• Applied Microscopy
• /
• v.28 no.1
• /
• pp.121-126
• /
• 1998

Detailed studies of high resolution TEM inages on the modulated structure caused by Zn vacancy ordering along [110] direction in BZT sintered at $1400^{\circ}C$ for 90 hours had revealed that the images which had hexagonal patterns were similar to those obtained from the structure which had no modulation, These images had appeared over the wide ranges from -30 nm to -42 nm in defocus values and from 2 nm to 20 nm in thickness. The computer simulated images showed that the modulation due to Zn vacancy ordering had made a small change in contrast in the interior of hexagonal pattern, which was very difficult to differenciate in experiments. The image which demonstrated the modulated structure very well was the one which obtained at -52 nm in defocus value and 16 nm in thickness.

• The Korean Journal of Ceramics
• /
• v.2 no.4
• /
• pp.242-245
• /
• 1996

The microstructure of $Ba (Zn_{1/3}Ta_{2/3})O_3$ (BZT) was investigated using X-ray diffractometry(XRD) and transmission electron microscopy (TEM). $Ba_{0.5}TaO_3$ and $Ba_3TaO_{5.5}$ (BT) phasses were observed on the surface of the sintered specimen by XRD. Furthermore, a new type of ordering along the [110] direction was found in sintered specimen by the XRD and TEM analysis. The wavelength of ordering was 0.9 nm which is three times larger than the interplanar distance of (110) plane and new type of ordering is considered to be a result of Zn vacancy ordering. The creation of Zn vacancies and formation of BT phases are attributed to the evaporation of volatile ZnO. A new mechanism for ZnO loss is suggested. In this mechanism, only Zn vacancies are created only when the amount of ZnO loss is small and as the amount of ZnO loss increases, BT phases are formed at the same time. A new unit cell of ordered structure is suggested as the superlattics containing three BZT unit cells.

• Applied Microscopy
• /
• v.34 no.2
• /
• pp.113-120
• /
• 2004

Microstructural characteristics of the Complex Perovskite (1-x) $(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$ (LNST) system have been investigated using the transmission electron microscopy (TEM). When $0.0{\leq}x{\leq}0.6$, the vacancy ordering forming the 1/2 (001) superlattice reflections due to the A-site cation deficiencies has apperaed. It could be confirmed by presence of ABPs. But it was difficult to form the vacancy ordering since vacancy concentration gradually lowered as the amount of the substituted Li ions decrease. Antiphase boundaries (APBs) were presented in microstructures of LNST when $0.8{\leq}x{\leq}1.0$. It was considered that these boundaries were caused by the 1:1 chemical ordering of A-site cations, Na and Sm ions. LNST had not only the antiphase tilting of oxygen octahedron but also the inphase tilting of oxygen octahedron and the antiparallel shift of cations all of them. It could be confirmed by presence of ferroelastic domains

• Applied Microscopy
• /
• v.27 no.2
• /
• pp.217-223
• /
• 1997

New type of ordering along 1110] direction was found In BZT sintered at $1400^{\circ}C$ for 90 hours by using X-ray diffraction analysis and high resolution transmission electron microscopy. The wavelength of the modulated structure was 0.9 nm which is three times larger than the interplanar distance of (110) plane. New type of ordering is considered to be formed as a result of Zn vancacy ordering and new structural model was proposed. The computer simulated electron diffraction and the structural images are in good agreement with those obtained by experiments.

• Journal of Powder Materials
• /
• v.13 no.2 s.55
• /
• pp.112-118
• /
• 2006

[ $R_{1/3}Sr_{2/3}FeO_{3}$ ](R=Pr, Nd, and Sm) was synthesized and their magnetic properties and charge ordering(CO) transition related with lattice dynamics and oxygen vacancy were systematically investigated. The charge disproportion ation(CD) in $R_{1/3}Sr_{2/3}FeO_{3}$(R=Pr,Nd) was in which two kins of iron with valence state $Fe^{3+}$ and $Fe^{5+}$ were found with ratio of 2:1. In this charge ordering state a sequence of $Fe^{3+}Fe^{3+}Fe^{5+}Fe^{3+}Fe^{3+}Fe^{5+}$ exists aligned along the [111] direction of the pseudocubic perovskite structure. The charge ordering exist in distorted structure involving $t_{pd}$ hybridization. The disordering phases coexist in distorted structure as temprature in creases that is controlled amount of oxygen vacancy. The magnetic hyperfine fields indicate charge tranfering temperature as it dissapeared drastically.

• Bulletin of the Korean Chemical Society
• /
• v.15 no.1
• /
• pp.64-74
• /
• 1994

The nonstoichiometric chalcogenides with NaCl-type structure were prepared and the physical and structural properties were studied. The homogeneous range and the structural change were studied based on X-ray powder diffractions using Rietveld-type full-profile fitting technique. Wide homogeneous ranges were observed in Y-S and Y-Se systems, and relatively narrow homogeneous ranges were observed in Yb-S and Yb-Se systems. Both in $Yb_{1-x}S\;and\;Yb_{1-x}Se$, a vacancy ordering transition occurred in (111) plane direction. The ordered superstructure had cubic symmetry(Fm$\bar{3}m) with doubled unit cell "a" parameter compared to the original NaCl-type. The superlattice developed in a continuous second-order transitiion was characterized by the reduced waved vector k= $(a^*+b^*+c^*)/2$. Y-S system had metallic, and YSe, YbSe system had semiconducting properties in their homogeneous ranges. It was observed that the change of electronic transport properties in extended homogeneous range did not depend on the relativeratio of metal to nonmetal, but on the quantities of vacancies.

• Applied Microscopy
• /
• v.34 no.1
• /
• pp.61-69
• /
• 2004

The microwave dielectric properties and microstructures of the Complex Perovskite (1-x)$(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$(LNST) system were investigated using the X-ray diffraction (XRD) and scanning electron microscopy (SEM). LNST had not only the antiphase tilting of oxygen octahedron but also the inphase tilting of oxygen octahedron and the antiparallel shift of cations. Also, when $0.0{\leq}x{\leq}0.4$, LNST had the vacancy ordering of A-sites because of the evaporation of Li ions. From the observation of the microstructure, abnormal grain growth phenomena were observed over the whole range of x. The temperature coefficient of resonant frequency ($T_{cf}$) of the $({Li_{1/2}}^{+1}{Sm_{1/2}}^{+3})TiO_3$(LST) system has a large negative value ($-220ppm/^{\circ}C$) but the $({Na_{1/2}}^{+1}{Sm_{1/2}}^{+3})TiO_3$(NST) system which substituted $Na^{+1}$ has a large positive value ($+173ppm/^{\circ}C$). The dielectric properties of ${\varepsilon}_r=103,\;Q*f_{0}=3,700GHz$ and $T_{cf}=+50ppm/^{\circ}C$ at 4GHz were obtained when x =0.4.

• 한국전자현미경학회:학술대회논문집
• /
• 1996.11a
• /
• pp.20-23
• /
• 1996

• Journal of the Korean Chemical Society
• /
• v.32 no.1
• /
• pp.9-14
• /
• 1988

Perovskite type compounds of the $La_{1-x}Ca_xFeO_{3-y}$ system were prepared from stoichiometric mixtures of La_2O_3,\;CaCO_3$, and Fe(NO-3)_3{\cdot}9H_2O$ by heating at 1100$^{\circ}C$ for 24 hours. The crystallographic structures of the solid solutions of all compositions were orthorhombic systems. X-ray diffraction and Mohr salt analysis revealed that at higher y value the phase transition due to vacancy ordering occured and that the lattice volume decreased when the x value was increased. The value of nonstoichiometric ratio y were found to be in the range of $0.0{\sim}0.5$. Electrical conductivities of this systems are measured in temperature range of -100 to 100$^{\circ}C$. Ionic contribution to total conductivity was found from activation energy in the phase containing the open pathway due to vacancy ordering.

• The Korean Journal of Ceramics
• /
• v.5 no.4
• /
• pp.371-374
• /
• 1999

Y2O3 and Nb2O5 co-doped tetragonal zirconia polycrystals((Y, Nb)-TZP) containing 10 to 30 vol% $Al_2O_3$ were prepared and hydrothermal stability of the composites was evaluated after aging for 5 h at the temperature range of $150^{\circ}C$ $250^{\circ}C$ under 4 MPa $H_2O$ vapor pressure in an autoclave. The (Y, Nb)-TZP/Al2O3 composites showed excellent phase stability under the hydrothermal conditions, as compared with the 3Y-TZP/$Al_2O_3$ composites, due to the combined effects of the Y-Nb ordering in the $t-ZrO_2$ lattice, the reduction of oxygen vacancy concentration, and the $Al_2O_3$ addition. The strength and fracture toughness of the (Y, Nb)-TZP/$Al_2O_3$ composite, containing 20 vol% of 2.8 $Al_2O_3$ particles, were 700 MPa and 8.1 MP.$am^{1/2}$, respectively.