• Title/Summary/Keyword: HR-XRD

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Synthesis of the Water Dispersible L-Valine Capped ZnS:Mn Nanocrystal and the Crystal Structure of the Precursor Complex: [Zn(Val)2(H2O)]

  • Hwang, Cheong-Soo;Lee, Na-Rae;Kim, Young-Ah;Park, Youn-Bong
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1809-1814
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    • 2006
  • The L-Valinate anion coordinating zinc complex, [$Zn(val)_2(H-2O)$], was isolated and structurally characterized by single crystal X-ray crystallography. The crystal possess orthorhombic symmetry with a space group $P2_12_12_1$, Z = 4, and a = 7.4279(2)$\AA$, b = 9.4342(2)$\AA$, c =20.5862(7)$\AA$ respectively. The compound features a penta-coordinate zinc ion in which the two valine anion molecules are directly coordinating the central zinc metal ion via their N (amine) and O (carboxylate) atoms, and an additional coordination to zinc is made by water molecule (solvent) to form a distorted square pyramidal structure. In addition, further synthesis of the valine capped ZnS:Mn nanocrystal from the reaction of [$Zn(val)_2(H-2O)$] precursor with $Na_2S$ and 1.95 weight % of $Mn^{2+}$ dopant is described. Obtained valine capped nanocrystal was water dispersible and was optically characterized by UV-vis and solution PL spectroscopy. The solution PL spectrum for the valine capped ZnS:Mn nanocrystal showed an excitation peak at 280 nm and a very narrow emission peak at 558 nm respectively. The measured and calculated PL efficiency of the nanocrystal in water was 15.8%. The obtained powders were characterized by XRD, HR-TEM, and EDXS analyses. The particle size of the nanocrystal was also measured via a TEM image. The measured average particle size was 3.3 nm.

Reaction between Calcium-doped Lanthanum Chromite and Yttria Stabilized Zirconia (칼슘이 첨가된 란탄-아크롬산 염과 이트리아 안정화 지르코니아 계면간의 반응)

  • Choe, Jin-Sam
    • Korean Journal of Materials Research
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    • v.11 no.6
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    • pp.460-464
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    • 2001
  • The ceramic diffusion coupling with the green body of calcium-doped lanthanum chromite(La$_{0.8}$Ca$_{0.2}$CrO$_3$CLC- G) and sintered calcium-doped lanthanum chromite(La$_{0.8}$Ca$_{0.2}$CrO$_3$ CLC) by Pechini's method on yttria stabilized zirconia(YSZ) plate has been investigated. The X-ray diffraction pattern of CLC sides at the reacted CLC-G/ CLC and CLC/YSZ interface were identified as La$_{1-x}$ Ca$_{x}$CrO$_3$ and the unreacted YSZ side was cubic-ZrO$_2$ at the treated condition, 1300~1500 C for 10 hr in air, respectively. The order of migration components between CLC/YSZ interface was Zr>La>>Cr>>>Ca and these changes were not dependent upon the treated conditions. The grain shape and size at the interface of CLC-G/CLC was appeared to have a uniform distribution with increasing temperature. The bonding reaction of YSZ/CLC was occurred without a large amount change of the compositions in SEM photos.os.otos.os.

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A Study on the Dielectric and Piezoelectric properties of the Pb(SbS11/2TSnS11/2T)OS13T-PbTiOS13T-PbZrOS13T Ceramics (Pb(Sb1/2Sn1/2)O3-PbTiO3-PbZrO3 세라믹스의 유전 및 압전 특성에 관한 연구)

  • 정장호;류기원;이성갑;이영희
    • The Transactions of the Korean Institute of Electrical Engineers
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    • v.41 no.5
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    • pp.517-524
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    • 1992
  • In this study, 0.10Pb(SbS11/2TSnS11/2T)OS13T-(0.90-x)PbZrOS13T (0.25 x 0.40) ceramics were fabricated by the atmospheric method. The sintering temperature and time were 1250[$^{\circ}C$] and 2[2hr], respectively. The structureal, dielectric and piezoelectric properties with composition of PbTiOS13T were studied. As the results of XRD ans SEM, the crystal structure of a specimen was rhombohedral, lattice constant and average grain size were decreased with increasing the contents of PbTiOS13T. Relative dielectric constant and Curie temperature were increased with increasing the contents of PbTiOS13T, 0.10PSS-0.40PT-0.50PZ specimen had the highest values of 904 and 265[$^{\circ}C$], respectively. In increasing of PbTiOS13T contents form 25[mol%] to 40[mol%], piezoelectric charge constant and electromechanical coupling factors were increased form 114[pC/N] to 142[pC/N], 17[%] to 24[%] and mechanical quality factor were decreased with increasing the contents of PbTiOS13T. In the 0.10PSS-0.40PT-0.50PZ specimens, those values were 14.2[kV/cm] and 9.43[x10S0-6TC/cmS02T], resectively.

Microwave Dielectric Properties of (1-X)$Mg_4Ta_2O_{9-x}TiO_2$(X=0, 0.3, 0.4) Ceramics with Sintering Temperature (소결온도에 따른 (1-x)$Mg_4Ta_2O_{9-x}TiO_2$(X=0, 0.3, 0.4) 세라믹스의 마이크로파 유전특성)

  • 김재식;최의선;이문기;이영희
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.53 no.2
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    • pp.67-72
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    • 2004
  • The microwave dielectric properties and microstructure of the (1-x)$Mg_4Ta_2O_{9-x}TiO_2$(X=0, 0.3, 0.4) ceramic were, investigated. The specimens were prepared by the conventional mixed oxide method with sintering temperature of $1350^{\circ}C$$1425^{\circ}C$. According to the XRD patterns, the (1-x)$Mg_4Ta_2O_{9-x}TiO_2$(X=0, 0.3, 0.4) ceramics have the $Mg_4Ta_2O_{9}$ phase(hexagonal). The dielectric constant($\varepsilon$$_{\gamma}$) and density increased with sintering temperature and mole fraction of x. To improve the quality factor and the temperature coefficient of resonant frequency, TiO$_2$($\varepsilon_{r}$=100, $Q{\times}f_{r}$=40,000GHz, $\tau$$_{f}$=+450 ppm/$^{\circ}C$) was added in $Mg_4Ta_2O_{9}$ ceramics. In the case of the $0.7Mg_4Ta_2O_{9}$-$0.3TiO_2$ and the $0.6Mg_4Ta_2O_{9}$-$0.4TiO_2$ceramics sintered at $1400^{\circ}C$ for 5hr., the microwave dielectric properties were $\varepsilon$$_{\gamma}$=11.72, $Q{\times}f_{r}$=126,419GHz, $\tau_{f}$=-31.82 ppm/$^{\circ}C$ and $\varepsilon_{r}$=12.19, $Q{\times}f_{r}$=109,411GHZ, $\tau$$_{f}$= -17.21 ppm/$^{\circ}C$, respectively.

Deposition of ZrO$_2$ and TiO$_2$ Thin Films Using RF Magnet ron Sputtering Method and Study on Their Structural Characteristics

  • Shin, Y.S.;Jeong, S.H.;Heo, C.H.;Bae, I.S.;Kwak, H.T.;Lee, S.B.;Boo, J.H.
    • Journal of the Korean institute of surface engineering
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    • v.36 no.1
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    • pp.14-21
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    • 2003
  • Thin films of ZrO$_2$ and TiO$_2$ were deposited on Si(100) substrates using RF magnetron sputtering technique. To study an influence of the sputtering parameters, systematic experiments were carried out in this work. XRD data show that the $ZrO_2$ films were mainly grown in the [111] orientation at the annealing temperature between 800 and $1000^{\circ}C$ while the crystal growth direction was changed to be [012] at above $1000^{\circ}C$. FT-IR spectra show that the oxygen stretching peaks become strong due to $SiO_2$ layer formation between film layers and silicon surface after annealing, and proved that a diffusion caused by either oxygen atoms of $ZrO_2$ layers or air into the interface during annealing. Different crystal growth directions were observed with the various deposition parameters such as annealing temperature, RF power magnitude, and added $O_2$ amounts. The growth rate of $TiO_2$ thin films was increased with RF power magnitude up to 150 watt, and was then decreased due to a sputtering effect. The maximum growth rate observed at 150 watt was 1500 nm/hr. Highly oriented, crack-free, stoichiometric polycrystalline $TiO_2$<110> thin film with Rutile phase was obtained after annealing at $1000^{\circ}C$ for 1 hour.

Fabrication of Ultra Fine β-phase Ti-Nb-Sn-HA Composite by Pulse Current Activated Sintering

  • Woo, Kee-Do;Wang, Xiaopeng;Kang, Duck-Soo;Kim, Sang-Hyuk;Woo, Jeong-Nam;Park, Sang-Hoon;Liuc, Zhiguang
    • Journal of Powder Materials
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    • v.17 no.6
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    • pp.443-448
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    • 2010
  • The $\beta$ phase Ti-Nb-Sn-HA bio materials were successfully fabricated by high energy mechanical milling and pulse current activated sintering (PCAS). Ti-6Al-4V ELI alloy has been widely used as biomaterial. But the Al has been inducing Alzheimer disease and V is classified as toxic element. In this study, ultra fine sized Ti-Nb-Sn-HA powder was produced by high energy mechanical milling machine. The $\beta$ phase Ti-Nb-Sn-HA powders were obtained after 12hr milling from $\alpha$ phase. And ultra fine grain sized Ti-Nb-Sn-HA composites could be fabricated using PCAS without grain growth. After sintering, the microstructures and phase-transformation of Ti-Nb-Sn-HA biomaterials were analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). The relative density was obtained by Archimedes principle and the hardness was measured by Vickers hardness tester. The $\beta$-Ti phase was obtained after 12h milling. As result of hardness and relative density, 12h milled Ti-Nb-Sn-HA composite has the highest values.

Characteristics and Processing Effects Of $HfO_2$ Thin Films grown by Metal-Organic Molecular Beam Epitaxy (금속 유기 분자 빔 에피택시로 성장시킨 $HfO_2$ 박막의 특성과 공정변수가 박막의 성장 및 특성에 미치는 영향)

  • Kim, Myoung-Seok;Ko, Young-Don;Nam, Tae-Hyoung;Jeong, Min-Chang;Myoung, Jae-Min;Yun, Il-Gu
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.07a
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    • pp.74-77
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    • 2004
  • [ $HfO_2$ ] dielectric layers were grown on the p-type Si(100) substrate by metalorganic molecular beam epitaxy(MOMBE). Hafnium $t-butoxide[Hf(O{\cdot}t-C_4H_9)_4]$ was used as a Hf precursor and Argon gas was used as a carrier gas. The thickness of the layers was measured by scanning electron microscopy (SEM) and high-resolution transmission electron measurement(HR-TEM). The properties of the $HfO_2$ layers were evaluated by X-ray diffraction(XRD), high frequency capacitance-voltage measurement(HF C-V), current-voltage measurement(I-V), and atomic force measurement(AFM). HF C-V measurements have shown that $HfO_2$ layer grown by MOMBE has a high dielectric constant(k=19-21). The properties of $HfO_2$ films are affected by various process variables such as substrate temperature, bubbler temperature, Ar, and $O_2$ gas flows. In this paper, we examined the relationship between the $O_2/Ar$ gas ratio and the electrical properties of $HfO_2$.

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Synthesis of Boron-doped Crystalline Si Nanoparticles Synthesized by Using Inductive Coupled Plasma and Double Tube Reactor (유도결합 플라즈마와 이중관 반응기를 이용하여 제조한 보론-도핑된 결정질 실리콘 나노입자의 합성)

  • Jung, Chun-Young;Koo, Jeong-Boon;Jang, Bo-Yun;Lee, Jin-Seok;Kim, Joon-Soo;Han, Moon-Hee
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.27 no.10
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    • pp.662-667
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    • 2014
  • B-doped Si nanoparticles were synthesized by using inductive coupled plasma and specially designed double tube reactor, and their microstructures were investigated. 0~10 sccm of $B_2H_6$ gas was injected during the synthesis of Si nanoparticles from $SiH_4$ gas. Highly crystalline Si nanoparticles were synthesized, and their crystallinity did not change with increase of $B_2H_6$ flow rates. From SEM measurement, their particle sizes were approximately 30 nm regardless of $B_2H_6$ flow rates. From SIMS analysis, almost saturation of B in Si nanoparticles was detected only when 1 sccm of $B_2H_6$ was injected. When $B_2H_6$ flow rate exceeded 5 sccm, higher concentration of B than solubility limit was detected even if any secondary phase was not detected in XRD or HR-TEM results. Due to their high electronic conductivity, those heavily B-doped Si nanoparticles can be a potential candidate for an active material in Li-ion battery anode.

Development of Ultra-Thin TiO2 Coated WO3 Inverse Opal Photoelectrode for Dye-Sensitized Solar Cells (염료감응형 태양전지로의 응용을 위한 얇은 TiO2가 코팅 된 WO3 역오팔 광전극의 개발)

  • Arunachalam, Maheswari;Kwag, Seoui;Lee, Inho;Kim, Chung Soo;Lee, Sang-Kwon;Kang, Soon Hyung
    • Korean Journal of Materials Research
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    • v.29 no.8
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    • pp.491-496
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    • 2019
  • In this study, we prepare pure $WO_3$ inverse opal(IO) film with a thickness of approximately $3{\mu}m$ by electrodeposition, and an ultra-thin $TiO_2$ layer having a thickness of 2 nm is deposited on $WO_3$ IO film by atomic layer deposition. Both sets of photoelectrochemical properties are evaluated after developing dye-sensitized solar cells(DSSCs). In addition, morphological, crystalline and optical properties of the developed films are evaluated through field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HR-TEM), X-ray diffraction(XRD) and UV/visible/infrared spectrophotometry. In particular, pure $WO_3$ IO based DSSCs show low $V_{OC}$, $J_{SC}$ and fill factor of 0.25 V, $0.89mA/cm^2$ and 18.9 %, achieving an efficiency of 0.04 %, whereas the $TiO_2/WO_3$ IO based DSSCs exhibit $V_{OC}$, $J_{SC}$ and fill factor of 0.57 V, $1.18mA/cm^2$ and 50.1 %, revealing an overall conversion efficiency of 0.34 %, probably attributable to the high dye adsorption and suppressed charge recombination reaction.

Effects of Co/Fe Sulfate Pigments on the Colour and Phase of Porcelain (Co/Fe 황화물의 혼합안료에 의한 도자기 표면의 상형성과 색변화)

  • Kim, Nam-Heun;Shin, Dae-Yong;Kim, Kyung-Nam
    • Korean Journal of Materials Research
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    • v.32 no.8
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    • pp.354-360
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    • 2022
  • In this study, an Co/Fe coated porcelain using a cobalt and ferrous sulfate was sintered at 1,250 ℃. The specimens were investigated by HR-XRD, FE-SEM (EDS), Dilatometer, and UV-vis spectrophotometer. The surface of the porcelain was uniformly fused with the pigment, and white ware and celadon body specimens were densely fused to a certain thickness from the surface. Other new compounds were produced by the chemical reaction of cobalt/ferrous sulfate with the porcelain body during the sintering process. These compounds were identified as cobalt ferrite spinel phases for white ware and white mixed ware, and an andradite phase for the celadon body, and the amorphous phase, respectively. As for the color of the specimens coated with cobalt and ferrous mixed pigments, it was found that the L* value was greatly affected by the white ware, and the a* and b* values were significantly changed in the celadon body. The L* values of the specimens fired with pure white ware, celadon body, and white mix ware were 72.1, 60.92, 82.34, respectively. The C7F3 pigment coated porcelain fired at 1,250 ℃ had L* values of 39.91, 50.17, and 40.53 for the white ware, celadon body, and white mixed ware, respectively; with a* values of -1.07, -2.04, and -0.19, and at b* values of 0.46 and 6.01, it was found to be 4.03. As a new cobalt ferrite spinel phase was formed, it seemed to have had a great influence on the color change of the ceramic surface.