• Proceedings of the Materials Research Society of Korea Conference
• /
• 2009.05a
• /
• pp.33.1-33.1
• /
• 2009

Lead-free (1-x)$(Na_{0.5}K_{0.5})NbO_3$-xBa($Ti_{0.9}Sn_{0.1})O_3$ [NKN-BTS-100x] ceramics doped with 1 mol% $MnO_2$ have been prepared by the conventional solid state method and their structural and piezoelectric properties were investigated. The NKN-BTS-100x ceramics exhibited a dense and homogeneous microstructure when they were sintered at $1030-1150^{\circ}C$. Grain growth was observed for the specimen sintered at relatively low temperature of $1050^{\circ}C$. A tetragonal/orthorhombic morphotropic phase boundary (MPB) in the perovskite structure was also appeared for the NKN-BTS-100x ceramics (0.04$1050^{\circ}C$. The enhanced piezoelectric properties in the NKN-BTS ceramics with a MPB composition were obtained. Especially, for the NKN-BTS-6 ceramics, a high dielectric constant (${\varepsilon}^T_3/\varepsilon_0=1,400$), piezoelectric constant ($d_{33}=237$) and electromechanical coupling factor ($k_p=0.42$) were obtained.

• Journal of the Korean Ceramic Society
• /
• v.50 no.1
• /
• pp.87-91
• /
• 2013

The doping effect of Sn on the microstructure evolution and dielectric properties was studied in $CaCu_3Ti_{4-x}Sn_xO_{12}$ polycrystals. Samples were produced by a conventional solid-state reaction method. Sintering was carried out at $1115^{\circ}C$ for 2-16 h in air. The dielectric constant and loss were examined at room temperature over a frequency range between $10^2$ and $10^6$ Hz. The microstructure was found to evolve into three stages. Addition of $SnO_2$ led to an increase in density and advanced formation of abnormal grains. The formation of coarse grains with a reduced thickness of the boundary brought about an enhanced dielectric constant and a lower dielectric loss below ~1 kHz. EDS data showed the Cu-rich phase along the grain boundary, which should contribute to the improved dielectric constant according to the internal barrier layer capacitor model. After all, $SnO_2$ was an effective dopant to elevate the dielectric characteristics of $CaCu_3Ti_{4-x}Sn_xO_{12}$ polycrystals as a promoter for abnormal grain growth.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.36 no.5
• /
• pp.505-512
• /
• 2023

This study investigated crystal structures, microstructures, and electric-field-induced strain (EFIS) properties of Bi-based lead-free ferroelectric/relaxor composites. Bi_1/2Na_0.82K_0.18)_1/2TiO₃ (BNKT) as a ferroelectric material and 0.78Bi_1/2(Na_0.78K_0.22)_1/2TiO₃-0.02LaFeO₃ (BNKT2LF) as a relaxor material were synthesized using a conventional solid-state reaction method, and the resulting BNKT2LF powders were subjected to high-energy ball milling (HEBM) after calcination. As a result, HEBM proved a larger average grain size of sintered samples compared to conventional ball milling (CBM). In addition, the increased sintering time led to grain growth. Furthermore, HEBM treatment and sintering time demonstrated a significant effect on EFIS of BNKT/BNKT2LF composites. At 6 kV/mm, 0.35% of the maximum strain (S_max) was observed in the HEBM sample sintered for 12 h. The unipolar strain curves of CBM samples were almost linear, indicating almost no phase transitions, while HEBM samples displayed phase transitions at 5~6 kV/mm for all sintering time levels, showing the highest S_max/E_max value of 700 pm/V. These results indicated that HEBM treatment with a long sintering time might significantly enhance the electromechanical strain properties of BNT-based ceramics.

• Journal of Powder Materials
• /
• v.30 no.6
• /
• pp.509-515
• /
• 2023

Lead-free perovskite ceramics, which have excellent energy storage capabilities, are attracting attention owing to their high power density and rapid charge-discharge speed. Given that the energy-storage properties of perovskite ceramic capacitors are significantly improved by doping with various elements, modifying their chemical compositions is a fundamental strategy. This study investigated the effect of Zn doping on the microstructure and energy storage performance of potassium sodium niobate (KNN)-based ceramics. Two types of powders and their corresponding ceramics with compositions of (1-x)(K,Na)NbO₃-xBi(Ni_2/3Ta_1/3)O₃ (KNN-BNT) and (1-x)(K,Na)NbO₃-xBi(Ni_1/3Zn_1/3Ta_1/3)O₃ (KNN-BNZT) were prepared via solid-state reactions. The results indicate that Zn doping retards grain growth, resulting in smaller grain sizes in Zn-doped KNN-BNZT than in KNN-BNT ceramics. Moreover, the Zn-doped KNN-BNZT ceramics exhibited superior energy storage density and efficiency across all x values. Notably, 0.9KNN-0.1BNZT ceramics demonstrate an energy storage density and efficiency of 0.24 J/cm³ and 96%, respectively. These ceramics also exhibited excellent temperature and frequency stability. This study provides valuable insights into the design of KNN-based ceramic capacitors with enhanced energy storage capabilities through doping strategies.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.30 no.3
• /
• pp.103-109
• /
• 2020

The effect of La₂O₃ addition on the crystalline phase, microstructure, and dielectric properties of BaTiO₃ has been studied as a function of the amounts of La₂O₃. 0.3 mol% TiO₂-excess BaTiO₃ powder was synthesized by solid-state reaction, and then the powder compacts with various amounts of La₂O₃ were sintered at 1250℃ for 2 hours. Room temperature XRD showed changes in the lattice parameters and a decrease of tetragonality (c/a) as the amounts of La₂O₃ increased. It can be explained that the phase transition from tetragonal to cubic phase occurred because La³⁺ replaced Ba²⁺ site, which increased the instability of the tetragonal phase. As La₂O₃ was added over 0.1 mol%, the critical driving force for growth (Δg_c) increased over maximum driving force (Δg_max). As the result, the grain size decreased with La₂O₃ addition. Dielectric constant decreased as the amounts of La₂O₃ increased, which was analyzed with crystal structure and microstructure.

• Applied Chemistry for Engineering
• /
• v.20 no.3
• /
• pp.317-321
• /
• 2009

In order to analyze the high temperature phase formation and the sinterability of super ionic conductor $K^+-{\beta}/{\beta}"-Al_2O_3$ which is commonly used as a solid oxide electrolyte, the pure $K^+-{\beta}/{\beta}"-Al_2O_3$ powder in the ternary system $K_2O-LiO_2-Al_2O_3$ was synthesized by solid state reaction and formed to tube and disk using slip casting method and cold isostatic pressing (CIP), respectively. The slip casting was conducted in an alumina mold with the slurry containing 40 wt% of solid contents and the CIP was carried out under 20 MPa. The samples were sintered at $1600^{\circ}C$, $1700^{\circ}C$ and $1750^{\circ}C$, respectively, and their phase formation and the sintering density were investigated according to the forming method. The samples produced by CIP showed far higher ${\beta}"-Al_2O_3$ fraction as compared with those by slip casting. On the other hand, the samples by slip casting showed slightly higher sintering density. The relative density reached to about 83% at $1750^{\circ}C$ and for 1 h, independent of the forming method. In the case of 90 min socking time, the density was decreased owing to the exaggerated grain growth and the pores by $K_2O$ evaporation.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.12 no.2
• /
• pp.87-90
• /
• 2002

$LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.23 no.6
• /
• pp.314-319
• /
• 2013

Fabrication of nanocomposite material for the $Fe_2O_3-Al$ system by mechanical alloying (MA) has been investigated at room temperature. It is found that ${\alpha}-Fe/Al_2O_3$ nanocomposite powders in which $Al_2O_3$ is dispersed in ${\alpha}-Fe$ matrix are obtained by mechanical alloying of $Fe_2O_3$ with Al for 5 hours. The change in magnetization and coercivity also reflects the details of the solid state reduction process of hematite by pure metal of Al during mechanical alloying. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $1000^{\circ}C$ and $1100^{\circ}C$ under 60 MPa. Shrinkage change after SPS of MA'ed sample for 5 hrs was significant above $700^{\circ}C$ and gradually increased with increasing temperature up to $1100^{\circ}C$. X-ray diffraction result shows that the average grain size of ${\alpha}-Fe$ in ${\alpha}-Fe/Al_2O_3$ nanocomposite sintered at $1100^{\circ}C$ is in the range of 180 nm. It can be also seen that the coercivity (Hc) of SPS sample sintered at $1000^{\circ}C$ is still high value of 88 Oe, suggesting that the grain growth of magnetic ${\alpha}-Fe$ phase during SPS process tend to be suppressed.

• Journal of the Korea Institute of Information and Communication Engineering
• /
• v.15 no.8
• /
• pp.1771-1776
• /
• 2011

In this paper, as an attempt to improve the preparation conditions of $YBa_2Cu_3Ox$ superconducting bulk samples, the properties of $YBa_2Cu_3Ox$ superconductor depending on the particle size of YBCO powder and $BaPbO_3$ as an additive have been investigated, and a study on the effects of additive to the density, grain alignment, and porosity of samples that affect the critical current of superconductor has been performed. In order to prepare superconductor, $YBa_2Cu_3Ox$ powder synthesized by sol-gel method, showing a size distribution of 0.2~1 ${\mu}m$ was used. The $BaPbO_3$ added to promote grain growth and to decrease porosities and weak links between grain boundaries of $YBa_2Cu_3Ox$ superconductors. In the samples prepared by sol-gel synthesized powder with 10, 20, and 30 wt% conductive $BaPbO_3$ additives, the sample with 20 wt% $BaPbO_3$ obtained the highest critical current of 4.74 A, showing 20 wt% higher critical current than that with solid state synthesized powder.

• Korean Journal of Materials Research
• /
• v.22 no.7
• /
• pp.346-351
• /
• 2012

$Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.