Tungsten carbide is widely used in carbide tools. However, its production process generates a significant number of end-of-life products and by-products. Therefore, it is necessary to develop efficient recycling methods and investigate the remanufacturing of tungsten carbide using recycled materials. Herein, we have recovered 99.9% of the tungsten in cemented carbide hard scrap as tungsten oxide via an alkali leaching process. Subsequently, using the recovered tungsten oxide as a starting material, tungsten carbide has been produced by employing a self-propagating high-temperature synthesis (SHS) method. SHS is advantageous as it reduces the reaction time and is energy-efficient. Tungsten carbide with a carbon content of 6.18 wt % and a particle size of 116 nm has been successfully synthesized by optimizing the SHS process parameters, pulverization, and mixing. In this study, a series of processes for the highefficiency recycling and quality improvement of tungsten-based materials have been developed.

The automotive industry has focused on the development of metallic materials with high specific strength, which can meet both fuel economy and safety goals. Here, a new class of ultrafine-grained high-Mn steels containing nano-scale oxides is developed using powder metallurgy. First, high-energy mechanical milling is performed to dissolve alloying elements in Fe and reduce the grain size to the nanometer regime. Second, the ball-milled powder is consolidated using spark plasma sintering. During spark plasma sintering, nanoscale manganese oxides are generated in Fe-15Mn steels, while other nanoscale oxides (e.g., aluminum, silicon, titanium) are produced in Fe-15Mn-3Al-3Si and Fe-15Mn-3Ti steels. Finally, the phases and resulting hardness of a variety of high-Mn steels are compared. As a result, the sintered pallets exhibit superior hardness when elements with higher oxygen affinity are added; these elements attract oxygen from Mn and form nanoscale oxides that can greatly improve the strength of high-Mn steels.

Effective control of the heat generated from electronics and semiconductor devices requires a high thermal conductivity and a low thermal expansion coefficient appropriate for devices or modules. A method of reducing the thermal expansion coefficient of Cu has been suggested wherein a ceramic filler having a low thermal expansion coefficient is applied to Cu, which has high thermal conductivity. In this study, using pressureless sintering rather than costly pressure sintering, a polymer solution synthesis method was used to make nano-sized Cu powder for application to Cu matrix with an AlN filler. Due to the low sinterability, the sintered Cu prepared from commercial Cu powder included large pores inside the sintered bodies. A sintered Cu body with Zn, as a liquid phase sintering agent, was prepared by the polymer solution synthesis method for exclusion of pores, which affect thermal conductivity and thermal expansion. The pressureless sintered Cu bodies including Zn showed higher thermal conductivity (180 W/m·K) and lower thermal expansion coefficient (15.8×10−6/℃) than did the monolithic synthesized Cu sintered body.

An optimum route to fabricate a hybrid-structured W powder composed of nano and micro size powders was investigated. The mixture of nano and micro W powders was prepared by a ball milling and hydrogen reduction process for WO3 and W powders. Microstructural observation for the ball-milled powder mixtures revealed that the nano-sized WO3 particles were homogeneously distributed on the surface of large W powders. The reduction behavior of WO3 powder was analyzed by a temperature programmed reduction method with different heating rates in Ar-10% H2 atmosphere. The activation energies for the reduction of WO3, estimated by the slope of the Kissinger plot from the amount of reaction peak shift with heating rates, were measured as 117.4 kJ/mol and 94.6 kJ/mol depending on reduction steps from WO3 to WO2 and from WO2 to W, respectively. SEM and XRD analysis for the hydrogen-reduced powder mixture showed that the nano-sized W particles were well distributed on the surface of the micro-sized W powders.

The effect of the mixing method on the characteristics of hybrid-structure W powder with nano and micro sizes is investigated. Fine WO3 powders with sizes of ~0.6 μm, prepared by ball milling for 10 h, are mixed with pure W powder with sizes of 12 μm by various mixing process. In the case of simple mixing with ball-milled WO3 and micro sized W powders, WO3 particles are locally present in the form of agglomerates in the surface of large W powders, but in the case of ball milling, a relatively uniform distribution of WO3 particles is exhibited. The microstructural observation reveals that the ball milled WO3 powder, heat-treated at 750oC for 1 h in a hydrogen atmosphere, is fine W particles of ~200 nm or less. The powder mixture prepared by simple mixing and hydrogen reduction exhibits the formation of coarse W particles with agglomeration of the micro sized W powder on the surface. Conversely, in the powder mixture fabricated by ball milling and hydrogen reduction, a uniform distribution of fine W particles forming nano-micro sized hybrid structure is observed.

Nanopowders provide better details for micro features and surface finish in powder injection molding processes. However, the small size of such powders induces processing challenges, such as low solid loading, high feedstock viscosity, difficulty in debinding, and distinctive sintering behavior. Therefore, the optimization of process conditions for nanopowder injection molding is essential, and it should be carefully performed. In this study, the powder injection molding process for Fe nanopowder has been optimized. The feedstock has been formulated using commercially available Fe nanopowder and a wax-based binder system. The optimal solid loading has been determined from the critical solid loading, measured by a torque rheometer. The homogeneously mixed feedstock is injected as a cylindrical green body, and solvent and thermal debinding conditions are determined by observing the weight change of the sample. The influence of the sintering temperature and holding time on the density has also been investigated. Thereafter, the Vickers hardness and grain size of the sintered samples have been measured to optimize the sintering conditions.

2ZrO2·P2O5 powder, which is not synthesized by solid reaction method, was successfully synthesized through PVA solution method. In this process, the firing temperature and the PVA content strongly affected the crystallization behavior and final particle size. A stable α-phase 2ZrO2·P2O5 was synthesized at a firing temperature of 1200 oC and holding time of 4 h. β-phase 2ZrO2·P2O5 was observed, with un-reacted ZrO2 phases, for firing temperatures lower than 1200 oC. In terms of the PVA content effect, the powder prepared with a PVA mixing ratio of 12:1 showed stable α-phase 2ZrO2·P2O5; however, the β-phase was found to co-exist at relatively higher PVA content. The synthesized α-phase 2ZrO2·P2O5 powder showed an average particle size of 100~250 nm and an average thermal expansion coefficient of −2.5 × 10−6/oC in the range of room temp. ~800 oC.

In order to identify changes in the nature of the particles due to changes in the inflow rate of the raw material solution, the present study was intended to prepare nano-sized cobalt oxide (Co3O4) powder with an average particle size of 50 nm or less by spray pyrolysis reaction using raw cobalt chloride solution. As the inflow rate of the raw material solution increased, droplets formed by the pyrolysis reaction showed more divided form and the particle size distribution was more uneven. As the inflow rate of the solution increased from 2 to 10 ml/min, the average particle size of the formed particles increased from about 25 nm to 40 nm, while the average particle size did not show significant changes when the inflow rate increased from 10 to 50 ml/min. XRD analysis showed that the intensity of the XRD peaks increased remarkably when the inflow rate of the solution increased from 2 to 10 ml/min. On the other hand, the peak intensity stayed almost constant when the inflow rate increased from 10 to 50 ml/min. With the increase in the inflow rate from 2 to 10 ml/min, the specific surface area of the particles decreased by approximately 20 %. On the contrary, the specific surface area stayed constant when the inflow rate increased from 10 to 50 ml/min.

The self-propagating high temperature synthesis approach was applied to synthesize amorphous boron nanopowders in argon atmospheres. For this purpose, we investigated the characteristics of a thermally induced combustion wave in the B2O3 + α Mg system(α = 1.0-8.0) in an argon atmospheres. In this study, the exothermic nature of the B2O3-Mg reaction was investigated using thermodynamic calculations. Experimental study was conducted based on the calculation data and the SHS products consisting of crystalline boron and other compounds were obtained starting with a different initial molar ratio of Mg. It was found that the B2O3 and Mg reaction system produced a high combustion temperature with a rapid combustion reaction. In order to regulate the combustion reaction, NaCl, Na2B4O7 and H3BO3 additives were investigated as diluents. In an experimental study, it was found that all diluents effectively stabilized the reaction regime. The final product of the B2O3 + α Mg system with 0.5 mole Na2B4O7 was identified to be amorphous boron nano-powders(< 100 nm).

Electronic products are a major part of evolving industry and human life style; however most of them are known to emit electromagnetic waves that have severe health hazards. Therefore, different materials and fabrication techniques are understudy to control or limit transfer of such waves to human body. In this study, nanocomposite powder is dispersed into epoxy resin and shielding effects such as absorption, reflection, penetration and multiple reflections are investigated. In addition, nano size powder (Ni, Fe2O3, Fe-85Ni, C-Ni) is fabricated by pulsed wire evaporation method and dispersed manually into epoxy. Characterization techniques such as X-ray diffraction, Scanning electron microscopy and Transmission electron microscopy are used to investigate the phase analysis, size and shape as well as dispersion trend of a nano powder on epoxy matrix. Shielding effect is measured by standard test method to investigate the electromagnetic shielding effectiveness of planar materials, ASTM D4935. At lower frequency, sample consisting nano-powder of Fe-85%Wt Ni shows better electromagnetic shielding effect compared to only epoxy, only Ni, Fe2O3 and C-Ni samples.

In this study, in order to increase surface ability of hardness and corrosion of magnesium alloy, anodizingand sealing with nano-diamond powder was conducted. A porous oxide layer on the magnesium alloy was successfullymade at 85℃ through anodizing. It was found to be significantly more difficult to make a porous oxide layer in themagnesium alloy compared to an aluminum alloy. The oxide layer made below 73℃ by anodizing had no porous layer.The electrolyte used in this study is DOW 17 solution. The surface morphology of the magnesium oxide layer wasinvestigated by a scanning electron microscope. The pores made by anodizing were sealed by water and aqueous nano-diamond powder respectively. The hardness and corrosion resistance of the magnesium alloy was increased by the anod-izing and sealing treatment with nano-diamond powder.

Using the spray pyrolysis process, nano-sized cobalt oxide powder with average particle size below 50 nm was prepared from cobalt chloride solution. The influences of the raw material solution on the properties of the powder formed examined. When the concentration of Co was low(20 g/L), the average particle size of the powder formed was roughly 20 nm, and the cohesion between these particles was significantly strong. When the concentration of Co increased to 100 g/L, the droplets nearly failed to exist in circular form and reflected a severely divided form. Furthermore, the average size of the particles formed was roughly 40 nm, and the particles reflected a polygonal form. When the solution was increased to nearly saturation level (Co at 200 g/L), the particle size distribution reflected significant unevenness due to severe droplet division while the surface also reflected significant unevenness. Furthermore, the average size of the particles formed increased significantly to 70 nm. The results of XRD analysis showed that the strength of the peaks reflected very little change when the concentration of Co was increased from 20 g/L to 50 g/L. Alternatively, when the concentration was increased to 100 g/L, the strength of the peaks increased compared to when the concentration was 50 g/L. However, when the concentration was increased to 200 g/L, the strength of the peaks failed to reflect significant change compared to when the concentration was 100 g/L. The specific surface area dramatically decreased by 30 % when the concentration of Co was increased from 20 g/L to 50 g/L. Alternatively, when the concentration of Co the solution increased to 100 g/L, the specific surface area decreased by roughly 15 %. Furthermore, when the concentration of Co was increased to nearly saturation level(200 g/L), the specific surface area decreased by roughly 35%.

In this study, nano-scale copper powders were reduction treated in a hydrogen atmosphere at the relativelyhigh temperature of 350℃ in order to eliminate surface oxide layers, which are the main obstacles for fabricating anano/ultrafine grained bulk parts from the nano-scale powders. The changes in composition and microstructure beforeand after the hydrogen reduction treatment were evaluated by analyzing X-ray diffraction (XRD) line profile patternsusing the convolutional multiple whole profile (CMWP) procedure. In order to confirm the result from the XRD lineprofile analysis, transmitted electron microscope observations were performed on the specimen of the hydrogen reduc-tion treated powders fabricated using a focused ion beam process. A quasi-statically compacted specimen from the nano-scale powders was produced and Vickers micro-hardness was measured to verify the potential of the powders as thebasis for a bulk nano/ultrafine grained material. Although the bonding between particles and the growth in size of theparticles occurred, crystallites retained their nano-scale size evaluated using the XRD results. The hardness results dem-onstrate the usefulness of the powders for a nano/ultrafine grained material, once a good consolidation of powders isachieved.

In this study, an aluminum oxide layer for sealing treatment of nano-diamond powder was synthesized byanodizing under constant current. The produced pore size and oxide thickness were investigated using scanning electronmicroscopy. The pore size increased as the treatment time increased, current density increased, sulfuric acid concentra-tion decreased, which is different from the results under constant voltage, due to a dissolution of the oxide layers. Theoxide layer thickness by the anodizing increased as temperature, time, and current density increased. The results of thisstudy can be applied to optimize the sealing treatment process of nano-diamond particles of 4-10 nm to enhance theresistances of corrosion and wear of the matrix.

Bulk nanostructured copper was fabricated by a shock compaction method using the planar shock wavegenerated by a single gas gun system. Nano sized powders, average diameter of 100 nm, were compacted into the cap-sule and target die, which were designed to eliminate the effect of undesired shock wave, and then impacted with analuminum alloy target at 400 m/s. Microstructure and mechanical properties of the shock compact specimen were ana-lyzed using an optical microscope (OM), scanning electron microscope (SEM), and micro indentation. Hardness resultsshowed low values (approximately 45~80 Hv) similar or slightly higher than those of conventional coarse grained com-mercial purity copper. This result indicates the poor quality of bonding between particles. Images from OM and SEMalso confirmed that no strong bonding was achieved between them due to the insufficient energy and surface oxygenlayer of the powders.

This study was aimed at synthesizing and characterizing cerium-doped titania. Cerium-doped anatase titania powders were prepared by sol-gel process, with ammonium (IV) nitrate and titanium (IV) butoxide as the raw materials. The characteristics of pure TiO2 and cerium-doped TiO2 were investigated by XRD, TG/DTA, FE-SEM, and UV-vis spectroscopy. The results of this study show that anatase type of TiO2 was obtained in as-prepared and calcined TiO2 and Ce-TiO2 powder. A DTA curve was also observed as the crystallization temperature decreased with increasing cerium contents. We found that the crystallite size of the obtained anatase particles decreased from 55 nm to 25 nm and the particle size decreased with increasing cerium contents. Moreover, UV-vis spectra showed that anatase titania powders with various cerium contents effectively extend the light absorption properties to the visible region.

In this study, nano-sized cobalt oxide powder with an average particle size below 50 nm was prepared from a cobalt chloride solution by the spray pyrolysis process. The influences of reaction temperature on the properties of the generated powder were examined. The average particle size of the particles formed based on the spray pyrolysis process at a reaction temperature of 700˚C is roughly 20 nm. Moreover, most of these particles cannot appear with an independent type, thereby coexisting in a droplet type. When the reaction temperature increases to 800˚C, the average particle size not only increases to roughly 40 nm but also shows a more dense structure while the ratio of particles which shows a polygonal form significantly increases. As the reaction temperature increases to 900˚C, the distribution of the particles is from roughly 70 nm to 100 nm, while most of the particle surface is more intricately close and forms a polygonal shape. When the reaction temperature increases to 1000˚C, the particle size distribution of the powder shows an existing form from 80 nm to at least 150 nm in an uneven form. As the reaction temperature increases, the XRD peak intensity gradually increases, yet the specific surface area gradually decreases.

In this study, by using nickel chloride solution as a raw material, a nano-sized nickel oxide powder with an average particle size below 50 nm was produced by spray pyrolysis reaction. A spray pyrolysis system was specially designed and built for this study. The influence of nozzle tip size on the properties of the produced powder was examined. When the nozzle tip size was 1 mm, the particle size distribution was more uniform than when other nozzle tip sizes were used and the average particle size of the powder was about 15 nm. When the nozzle tip size increases to 2 mm, the average particle size increases to roughly 20 nm, and the particle size distribution becomes more uneven. When the tip size increases to 3 mm, particles with an average size of 25 nm and equal to or less than 10 nm coexist and the particle size distribution becomes much more uneven. When the tip size increases to 5 mm, large particles with average size of 50 nm partially exist, mostly consisting of minute particles with average sizes in the range of 15~25 nm. When the tip size increases from 1 mm to 2 mm, the XRD peak intensities greatly increase while the specific surface area decreases. When the tip size increases to 3 mm, the XRD peak intensities decrease while the specific surface area increases. When the tip size increases to 5 mm, the XRD peak intensities increase again while the specific surface area decreases.

In this study, using a tin chloride solution as the raw material, a nano-sized tin oxide powder with an average particle size below 50 nm is generated by a spray pyrolysis process. The properties of the tin oxide powder according to the nozzle tip size are examined. Along with an increase in the nozzle tip size from 1 mm to 5 mm, the generated particles that appear in the shape of droplets maintain an average particle size of 30 nm. When the nozzle tip size increases from 1 mm to 2 mm, the average size of the generated particles is around 80-100 nm, and the ratio of the independent particles with a compact surface structure increases significantly. When the nozzle tip size is at 3 mm, the majority of the generated particles maintain the droplet shape, the average size of the droplet-shaped particles increases remarkably compared to the cases of other nozzle tip sizes, and the particle size distribution also becomes extremely irregular. When the nozzle tip size is at 5 mm, the ratio of droplet-shaped particles decreases significantly and most of the generated particles are independent ones with incompact surface structures. Along with an increase in the nozzle tip size from 1 mm to 3 mm, the XRD peak intensity increases, whereas the specific surface area decreases greatly. When the nozzle tip size increases up to 5 mm, the XRD peak intensity decreases significantly, while the specific surface area increases remarkably.