Lithium (Li) is a key resource driving the rapid growth of the electric vehicle industry globally, with demand and prices continually on the rise. To address the limited reserves of major lithium sources such as rock and brine, research is underway on seawater Li extraction using electrodialysis and Li-ion selective membranes. Lithium lanthanum titanate (LLTO), an oxide solid electrolyte for all-solid-state batteries, is a promising Li-ion selective membrane. An important factor in enhancing its performance is employing the powder synthesis process. In this study, the LLTO powder is prepared using two synthesis methods: sol-gel reaction (SGR) and solid-state reaction (SSR). Additionally, the powder size and uniformity are compared, which are indices related to membrane performance. X-ray diffraction and scanning electron microscopy are employed for determining characterization, with crystallite size analysis through the full width at half maximum parameter for the powders prepared using the two synthetic methods. The findings reveal that the powder SGR-synthesized powder exhibits smaller and more uniform characteristics (0.68 times smaller crystal size) than its SSR counterpart. This discovery lays the groundwork for optimizing the powder manufacturing process of LLTO membranes, making them more suitable for various applications, including manufacturing high-performance membranes or mass production of membranes.

In this study, we evaluated the effects of acid leaching on the properties of Cr powder synthesized using self-propagating high-temperature synthesis (SHS). Cr powder was synthesized from a mixture of Cr2O3 and magnesium (Mg) powders using the SHS Process, and the byproducts after the reaction were removed using acid leaching. The properties of the recovered Cr powder were analyzed via X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), particle size analysis (PSA), and oxygen content analysis. The results show that perfect selective leaching of Cr is challenging because of various factors such as incomplete reaction, reaction kinetics, the presence of impurities, and incompatibility between the acid and metal mixture. Therefore, this study provides essential information on the properties under acidic conditions during the production of high-quality Cr powder using a self-propagating high-temperature synthesis method.

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.

W2C is synthesized through a reaction-sintering process from an ultrafine-W and WC powder mixture using spark plasma sintering (SPS). The effect of various parameters, such as W:WC molar ratio, sintering temperature, and sintering time, on the synthesis behavior of W2C is investigated through X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) analysis of the microstructure, and final sintered density. Further, the etching properties of a W2C specimen are analyzed. A W2C sintered specimen with a particle size of 2.0 μm and a relative density over 98% could be obtained from a W-WC powder mixture with 55 mol%, after SPS at 1700℃ for 20 min under a pressure of 50 MPa. The sample etching rate is similar to that of SiC. Based on X-ray photoelectron spectroscopy (XPS) analysis, it is confirmed that fluorocarbon-based layers such as C-F and C-F2 with lower etch rates are also formed.

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.

In this work, ultra-fine calcium oxide (CaO) powder derived from eggshells is used as the starting material to synthesize mineral trioxide aggregate (MTA). The prepared CaO powder is confirmed to have an average particle size of 500 nm. MTAs are synthesized with three types of fine CaO-based powders, namely, tricalcium silicate (C3S), dicalcium silicate (C2S), and tricalcium aluminate (C3A). The synthesis behavior of C3S, C2S and C3A with ultra-fine CaO powder and the effects of C3A content and curing time on the properties of MTA are investigated. The characteristics of the synthesized MTA powders are examined by X-ray diffraction (XRD), field emission-scanning electron microscope (FE-SEM), and a universal testing machine (UTM). The microstructure and compressive strength characteristics of the synthesized MTA powders are strongly dependent on the C3A wt.% and curing time. Furthermore, MTA with 5 wt.% C3A is found to increase the compressive strength and shorten the curing time.

Despite numerous advances in the preparation and use of GaN, and many leading-edge applications in lighting technologies, the preparation of high-quality GaN powder remains a challenge. Ammonolytic preparations of polycrystalline GaN have been studied using various precursors, but all were time-consuming and required high temperatures. In this study, an efficient and low-temperature method to synthesize high-purity hexagonal GaN powder is developed using sub-micron Ga2O3 powder as a starting material. The sub-micron Ga2O3 powder was prepared by an ultrasonic spray pyrolysis process. The GaN powder is synthesized from the sub-micron Ga2O3 powder through a nitridation treatment in an NH3 flow at 800℃. The characteristics of the synthesized powder are systematically examined by X-ray diffraction, scanning and transmission electron microscopy, and UV-vis spectrophotometer.

One-dimensional rutile TiO2 is an important inorganic compound with applicability in sensors, solar cells, and Li-based batteries. However, conventional synthesis methods for TiO2 nanowires are complicated and entail risks of environmental contamination. In this work, we report the growth of TiO2 nanowires on a Ti alloy powder (Ti-6wt%Al- 4wt%V, Ti64) using simple thermal oxidation under a limited supply of O2. The optimum condition for TiO2 nanowire synthesis is studied for variables including temperature, time, and pressure. TiO2 nanowires of ~5 μm in length and 100 nm in thickness are richly synthesized under the optimum condition with single-crystalline rutile phases. The formation of TiO2 nanowires is greatly influenced by synthesis temperature and pressure. The synthesized TiO2 nanowires are characterized using field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HR-TEM).

A Nanosized WO3 and CuO powder mixture is prepared using novel high-energy ball milling in a bead mill to obtain a W-Cu nanocomposite powder, and the effect of milling time on the structural characteristics of WO3-CuO powder mixtures is investigated. The results show that the ball-milled WO3-CuO powder mixture reaches at steady state after 10 h milling, characterized by the uniform and narrow particle size distribution with primary crystalline sizes below 50 nm, a specific surface area of 37 m2/g, and powder mean particle size (D50) of 0.57 μm. The WO3-CuO powder mixtures milled for 10 h are heat-treated at different temperatures in H2 atmosphere to produce W-Cu powder. The XRD results shows that both the WO3 and CuO phases can be reduced to W and Cu phases at temperatures over 700oC. The reduced W-Cu nanocomposite powder exhibits excellent sinterability, and the ultrafine W-Cu composite can be obtained by the Cu liquid phase sintering process.

An optimum route to fabricate oxide dispersion strengthened ferritic superalloy with desired microstructure was investigated. Two methods of high energy ball milling or polymeric additive solution route for developing a uniform dispersion of Y2O3 particles in Fe-Cr-Al-Ti alloy powders were compared on the basis of the resulting microstructures. Microstructural observation revealed that the crystalline size of Fe decreased with increases in milling time, to values of about 15-20 nm, and that an FeCr alloy phase was formed. SEM and TEM analyses of the alloy powders fabricated by solution route using yttrium nitrate and polyvinyl alcohol showed that the nano-sized Y-oxide particles were well distributed in the Fe based alloy powders. The prepared powders were sintered at 1000 and 1100 oC for 30 min in vacuum. The sintered specimen with heat treatment before spark plasma sintering at 1100 oC showed a more homogeneous microstructure. In the case of sintering at 1100 oC, the alloys exhibited densified microstructure and the formation of large reaction phases due to oxidation of Al.

Photoelectron-hole separation efficiency plays an important role in the enhancement of the photocatalytic activity of photocatalysts towards the degradation of organic molecules. In this study, TiO2/TiOF2 heterostructured composite powders with suitable band structures, which structures are able to separate photoelectron-hole pairs, have been synthesized using a simple and versatile ultrasonic spray pyrolysis process. In addition, their phase volume fractions have been controlled by varying the pyrolysis temperature from 400 oC to 800 oC. The structural and optical properties of the synthesized powders have been characterized by X-ray diffraction, scanning electronic microscopy and UV-vis spectroscopy. The powder with a phase volume ratio close to 1, compared with single TiOF2 and other composite powders with different phase volume fractions, was found to have superior photocatalytic activity for the degradation of rhodamine B. This result shows that the TiO2/TiOF2 heterostructure promotes the separation of the photoinduced electrons and holes and that this powder can be applicable to environmental cleaning applications.

TiOF2, which has remarkable electrochemical and optical properties, is used in various applications such as Li-ion batteries, electrochemical displays, and photocatalysts. In addition, it is possible to utilize the template which is allowed to synthesize fluorine doped TiO2 powders with hollow or faceted structures. However, common synthesis methods of TiOF2 powders have some disadvantages such as the use of expensive and harmful precursors and batchtype processes with a limited production scale. In this study, we report a synthetic route for preparing TiOF2 powders by using an inexpensive and harmless precursor and a continuous ultrasonic spray pyrolysis process under a controlled atmosphere to address the aforementioned problems. The synthesized powder has an average size of 1 μm, a spherical shape, a pure TiOF2 phase, and exhibits a band-gap energy of 3.2 eV.

A Ni-Ti-B alloy powder prepared by mechanical alloying (MA) of individual Ni, Ti, and B components is examined with the aim of elucidating the phase transitions and crystallization during heat treatment. Ti and B atoms penetrating into the Ni lattice result in a Ni (Ti, B) solid solution and an amorphous phase. Differential thermal analysis (DTA) reveals peaks related to the decomposition of the metastable Ni (Ti, B) solid solution and the separation of equilibrium Ni3Ti, TiB2, and τ-Ni20Ti3B6 phases. The exothermal effects in the DTA curves move to lower temperatures with increasing milling time. The formation of a TiB2 phase by annealing indicates that the mechanochemical reaction of the Ni-Ti-B alloy does not comply with the alloy composition in the ternary phase diagram, and Ti-B bonds are found to be more preferable than Ni-B bonds.

Electrochemical synthesis was employed to prepare a novel hydroxyapatite/graphene (HAP/ Gr) composite powder suitable for medical applications as a hard tissue implant (scaffold). The synthesis was performed in a homogeneous dispersion containing Na2H2EDTA·2H2O, NaH2PO4 and CaCl2 with a Ca/EDTA/PO4 3− concentration ratio of 0.25/0.25/0.15M, along with 0.01 wt% added graphene nanosheets, at a current density of 137 mA cm−2 and pH value of 9.0. The field emission scanning electron microscopy and transmission electron microscopy observations of the composite HAP/Gr powder indicated that nanosized hydroxyapatite particles were uniformly placed in the graphene overlay. Raman spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction confirmed graphene incorporation in the HAP/Gr powder. The electrochemically prepared HAP/Gr composite powder exhibited slight antibacterial effect against the growth of the bacterial strain Staphylococcus aureus.

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).

The synthesis of NiTi alloy powders by hydrogen reduction and dehydrogenation process of NiO and TiH2 powder mixtures is investigated. Mixtures of NiO and TiH2 powders are prepared by simple mixing for 1 h or ball milling for 24 h. Simple-mixed mixture shows that fine NiO particles are homogeneously coated on the surface of TiH2 powders, whereas ball milled one exhibits the morphology with mixing of fine NiO and TiH2 particles. Thermogravimetric analysis in hydrogen atmosphere reveals that the NiO and TiH2 phase are changed to metallic Ni and Ti in the temperature range of 260 to 290oC and 553 to 639oC, respectively. In the simple-mixed powders by heat-up to 700oC, agglomerates with solid particles and solidified liquid phase are observed, and the size of agglomerates is increased at 1000oC. From the XRD analysis, the presence of liquid phase is explained by the formation and melting of NiTi2 intermetallic compound due to an exothermic reaction between Ni and Ti. The simple-mixed powders, heated to 1000oC, lead to the formation of NiTi phase but additional Ni-, Ti-rich and Ti-oxide phases. In contrast, the microstructure of ball-milled powders is characterized by the neck-grown particles, forming Ni3Ti, Ti-oxide and unreacted Ni phase.

투명 전도성 산화물로서 알루미늄과 붕소가 함께 도핑된 아연산화물(AZOB)이 900℃에서 분무 열분해법에 의해 제조되었다. 얻어진 마이크론 크기의 AZOB 분말은 알루미늄, 붕소 및 아연의 수용액으로부터 얻어진다. 분무 열분해로 얻어진 마이크론 크기의 AZOB 분말은 700℃에서 두 시간동안의 후 소성 과정과 24 시간 동안의 볼 밀링을 통해 나노 크기의 AZOB으로 변환된다. AZOB을 구성하는 일차 입자의 크기를 Debye-Scherrer 식에 의해 계산하였고 압축된 AZOB 펠렛의 표면 저항을 측정하였다.

마이크론 크기를 가지는 ITO(indium tin oxide) 입자들은 인듐과 틴의 수용성 전구체들과 유기 첨가제를 분무 열분해하여 얻었다. 유기 첨가제로서는 에틸렌글리콜과 시트르산을 이용하였다. 분무 열분해 시 에틸렌글리콜과 시트르산과 같은 유기첨가제를 첨가하지 않고 얻어진 ITO 입자들은 구형이며 속이 꽉찬 형태를 가지는데 비해 유기 첨가제를 첨가하여 분무 열분해를 하면 얻어지는 ITO 입자들은 유기 첨가제의 양이 증가 할수록 껍질이 얇고 다공성이 증대된 중공 입자가 얻어진다. 유기첨가제를 첨가하지 않고 분무 열분해를 통해 얻어지는 마이크론 크기를 가지는 ITO는 700℃에서 두 시간 동안의 후소성과 24 시간동안의 습식 볼밀링에 의해 나노 크기의 ITO로 전환되지 않으나, 유기첨가제를 첨가하고 분무 열분해를 통해 얻어지는 마이크론 크기를 가지는 ITO는 700℃에서 두 시간 동안의 후소성과 24 시간 동안의 습식 볼밀링에 의해 나노 크기의 ITO로 쉽게 전환되었다. 응집된 나노 크기의 ITO의 일차 입자의 크기를 Debye-Scherrer 식에 의해 계산하였고 ITO 입자를 압축하여 만든 펠렛의 표면저항을 측정하였다.

In this research, a precipitation method was used to synthesize β-Ga2O3 powders with various particle morphologies and sizes under varying precipitation conditions, such as gallium nitrate concentration, pH, and aging temperature, using ammonium hydroxide and ammonium carbonate as precipitants. The obtained powders were characterized in detail by XRD, SEM, FT-IR, and TG-DSC. From the TG-DSC result, GaOOH phase was transformed to β-Ga2O3 at around 742˚C, and weight loss percent was about 14 % when NH4OH was used as a precipitant. Also, β-Ga2O3 formed at 749˚C and weight loss percent was about 15 % when (NH)2CO3 was used as a precipitant. XRD results showed that the obtained Ga2O3 had pure monoclinic phase in both cases. When (NH)2CO3 was used as a precipitant, the particle shape changed and became irregular. The range of particle size was about 500nm-4μm based on various concentrations of gallium nitrate solution with NH4OH. The particle size was increased from 1-2μm to 3-4μm and particle shape was changed from spherical to bar type by increasing aging temperature over 80˚C.