• Bulletin of the Korean Chemical Society
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• v.21 no.1
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• pp.75-80
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• 2000

The positions of Xe atoms encapsulated in the molecular-dimensioned cavities of fully dehydrated Na-A have been determined. Na-A was exposed to 1050atm of xenon gas at 400 $^{\circ}C$ for seven days, followed by cooling at pressure to encapsulate Xe atoms. The resulting crystal structure of Na-A(7Xe) (a = 12.249(1) $\AA$, $R_1$ = 0.065, and $R_2$ = 0.066) were determined by single-crystal X-ray diffraction techniques in the cubic space group Pm3m at 21(1) $^{\circ}C$ and 1 atm. In the crystal structure of Na-A(7Xe), seven Xe atoms per unit cell are distributed over four crystallographically distinct positions: one Xe atom at Xe(1) lies at the center of the sodalite unit, two Xe atoms at Xe(4) are found opposite four-rings in the large cavity, and four Xe atoms, two at Xe(2) and others at Xe(3), respectively, occupy positions opposite and between eight- and six-rings in the large cavity. Relatively strong interactions of Xe atoms at Xe(2) and Xe(3) with $Na^+$ ions of four-, eight-, and six-rings are observed:Na(1)-Xe(2) = 3.09(6), Na(2)-Xe(3) = 3.11(2), and Na(3)-Xe(2) = 3.37(8) $\AA$. In each sodalite unit, one Xe atom is located at its center. In each large cavity, six Xe atoms are found, forming a distorted octahedral arrangement with four Xe atoms, at equatorial positions (each two at Xe(2) and Xe(3)) and the other two at axial positions (at Xe(4)). With various reasonable distances and angles, the existence of $(Xe)_6$ cluster is proposed (Xe(2)-Xe(3) = 4.78(6) and 4.94(7), Xe(2)-Xe(4) = 4.71(6) and 5.06(6), Xe(3)-Xe(4) = 4.11(3) and 5.32(4) $\AA$, Xe(2)-Xe(3)-Xe(2) = 93(1), Xe(3)-Xe(2)-Xe(3) = 87(1), Xe(2)-Xe(4)-Xe(2) = 91(4), Xe(2)-Xe(4)-Xe(3) = 55(2), 59(1), 61(1), and 68(1), and Xe(3)-Xe(4)-Xe(3) = 89($^{\circ}1$)). These arrangements of the encapsulated Xe atoms in the large cavity are stabilized by alternating dipoles induced on Xe(2), Xe(3), and Xe(4) by eight- and six-ring $Na^+$ ions as well as four-ring oxygens, respectively.

• Bulletin of the Korean Chemical Society
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• v.14 no.5
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• pp.603-610
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• 1993

The crystal structure of dehydrated $Ag_{5.6}K_{6.4}-A$, zeolite A ion-exchanged with $K^+\;and\;Ag^+$ as indicated and dehydrated at 360$^{\circ}$C, has been determined by single-crystal X-ray diffraction techniques. Also determined were the structures of the products of the reactions of this zeolite with 0.1 Torr of Cs vapor at 250$^{\circ}$C for 48 h and 72 h, and with 0.1 Torr of Rb vapor at 250$^{\circ}$C for 24 h. The structures were solved and refined in the cubic space group Pm3m at 21(l)$^{\circ}$C (a= 12.255(l) ${\AA}$ , 12.367(l) ${\AA}$, 12.350(l) ${\AA}$, and 12.263(l) ${\AA}$, respectively). Dehydrated $Ag_{5.6}K_{6.4}$-A was refined to the final error indices $R_1= 0.044\;and\;R_2=0.037$ with 202 reflections for which I>3${\sigma}$(I). The crystal structures of the reaction products were refined to $R_1=0.087\;and\;R_2= 0.089$ with 157 reflections, $R_1=0.080\;and\;R_2= 0.087$ with 161 reflections, and $R_1= 0.071\;and\;R_2=0.061$ with 88 reflections, respectively. In the structure of $Ag_{5.6}K_{6.4}-A,\;K^+$ ions block all 8-oxygen rings, and one reduced Ag atom is found per sodalite cavity. Also, ca. 4.6 $Ag^+ ions\;and\;3.4 K^+ ions$ are found at 6-ring sites in the large cavity. The crystal structures of the reaction products show that all $K^+$ and $Ag^+$ ions have been reduced, and that all K^+$ atoms have left the zeolite. Cs or Rb species are found at three different crystallographic sites: 3.0 $Cs^+\;or\;3.0Rb^+$ ions per unit cell occupy 8-ring centers, ca. 8.0 $Cs^+ ions\;or\;5.7 Rb^+$ ions, are found on threefold axes opposite 6-rings deep in the large cavity, and ca. 2.5 $Cs^+\;or\;2.3 Rb^+ ions are found on threefold axes in the sodalite unit. Also, 1 $Rb^+$ ion lies opposite a 4-ring. Silver atoms, corresponding to 75% or 40% occupancy of hexasilver clusters stabilized by coordination to $Cs^+\;or\;Rb^+$ ions, are found at the centers of the large cavities. In the crystal structures of dehydrated Ag_{5.6}K_{6.4}-A$ reacted with Cs vapor, excess Cs atoms are absorbed and these form (locally) cationic clusters such as $(Cs_4)3^+\;and\;(Cs_6)4^+$.

• Bulletin of the Korean Chemical Society
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• v.17 no.7
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• pp.631-637
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• 1996

The structures of fully dehydrated Ca2+- and Rb+-exchanged zeolite X, Ca31Rb30Si100Al92O384(Ca31Rb30-X; a=25.009(1) Å) and Ca28Rb36Si100Al92O384(Ca28Rb36-X; a=24.977(1) Å), have been determined by single-crystal X-ray diffraction methods in the cubic space group Fd&bar{3} at 21(1) ℃. Their structures were refined to the final error indices R1=0.048 and R2=0.041 with 236 reflections for Ca31Rb30-X, and R1=0.052 and R2=0.043 with 313 reflections for Ca28Rb36-X; I>3σ(I). In both structures, Ca2+ and Rb+ ions are located at six different crystallographic sites. In dehydrated Ca31Rb30-X, sixteen Ca2+ ions fill site I, at the centers of the double 6-rings (Ca-O=2.43(1) Å and O-Ca-O=93.3(3)°). Another fifteen Ca2+ ions occupy site II (Ca-O=2.29(1) Å, O-Ca-O=119.5(5)°) and fifteen Rb+ ions occupy site II opposite single six-rings in the supercage; each is 1.60 Å from the plane of three oxygens (Rb-O=2.77(1) Å and O-Rb-O=91.1(4)°). About two Rb+ ions are found at site II', 1.99 Å into sodalite cavity from their three-oxygen plane (Rb-O=2.99(1) Å and O-Rb-O=82.8(4)°). The remaining thirteen Rb+ ions are statistically distributed over site III, a 48-fold equipoint in the supercages on twofold axes (Rb-O=3.05(1) Å and Rb-O=3.38(1) Å). In dehydrated Ca28Rb36-X, sixteen Ca2+ ions fill site I (Ca-O=2.41(1) Å and O-Ca-O=93.6(3)°) and twelve Ca2+ ions occupy site II (Ca-O=2.31(1) Å, O-Ca-O=119.7(4)°). Sixteen Rb+ ions occupy site II; each is 1.60 Å from the plane of three oxygens (Rb-O=2.81(1) Å and O-Rb-O=90.6(3)°) and four Rb+ ions occupy site II'; each is 1.88 Å into sodalite cavity from their three-oxygen plane (Rb-O=2.99(1) Å and O-Rb-O=83.8(2)°). The remaining sixteen Rb+ ions are found at III site in the supercage (Rb-O=2.97(1) Å and Rb-O=3.39(1) Å). It appears that Ca2+ ions prefer sites I and II in that order, and that Rb+ ions occupy the remaining sites. Rb+ ions are too large to be stable at site I, when they are competing with other smaller cations like Ca2+ ions.

• Bulletin of the Korean Chemical Society
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• v.9 no.6
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• pp.338-341
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• 1988

Two crystal structures of fully dehydrated silver and potassium exchanged zeolite A, stoichiometries of $Ag_{9.3}K_{{2.7}^-}A$ (${\alpha}$ = 12.282(2) ${\AA}$) and $Ag_{10.7}K_{{1.3}^-}{\AA}$ (${\alpha}$ = 12.287(2) A) per unit cell, have been determined from 3-dimensional x-ray diffraction data gathered by counter methods. All structures were solved and refined in the cubic space group Pm3m at 21(1)$^{\circ}C$ . The crystals of $Ag_{9.3}K_{{2.7}^-}A$ and $Ag_{10.7}K_{{1.3}^-}A$ were prepared by flow method using exchange solutions in which mole ratios of $AgNO_3$ and $KNO_3$ were 1:10 and 1:5, respectively, with total concentration of 0.05M. The structures of the dehydrated $Ag_{9.3}K_{{2.7}^-}A$ and $Ag_{10.7}K_{{1.3}^-}A$ were refined to yield the final error indices $R_1$ = 0.037 and $R_2$ = 0.040 with 321 reflections, and $R_1$ = 0.042 and $R_2$ = 0.043 with 371 reflections, repectively, for which I > 3${\sigma}$(I). In both structures, eight $Ag^+$ ions are found nearly at 6-ring centers and each $Ag^+$ ion is nearly in the (1 1 1) plane at its O(3) ligands. The 8-ring sites are preferentially occupied by $K^+$ ions in both structures. 1.3 and 1.7 reduced silver atoms per unit cell were found inside of sodalite units of $Ag_{9.3}K_{{2.7}^-}A$ and that of $Ag_{10.7}K_{{1.3}^-}A$, respectively. These reduced silver species were presumably formed from the reduction of $Ag^+$ ions by oxide ions of residual water molecule or of the zeolite framework. These two crystals may be presented as hexasilver cluster in 21.7% and 28.3% of sodalite unit cells for $Ag_{9.3}K_{{2.7}^-}A$ and $Ag_{10.7}K_{{1.3}^-}A$, repectively.

• Bulletin of the Korean Chemical Society
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• v.22 no.2
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• pp.164-170
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• 2001

The crystal structures of fully dehydrated Ni2+- and Tl+ -exchanged zeolite X (Ni17Tl58-X, and Ni12Tl68-X; X=Si100Al92O384) have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd3 at $21(1)^{\circ}C$ (a=24.380(4) $\AA$, 24.660(4) $\AA$, respectively). Their structures have been refined to the final error indices R1=0.037 and R2=0.043 with 485 reflections, and R1=0.039 and R2=0.040 with 306 reflections, respectively, for which I >36(I). In Ni17Tl58-X, 17 Ni2+ ions per unit cell were found at only two sites: 15 at site I at the center of the hexagonal prism (Ni-O=2.203(9) $\AA)$ and the remaining 2 at site II near single six-oxygen rings in the supercage (Ni-O=2.16(3) $\AA).$ Fifty-eight Tl+ ions were found at five crystallographic sites: 28 at site II (Tl-O=2.626(8) $\AA)$, 2 at site I' in the sodalite cavity near the hexagonal prism (Tl-O=2.85(1) $\AA)$, another 2 at site II' in the sodalite cavity (Tl-O=2.77(1) $\AA).$ The remaining 26 were found at two nonequivalent Ⅲ' sites with occupancies of 23 and 3. In Ni12Tl68-X, 12 Ni2+ ions per unit cell were found at two sites: 10 at site I (Ni-O=2.37(2) $\AA)$ and the remaining 2 at site II (Ni-O=2.13(2) $\AA).$ Sixty-eight Tl+ ions were found at five crystallographic sites: 28 at site II (Tl-O=2.63(1) $\AA)$, 12 at site I' (Tl-O=2.62(1) $\AA)$, 2 at site II' (Tl-O=3.01(2) $\AA)$, and the remaining 26 at two III' sites with occupancies of 23 and 3. It appears that Ni 2+ ions prefer to occupy site I and II, in that order. The large Tl+ ions occupy the remaining sites, I', II, II' and two different III' sites. In both crystals, only the Ni2+ ions at site II were reduced and migrated to the external surface of zeolite X when these crystals were treated with hydrogen gas.

• Journal of Environmental Science International
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• v.12 no.7
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• pp.817-824
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• 2003

Various kinds of zeolites, such as analcime (ANA), cancrinite (CAN), Na-Pl and sodalite octahydrate (SOD) could be synthesized from Hwangto by hydrothermal reaction in a high-pressure vessel. The adsorption characteristics of Cu(II) and Cd(II) by Hwangto and its synthetic zeolites were investigated using the chemical and electrochemical surface parameters of these adsorbents. The heavy metal adsorptivity among the adsorbents decreased in the following sequences: Na-Pl > SOD > ANA > CAN > Hwangto. This sequence was the same with the values of surface site density (Ns) of these adsorbents and was correlated inversely with the values of pHpzc (pH of the point of zero charge) and the va]ues of K$\_$a2/(int) (intrinsic surface deprotonation constant) of the adsorbents for synthetic zeolites, i.e., the adsorbents with higher values of Ns and with lower values of pHpzc and K$\_$a2/(int) for synthetic zeolites showed higher heavy metal adsorptivity. With increasing pH, the heavy metal adsorptivity increased greatly between pHpzc and pH 6 or 7 because of the steep increase of negatively charged sites for synthetic zeolites, but for Hwangto, it increased broadly because of slow increase of negatively charged sites based on its lower surface sites.

• Journal of the Microelectronics and Packaging Society
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• v.7 no.1
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• pp.7-12
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• 2000

As an essential technology for the FED, VFD and PDP packaging having merits of no glass frit and no glass tube usage, two sodalime glass substrates were electrostatically-bonded in a vacuum environment, and the bond properties were compared with the case of bonding in atmosphere. The glass wafer pairs bonded in vacuum using a-Si interlayer had a relatively lower bond strength than the ones bonded in atmosphere under same bonding conditions (temperature and voltage). And the bond strength was increased in the case of oxygen ambient. Through the XPS and SIMS analyses fur the surface region of a-silicon and bulk glass, it might be concluded that the lower bonding strength was originated from the inactive silicon oxide growth occurred during the electrostatic bonding process due to oxygen deficiency in vacuum.

• Journal of the Korean Applied Science and Technology
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• v.16 no.3
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• pp.217-221
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• 1999

This study was carried out to synthesis the zeolite using the bituminous coal fly ash emitted from power plant that occurs several environmental problems. In spite of fly ash has contained high content of $SiO_2$ and $Al_2O_3$, it disposed mainly landfill. If the effective methods to recover the $SiO_2$ and $Al_2O_3$ were developed, the fly ash could be utilized valuable raw materials. In this study, fly ash was used as raw material to synthesize the zeolite by pressurized hydrothermal reaction. Also, experimental parameters included temperature($70{\sim}110^{\circ}C$, and pressure($140{\sim}200$ psi) of crystallization were investigated. The more crystallization pressure was increased, the more Zeolite 4A was synthesized at 70 and $90^{\circ}C$. Zeolite 4A of metastable phase tend to be transformed into sodalite of stable phase at $110^{\circ}C$.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2005.11b
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• pp.176-181
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• 2005

The electrolytic reduction process and the electrorefining process, which are being developed at the Korea Atomic Energy Research Institute (KAERI), are to generate molten waste salts such as LiCI salt and LiCI-KCI eutectic salt, respectively. Our goal in waste salt management is to minimize a total waste generation and fabricate a very low­leaching waste form such as a ceramic waste form. Zeolite has been known to one of the most desirable media to immobilize waste salt, which is water soluble and easily radiolyzed. Zeolite can be also used to the removal of fission products from the spent waste salt. Molten LiCI salt is mixed with zeolite A at $650^{\circ}C$ to form a salt-loaded zeolite, and then thermally treated in above $900^{\circ}C$ to become an immobilized product with crystal phase of $Li_{8}Cl_{2}$-Sodalite. In this work, a crystal phase changes of immobilization medium, zeolite, during immobilization of molten LiCI salt using zeolite A is introduced.

• Journal of Korean Society on Water Environment
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• v.20 no.5
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• pp.466-472
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• 2004

Red mud is formed as a waste during bauxite refining known as Bayer's process. Its main constituents are iron, aluminium, sodium and silica. The disposal of large quantities of wasted red mud causes a serious ecological problem. In this study, the red mud wasted from the bauxite refinery was studied for phosphate removal from aqueous solution according to activation methods. The influence of heat treatment, and neutralization with sea water and acid treatment level for the optimum conditions for phosphate removal have been determined. Heat treatment combined with acid treatment is most suitable for the removal of phosphate from aqueous solution. The optimal condition was activated with 1 N HCl solution after heating in $600^{\circ}C$ during 4 hours. Acid and heat treatment causes sodalite compounds which hinder the phosphate adsorption to leach out. The adsorption data obtained followed a first-order rate expression and fitted well with the Freundlich Isotherm well.