• Journal of the Korean Crystal Growth and Crystal Technology
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• v.12 no.3
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• pp.144-148
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• 2002

Hydroxyapatite/titanium composites were prepared as 4-layered functionally graded materials (FGM) using a spark plasma sintering (SPS) apparatus. The maximum density and the biaxial strength of hydroxyapatite/titanium composites were achieved by SPS with a holding time 8 minutes at $1200^{\circ}C$. However, the hydroxyapatite was decomposed tetracalcium phosphate (TetCP) at $1100^{\circ}C$, and calcium titanate compounds ($CaTiO_3$) were formed. When titanium was added to hydroxyapatite, decomposition of hydroxyapatite was occurred easily at the low temperature.

• Applied Chemistry for Engineering
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• v.9 no.4
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• pp.585-590
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• 1998

Fibrous $Na_xTi_nO_{2n+1}$ whisker was prepared by $H^+/Na^+$ ion-exchange on layered hydrous titanium dioxide ($H_2Ti_4O_9{\cdot}nH_2O$). The ion-exchange reaction was proceeded at 0.5~2.0 M NaOH solution. In the ion-exchange at 2.0 M NaOH solution, 73% of sodium was exchanged and the prepared $Na_xTi_nO_{2n+1}$ whisker was a fibrous crystal of about $10{\sim}20{\mu}m$ of length and about $0.7{\mu}m$ of diameter. The phase transition of the ion-exchange phases identified by the thermal analysis. The result showed that the $Na_xTi_nO_{2n+1}$ whisker was decomposed into $Na_2Ti_6O_{13}$ and $TiO_2$ in the temperature of $200{\sim}600^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.43 no.11 s.294
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• pp.688-692
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• 2006

Ferroelectric lanthanides-substituted $Bi_4Ti_3O_{12}$ $(Bi_{4-x}Ln_xTi_3O_{12}, BLnT)$ thin films approximately 200 nm in thickness were deposited by metal organic chemical vapor deposition onto Pt(111)/Ti/SiO$_2$/Si(100) substrates. Many researchers reported that the lanthanides substitution for Bi in the pseudo-perovskite layer caused the distortion of TiO$_6$ octahedron in the a-b plane accompanied with a shift of the octahedron along the a-axis. In this study, the effect of lanthanides (Ln=Pr, Eu, Gd, Dy)-substitution and crystallization temperature on their ferroelectric properties of bismuth titanate $(Bi_4Ti_3O_{12}, BIT)$ thin films were investigated. As BLnT thin films were substituted to lanthanide elements (Pr, Eu, Gd, Dy) with a smaller ionic radius, the remnant polarization (2P$_r$) values had a tendency to increase and made an exception of the Eu-substituted case because $Bi_{4-x}Eu_xTi_3O_{12}$ (BET) thin films had the smaller grain sizes than the others. In this study, we confirmed that better ferroelectric properties can be expected for films composed of larger grains in bismuth layered peroskite materials. The crystallinity of the thin films was improved and the average grain size increased as the crystallization temperature,increased from 600 to 720$^{\circ}C$. Moreover, the BLnT thin film capacitor is characterized by well-saturated polarization-electric field (P-E) curves with an increase in annealing temperature. The BLnT thin films exhibited no significant degradation of switching charge for at least up to $1.0\times10^{11}$ switching cycles at a frequency of 1 MHz. From these results, we can suggest that the BLnT thin films are the suitable dielectric materials for ferroelectric random access memory applications.

• Bulletin of the Korean Chemical Society
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• v.25 no.7
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• pp.1051-1054
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• 2004

The structural transformation behavior of $Na_2Ti_3O_7$ by hydrolysis was investigated in mild and strong acidic aqueous medium. Compared with $K_2Ti_4O_9,\;Na_2Ti_3O_7$ exhibits quite different structural and morphological transformation behavior despite their similar layered structural characteristics. $TiO_2(B)$ obtained by heat treatment of $H_2Ti_3O_7\;at\;350^{\circ}C$ transforms to rutile $H_2Ti_3O_7\;at\;900^{\circ}C$. This temperature is much lower than $1200{\circ}C$, the temperature for anatase to rutile transition when $K_2Ti_4O_9$ is used as a starting titanate. A rectangular rod shape and size of $TiO_2(B)$ particles obtained from $Na_2Ti_3O_7$ is also different from a fibrous structure of $TiO_2(B)$ prepared using $K_2Ti_4O_9$. Rutile crystals of 100 nm diameter with a corn-like morphology and large surface area are directly obtained when the hydrolysis of $Na_2Ti_3O_7$ is carried out at $100^{\circ}C$ in a strong acid solution. The structure of starting titanates and the hydrolysis conditions are an important factor to decide the particle size and morphology of $TiO_2(B)\;and\;TiO_2$.

• Korean Journal of Materials Research
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• v.27 no.3
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• pp.132-136
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• 2017

We synthesized potassium hexatitanate, ($K_2Ti_6O_{13}$, PT6), with a non-fibrous shape, by acid leaching and subsequent thermal treatment of potassium tetratitanate ($K_2Ti_4O_9$, PT4), with layered crystal structure. By controlling nucleation and growth of PT4 crystals, we obtained splinter-type crystals of PT6 with increased width and reduced thickness. The optimal holding temperature for the layered PT4 was found to be ${\sim}920^{\circ}C$. The length and width of the PT4 crystals were increased when the nucleation and growth time were increased. After a proton exchange reaction using aqueous 0.3 M HCl solution, and subsequent heat treatment at $850^{\circ}C$, the PT4 crystal transformed into splinter-type PT6 crystals. The frictional characteristics of the friction materials show that as the particle size of PT6 increases, the coefficient of friction (COF) and wear amounts of both the friction materials and counter disc increase.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.20 no.3
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• pp.223-227
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• 2007

The effect of Eu contents on the ferroelectric properties of $Bi_{4-x}Eu_xTi_3 O_{12}$ (BET) thin films has been investigated. Bismuth Europium titanate thin films with a Eu contents were prepared on the $Pt/Ti/SiO_2/Si$ substrate by metal-organic decomposition technique. The structure and the morphology of the films were analyzed using X-ray diffraction (XRD) and field emission scanning microscopy (FE-SEM), respectively. From the XRD analysis, it was found that BET thin films have polycrystalline structure, and the layered-perovskite phase is obtained when the Eu contents exceeds 0.2 (x > 0.2). Also, the ferroelectric characteristics of the BET thin films were found to be dependent on the Eu content. Particularly, the BET films doped with x = 0.75 show better ferroelectric properties (remanent polarization 2Pr = 60.99 C/$cm^2$ and only a little polarization fatigue up to $3.5{\times}10^9$ bipolar switching cycling) than those doped with other Eu contents.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.15 no.9
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• pp.764-769
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• 2002

The effect of excess Bi contents on the ferroelectric properties of B $i_{3.25}$ L $a_{0.75}$ $Ti_3$ $O_{12}$ (BLT) thin films has been investigated. Bismuth lanthanum titanate thin films with excess Bi contents were prepared onto Pt/Ti/ $SiO_2$/Si substrate by metalorganic decomposition (MOD) technique. The structure and morphology of the films were analyzed using X-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. From the XRD analysis, BLT thin films show polycrystalline structure and the layered-perovskite phase was obtained over 10% excess of Bi contents. As a result of ferroelectric characteristics related to the Bi content of the BLT thin film, the remanent polarization and dielectric constant decreased with increasing over Bi content of 10% excess. The BLT film with Bi content of 10% excess was measured to have a dielectric constant of 326 and dielectric loss of 0.024. The BLT thin films showed little polarization fatigue test up to 3.5$\times$10$^{9}$ bipolar switching cycling.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.6
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• pp.278-282
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• 2010

The doping effect of thulium on electrical properties and degradation behavior in barium titanate ceramics ($BaTiO_3$) was investigated in terms of generations of core-shell structure and micro-chemical changes through highly accelerated degradation test. The dielectric specimens of pellet type and multi-layered sheets were prepared by using $BaTiO_3$ with undoped and doped with 1 mol% $Tm_2O_3$. The $BaTiO_3$ ceramics doped with 1 mol% $Tm_2O_3$ had 40% higher dielectric constant (${\varepsilon}$ = 2700) than that of the undoped $BaTiO_3$ specimen at curie temperature and met X7R specification. According to the result of highly accelerated degradation test conducted at $150^{\circ}C$, 70 V, and 24 hr, the oxygen diffusion was declined in dielectrics doped with 1 mol% $Tm_2O_3$. The $Tm^{3+}$ ion substituted selectively Ba site and Ti site and contributed to the generation of the core-shell structure. Oxygen vacancies occurred by substitution for Ti site could reduce excess oxygen that reacted to the Ni electrode.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.319-319
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• 2013

Even though the fabrication methods of metal oxide based thin film capacitor have been well established such as RF sputtering, Sol-gel, metal organic chemical vapor deposition (MOCVD), ion beam assisted deposition (IBAD) and pulsed laser deposition (PLD), an applicable capacitor of printed circuit board (PCB) has not realized yet by these methods. Barium Strontium Titanate (BST) and other high-k ceramic oxides are important materials used in integrated passive devices, multi-chip modules (MCM), high-density interconnect, and chip-scale packaging. Thin film multi-layer technology is strongly demanded for having high capacitance (120 nF/$mm^2$). In this study, we suggest novel multi-layer thin film capacitor design and fabrication technology utilized by plasma assisted deposition and photolithography processes. Ba0.6Sr0.4TiO3 (BST) was used for the dielectric material since it has high dielectric constant and low dielectric loss. 5-layered BST and Pt thin films with multi-layer sandwich structures were formed on Pt/Ti/$SiO_2$/Si substrate by RF-magnetron sputtering and DC-sputtering. Pt electrodes and BST layers were patterned to reveal internal electrodes by photolithography. SiO2 passivation layer was deposited by plasma-enhanced chemical vapor deposition (PE-CVD). The passivation layer plays an important role to prevent short connection between the electrodes. It was patterned to create holes for the connection between internal electrodes and external electrodes by reactive-ion etching (RIE). External contact pads were formed by Pt electrodes. The microstructure and dielectric characteristics of the capacitors were investigated by scanning electron microscopy (SEM) and impedance analyzer, respectively. In conclusion, the 0402 sized thin film multi-layer capacitors have been demonstrated, which have capacitance of 10 nF. They are expected to be used for decoupling purpose and have been fabricated with high yield.

• Proceedings of the Materials Research Society of Korea Conference
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• 2010.05a
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• pp.48.2-48.2
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• 2010

The effect of additives as rare-earth in dielectric materials has been studied to meet the development trend in electronics on the miniaturization with increasing the capacitance of MLCCs (multi-layered ceramic capacitors). It was reported that the addition of rare-earth oxides in dielectrics would contribute to enhance dielectric properties and high temperature stability. Especially, dysprosium and thulium are well known to the representative elements functioned as selective substitution in barium titanate with perovskite structure. The effects of these additives on microstructure and electric properties were studied. The 0.8 mol% Dy doped $BaTiO_3$ and the 1.0 mol% Tm doped $BaTiO_3$ had the highest electric properties as optimized composition, respectively. According to the increase of rare-earth contents, the growth of abnormal grains was suppressed and pyrochlore phase was formed in more than solubility limits. Furthermore, the effect of two rare-earth elements co-doped $BaTiO_3$ on the dielectric properties and insulation resistance was investigated with different concentration. The dielectric specimens with $BaTiO_3-Dy_2O_3-Tm2O_3$ system were prepared by design of experiment for improving the electric properties and sintered at $1320^{\circ}C$ for 2h in a reducing atmosphere. The dielectric properties were evaluated from -55 to $125^{\circ}C$ (at $1KHz{\pm}10%$ and $1.0{\pm}0.2V$) and the insulation resistance was examined at 16V for 2 min. The morphology and crystallinity of the specimens were determined by microstructural and phase analysis.