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

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Irradiation enduced In-plane magnetization in Fe/MgO/Fe/Co multilayers

  • Singh, Jitendra Pal;Lim, Weon Cheol;Song, Jonghan;Kim, Jaeyeoul;Asokan, K.;Chae, Keun Hwa
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.188.1-188.1
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    • 2015
  • For present investigation Fe/MgO/Fe/Co multilayer stack is grown on Si substrate using e-beam evaporation in ultrahigh vacuum. This stack is irradiated perpendicularly by 120 MeV $Ag^{8+}$ at different fluences ranging from $1{\times}10^{11}$ to $1{\times}10^{13}ions/cm^2$ in high vacuum using 15UD Pelletron Accelerator at Inter University Accelerator Centre, New Delhi. Magnetic measurements carried out on pre and post irradiated stacks show significant changes in the shape of perpendicular hysteresis which is relevant with previous observation of re-orientation of magnetic moment along the direction of ion trajectory. However increase in plane squareness may be due to the modification of interface structure of stacks. X-ray reflectivity measurements show onset of interface roughness and interface mixing. X-ray diffraction measurements carried out using synchrotron radiation shows amorphous nature of MgO and Co layer in the stack. Peak corresponding body centered Fe [JCPDS-06-0696] is observed in X-ray diffraction pattern of pre and post irradiated stacks. Peak broadening shows granular nature of Fe layer. Estimated crystallite size is $22{\pm}1nm$ for pre-irradiated stack. Crystallite size first increases with irradiation then decreases. Structural quality of these stacks was further studied using transmission electron microscopic measurements. Thickness from these measurements are 54, 36, 23, 58 and 3 nm respectively for MgO, Fe, MgO, Fe+Co and Au layers in the stack. These measurements envisage poor crystallinity of different layers. Interfaces are not clear which indicate mixing at interface. With increase fluence mixing and diffusion was increased in the stack. X-ray absorption spectroscopic measurements carried out on these stacks show changes of Fe valence state after irradiation along with change of O(2p)-metal (3d) hybridized state. Valence state change predicts oxide formation at interface which causes enhanced in-plane magnetization.

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Elastic Behavior of Zeolite Mesolite under Hydrostatic Pressure (제올라이트 메소라이트의 수압 하 탄성특성)

  • Lee, Yong-Jae;Lee, Yong-Moon;Seoung, Dong-Hoon;Jang, Young-Nam
    • Economic and Environmental Geology
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    • v.42 no.5
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    • pp.509-512
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    • 2009
  • Powder diffraction patterns of the zeolite mesolite ($Na_{5.33}Ca_{5.33}Al_{16}Si_{24}O_{80}{\cdot}21.33H_2O$), with a natrolite framework topology were measured as a function of pressure up to 5.0 GPa using a diamond-anvil cell and a $200{\mu}m$-focused monochromatic synchrotron X-ray. Under the hydrostatic conditions mediated by pore-penetrating alcohol and water mixture, the elastic behavior of mesolite is characterized by continuous volume expansion between ca. 0.5 and 1.5 GPa, which results from expansion in the ab-plane and contraction along the c-axis. Subsequent to this anomalous behavior, changes in the powder diffraction patterns suggest possible reentrant order-disorder transition. The ordered layers of sodium- and calcium-containing channels in a 1:2 ratio along the b-axis attribute to the $3b_{natrolite}$ cell below 1.5 GPa. When the volume expansion is completed above 1.5 GPa, such characteristic ordering reflections disappear and the $b_{natrolite}$ cell persists with marginal volume contraction up to ca. 2.5 GPa. Further increase in pressure leads to progressive volume contraction and appears to generate another set of superlattice reflections in the $3c_{natrolite}$ cell. This suggests that mesolite in the pressure-induced hydration state experiences order-disorder-order transition involving the motions of sodium and calcium cations either through cross-channel diffusion or within the respective channels.

Phase Transition Study on Ilmenite under High Pressure and Temperature (고온-고압하에서 티탄철석에 대한 상면이 연구)

  • Kim, Young-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.3
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    • pp.161-169
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    • 2002
  • high pressure and temperature conditions. However, those results are not consistent with one another, and phase boundary between ilmenite and perovskite phases determined only from the quenching method may be not so reliable at all. Therefore, in-situ high pressure-temperature (hP-T) X-ray diffraction measurements were performed up to 19 GPa and $700^{\circ}C$ in a large volume press apparatus using synchrotron radiation. Experimental results show that perovskite phase is stable at pressures above 16 GPa, and transforms back to $LiNbO_3$phase near 15 CPa at room temperature, and that the perovskite-ilmenite transition is back and forth near 15 CPa at $500^{\circ}C$. LiNbO$_3$phase transforms to ilmenite at 13 CPa and $300^{\circ}C$ and at 10.8 CPa and $400^{\circ}C$, respectively. These data indicate that $LiNbO_3$phase may have a stability region in the hP-T phase diagram and that the perovskite-ilmenite phase boundary would be quite different from that previously reported.

Effect of Thermal Treatment on the Performance and Nanostructures in Polymer Solar Cells with PTB7-Th:PC71BM Bulk Heterojunction Layers

  • Lee, Sooyong;Seo, Jooyeok;Jeong, Jaehoon;Lee, Chulyeon;Song, Myeonghun;Kim, Hwajeong;Kim, Youngkyoo
    • Current Photovoltaic Research
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    • v.5 no.3
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    • pp.69-74
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    • 2017
  • Here we report the influence of thermal treatment on the performance of high efficiency polymer solar cells with the bulk heterojunction films of poly[4,8-bis(5-(2-ethylhexyl)thiophen-2-yl)benzo[1,2-b:4,5-b'] dithiophene-alt-3-fluorothieno[3,4-b]thiophene-2-carboxylate] (PTB7-Th) and [6,6]-phenyl $C_{71}$ butyric acid methyl ester ($PC_{71}BM$). The crystalline nanostructure of PTB7-Th:$PC_{71}BM$ layers, which were annealed at three different temperatures, was investigated by employing synchrotron radiation grazing incidence X-ray diffraction (GIXD) technique. Results showed that the device performance was slightly reduced by thermal annealing at $50^{\circ}C$ but became significantly poor by thermal annealing at $100^{\circ}C$. The poor device performance by thermal annealing was attributed to the collapse in the crystalline nanostructure of PTB7-Th in the PTB7-Th:$PC_{71}BM$ layers as evidenced by the GIXD measurements that exhibited huge reduction in the intensity of PTB7-Th (100) peak even at $50^{\circ}C$.

Single-Crystal Structures of Li+-exchanged Zeolite X (FAU, Si/Al = 1.09) from Aqueous Solution Depends on Ion-exchange Temperatures at 293 and 333 K

  • Kim, Hu-Sik;Ko, Seong-Oon;Lim, Woo-Taik
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3303-3310
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    • 2012
  • Two single crystals of fully dehydrated partially $Li^+$-exchanged zeolite X were prepared by the exchange of Na-X, $Na_{92}Si_{100}Al_{92}O_{384}$ (Si/Al = 1.09), with $Li^+$ using aqueous 0.1 M $LiNO_3$ at 293 (crystal 1) and 333 K(crystal 2), followed by vacuum dehydration at 623 K and $1{\times}10^{-6}$ Torr for 2 days. Their structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd{\overline{3}}$ at 100(1) K. Their structures were refined using all intensities to the final error indices (using the 1281 and 883 reflections for which ($F_o$ > $4{\sigma}(F_o)$) $R_1/R_2$ = 0.075/0.244 and 0.074/0.223 for crystals 1 and 2, respectively. Their compositions are seen to be ${\mid}Li_{86}Na_6{\mid}[Si_{100}Al_{92}O_{384}]$-FAU and ${\mid}Li_{87}Na_5{\mid}[Si_{100}Al_{92}O_{384}]$-FAU, respectively. In crystal 1, 17 $Li^+$ ions per unit cell are at site I', 15 another site I', 30 at site II, and the remaining 16 at site III; 2 $Na^+$ ions are at site II and the remaining 4 at site III'. In crystal 2, 32 and 30 $Li^+$ ions per unit cell fill sites I' and II, respectively, and the remaining 25 at site III'; 2 and 3 $Na^+$ ions are found at sites II and III', respectively. The extent of $Li^+$ exchange increases slightly with increasing ion exchange temperature from 93% to 95%.

Crystallization and Preliminary X-Ray Diffraction Analysis of 5,10-Methylenetetrahydrofolate Dehydrogenase/Cyclohydrolase from Thermoplasma acidophilum DSM 1728

  • Kim, Jae-Hee;Sung, Min-Woo;Lee, Eun-Hye;Nam, Ki-Hyun;Hwang, Kwang-Yeon
    • Journal of Microbiology and Biotechnology
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    • v.18 no.2
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    • pp.283-286
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    • 2008
  • The methylenetetrahydrofolate dehydrogenase/cyclohydrolase (MTHFDC) from the thermoacidophilic archaeon Thermoplasma acidophilum is a 30.6kDa molecular-mass enzyme that sequentially catalyzes the conversion of formyltetrahydrofollate to methylenetetrahydrofolate, with a preference for NADP as a cofactor, rather than NAD. In order to elucidate the functional and structural features of MTHFDC from archaeons at a molecular level, it was overexpressed in Escherichia coli and crystallized in the presence of its cofactor, NADP, at 295K using polyethylene glycol (PEG) 4000 as a precipitant. The crystal is a member of the monoclinic space group $P2_1$, with the following unit cell parameters: $a=66.333{\AA},\;b=52.868{\AA},\;c=86.099{\AA},\;and\;{\beta}=97.570^{\circ}$, and diffracts to a resolution of at least $2.40{\AA}$ at the synchrotron. Assuming a dimer in the crystallographic asymmetric unit, the calculated Matthews parameter $(V_M)\;was\;2.44{\AA}^3/Da$ and the solvent content was 49.7%.

Influence on mechanical property of C-S-H(I) due to its structural modification (C-S-H(I)의 분자구조변형을 통한 기계적 거동의 변화)

  • Oh, Jae-Eun;Monteiro, Paulo J.M.
    • Proceedings of the Korea Concrete Institute Conference
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    • 2010.05a
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    • pp.473-474
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    • 2010
  • This high pressure synchrotron X-ray diffraction study examined the change of bulk modulus of C-S-H(I), core material creating strength in alkali-activated slag cement as well as structural model of C-S-H, mainly attributed to Al-substitution for Si, which occurs at the bridging tetrahedral sites in dreierketten silicate chains in the nanostructure of C-S-H(I). This study presents that Al-substitution in C-S-H(I) does not affect the bulk modulus of C-S-H(I), which is surprising because many researchers have expected that Al-substitution should induce some critical change in mechanical properties of C-S-H(I).

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A Study on the SH Structure Change of Myosin Head by Temperature Effect (온도 영향에 따른 Myosin Head의 SH 구조 변화 연구)

  • 김덕술;송주영
    • Journal of Life Science
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    • v.9 no.6
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    • pp.646-652
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    • 1999
  • The effect of temperature on the structure change of the SH of myosin head have been investigated with improved resolution by x-ray diffraction using synchrotron radiation. The movement of myosin head and conformational change of contractile molecules were occurred in the muscle contraction. IASL (iodo acetamide) and MSL (maleimide) disordered the orderly helix arrangement of myosin in the rest state of spin level. The temperature effect on the structure change was great at the UL in the equatorial reflection. But those of IASL and MSL were minor. Equatorial reflection (10, 11) change inferred that myosin head was moved to the vicinity of actin filament by temperature change (from $25^{\circ}C$ to $0^{\circ}C$) at UL, but spin level was not changed. The intensity change of 143 $\AA$ and 72 $\AA$ could offer information of the mass profection of population of myosin heads along the filament axis. The slope of intensity profile of the mass profection of 143$\AA$ and reflection of MSL is appeared sharply and those of UL and IASL were not changed. The decrease of MSL actin reflection at 51 $\AA$ and 59 $\AA$ in the actin reflection change refers that the shifted myosin head binds a certain actin or changes an actin structure. From these results, we could conclude that IASL and MSL were spin labeled on SH of myosin head and disordered the helix arrangement of actin.

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A Thermostable Xylose Isomerase from Thermus thermophilus: Biochemical Characterization, Crystallization, and Preliminary X-ray Analyses

  • Chang, Changsoo;Park, Byung-Chul;Lee, Dae-Sil;Suh, Se-Won
    • BMB Reports
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    • v.31 no.6
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    • pp.600-603
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    • 1998
  • A highly thermostable xylose isomerase from Thermus thermophilus has been expressed in Escherichia coli and crystallized. The purified enzyme shows its optimum temperature at $90^{\circ}C$. It has been crystallized at room temperature using polyethylene glycol 4000 as the precipitant. The crystal belongs to the orthorhombic space group $P2_12_12_1$, with unit cell parameters of a = 73.34 ${\AA}$, b = 144.05 ${\AA}$, c = 155.07 ${\AA}$. The presence of one molecule of tetrameric xylose isomerase in the asymmetric unit gives a crystal volume per protein mass ($V_m$) of 2.32 ${\AA}^3/Da$ and the solvent content of 47.0% by volume. The diffraction pattern extends to 1.9 ${\AA}$ Bragg spacing with synchrotron radiation and a set of native data has been collected to 2.3 ${\AA}$.

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Dielectric Properties and Phase Transformation of Poled <001>-Oriented Pb(Mg1/3Nb2/3)O3-PbTiO3 Single Crystals (분극된 <001> 방위 Pb(Mg1/3Nb2/3)O3-PbTiO3 단결정의 유전 특성 및 상전이)

  • Lee, Eun-Gu;Lee, Jae-Gab
    • Korean Journal of Materials Research
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    • v.22 no.7
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    • pp.342-345
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    • 2012
  • The dielectric properties and phase transformation of poled <001>-oriented $Pb(Mg_{1/3}Nb_{2/3})O_3-x%PbTiO_3$(PMN-x%PT) single crystals with compositions of x = 20, 30, and 35 mole% are investigated for orientations both parallel and perpendicular to the [001] poling direction. An electric-field-induced monoclinic phase was observed for the initial poled PMN-30PT and PMN-35PT samples by means of high-resolution synchrotron x-ray diffraction. The monoclinic phase appears from $-25^{\circ}C$ to $100^{\circ}C$ and from $-25^{\circ}C$ to $80^{\circ}C$ for the PMN-30PT and PMN-35PT samples, respectively. The dielectric constant (${\varepsilon}$)-temperature (T) characteristics above the Curie temperature were found to be described by the equation$(1/{\varepsilon}-1/{\varepsilon}_m)^{1/n}=(T-T_m)/C$, where ${\varepsilon}_m$ is the maximum dielectric constant and $T_m$ is the temperature giving ${\varepsilon}_m$, and n and C are constants that change with the composition. The value of n was found to be 1.82 and 1.38 for 20PT and 35PT, respectively. The results of mesh scans and the temperature-dependence of the dielectric constant demonstrate that the initial monoclinic phase changes to a single domain tetragonal phase and a to paraelectric cubic phase. In the ferroelectric tetragonal phase with a single domain state, the dielectric constant measured perpendicular to the poling direction was dramatically higher than that measured in the parallel direction. A large dielectric constant implies easier polarization rotation away from the polar axis. This enhancement is believed to be related to dielectric softening close to the morphotropic phase boundary.