• Title/Summary/Keyword: synchrotron X-ray diffraction

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High-Resolution X-Ray Photoelectron Spectroscopy Study of a Sb2Te3 Thin Film with the Polycrystalline Phase (고해상도 엑스선 광전자 분광법을 이용한 다결정구조의 안티몬-테레니움 박막 연구)

  • Lee, Y.M.;Kim, K.;Shin, H.J.;Jung, M.C.;Qi, Y.
    • Journal of the Korean Vacuum Society
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    • v.21 no.6
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    • pp.348-353
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    • 2012
  • We investigated chemical states of a $Sb_2Te_3$ thin film with the polycrystalline phase by using high-resolution x-ray photoelectron spectroscopy with synchrotron radiation. The $Sb_2Te_3$ thin film was formed by sputtering. The rhombohedral phase was confirmed by x-ray diffraction. To remove the surface oxide, we performed $Ne^+$ ion sputtering for 1 hour with the beam energy of 1 kV and post-annealing at $100^{\circ}C$ for 5 min in ultra-high vacuum. We obtained the Te and Sb 4d core-levels spectra with the peaks at the binding energies of 40.4 and 33.0 eV, respectively. The full-width of half maximum of both the Te and Sb $4d_{5/2}$ core-levels is 0.9 eV. The Te and Sb core-levels only show a single chemical state, and we also confirmed the stoichiometry of approximately 2 : 3.

Compressibility of $FeS_{2}$ ($FeS_{2}$의 압축성 연구)

  • Kim, Young-Ho;Hwang, Gil-Chan;Cho, Hyen-Goo
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.3 s.49
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    • pp.189-195
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    • 2006
  • Compression work on a pyrite powder has been carried out using energy dispersive X-ray diffraction (EDXRD) with Mao-Bell type diamond anvil cell (DAC) and synchrotron radiation(SR) at room temperature. It has been reported the bulk moduli of pyrite show the large variations depending on the experimental conditions as well as the apparatus used. Thus, two kinds of sample in different pressure transmitting media of both NaCl and MgO powder emerged in alcoholic fluids were subjected to measure their compressibilities. Bulk moduli thus obtained are 138.9 GPa and 198.2 GPa, respectively, and this result contradicts to the anticipated values according to the hydrostaticity conditions of the sample chamber. This might be due to the alcoholic fluids phase transition mainly with the side effects from the difference of both solid state detector (SSD) used and E*d value applied. All experiments were performed at the Beam Line 1B2 of Pohang Light Source (PLS).

Isotropic Compression Behavior of Lawsonite Under High-pressure Conditions (로소나이트(Lawsonite)의 압력에 따른 등방성 압축거동 연구)

  • Im, Junhyuck;Lee, Yongjae
    • Economic and Environmental Geology
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    • v.49 no.1
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    • pp.23-30
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    • 2016
  • Powder samples of natural lawsonite (Ca-lawsonite, $CaAl_2Si_2O_7(OH)_2{\cdot}H_2O$) was studied structurally up to 8 GPa at room temperature using monochromatic synchrotron X-ray powder diffraction and a diamond anvil cell (DAC) with a methanol : ethanol : water (16 : 3 : 1 by volume) mixture solution as a penetrating pressure transmitting medium (PTM). Upon pressure increase, lawsonite does not show any apparent pressure induced expansion (PIE) or phase transition. Pressure-volume data were fitted to a second-order Birch-Murnaghan equation of state using a fixed pressure derivative of 4 leading to a bulk modulus ($B_0$) of 146(6) GPa. This compression is further characterized to be isotropic with calculated linear compressibilities of ${\beta}^a=0.0022GPa^{-1}$, ${\beta}^b=0.0024GPa^{-1}$, and ${\beta}^c=0.0020GPa^{-1}$.

Effect of vacuum annealing and characterization of diecast ADC12 aluminum alloys (다이캐스팅 공정으로 제조한 ADC12 알루미늄 합금의 물성 향상 및 진공 열처리 효과)

  • Jo, Jihoon;Ham, Daseul;Oh, Seongchan;Cha, Su Yeon;Kang, Hyon Chol
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.1
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    • pp.24-31
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    • 2021
  • We report structural, mechanical, and thermal properties of diecast ADC12 aluminum alloys characterized using synchrotron X-ray diffraction (XRD), scanning electron microscopy, energy dispersive X-ray (EDX) analysis, thermal conductivity (λ), Vickers hardness (Hv), and stress-strain measurements. We also studied the effect of post-annealing performed in a vacuum atmosphere on the mechanical properties of diecast ADC12 alloys. EDX and XRD results revealed that Al2Cu and AlCu3 grains are formed, well dispersed in Al base and highly crystalline. Ultimate tensile strength (UTS) of 307.9 ± 9.1 MPa and elongation of 2.98 ± 0.62 % were estimated. λ was 129.3 ± 0.27 W/m·K and Hv was approximately 130. Both values were significantly higher than the reported values. At annealing temperatures ranging from 25 to 200℃, UTS and Hv values remained constant, while as the annealing temperature increased to 500℃, these values gradually decreased. This is because stabilization of the microstructure improves toughness and ductility.

Comparative Compressional Behavior of Zeolite-W in Different Pressure-transmitting Media (제올라이트-W의 압력전달매개체에 따른 체적탄성률 비교 연구)

  • Seoung, Donghoon;Kim, Hyeonsu;Kim, Pyosang;Lee, Yongmoon
    • Korean Journal of Mineralogy and Petrology
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    • v.34 no.3
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    • pp.169-176
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    • 2021
  • This study aimed to fundamentally understand structural changes of zeolite under pressure and in the presence of different pressure-transmitting media (PTM) for application studies such as immobilization of heavy metal cation or CO2 storage using pressure. High-pressure X-ray powder diffraction study was conducted on the zeolite-W (K6.4Al6.5Si25.8O64× 15.3H2O, K-MER) to understand linear compressibility and the bulk moduli in different PTM conditions. Zeolite-w is a synthetic material having the same framework as natural zeolite merlinoite ((K, Ca0.5, Ba0.5, Na)10 Al10Si22O64× 22H2O). The space group of the sample was identified as I4/mmm belonging to the tetragonal crystal system. Water, carbon dioxide, and silicone-oil were used as pressure-transmitting media. The mixture of sample and each PTM was mounted in a diamond anvil cell (DAC) and then pressurized up to 3 GPa with an increment of ca. 0.5 GPa. Pressure-induced changes of powder diffraction patterns were measured using a synchrotron X-ray light source. Lattice constants, and bulk moduli were calculated using the Le-Bail method and the Birch-Murnaghan equation. In all PTM conditions, linear compressibility of c-axis (𝛽c) was 0.006(1) GPa-1 or 0.007(1) GPa-1. On the other hand, the linear compressibility of a(b)-axis (𝛽a) was 0.013(1) GPa-1 in silicone-oil run, which is twice more compressible than the a(b)-axis in water and carbon dioxide runs, 𝛽a = 0.006(1) GPa-1. The bulk moduli were measured as 50(3) GPa, 52(3) GPa, and 29(2) GPa in water, carbon dioxide, and silicone-oil run, respectively. The orthorhombicities of ac-plane in the water, and carbon dioxide runs were comparatively constant, near 0.350~0.353, whereas the value decreased abruptly in the silicone-oil run following formula, y = -0.005(1)x + 0.351(1) by non-penetrating pressure fluid condition.

Characterization of Li+-ion Exchanged Zeolite Y using Organic Solvents

  • Kim, Hu Sik;Lee, Seok Hee;Park, Kyun Hye;Park, Yong Hyun;Park, Jun Woo;Hwang, Ji Hyun;Park, Jong Sam;Choi, Sik Young;Lim, Woo Taik
    • Korean Journal of Soil Science and Fertilizer
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    • v.48 no.3
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    • pp.180-188
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    • 2015
  • To investigate the tendency of $Li^+$ exchange from polar organic solvents, $Li^+$-ion exchange into zeolite Y (Si/Al = 1.56) was attempted by undried methanol (crystal 1) and formamide (crystal 2) solvent. Two single crystals of Na-Y were treated with 0.1 M LiNO3 in each of the two solvents at 323 K, followed by vacuum dehydration at 723 K. Their structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd{\bar{3}}m$, at 100(1) K. In both structures, $Li^+$ for $Na^+$ ions filled preferentially sites I' and II. The remaining $Na^+$ ions occupied sites I', II, and III' in both structures, in additional to above sites, and $Na^+$ ions occupied site I in crystal 2. While the 68 % exchange of $Li^+$ for $Na^+$ was achieved from undried methanol, only 40 % exchange was observed from undried formamide, indicating that the undried methanol was more effective than undried formamide as solvent for $Li^+$ exchange under the conditions employed.

The Effect of Co2+-Ion Exchange Time into Zeolite Y (FAU, Si/Al = 1.56): Their Single-Crystal Structures

  • Seo, Sung Man;Kim, Hu Sik;Chung, Dong Yong;Suh, Jeong Min;Lim, Woo Taik
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.243-249
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    • 2014
  • Three single crystals of fully dehydrated $Co^{2+}$-exchanged zeolite Y (Si/Al = 1.56) were prepared by the exchange of $Na_{75}$-Y ($|Na_{75}|[Si_{117}Al_{75}O_{384}]$-FAU) with aqueous streams 0.05 M in $Co(NO_3)_2$, pH = 5.1, at 294 K for 6 h, 12 h, and 18 h, respectively, followed by vacuum dehydration at 673 K. Their single-crystal structures were determined by synchrotron X-ray diffraction techniques in the cubic space group Fd3m at 100(1) K. They were refined to the final error indices $R_1/wR_2$ = 0.0437/0.1165, 0.0450/0.1228, and 0.0469/0.1278, respectively. Their unit-cell formulas are $|Co_{29.1}Na_{11.8}H_{5.0}|[Si_{117}Al_{75}O_{384}]$-FAU, $|Co_{29.8}Na_{11.0}H_{4.4}|[Si_{117}Al_{75}O_{384}]$-FAU, and $|Co_{30.3}Na_{9.5}H_{4.9}|[Si_{117}Al_{75}O_{384}]$-FAU, respectively. In all three crystals, $Co^{2+}$ ions occupy sites I, I' and II; $Na^+$ ions are also at site II. The tendency of $Co^{2+}$ exchange slightly increases with increasing contact time as $Na^+$ content and the unit cell constant of the zeolite framework decrease.

Epitaxial Growth of ZnO Nanowires on Sapphire (001) Substrates Using a Hydrothermal Process (수열합성법을 이용한 산화아연 나노와이어의 에피택시 성장)

  • Ham, Daseul;Jeong, Byeong Eon;Yang, Myeong Hun;Lee, Jong Kwan;Choi, Young Bin;Kang, Hyon Chol
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.31 no.7
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    • pp.502-509
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    • 2018
  • Epitaxial ZnO nanowires (NWs) were synthesized on sapphire (001) substrates using a hydrothermal process. The effects of the pH value of the precursor solution on the structural and optical properties of the resulting NWs was studied. The epitaxial relationship and the domain matching configuration between the sapphire (001) substrate and the as-grown ZnO NWs were determined using synchrotron X-ray diffraction measurements. The (002) plane of $w{\ddot{u}}rtzite$ ZnO NW grows in the surface normal direction parallel to the sapphire (001) direction. However, three types of in-plane domain matching configurations were observed, such as the on-position, $30^{\circ}$-rotated position, and ${\pm}8.5^{\circ}$-rotated position relative to the on-position, which might be attributed to inheriting the in-plane domain configuration of the ZnO seed layer.

Single-Crystal Structure of |Li50Na25|[Si117Al75O384]-FAU

  • Kim, Hu Sik;Suh, Jeong Min;Kang, Jum Soon;Lim, Woo Taik
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.12-19
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    • 2013
  • The single-crystal structure of fully dehydrated partially $Li^+$-exchanged zeolite Y, ${\mid}Li_{50}Na_{25}{\mid}[Si_{117}Al_{75}O_{384}]$-FAU, was determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd\bar{3}m$ at 100(1) K. Ion exchange was accomplished by flowing stream of 0.1 M aqueous $LiNO_3$ for 2 days at 293 K, followed by vacuum dehydration at 623 K and $1{\times}10^{-6}$ Torr for 2 days. The structure was refined using all intensities to the final error indices (using only the 801 reflections with ($F_o$ > $4{\sigma}(F_o)$) $R_1/R_2=0.043/0.140$. The 50 $Li^+$ ions per unit cell are found at three different crystallographic sites. The 19 $Li^+$ ions occupy at site I' in the sodalite cavity: the $Li^+$ ions are recessed 0.30 ${\AA}$ into the sodalite cavity from their 3-oxygens plane (Li-O = 1.926(5) ${\AA}$ and $O-Li-O=117.7(3)^{\circ}$). The 20 $Li^+$ ions are found at site II in the supercage, being recessed 0.23 ${\AA}$ into the supercage (Li-O = 2.038(5) ${\AA}$ and $O-Li-O=118.7(3)^{\circ}$). Site III' positions are occupied by 11 $Li^+$ ions: these $Li^+$ ions bind strongly to one oxygen atom (Li-O = 2.00(8) ${\AA}$). About 25 $Na^+$ ions per unit cell are found at four different crystallographic sites: 4 $Na^+$ ions are at site I, 5 at site I', 12 at site II, and the remaining 4 at site III'.

The Study on Phase Transition Pressure of Donor doped Pb(Zr0.52Ti0.48)O3 Ceramics with Diamond Anvil Cell (다이아몬드 엔빌 셀을 이용한 Donor doped Pb(Zr0.52Ti0.48)O3 세라믹스의 상전이 압력 연구)

  • Cho, Kyung-Ho;Ko, Young-Ho;Seo, Chang-Eui;Kim, Kwang-Joo
    • Journal of the Korean Ceramic Society
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    • v.48 no.5
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    • pp.471-478
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    • 2011
  • Investigations of crystal structure and phase transition of $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics doped with A-site substitution impurity (La, Nd) or B-site substitution impurity (Sb, Nb) at 2 mol% concentration were carried out. X-ray diffraction patterns of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics have been measured at pressures up to ~5 GPa with diamond anvil cell and synchrotron radiation. The patterns were obtained at room temperature using methanol-ethanol mixture as pressure-transmitting media. In order to refine the crystal structure, Rietveld analysis has been performed. The structures of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics are tetragonal in space group P4mm at ambient pressure and are transformed into a cubic phase in space group Pm$\bar{3}$m as the pressure increases. In this study, when A-site substitution donor $La^{3+}$ or $Nd^{3+}$ ion was added to $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics, the phase transition phenomena showed up at the pressure of 2.5~4.6 GPa, but when B-site substitution donor $Nb^{5+}$ or $Sb^{5+}$ ion was added to it, the phase transition appeared at relatively lower pressure of 1.7~2.6 GPa.