In this study, a core-shell powder and sintered specimens using a mechanically alloyed (MAed) Ti-Mo powder fabricated through high-energy ball-milling are prepared. Analysis of sintering, microstructure, and mechanical properties confirms the applicability of the powder as a sputtering target material. To optimize the MAed Ti-Mo powder milling process, phase and elemental analyses of the powders are performed according to milling time. The results reveal that 20 h of milling time is the most suitable for the manufacturing process. Subsequently, the MAed Ti-Mo powder and MoO3 powder are milled using a 3-D mixer and heat-treated for hydrogen reduction to manufacture the core-shell powder. The reduced core-shell powder is transformed to sintered specimens through molding and sintering at 1300 and 1400oC. The sintering properties are analyzed through X-ray diffraction and scanning electron microscopy for phase and porosity analyses. Moreover, the microstructure of the powder is investigated through optical microscopy and electron probe microstructure analysis. The Ti-Mo core-shell sintered specimen is found to possess high density, uniform microstructure, and excellent hardness properties. These results indicate that the Ti-Mo core-shell sintered specimen has excellent sintering properties and is suitable as a sputtering target material.
The theoretical capacity of silicon-based anode materials is more than 10 times higher than the capacity of graphite, so silicon can be used as an alternative to graphite anode materials. However, silicon has a much higher contraction and expansion rate due to lithiation of the anode material during the charge and discharge processes, compared to graphite anode materials, resulting in the pulverization of silicon particles during repeated charge and discharge. To compensate for the above issues, there is a growing interest in SiOx materials with a silica or carbon coating to minimize the expansion of the silicon. In this study, spherical silica (SiO2) was synthesized using TEOS as a starting material for the fabrication of such SiOx through heating in a reduction atmosphere. SiOx powder was produced by adding PVA as a carbon source and inducing the reduction of silica by the carbothermal reduction method. The ratio of TEOS to distilled water, the stirring time, and the amount of PVA added were adjusted to induce size and morphology, resulting in uniform nanosized spherical silica particles. For the reduction of the spherical monodisperse silica particles, a nitrogen gas atmosphere mixed with 5 % hydrogen was applied, and oxygen atoms in the silica were selectively removed by the carbothermal reduction method. The produced SiOx powder was characterized by FE-SEM to examine the morphology and size changes of the particles, and XPS and FT-IR were used to examine the x value (O/Si ratio) of the synthesized SiOx.
This study compares the characteristics of a compact TiO2 (c-TiO2) powdery film, which is used as the electron transport layer (ETL) of perovskite solar cells, based on the manufacturing method. Additionally, its efficiency is measured by applying it to a carbon electrode solar cell. Spin-coating and spray methods are compared, and spraybased c-TiO2 exhibits superior optical properties. Furthermore, surface analysis by scanning electron microscopy (SEM) and atomic force microscopy (AFM) exhibits the excellent surface properties of spray-based TiO2. The photoelectric conversion efficiency (PCE) is 14.31% when applied to planar perovskite solar cells based on metal electrodes. Finally, carbon nanotube (CNT) film electrode-based solar cells exhibits a 76% PCE compared with that of metal electrodebased solar cells, providing the possibility of commercialization.
화석연료의 사용에 따른 지구 온난화 및 기상 이변으로 인하여 온실가스 저감 문제가 대두되고 있으며, 그에 따 라 에너지 소모 없이 셀프 쿨링이 가능한 소재에 대한 연구가 활발히 진행되고 있다. 그 중에서도 실크는 천연 쿨링 소재로 알려져 있으나, 기존의 혼합 공정에서는 실크를 화학적으로 분말화 시키기 때문에 복사 냉각 효과가 사라지는 문제점이 있어, 복사냉각을 위한 필름 또는 코팅제 형태로 제조하는데 어려움을 겪고 있다. 본 연구에서는 실크 피브로인의 고유구조를 훼손 하지 않는 물리적 분쇄 공정을 거친 실크 분말을 사용하여 다양한 형태의 막을 제조하고, 코팅제로서의 적용가능성을 살펴보 고자 연구를 수행하였다. 이를 위해 실크 피브로인 분말이 도입된 전기방사 복합막 및 평막 형태의 복합막을 제조하였으며, 용액의 점도가 막 제조 및 제조된 막의 물성에 큰 영향을 미치는 것을 관찰하였다.
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.
Laser cladding a surface treatment process that grants superior characteristics such as toughness, hardness, and corrosion resistance to the surface, and rebuilds cracked molds; as such, it can be a strong tool to prolong service life of mold steel. Furthermore, compared with the other similar coating processes – thermal spray, etc., laser cladding provides superior bonding strength and precision coating on a local area. In this study, surface characteristics are studied after laser cladding of low carbon steel using 18%Cr-2.5%Ni-Fe powder (Rockit404), known for its high hardness and excellent corrosion resistance. A diode laser with wavelength of 900-1070 nm is adopted as laser source under argon atmosphere; electrical power for the laser cladding process is 5, 6, and 10 kW. Fundamental surface characteristics such as crossectional microstructure and hardness profile are observed and measured, and special evaluation, such as a soldering test with molten ALDC12 alloy, is conducted to investigate the corrosion resistance characteristics. As a result of the die-soldering test by immersion of low carbon alloy steel in ALDC12 molten metal, the clad layer's soldering thickness decreases.
Macro-porous carbon foams are fabricated using cured spherical phenolic resin particles as a matrix and furfuryl alcohol as a binder through a simple casting molding. Different sizes of the phenolic resin particles from 100– 450 μm are used to control the pore size and structure. Ethylene glycol is additionally added as a pore-forming agent and oxalic acid is used as an initiator for polymerization of furfuryl alcohol. The polymerization is performed in two steps; at 80oC and 200oC in an ambient atmosphere. The carbonization of the cured body is performed under Nitrogen gas flow (0.8 L/min) at 800oC for 1 h. Shrinkage rate and residual carbon content are measured by size and weight change after carbonization. The pore structures are observed by both electron and optical microscope and compared with the porosity results achieved by the Archimedes method. The porosity is similar regardless of the size of the phenolic resin particles. On the other hand, the pore size increases in proportion to the phenol resin size, which indicates that the pore structure can be controlled by changing the raw material particle size.
Nb-Si-B alloys with Nb-rich compositions are fabricated by spark plasma sintering for high-temperature structural applications. Three compositions are selected: 75 at% Nb (Nb0.7), 82 at% Nb (Nb1.5), and 88 at% Nb (Nb3), the atomic ratio of Si to B being 2. The microstructures of the prepared alloys are composed of Nb and T2 phases. The T2 phase is an intermetallic compound with a stoichiometry of Nb5Si3-xBx (0 ≤ x ≤ 2). In some previous studies, Nb-Si- B alloys have been prepared by spark plasma sintering (SPS) using Nb and T2 powders (SPS 1). In the present work, the same alloys are prepared by the SPS process (SPS 2) using Nb powders and hypereutectic alloy powders with composition 67at%Nb-22at%Si-11at%B (Nb67). The Nb67 alloy powders comprise T2 and eutectic (T2 + Nb) phases. The microstructures and hardness of the samples prepared in the present work have been compared with those previously reported; the samples prepared in this study exhibit finer and more uniform microstructures and higher hardness.
A powder mixture of 70 wt% Al2O3 and 30 wt% hydroxyapatite (HA) is sintered at 1300 ℃ or 1350 ℃ for 2 h at normal pressure. An MgF2-added composition to make HA into fluorapatite (FA) is also prepared for comparison. The samples without MgF2 show α & β-tricalcium phosphates (TCPs) and Al2O3 phases with no HA at either of the sintering temperatures. In the case of 1,350 ℃, a CaAl4O7 phase is also found. Densification values are 69 and 78 %, and strengths are 156 and 104MPa for 1,300 and 1,350 ℃, respectively. Because the decomposition of HA produces a H2O vapor, fewer large pores of 5-6 μm form at 1,300 ℃. The MgF2-added samples show FA and Al2O3 phases with no TCP. Densification values are 79 and 87%, and strengths are 104 and 143 MPa for 1,300 and 1,350 ℃, respectively. No large pores are observed, and the grain size of FA (1-2 μm) is bigger than that of TCP (0.7 μm ≥) in the samples without MgF2. The resulting TCP/Al2O3 and FA/Al2O3 composites fabricated in situ exhibit strengths 6-10 times higher than monolithic TCP and HA.
Metallic tantalum powder is manufactured by reducing tantalum oxide (Ta2O5) with magnesium gas at 1,073–1,223 K in a reactor under argon gas. The high thermodynamic stability of magnesium oxide makes the reduction reaction from tantalum oxide into tantalum powder possible. The microstructure after the reduction reaction has the form of a mixture of tantalum and magnesium oxide, and the latter could be entirely eliminated by dissolving in weak hydrochloric acid. The powder size in SEM microstructure for the tantalum powder increases after acid leaching in the range of 50–300 nm, and its internal crystallite sizes are observed to be 11.5 to 24.7 nm with increasing reduction temperatures. Moreover, the optimized reduction temperature is found to be 1,173 K as the minimum oxygen concentration is approximately 1.3 wt.%.
W-10 wt% Ti alloys that have a homogeneous microstructure are prepared by thermal decomposition of WO3-TiH2 powder mixtures and spark plasma sintering. The reduction and dehydrogenation behavior of WO3 and TiH2 are analyzed by temperature programmed reduction and a thermogravimetric method, respectively. The X-ray diffraction analysis of the powder mixture, heat-treated in an argon atmosphere, shows W- oxides and TiO2 peaks. Conversely, the powder mixtures heated in a hydrogen atmosphere are composed of W, WO2 and TiO2 phases at 600 ℃ and W and W-rich β phases at 800 ℃. The densified specimen by spark plasma sintering at 1500 ℃ in a vacuum using hydrogen-reduced WO3-TiH2 powder mixtures shows a Vickers hardness value of 4.6 GPa and a homogeneous microstructure with pure W, β and Ti phases. The phase evolution dependent on the atmosphere and temperature is explained by the thermal decomposition and reaction behavior of WO3 and TiH2.
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 300oC shows Cu, MoO3, and Cu2MoO5 phases. In contrast, the powder mixture heated at 400oC 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 700oC, shows the dispersion of nano-sized Cu agglomerates on the surface of Mo powders.
This study focuses on the fabrication of a WC/Co composite powder from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere for the recycling of WC/Co hardmetal. Mixed powders are manufactured by mechanically milling the oxide powder of WC-13 wt% Co hardmetal scrap and carbon black with varying powder/ball weight ratios. The oxide powder of WC-13 wt% Co hardmetal scrap consists of WO3 and CoWO4. The mixed powder mechanically milled at a lower powder/ball weight ratio (high mechanical milling energy) has a more rapid carbothermal reduction reaction in the formation of WC and Co phases compared with that mechanically milled at a higher powder/ball weight ratio (lower mechanical milling energy). The WC/Co composite powder is fabricated at 900℃ for 6 h from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere. The fabricated WC/Co composite powder has a particle size of approximately 0.25-0.5 μm.
SiAlON-based ceramics are some of the most typical ceramic materials used as cutting tools for HRSA(Heat Resistant Super-Alloys). SiAlON can be fabricated using ceramic processing, such as mixing, granulation, compaction, and sintering. Spray drying is a widely-used method for producing a granular powder of controlled morphology and size with flowability. In this study, we report a systematic investigation aimed at optimizing spherical granule morphology by controlling spray-drying parameters such as gas flow and feed rate. Before spray drying, the viscosities of the raw material slurries were also optimized with the amount of dispersant added.
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 WO2.9, 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℃, 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℃ 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.
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.
ZnS powder was synthesized using a relatively facile and convenient glycothermal method at various reaction temperatures. ZnS was successfully synthesized at temperatures as low as 125 oC using zinc acetate and thiourea as raw materials, and diethylene glycol as the solvent. No mineralizers or precipitation processes were used in the fabrication, which suggests that the spherical ZnS powders were directly prepared in the glycothermal method. The phase composition, morphology, and optical properties of the prepared ZnS powders were characterized using XRD, FE-SEM, and UV-vis measurements. The prepared ZnS powders had a zinc blende structure and showed average primary particles with diameters of approximately 20~30 nm, calculated from the XRD peak width. All of the powders consisted of aggregated secondary powders with spherical morphology and a size of approximately 0.1~0.5 μm; these powders contained many small primary nanopowders. The as-prepared ZnS exhibited strong photo absorption in the UV region, and a red-shift in the optical absorption spectra due to the improvement in powder size and crystallinity with increasing reaction temperature. The effects of the reaction temperature on the photocatalytic properties of the ZnS powders were investigated. The photocatalytic properties of the assynthesized ZnS powders were evaluated according to the removal degree of methyl orange (MO) under UV irradiation (λ = 365 nm). It was found that the ZnS powder prepared at above 175 oC exhibited the highest photocatalytic degradation, with nearly 95 % of MO decomposed through the mediation of photo-generated hydroxyl radicals after irradiation for 60 min. These results suggest that the ZnS powders could potentially be applicable as photocatalysts for the efficient degradation of organic pollutants.
Fe3O4/Fe/graphene nanocomposite powder is synthesized by electrical wire explosion of Fe wire and dispersed graphene in deionized water at room temperature. The structural and electrochemical characteristics of the powder are characterized by the field-emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy, field-emission transmission electron microscopy, cyclic voltammetry, and galvanometric discharge-charge method. For comparison, Fe3O4/Fe nanocomposites are fabricated under the same conditions. The Fe3O4/Fe nanocomposite particles, around 15-30 nm in size, are highly encapsulated in a graphene matrix. The Fe3O4/Fe/graphene nanocomposite powder exhibits a high initial charge specific capacity of 878 mA/g and a high capacity retention of 91% (798 mA/g) after 50 cycles. The good electrochemical performance of the Fe3O4/Fe/graphene nanocomposite powder is clearly established by comparison of the results with those obtained for Fe3O4/Fe nanocomposite powder and is attributed to alleviation of volume change, good distribution of electrode active materials, and improved electrical conductivity upon the addition of graphene.