• Journal of the Korean Ceramic Society
• /
• v.24 no.3
• /
• pp.235-242
• /
• 1987

This study was about to make zirconia ceramics with yttria, using spraying precipitation method for the purpose of powder control. The powder properties and the characterization of sintered body, were studied. As the results, 1. The synthesized powder had homogeneity of spherical shape, and average particle size was 2-3 um. 2. Crystallization temperature increased with Y2O3 content. 3. Apparent density of sintered body (fired above 1500$^{\circ}C$) was higher than 98% of theoretical value in 3 mol% Y2O3 content. 4. High KIC values(19kg/㎣/2) in 3 mol % Y2O3 content resulted from sintering density increasement.

• Transactions of the Korean hydrogen and new energy society
• /
• v.23 no.6
• /
• pp.670-677
• /
• 2012

Perovskite-type oxides such as doped barium zirconate ($BaZrO_3$) show high proton conductivity and chemical stability when they are exposed to hydrogen and water vapour containing atmospheres, thus it can be applicable to the hydrogen separation and the fuel cell electrolyte membranes. However the high temperature ($1700-1800^{\circ}C$) and long sintering times (24h) are generally required to prepare the fully densified $BaZrO_3$ pellets. These sintering conditions lead to the limitation of the grain size growth and the degradation of conductivity due to the acceleration of BaO evaporation at $1200^{\circ}C$. Here we demonstrate NiO-doped $BaZr_{0.85}Y_{0.15}O_{3-{\delta}}$ with lower calcination and sintering temperature, less experimental procedure and lower process cost than the conventional mixing method. The stoichiometry of $BaZr_{0.85}Y_{0.15}O_{3-{\delta}}$ was optimized by the control of excess amount of Ba (5mol%) to minimized BaO evaporation. We found that the crystal size of NiO-doped $BaZr_{0.85}Y_{0.15}O_{3-{\delta}}$ was increased with increase of calcination temperature from XRD analysis. NiO-doped $BaZr_{0.85}Y_{0.15}O_{3-{\delta}}$ powder was calcined at $1000^{\circ}C$ for 12h when its showed the highest conductivity of $3.3{\times}10^{-2}s/cm$.

• Korean Journal of Materials Research
• /
• v.22 no.5
• /
• pp.220-226
• /
• 2012

Pure zirconia and $x$ mol% calcia partially stabilized zirconia ($x$ = 1.5, 3, and 8) nanopowders were synthesized by hydrothermal method with various reaction temperatures for 24 hrs. The precipitated precursor of pure zirconia and $x$ mol% calcia doped zirconia was prepared by adding $NH_4OH$ to starting solutions; resulting sample was then put into an autoclave reactor. The optimal experimental conditions, such as reaction temperatures and times and amounts of stabilizer CaO, were carefully studied. The synthesized $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5, 3, and 8) powders were characterized by XRD, SEM, TG-DTA, and Raman spectroscopy. When the hydrothermal temperature was as low as $160^{\circ}C$, pure $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5 and 3) powders were identified as a mixture of monoclinic and tetragonal phases. However, a stable tetragonal phase of zirconia was observed in the 8 mol% calcia doped zirconia nanopowder at hydrothermal temperature above $160^{\circ}C$. To observe the phase transition, the 3 mol% CaO-$ZrO_2$ and 8 mol% CaO-$ZrO_2$ nanopowders were heat treated from 600 to $1000^{\circ}C$ for 2h. The 3 mol% CaO-$ZrO_2$ heat treated at above $1000^{\circ}C$ was found to undergo a complete phase transition from mixture phase to monoclinic phase. However, the 8 mol% calcia doped zirconia appeared in the stable tetragonal phase after heat treatment. The result of this study therefore should be considered as the preparation of 8 mol% CaO-$ZrO_2$ nanopowders via the hydrothermal method.

• Journal of the Korean Ceramic Society
• /
• v.24 no.6
• /
• pp.586-592
• /
• 1987

The role of the strain energy and phase stability in the diffuse phase transition have been investigated in the highly disordered solid solution, (Pb1-xBax)(Zr0.4Ti0.6)O3 (0.2 x 0.4). X-ray diffraction analysis indicates that tetragonality (c/a) decreases with the increasing Ba content. Also as the Ba content increases, phase transition becomes more diffuse and at the same time dielectric relaxation as a function of measured frequencies in the 1KHz-10MHz range occurs very pronouncedly. In the Ba content range, 0.2 x 0.35, hysteresis loops are routinely observed and the loop is observed to narrow shape as the Ba content increases but becomes very slim at 40mol% Ba content. Moreover thermal analysis shows that there is no abrupt change in the thermal expansion coefficient below the apparent transition temperature at which dielectric constant becomes maximum. From the above results, it has been concluded that creation of the strain energy due to the distorthion that occurred during the phase transition suppresses diffuse phase transition.

• Transactions on Electrical and Electronic Materials
• /
• v.4 no.2
• /
• pp.24-28
• /
• 2003

(Ba,Sr,Ca)TiO$_3$ powders, prepared by the sol-gel method, were mixed with organic binder and the BSCT thick films were fabricated by the screen printing techniques on alumina substrates. All the BSCT thick films, sintered at 1420$^{\circ}C$, showed the typical XRD patterns of a perovskite polycrystalline structure. The average grain sizes decreased with increasing amounts of ZrO$_2$, and the BSCT(40/40/20) thick films doped with 2wt% MnO$_2$ showed a value of 8$\mu\textrm{m}$. The thickness of thick films by four-cycle on printing/drying was approximately 951$\mu\textrm{m}$. The relative dielectric constant decreased with increasing Ca content and MnO$_2$ doping amount. The relative dielectric constant, dielectric loss and tunability of the BSCT(50/40/10) thick films doped with 2.0wt% ZrO$_2$ were 772, 0.184％ and 15.62%, respectively.

• Journal of Radiation Protection and Research
• /
• v.8 no.2
• /
• pp.15-35
• /
• 1983

High voltage paper-electrophoresis of fission products from 24 hour neutron-irradiated and 150 days-decayed 90% highly enriched uranyl nitrate solution has been carried out by using the specially designed migration apparatus. The separation of Zr-95 and Nb-95 from the other fission products is possible under the migration condition of 0.1 $M-HClO_4$ (pH=0.85), 0.05 M-HCl+0.09M-KCl (pH=0.9), 0.1M-HCl (pH=1.1) and 0.01 M-HCl (pH=2.0). Zr-95 and Nb-95 are separated out at+1cm from the fiducial point. The separation of Zr-95 and Nb-95 from each other is possible under the migration condition of 0.1 $M-HClO_4$, 0.05 M-HCl+0.09 M-KCl, 0.1 M-HCl and 0.1 M-HAc+0.1 M-NaAc (pH=4.68) together with 2% ammonium oxalate. Nb-95 is separated out at $-6{\sim}-7cm$ from the fiducial point and Zr-95 at $+1{\sim}-lcm$. The separation of Ru-103 from the other fission products is possible under the migration condition of 0.025 $M-Na_2CO_3+0.025\;M-NaHCO_3$ (pH=10.0), 0.01M-$Na_3PO_4$ (pH=11.7) and 0.1 M-NaOH (pH=13.2). Ru-103 migrates towards the anode -6cm, -4cm and -3cm, respectively.

• Journal of the Korean Ceramic Society
• /
• v.24 no.2
• /
• pp.123-132
• /
• 1987

Yttria-stabilized zirconia with erbia-lanthana were investigated with respect to the amount of Ln2O3 (Ln; Er, La) addition in the range of 0.5∼5 mol% to the base composition of 8 mol% yttriazirconia. Following analysis and measurement were adopted for the characterization of synthesizes of solid electrolyte; phase transformation, lattice parameter, crystallite size, relative density, chemical composition and SEM/EDS. Electrical conductivity by two-probe method versus temperature from 350$^{\circ}C$ to 800$^{\circ}C$ and frequency in the range of 5Hz∼13MHz by complex impedance method was also conducted together with the determination of oxygen ion transference number by EMF method for the evaluation of their electrical properties. The results were as followsing; Electrical conductivity were decreased with increase in Ln2O3 content, but their activation energies increased. In the case of La2O3 addition, espicially, its electrical conductivity was decreased owing to the segregation of second phases at the grain-boundary. Grain-boundary conductivity of the specimen contained 0.5 mol% Er2O3 exhibited a maximum conductivity among thecompositions experimented. However, their bulk conductivities decreased in both case. Oxygen ion transference number was also reduced with decrease in oxygen partial pressure. For example, in the case of Er2O3 addition it retained value in the range of 0.97∼0.94 abvove 4.74${\times}$10-2in oxygen partial pressure. With the increase in the quantities of the evaporation of additive components, the crystallite size of stabilized zirconia decreased, and their relative density also reduced owing to the formation of porosity in their matrices. In the case of La2O3 the sinterbility was improved in the limited amount of addition up to 0.5 mol%, in the same range of addition the strength of sintered bodies were improved perhaps owing to the precipitation of metastable tetragonal phase in the fully stabilized zirconia.

• Clean Technology
• /
• v.24 no.1
• /
• pp.35-40
• /
• 2018

$Co_3O_4$ catalysts for $N_2O$ decomposition were prepared by co-precipitation method. Ce and Zr were added during the preparation of the catalyst as promoter with the molar ratio (Ce or Zr) / Co = 0.05. Also, 1 wt% $K_2CO_3$ was doped to the prepared catalyst with impregnation method to investigate the effect of K on the catalyst performance. The prepared catalysts were characterized with SEM, BET, XRD, XPS and $H_2-TPR$. The $Co_3O_4$ catalyst exhibited a spinel crystal phase, and the addition of the promoter increased the specific surface area and reduced the particle and crystal size. It was confirmed that the doping of K improves the catalytic activity by increasing the concentration of $Co^{2+}$ in the catalyst which is an active site for catalytic reaction. The catalytic activity tests were carried out at a GHSV of $45,000h^{-1}$ and a temperature range of $250{\sim}375^{\circ}C$. The K-impregnated $Co_3O_4$ catalyst showed much higher activity than $Co_3O_4$ catalysts with promoter only. It is found that the K-impregnation increased the concentration of $Co^{2+}$ more than the added of promoter did, and lowered the reduction temperature to a great extent.

• Environmental Engineering Research
• /
• v.25 no.2
• /
• pp.186-196
• /
• 2020

Pillared clays with Zr and Fe/Cu/Zr polycations have been prepared from natural clays found in large deposits of Kazakhstan and assessed as catalysts for the catalytic wet peroxide oxidation (CWPO), using 4-nitrophenol (4-NP) as model compound. The performance of the catalysts was followed by measuring the concentration of 4-NP, H₂O₂ and the total organic carbon (TOC), considering C_4-NP = 5 g L^-1, $C_{H_2O_2}$ = 17.8 g L^-1, C_cat = 2.5 g L^-1, initial pH = 3.0 and T = 50℃. At those selected conditions, the pillared clays showed higher activity than natural clays in the CWPO of 4-NP. The conversion of the model pollutant was complete when Fe/Cu/Zr-PILCs were used, with the TOC removal reaching 78.4% after 24 h with the best Fe/Cu/Zr-PILC. The H₂O₂, 4-NP and TOC time-evolution was well described by a kinetic model based on TOC lumps in three blocks, considering the initial TOC (corresponding to 4-NP), the production of oxidizable intermediates and the formation of refractory products.

• Transactions of the Korean hydrogen and new energy society
• /
• v.24 no.1
• /
• pp.29-35
• /
• 2013

A dense mixed ionic and electronic conducting ceramic membrane is one of the most promising materials because it can be used for separation of oxygen from the mixture gas. The $ABO_3$ perovskite structure shows high chemical stability at high temperatures under reduction and oxidation atmospheres. $BaCo_{1-x-y}Fe_xZr_yO_{3-{\delta}}$ (BCFZ) was well-known material as high mechanical strength, low thermal conductivity and stability in the high valence state. Glycine Nitrate Process (GNP) is rapid and effective method for powder synthesis using glycine as a fuel and show higher product crystallinity compared to solid state reaction and citrate-EDTA method. BCFZ was fabricated by modified glycine nitrate process. In order to control the burn-up reaction, $NH_4NO_3$ was used as extra nitrate. According to X-Ray Diffraction (XRD) results, BCFZ was single phase regardless of Zr dopants from y=0.1 to 0.3 on B sites. The green compacts were sintered at $1200^{\circ}C$ for 2 hours. Oxygen permeability, methane partial oxidation rate and hydrogen production ability of the membranes were characterized by using Micro Gas Chromatography (Micro GC) under various condition. The high oxygen permeation flux of BCFZ 1-451 was about $1ml{\cdot}cm^{-2}s^{-1}$. Using the humidified Argon gas, BCFZ 1-433 produced hydrogen about $1ml{\cdot}cm^{-2}s^{-1}$.