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.
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.
MgB2 bulk superconductors are synthesized by the solid state reaction of (MgB4+xMg) precursors withexcessive Mg compositions (x=1.0, 1.4, 2.0 and 2.4). The MgB4 precursors are synthesized using (Mg+B) powders. Thesecondary phases (MgB4 and MgO) present in the synthesized MgB4 are removed by HNO3 leaching. It is found thatthe formation reaction of MgB2 is accelerated when Mg excessive compositions are used. The magnetization curves ofMg1+xB2 samples show that the transition from the normal state to the superconducting state of the Mg excessive sam-ples with x=0.5 and x=0.7 are sharper than that of MgB2. The highest Jc-B curve at 5 K and 20 K is achieved forx=0.5. Further addition of Mg decreases the Jc owing to the formation of more pores in the MgB2 matrix and smallervolume fraction of MgB2.
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.
The effect of Al content on the processing of reaction-bonded Al2O3 (RBAO) ceramics using 40v/o ~ 80v/o Al- Zn-Mg alloy powder was studied in order to improve traditional RBAO ceramic processes that use ~ 40v/o pure Al powder. The influence of high Al content in starting Al2O3-Al alloy powder mixtures on its particulate characteristics, reaction-bonding, microstructure, physical and mechanical properties was revealed. Starting Al2O3-Al alloy powder mixtures with 40v/o ~ 80v/o Al alloy powder were milled, reaction-bonded, post-sintered, and characterized. With an increasing Al alloy content, the milling efficiency of Al alloy powder was lowered, resulting in a larger particle size after milling. However, in spite of the larger particle size of Al alloy powder, the oxidation, i.e., reaction-bonding, of the Al alloy was successfully completed via solid and liquid state oxidation, in which the activation energy of the oxidation was nearly the same regardless of Al alloy content. After reaction-bonding and post-sintering at 1600 oC, RBAO ceramics from 80v/o Al alloy content showed a relative density of ~97% and a flexural strength of 251 MPa compared to ~ 96% and 353 MPa for RBAO ceramics from 40v/o Al alloy content, respectively. The lower flexural strength at 80v/o Al alloy content was due to the weak spinel phase that formed from Zn, Mg alloying elements in Al.
Fabrication of reaction-bonded Al2O3 (RBAO) ceramics using Al-Zn-Mg alloy powder was studied in order to improve traditional RBAO ceramic processing using Al powder. The influence on reaction-bonding and microstructure, as well as on physical and mechanical properties, of the particulate characteristics of the Al2O3-Al alloy powder mixtures after milling, was revealed. Variation of the particulate characteristics of this Al2O3-Al alloy powder mixture with milling time was reported previously. To start, the Al2O3-Al alloy powder mixture was milled, reaction-bonded, post-sintered, and characterized. During reaction-bonding of the Al2O3-Al alloy powder mixture compacts, oxidation of the Al alloy took place in two stages, that is, there was solid- and liquid-state oxidation of the Al alloy. The solid-state oxidation exhibited strong dependence on the density of surface defects on the Al-alloy particles formed during milling. Higher milling efficiency resulted in less participation of the Al alloy in reaction-bonding. This was because of its consumption by chemical reactions during milling, and subsequent powder handling, and could be rather harmful in the case of over-milling. In contrast to very little dependence of oxidation of the Al alloy on its particle size after milling, the relative density, microstructure, and flexural strength were strongly dependent on particle size after milling (i.e., on milling efficiency). The relative density and 4-point flexural strength of the RBAO ceramics in this study were ~98% and ~365 MPa, respectively, after post-sintering at 1,600˚C.
The milling and particulate characteristics of Al alloy-Al2O3 powder mixtures for a reaction-bonded Al2O3 (RBAO) process were studied. A commercially available prealloyed Al powder with Zn, Mg, Cu and Cr alloying elements (7475 series) was mixed with a calcined sinter-active Al2O3 powder and then milled in centrifugal milling equipment for ~48 hrs. The Al alloy-Al2O3 powder mixtures after milling were characterized and evaluated in various ways to reveal their particulate characteristics during milling. The milling efficiency of the Al alloy increased with a longer milling time. Comminution of the Al alloy particles started with its elongation, showing a high aspect ratio. With a longer milling time, the elongated Al alloy particle changed in terms of its shape and size, becoming equiaxially fine particles. Regardless of the milling efficiency of the Al alloy particles, all of the Al alloy particles repeatedly experienced strong plastic deformation during milling, giving rise to higher density of surface defects, such as microcracks, and leading to higher residual microstress within the Al alloy particles. The chemical reactions, oxidation behavior and hydration behavior of the Al alloy particles and the hydrolysis characteristics of their reaction with the environment were also observed during the milling process and during the subsequent powder handling steps.
TiB2-reinforced iron matrix composite (Fe-TiB2) powder was in-situ fabricated from titanium hydride (TiH2) and iron boride (FeB) powders by the mechanical activation and a subsequent reaction. Phase formation of the composite powder was identified by X-ray diffraction (XRD). The morphology and phase composition were observed and measured by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The results showed that TiB2 particles formed in nanoscale were uniformly distributed in Fe matrix. Fe2B phase existed due to an incomplete reaction of Ti and FeB. Effect of milling process and synthesis temperature on the formation of composite were discussed.
GdBa2Cu3O7-y(Gd123) powders were synthesized by the solid-state reaction method using Gd2O3 (99.9% purity), BaCO3 (99.75%) and CuO (99.9%) powders. The synthesized Gd123 powder and the Gd123 powder with Gd2O3 addition (Gd1.5Ba2Cu3O7-y(Gd1.5)) were used as raw powders for the fabrication of Gd123 bulk superconductors. The Gd123 and Gd1.5 bulk superconductors were fabricated by sintering or a top-seeded melt growth (TSMG) process. The superconducting transition temperature (Tc,onset) of the sintered Gd123 was 93 K and the transition width was as large as 20 K. The Tc,onset of the TSMG processed Gd123 was 82 K and the transition width was also as large as 12 K. The critical current density (Jc) at 77 K and 0 T of the sintered Gd123 and TSMG processed Gd123 were as low as a few hundreds A/cm2. The addition of 0.25 mole Gd2O3 and 1 wt.% CeO2 to Gd123 enhanced the Tc, Jc and magnetic flux density (H) of the TSMG processed Gd123 sample owing to the formation of the superconducting phase with high flux pinning capability. The Tc of the TSMG processed Gd1.5 was 92 K and the transition width was 1 K. The Jcs at 77 K (0 T and 2 T) were 3.2×104 A/cm2 and 2.5×104 A/cm2, respectively. The H at 77 K of the TSMG-processed Gd1.5 was 1.96 kG, which is 54% of the applied magnetic field (3.45 kG).
(Y123) powders for the fabrication of bulk superconductors were synthesized by the powder reaction method using (99.9% purity), (99.75%) and CuO (99.9%) powders. The raw powders were weighed to the cation ratio of Y:Ba:Cu=1:2:3, mixed and calcined at in air with intermediate repeated crushing steps. It was found that the formation of Y123 powder was more sensitive to reaction temperature than reaction time. The calcined Y123 powder and a mixture of (Y123 + 0.25 mole + 1 wt.% , (Y1.5)) were used as raw powders for the fabrication of poly-grain or single grain superconductors. The superconducting transition temperature () of the sintered Y123 sample was 91 K and the transition width was as large as 11 K, whereas the of the melt-grown Y1.5 sample was 90.5 K and the transition width was 3.5 K. The critical current density () at 77 K and 0 T of the sintered Y123 was 700 , whereas the of the top-seeded melt growth (TSMG) processed Y1.5 sample was . The magnetic flux density (H) at 77 K of the TSMG-processed Y123 and Y1.5 sample showed the 0.53 kG and 2.45 kG, respectively, which are 15% and 71% of the applied magnetic field of 3.5 kG. The high H value of the TSMG-processed Y1.5 sample is attributed to the formation of the larger superconducting grain with fine Y211 dispersion.
Fe-TiC composite powder was fabricated via two steps. The first step was a high-energy milling of FeO and carbon powders followed by heat treatment for reduction to obtain a (Fe+C) powder mixture. The optimal condition for high-energy milling was 500 rpm for 1h, which had been determined by a series of preliminary experiment. Reduction heat-treatment was carried out at for 1h in flowing argon gas atmosphere. Reduced powder mixture was investigated by X-ray Diffraction (XRD), Field Emission-Scanning Electron Microscopy (FE-SEM) and Laser Particle Size Analyser (LPSA). The second step was a high-energy milling of (Fe+C) powder mixture and additional powder, and subsequent in-situ synthesis of TiC particulate in Fe matrix through a reaction of carbon and Ti. High-energy milling was carried out at 500 rpm for 1 h. Heat treatment for reaction synthesis was carried out at for 1 h in flowing argon gas atmosphere. X-ray diffraction (XRD) results of the fabricated Fe-TiC composite powder showed that only TiC and Fe phases exist. Results from FE-SEM observation and Energy-Dispersive X-ray Spectros-copy (EDS) revealed that TiC phase exists uniformly dispersed in the Fe matrix in a form of particulate with a size of submicron.
Recovery of copper powder from copper chloride solution used in leaching process was carried out using a cementation method. Cementation is a simple and economical process, necessitating less energy compared with other recovery methods. Cementation utilizes significant difference in standard reduction potential between copper and iron under standard condition. In the present research, Cementation process variables of temperature, time, and added amount of iron scraps were optimized by using design of experiment method and individual effects on yield and efficiency of copper powder recovery were investigated using bench-scale cementation reaction system. Copper powders thus obtained from cementation process were further characterized using various analytical tools such as XRF, SEM-EDS and laser diffraction and scattering methods. Cementation process necessitated further purification of recovered copper powders and centrifugal separation method was employed, which successfully yielded copper powders of more than 99.65% purity and average in size.
Nanocrystalline powder could be synthesized by solid-state reaction using the mixture which was prepared by a high energy milling process in a bead mill for and nanocrystalline powders mixture. Effect of the milling time on the powder characteristic of the synthesized powder was investigated. Nanocrystalline with a particle size of 50 nm was obtained at . High tetragonal powder with a tetragonality(=c/a) of 1.009 and a specific surface area of was acquired after heat-treatment at for 2 h. High energy ball milling was effective in decreasing the reaction temperature and increasing the tetragonality.
In chemistry, the study of sonochemistry is concerned with understanding the effect of sonic waves and wave properties on chemical systems. In the area of chemical kinetics, it has been observed that ultrasound can greatly enhance chemical reactivity in a number of systems by as much as a million-fold. Nano-technology is a super microscopic technology in which structures of 100 nanometers or smaller can be investigated. This technology has been used to develop TiO2 materials and TiO2 devices of that size. Thus far, electrochemistry methods and photochemistry methods have generally been used to create TiO2 nano-size particles. However, these methods are complicated and create pollutants as a by-product. In the present study, nano-scale silver particles (5 nm) were prepared in a sonochemistry method. Sonochemistry deals with mechanical energy that is provided by the collapse of cavitation bubbles that form in solutions during exposure to ultrasound. TiO2 powders 25 nm in size doped with Ag were formed using an ultrasonic sound technique. The experimental results showed the high possibility of removing pollution through the action of a photocatalyst. This powder synthesis technique can be considered as an environmentally friendly powder-forming processing owing to its energy saving characteristics.
High-energy mechanical milling (HEMM) and sintering into Al-Mg alloy melt were employed tofabricate an Al alloy matrix composite reinforced with submicron and micron sized Al2O3 particles. Al-basedmetal matrix composite (MMC) reinforced with submicron and micron sized Al2O3 particles was successfullyfabricated by sintering at 1000oC for 2h into Al-Mg alloy melt, which used high energy mechanical milled Al-SiO2-CuO-ZnO composite powders. Submicron/micron-sized Al2O3 particles and eutectic Si were formed by in situdisplacement reaction between Al, SiO2, CuO, and ZnO during sintering for 2h into Al-Mg alloy melt and werehomogeneously distributed in the Al-Si-(Zn, Cu) matrix. The refined grains and homogeneously distributedsubmicron/micron-sized Al2O3 particles had good interfacial adhesive, which gives good wear resistance withhigher hardness.
In the present study, the focus is on the synthesis of nanosized WC powder by the chemical vapor condensation proces. The synthesized W-C system powder by the CVC process shows W2C, W, WO3 phases and can not shows WC phase. After recarburization heat treatment under mixture gas atmosphere of argon and hydrogen gases, the synthesized W-C system powder fully transformed to the pure WC. The synthesized WC powder after recarburization heat treatment has an average particle size of 20 nm. The nano-sized WC powder can be prepared by the combination of the CVC process and heat treatment methods.