• Title/Summary/Keyword: tetragonal phase

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Structural and Electrochemical characterization of LiCoO2 Nano Cathode Powder Fabricated by Mechanochemical Process (기계 화학법에 의해 제작된 나노 LiCoO2 양극 분말의 구조 및 전기화학적 특성)

  • Choi, Sun-Hee;Kim, Joo-Sun;Yoon, Young-Soo
    • Journal of the Korean Ceramic Society
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    • v.41 no.1
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    • pp.86-91
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    • 2004
  • $LiCoO_2$ cathode powders with round particle shaped and nano grain sized of 70-300nm were synthesized by a mechanochemical method. The surface of Li-Co precursor prepared by freeze drying method was modified by $K_2SO_4$ coating and ball milling was used for the coating process. The precursor was crystallized to high temperature form of $LiCoO_2$ at $800^{\circ}C$ and the grain growth was inhibited by the $K_2SO_4$ coating effect. The $K_2SO_4$ coating was not decomposed at $800^{\circ}C$ and prevented the contact in the Li-Co precursor particles. The nano-sized $LiCoO_2$ powder had tetragonal phase and it affected the Li diffusion through the surface of particles. It means that the anode materials for hight performance battery should be satisfied not only small particle size but phase contol on the surface of particles. In this study, the powder characteristics and rate capabilities were compared with a commercial powder and the nano-sized $LiCoO_2$ powder fabricated by the mechanochemical method. And the crucial factor which affects on battery performance was also examined.

Hydrothermal Preparation and Sintering of Fine PSZT Powder (미세 PSZT분말의 수열합성 및 소결)

  • Oh, Jung Kang;Seo, Kyung Won
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.654-660
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    • 1998
  • In preparing PSZT powder by hydrothermal synthesis, effects of reaction temperature, concentration of raw materials and mineralizer on crystallinity, particle size distribution, and dielectric constant were investigated. By varying the concentration of mineralizer and the ratio of Pb to Sr or Zr to Ti, crystalline PSZT powder, having the mean particle size of $0.3{\sim}15{\mu}m$, was prepared by hydrothermal synthesis in the temperature range of $120{\sim}200^{\circ}C$ for a 2h reaction. PSZT ceramics, having dielectric constant of 1000~3000, were prepared at $1150^{\circ}C$ for a 2h sintering reaction of the PSZT powders. Experimental results showed that the weight mean particle size of $0.5{\mu}m$ was obtained when the concentration of KOH in the solution was 10 wt % and the ratio of Pb to Sr was 0.95/0.05, that of Zr to Ti was 0.52/0.48. It also showed that the ceramics of dielectric constant of 2900 were prepared through sintering of this PSZT powder. Size of PSZT particles became smaller with its narrow distribution as the concentration of KOH increased up to 10 wt %. However, it came to be larger at this concentration and above. By adding small amount of Sr that would not affect that crystallinity of particles we can improve dielectric property of sintered materials. Addition of Zr may shift the major crystal phase of synthetic PSZT powder from tetragonal to rhombohedral phase.

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Effect of coloring liquids on biaxial flexural strength of monolithic zirconia (착색 용액이 단일 구조 지르코니아의 이축 굴곡 강도에 미치는 영향)

  • Jung, Chaeyul;Kim, Min-Jeong;Kim, Jae-Hyun
    • The Journal of Korean Academy of Prosthodontics
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    • v.59 no.2
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    • pp.190-200
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    • 2021
  • Purpose. The aim of this study was to evaluate biaxial flexural strength and hardness of colored monolithic zirconia after dipping in different time intervals of coloring solution. Materials and Methods. Disk shaped specimens were prepared from monolithic zirconia (Eclipse V2.0, AMS, Gimpo, Korea). Four experimental groups were categorized (n = 12) due to coloring time (PU (0s); ST (8s); OV (1 min); PS (preshade)), to evaluate biaxial flexural strength and Vickers hardness. After fracture, X-ray diffraction analysis was performed using fractured specimens. Results were analyzed with one-way ANOVA test. Results. There was no significant difference between groups in the biaxial flexural strength test. However, in the Vickers hardness test, the group with standard dipping time (ST) showed significantly higher value than the group without dipping in coloring liquid (PU)(P=.038). Also, there was no significant difference in the rest of the groups (P>.05). As a result of X-ray diffraction analysis, specific peaks of tetragonal phase were shown and the volume of monoclinic phase fraction was lower than 25%. Conclusion. Although this study has several limitations, coloring liquids had no significant effect on biaxial flexural strength. Vickers hardness was significantly different between the group to which the coloring liquid was applied and the group to which the coloring solution was not applied, but there was no significant difference between the other groups. Also, the flexural strength of monolithic zirconia corresponds to Class 5 of the minimal flexural strength standard according to the use of dental ceramics.

Dielectric Properties of (Ba0.7Sr0.3-3x/2Lax)(Ti0.9Zr0.1)O3 Ceramics with La3+ Substitution for Sr2+-Site ((Ba0.7Sr0.3-3x/2Lax)(Ti0.9Zr0.1)O3 세라믹의 Sr2+-자리에 대한 La3+ 치환에 따른 유전 특성)

  • Si Hyun Kim;Ju Hye Kim;Eung Soo Kim
    • Korean Journal of Materials Research
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    • v.33 no.11
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    • pp.465-474
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    • 2023
  • The effects of La3+ substitution for Sr2+-site on the crystal structure and the dielectric properties of (Ba0.7Sr0.3-3x/2Lax) (Ti0.9Zr0.1)O3 (BSLTZ) (0.005 ≤ x ≤ 0.02) ceramics were investigated. The structural characteristics of the BSLTZ ceramics were quantitatively evaluated using the Rietveld refinement method from X-ray diffraction (XRD) data. For the specimens sintered at 1,550 ℃ for 6 h, a single phase with a perovskite structure and homogeneous microstructure were observed for the entire range of compositions. With increasing La3+ substitution (x), the unit cell volume decreased because the ionic size of La3+ (1.36 Å) ions is smaller than that of Sr2+ (1.44 Å) ions. With increasing La3+ substitution (x), the tetragonal phase fraction increased due to the A-site cation size mismatch effect. Dielectric constant (εr) increased with the La3+ substitution (x) due to the increase in tetragonality (c/a) and the average B-site bond valence of the ABO3 perovskite. The BSLTZ ceramics showed a higher dielectric loss due to the smaller grain size than that of (Ba0.7Sr0.3)(Ti0.9Zr0.1)O3 ceramics. BSLTZ (x = 0.02) ceramics met the X7R specification proposed by the Electronic Industries Association (EIA).

Magnetic Properties of $ThMn_{12}-type$$NdFe_{10.7}Ti_{1.2}Mo_{0.1}$>$Ti_{1.2}Mo_{0.1}$ ($ThMn_{12}$$NdFe_{10.7}Ti_{1.2}Mo_{0.1}$의 미세구조 및 자기적 성질 연구)

  • 안성용;이승화;김철성;김윤배;김창석
    • Journal of the Korean Magnetics Society
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    • v.7 no.2
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    • pp.90-96
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    • 1997
  • We have studied crystallographic and magnetic properties of $NdFe_{10.7}Ti_ {1.2}Mo_{0.1}$ by Mossbauer spectroscopy, X-ray diffraction and vibrating sample magnetometer (VSM). The alloys were prepared by arc-melting under an argon atmosphere. The $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ has pure a single phase, whereas $NdFe_{10.7}Ti_{1.3}$ contains some $\alpha$-Fe, conformed with X-ray diffractometry and Mossbauer measurements. The $NdFe_{10.7}Ti_ {1.2}Mo_{0.1}$ has a $ThMn_{12}-type$ tetragonal structure with $a_0=8.637{\AA}$ and $c_0=4.807{\AA}$. The Curie temperature ($T_c$) is 600 K from the result of Mossbauer measurement performed at various temperatures ranging from 13 to 800 K. Each spectrum of below $T_c$ is fitted with five subspectra of Fe sites in the structure ($8i_1, 8i_2, 8j_2, 8j_1, 8f$). The area fractions of the subspectra at room temperature are 12.3%, 14.0%, 21.0% 11.8%, 40.9%, respectively. Magnetic hyperfine fields for the Fe sites decrease in the order, $H_{hf}(8i)>H_{hf}(8j)>H_{hf}(8f)$. The abrupt changes in the magnetic hyperfine field, an magnetic moment observed at about 160 K in $NdFe_ {10.7} Ti_{1.2}Mo_{0.1}$ are attributed to spin reorientations. The average hyperfine field of the $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ shows a temperature dependence of $[H_{hf}(T)-H_{hf}(0)]/H_{hf}(0)=-0.34(T/T_C)^{3/2}-0.14(T/T_C)^{5/2}$ for $T/T_c<0.7$, indicative of spin wave excitation. The Debye temperatures of $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ is found to be Θ=340$\pm$5 K.

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The Effect of Au Addition on the Hardening Mechanism in Ag-30wt%Pd-10wt%Cu Alloy (Ag-30wt% Pd-10wt% Cu 3원합금(元合金) 및 Au 첨가합금(添加合金)의 시효경화특성(時效硬化特性))

  • Lee, K.D.;Nam, S.Y.
    • Journal of Technologic Dentistry
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    • v.21 no.1
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    • pp.27-41
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    • 1999
  • The Ag-Pd-Cu alloys containing a small amount of Au is commonly used for dental purposes, because this alloy cheaper than Au-base alloys for clinical use. However, the most important characteristic of this alloy is age-hardenability, which is not exhibited by other Ag-base dental alloys. The specimens used were Ag-30Pd-10Cu ternary alloy and Au addition alloy. These alloys were melted and casted by induction electric furnace and centrifugal casting machine in Ar atmosphere. These specimens were solution treated for 2hr at $800^{\circ}C$ and were then quenched into iced water, and aged at 350-$550^{\circ}C$ Age-hardening characteristic of the small Au-containing Ag-Pd-Cu dental alloys were investigated by means of hardness testing, X-ray diffraction and electron microscope observations, electrical resistance, differential scanning calorimetric, energy dispersed spectra and electron probe microanalysis. Principal results are as follows ; Maximum hardening occured in two co-phases of ${\alpha}_2$ + PdCu In stage II, decomposition of the $\alpha$ solid solution to a PdCu ordered phase($L1_o$ type) and an Ag-rich ${\alpha}_2$ phase occurred and a discontinuous precipitation occurred at the grain boundary. From the electron microscope study, it was concluded that the cause of age-hardening in this alloy is the precipitation of the PdCu redered phase, which has AuCu I type face-centered tetragonal structure. Precipitation procedure was ${\alpha}{\to}{\alpha}_1+PdCu{\to}{\alpha}_2+PdCu$ at Pd/Cu = 3 Pd element of Ag-Pd-Cu alloy is more effective dental alloy on anti-corrosion and is suitable to isothermal ageing at $450^{\circ}C$.

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Flexural strength and reliability of highly translucent colored zirconia (고반투명 유색 지르코니아의 굽힘강도와 신뢰도에 대한 연구)

  • Kong, Hyun-Jun
    • Journal of Dental Rehabilitation and Applied Science
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    • v.36 no.1
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    • pp.41-47
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    • 2020
  • Purpose: The purpose of this study was to evaluate the flexural strength and reliability of highly translucent colored zirconia for all ceramic restoration. Materials and Methods: Bar-shaped specimens (25 × 4 × 2.5 mm) were prepared from highly translucent monolithic zirconia. Three experimental groups were set up according to color (shade A0, A1, and A3). For each group, 20 specimens were prepared. Flexural strength was determined using a 3-point flexural test and results were analyzed with one-way ANOVA test. Weibull statistical analysis provided 2 parameter estimates: Weibull modulus and characteristic strength. X-ray diffraction (XRD) analysis was performed. Results: There was statistically significant difference between uncolored (Shade A0) and colored (shade A1 and A3) (P < 0.05), but there was no difference between colored groups (P > 0.05). The uncolored group had higher reliability compared with colored study groups. On x-ray diffraction analysis of each group, typical peaks of tetragonal phase appeared in all groups. Conclusion: Within the limitations of this in vitro study, coloring highly translucent zirconia had significant effect on flexural strength and reliability. Therefore, clinicians should be careful when using highly translucent colored zirconia to prevent breakage of veneering ceramic and enhance aesthetics.

The Study on the Improvement of Piezoelectric and Electrical Characteristics of Bi0.5(Na0.78K0.22)0.5TiO3 Ceramics Modified by the La-based ABO3 Pervskite Structure (La 기반의 ABO3 구조를 갖는 첨가물에 따른 Bi0.5(Na0.78K0.22)0.5TiO3의 압전 및 전기적인 특성 향상 연구)

  • Lee, Ku Tak;Park, Jung Soo;Yun, Ji Sun;Cho, Jeong Ho;Jeong, Young Hun;Paik, Jong Hoo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.27 no.11
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    • pp.707-711
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    • 2014
  • The $0.99Bi_{0.5}(Na_{0.78}K_{0.22})_{0.5}TiO_3-0.01LaAlO_3$, $0.01LaMnO_3$ or $0.01LaFeO_3$ (0.99BNKT-0.01LA, 0.01LM or 0.01LF) ceramics were prepared by a conventional mixed mothod. The structure and morphology of the lead free ceramics were characterized by XRD (X-ray diffraction) and FE-SEM (field emission scanning electron microscopy). XRD results indicated that the BNKT ceramics modified by LA, LM or LF induced a transition from a ferroelectric tetragonal to a non-polar pseudo-cubic phase, leading to decrease in the remnant polarization ($P_r$) and coercive field ($E_c$) in the P-E hysterisis loops. The effects of the BNKT ceramics modified by La-based $ABO_3$ pervskite structure on the electric-field induced strain were investigated, and the largest normalized unipolar strain ($S_{max}/E_{max}$) was found in BNKT-0.01LF ceramic.

The Role of H2O as PCA and the Precipitation Behavior in Mechanically Alloyed Ni-20Cr-20Fe-5Nb Alloy (기계적합금화로 제조된 Ni-20Cr-20Fe-5Nb 합금에서 PCA로서 H2O의 역할과 시효석출거동)

  • Kim Il-Ho;Kwun S.I.;Lee Won-Sik;Chae S.W.;Hwang S.K.;Kim M.H.
    • Journal of Powder Materials
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    • v.13 no.3 s.56
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    • pp.178-186
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    • 2006
  • The effect of use of $H_2O$ as PCA(process control agent) to prevent the carbon contamination during mechanical alloying process and the precipitation behavior in Ni-20Cr-20Fe-5Nb bulk alloy after aging were investigated. NbC and $Cr_2O_3$ were formed during mechanical alloying and consolidation processes in the Ni-20Cr-20Fe-5Nb alloy in which methanol($CH_3OH$) was added as PCA. Formation of NbC in this alloy decreased the amount of Nb dissolved in the Ni matrix. The use of $H_2O$ as PCA in Ni-20Cr-20Fe-5Nb alloy prevented the formation of NbC and increased the hardness. The increase of hardness in this alloy was attributed to the increased amount of Nb dissolved in the Ni matrix. After aging treatment for 20 hours at $600^{\circ}C\;and\;720^{\circ}C$ of Ni-20Cr-20Fe-5Nb bulk alloy in which $H_2O$ added as PCA, ${\gamma}"$$(Ni_3Nb,\;tetragonal)\;and\;{\delta}\;(Ni_3Nb,\;orthorhombic)$ precipitates were formed, respectively. The precipitation temperatures of ${\gamma}"$ and ${\delta}$ in this bulk alloy were lower than those in commercial IN 718 alloy. It seemed that the lower precipitation temperatures for ${\gamma}"$ and ${\delta}$ in this bulk alloy than in commercial IN 718 alloy were due to severe plastic deformation during mechanical alloying.

Effects of the Addition of Alumina on the Mechanical Properties of Cast Zirconia Sintered Body (주입성형한 지르코니아 소결체의 기계적 성질에 미치는 알루미나 첨가의 영향)

  • Lee, Dong-Yoon;Jo, Jun-Ho;Seo, Jeong-Il;Bae, Won-Tae
    • Journal of Technologic Dentistry
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    • v.34 no.2
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    • pp.113-119
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    • 2012
  • Purpose: Zirconia blocks for all ceramic dentures are divided into two groups. One is pre-heated block and the other is binder added block. In this study, the possibility of recycling the remained parts of binder added block after CAD/CAM machining with slip casting process was investigated. Methods: Owing to the binder added block contain large amount of organic matter, Binder burn-out was must be carried out before ball milling for preparing the casting slip. Binder burn-out was accomplished at $600^{\circ}C$ for 10 hours. Ball milling was performed with 5mm zirconia ball and 60mm polyethylene bottle. From 0% to 5% at 1% intervals of alumina was added to zirconia powder for preparing slip. Solid casting was achieved with plaster mold. Cast bodies were dried and sintered at $1,500^{\circ}C$ for 1 hour. Linear shrinkage, apparent porosity, water absorption, bulk density, and flexural strength were tested. Microstructures were observed by SEM, EDS and XRD analysis were executed. Results: Optimum slips for casting was prepared with 300g ball, 100g powder, and 180g distilled water. Cast body without alumina showed 26% of linear shrinkage, 6.07 of apparent density, and 470MPa of three point bend strength. On the other hand, as received zirconia block, which was sintered at the same conditions, showed 23% of linear shrinkage, 6.10 of apparent density, and 680MPa of three point bend strength. When 3% of alumina was added to zirconia, sintered body showed 23% of linear shrinkage, 6.10 of apparent density, and 780MPa of three point bend strength. SEM photomicrographs and EDS analysis showed alumina particles uniformly dispersed in zirconia matrix, and XRD analysis showed no phase transformation of tetragonal zirconia particles was occurred when alumina was added. Conclusion: According to the all of this experimental results, 3% of alumina added cast zirconia body showed excellent mechanical properties more than as received binder containing zirconia block.