to 0.840 g/cm³, respectively. It demonstrates that pore properties of SUS316L powder porous metal are controllable by template type and quantity of powder coating.

Plastic pollution is threatening human health and ecosystems, resulting in one of the biggest challenges that humanity has ever faced. Therefore, this study focuses on the preparation of macroporous carbon from biowaste (MC)-supported manganese oxide (MnO₂) as an efficient, reusable, and robust catalyst for the recycling of poly(ethylene terephthalate) (PET) waste. As-prepared MnO₂/MC composites have a hierarchical pore network and a large surface area (376.16 m²/g) with a narrow size distribution. MnO₂/MC shows a maximum yield (98%) of bis(2-hydroxyethyl)terephthalate (BHET) after glycolysis reaction for 120 min. Furthermore, MnO₂/MC can be reused at least nine times with a negligible decrease in BHET yield. Based on this remarkable catalytic performance, we expect that MnO₂-based heterogeneous catalysts have the potential to be introduced into the PET recycling industry.

In this study, we synthesize tungsten oxide thin films by electrodeposition and characterize their electrochromic properties. Depending on the deposition modes, compact and porous tungsten oxide films are fabricated on a transparent indium tin oxide (ITO) substrate. The morphology and crystal structure of the electrodeposited tungsten oxide thin films are investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD). X-ray photoelectron spectroscopy is employed to verify the chemical composition and the oxidation state of the films. Compared to the compact tungsten oxides, the porous films show superior electrochemical activities with higher reversibility during electrochemical reactions. Furthermore, they exhibit very high color contrast (97.0%) and switching speed (3.1 and 3.2 s). The outstanding electrochromic performances of the porous tungsten oxide thin films are mainly attributed to the porous structure, which facilitates ion intercalation/deintercalation during electrochemical reactions.

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• A fast-response electrochromic device based on a composite gel film comprising triphenylamine derivatives and WO3
  Xuejian Zhang, Jinming Zeng, Zipeng Xu, Mimi Zhu, Ping Liu
  New Journal of Chemistry.2021; 45(12): 5503.     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.

Ceramic powder, such as MgO, is added as a binder to prepare the green compacts of molten salts of an electrolyte for a thermal battery. Despite the addition of a binder, when the thickness of the electrolyte decreases to improve the battery performance, the problem with the unintentional short circuit between the anode and cathode still remains. To improve the current powder molding method, a new type of electrolyte separator with porous MgO preforms is prepared and characteristics of the thermal battery are evaluated. A Spherical PMMA polymer powder is added as a pore-forming agent in the MgO powder, and an organic binder is used to prepare slurry appropriate for tape casting. A porous MgO preform with 300 μm thickness is prepared through a binder burnout and sintering process. The particle size of the starting MgO powder has an effect, not on the porosity of the porous MgO preform, but on the battery characteristics. The porosity of the porous MgO preforms is controlled from 60 to 75% using a pore-forming agent. The batteries prepared using various porosities of preforms show a performance equal to or higher than that of the pellet-shaped battery prepared by the conventional powder molding method.