• Macromolecular Research
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• v.15 no.4
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• pp.285-290
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• 2007

Ag nanoparticles were distributed onto polystyrene nanoparticle (PS-Ag) beads using two synthetic methodologies. In the first methodology, polystyrene (PS) beads were prepared via emulsion polymerization, with Ag nanoparticles subsequently loaded onto the surface of the PS beads. The polymerization of styrene was radiolytically induced in an ethanol (EtOH)/water medium, generating PS beads. Subsequently, Ag nanoparticles were loaded onto the PS beads via the reduction of Ag ions. The results from the morphological studies, using field emission transmission electron microscopy (FE-TEM), reveal the PS particles were spherical and nanosized, and the average size of the PS spherical particles decreased with increasing volume % of water in the polymerization medium. The size of the PS spherical particles increases with increasing radiation dose for the polymerization. Also, the amount of Ag nanoparticle loading could be increased by increasing the irradiation dose for the reduction of the Ag ions. In the second methodology, the polymerization of styrene and reduction of Ag ions were simultaneously performed by irradiating a solution containing styrene and Ag ions in an EtOH/water medium. Interestingly, the Ag nanoparticles were preferentially homogeneously distributed within the PS particles (not on the surface of the PS particles). Thus, Ag nanoparticles were distributed onto the surface of the PS particles using the first approach, but into the PS clusters of the particles via the second. The antimicrobial efficiency of a cloth coated with the Ag-PS composite nanoparticles was tested against bacteria, such as Staphylococcus aureus and Klebsiella pneumoniase, for 100 water washing cycles.

• Bulletin of the Korean Chemical Society
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• v.8 no.2
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• pp.69-72
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• 1987

The structures of dehydrated $Ag_9Cs_3$-A treated with hydrogen gas at three different temperatures have been determined by single-crystal X-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at 23(1) $^{\circ}C$. All crystals were ion exchanged in flowing streams of aqueous $AgNO_3$/$CsNO_3$ with a mole ratio 1:3.0 to achieve the desired crystal composition. The structures treated with hydrogen at $23^{\circ}C(a=12.288(1)\;{\AA})\;and\;310^{\circ}C(a=12.291(2)\;{\AA})$ refined to the final error indices R1 = 0.091 and R2 = 0.079, and 0.065 and 0.073, respectively, using the 216 and 227 reflections, respectively, for which I >3${\sigma}$(I). In both of these structures, eight $Ag^+$ ions are found nearly at 6-ring centers, and three $Cs^+$ ions lie at the centers of the 8-rings at sites of $D_{4h}$ symmetry. One $Ag^{\circ}atom$, presumably formed from the reduction of a $Ag^+$ ion by an oxide ion of a residual water molecule or of the zeolite framework during the dehydration process, is retained within the zeolite, perhaps in a cluster. In these two structures hydrogen gas could not enter the zeolite to reduce the $Ag^+$ ions because the large $Cs^+$ ions blocked all the 8-windows. However, hydrogen could slowly diffuse into the zeolite and was able to reach and to reduce about half of the $Ag^+$ ions in the structure only at high temperature ($470^{\circ}C$). The silver atoms produced migrated out of the zeolite framework, and the protons generated led to substantial crystal damage.

• Bulletin of the Korean Chemical Society
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• v.5 no.3
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• pp.117-121
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• 1984

The structure of $CS_{7.3}Ag_{4.7}Si_{12}Al_{12}O_{48}$, vacuum dehydrated zeolite A with all Na+ ions replaced by $Cs^+$ and $Ag^+$ as indicated, has been determined by single-crystal x-ray diffraction techniques in the cubic space group, Pm3m (a = 12.282 (1) ${\AA}$). The structure was refined to the final error indices $R_1$$R_2$ (weighted) = 0.099 using 347 independent reflections for whind intlch $I_0\;>\;3{\sigma}(I_0)$. Although deydration occurred at $360^{\circ}C$, no silver atoms or clusters have been observed. The 8-ring sites are occupied only by $Cs^+$ ion, and the 4-ring sites only by a single $Ag^+$ ion. The 6-ring sites contain $Ag^+$ and $Cs^+$ ions with $Ag^+$ nearly in 6-ring planes and $Cs^+$ well off them, one on the sodalite unit side. With regard to the 6-rings, the structure can be represented as a superposition of two types of unit cells: about 70 % have $4Ag^+$ and $4Cs^+$ ions, and the remaining 30 % have $3Ag^+$ and $5Cs^+$. In all unit cells, $3Cs^+$ ions lie at the centers of the 8-rings at sites of D4h symmetry; these ions are approximately 0.3 ${\AA}$ further from their nearest framework-oxygen neighbors than the sum of the appropriate ionic radii would indicate. To minimize electrostatic repulsions, the $Cs^+$ ions at Cs(1) are not likely to occupy adjacent 6-rings in the large cavity; they are likely to be tetrahedrally arranged when there are 4.

• Macromolecular Research
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• v.16 no.2
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• pp.108-112
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• 2008

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) analysis of nonpolar polymeric materials is affected by the sample preparation as well as the matrix and cationizing agent. This study examined the influence of silver salt types on the MALDI analysis of polybutadiene (PB). Silver trifluoroacetate (AgTFA), silver benzoate (AgBz), silver nitrate ($AgNO_3$), and silver p-toluenesulfonate (AgTS) were used as the silver salts to compare the MALDI mass spectra of PB. The mixture solution of PB and 2,5-dihydroxybenzoic acid (DHB), as a matrix dissolved in THF, was spotted on the sample plate and dried. A droplet of the aqueous silver salt solution was placed onto the mixture. The mass spectrum with AgBz showed the clear $[M+Ag]^+$ ion distribution of PB while the mass spectrum with AgTFA did not show $[M+Ag]^+$ ions but only silver cluster ions. The mass spectra with $AgNO_3$ and AgTS did not show a clear $[M+Ag]^+$ ion distribution. The difference in the formation of $[M+Ag]^+$ ions of PB depending on the silver salts was attributed to the silver cation transfer reaction between the silver salt and the matrix (DHB). The mass spectrum showed a clear $[M+Ag]^+$ ion distribution of PB when the conjugate acid of the silver salt was less acidic than the matrix.

• Korean Journal of Crystallography
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• v.6 no.2
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• pp.118-124
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• 1995

The crystal structure of an iodine sorption complex of vacumm-dehydrated Ag+ and Ca2+ exchanged zeolite A(a=12.174(3)Å) has been determined at 21℃ by single-crystal X-ray diffraction techniques in the cubic space group Pm3m. The crystal was prepared by flow method for three days using exchange solution in solution in which mole ratio of AgNO3 and Ca(NO3)2 was 1:150 with total concentration of 0.05 M. The complex was prepared by dehydration at 360℃ and 2×10-6 Torr for 2 days, followed by exposure to about 14.3 Torr of iodine vaporat 80℃ for 24 hours. Full-matrix least-squares refinement converged to the final error indices of R1=0.082, R2=0.068 using 122 reflections for which I > 3σ(I). Two Ag+ ions, 1.1 Ag+ ions, and 4.45 Ca2+ ions per unit cell are located on three different three-fold axes associated with 6-ring oxygens. Two Ag+ ions per unit cell are in the large cavity, 1.399(4)Å from the (111) plane of three oxygens. Another 1.1 Ag+ ions are found at opposite sites. Six iodine molecules are sorbed per unit cell. Each I2 molecule approaches a framework oxide ion axially (O-I=3.43(2)Å, I-I=2.92Å, I-I-O;166.1(3)°), by a charge transfer complex interaction. Two Ag+ ions make a close approach to the iodine molecules (Ag-I ; 2.73(2)Å).

• Analytical Science and Technology
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• v.12 no.2
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• pp.159-165
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• 1999

The adsorption and separation behaviors of transition metal ions using a merrifield resin bound 1,12-diaza-3,4:9,10-dibenzo-5,8-dioxacyclopentadecane (NTOE) and 1,12,15-triaza-3,4:9,10-dibenzo-5,8-dioxacycloheptadecane(NDOE) were investigated in aqueous solution. The orders of adsorption degree(E) and distribution ratio(D) of transition metal ions were Cu(II)$t_R$) of metal ions were affected by adsorption degree(E) and distribution ratio(D). This results showed good separation efficiency of Ag(I) from mixed metal solution.

• Journal of the Korean Vacuum Society
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• v.6 no.S1
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• pp.27-33
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• 1997

Recently ion beam assistant deposition (IBAD) was successfully used to produce a dense ultra-adherent and pinhole-free hydroxyapatite (HAp) layer on alumina substrate. After that the HAp-coated alumina was immersed in 20ppm and 100ppm $AgNO_3$ solution at room temperature for 48 hours to carry out the ions exchange between $Ag^+\;and\;Ca^+$ in HAp. The obvious antimicrobial effect against E.Coli, P. Aeruginosa and S. Epidermidis was observed in the samples treated with 20ppm $AgNO_3$ Solution, In contrast to this the untreated samples did not show any bactericidal effect. Scanning electron microscope(SEM) study showed that Ag homogeneously distributed on the surface. X-ray diffraction (XRD) demonstrated that the surface structure in the samples without Ag was HAp whereas with Ag is HAp and AgCaP. It appears that silver ions exchange with calcium ions in HAp does not cause significant changes in the structure of HAp coatings.

• 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 $(Cs_4)3^+\;and\;(Cs_6)4^+$.

• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.18-24
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• 1989

Two crystal structures of dehydrated $Ag^+$ and $Rb^+$ exchanged zeolite A, stoichiometries of $Ag_{9}Rb_{3}-A$ (a = 12.278(2)${\AA}$) and $Ag_{10}Rb_{2}-A$ (a = 12.286(2)${\AA}$) per unit cell, have been determined by single crystal x-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at 21(1)$^{\circ}$C. The crystals of $Ag_{10}Rb_{2}-A$ and $Ag_{10}Rb_{2}-A$ were prepared by flow methods using exchanged solution in which mole ratios of AgNO$_3$ and RbNO$_3$ were 1:5 and 1:50, respectively, with the total concentration of 0.05 M. The structures of the dehydrated $Ag_{9}Rb_{3}-A$ and the $Ag_{10}Rb_{2}-A$ were refined to the final error indices, $R_1$ = 0.064 and $R_2$ = 0.060 with 291 reflections, and $R_1$ = 0.063 and $R_2$ = 0.080 with 416 reflections respectively, for which I >3${\sigma}$(I). In both structures, one reduced silver atom per unit cell was found inside the sodalite cavity. It may be present as a hexasilver cluster in 1/6 of the sodalite units or as an isolated Ag atom coordinated to 4 $Ag^+$ ions in each sodalite unit to give $(Ag_5)^{4+}$, symmetry 4 mm. In the structure of dehydrated $Ag_{9}Rb_{3}-A$, 8 $Ag^+$ ions lie on the threefold axis and each is nearly at the center of the 8-rings at the sites of $D_{4h}$ symmetry. In the structure of dehydrated $Ag_{10}Rb_{2}-A$, two crystallographically different eight 6-ring $Ag^+$ ions were found; $7Ag^+$ ions in the (111) planes of their O(3) framework oxygens and one $Ag^+$ ion inside of sodalite cavity. Two crystallographically different 8-ring cations were also found; two $Rb^+$ ions at the centers of the 8-oxygen rings and one $Ag^+$ ion into the large cavity. Both structures indicate that $Rb^+$ ions prefer to occupy the 8-ring sites, while $Ag^+$ ions prefer to occupy the 6-ring sites.

• Bulletin of the Korean Chemical Society
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• v.7 no.3
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• pp.190-193
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• 1986

The structure of partially $Ag^+$-exchanged zeolite 4A, $Ag_{7.6}Na_{4.4}-A$, vacuum dehydrated at $370^{\circ}C$, has been determined by single-crystal x-ray diffraction techniques in the cubic space group, Pm3m (a = 12.311(1)${\AA}$) at $24(1)^{\circ}}C$. The structure was refined to the final error indices $R_1$ = $R_2$ (weighted) = 0.064 using 266 independent reflections for which $I_0$>$3{\sigma}(I_0)$. Three $Na^+$ ions occupy the 3 8-ring sites, and the remaining ions, 1.4 $Na^+$ and 6.6 $Ag^+$, fill the 8 6-ring sites; each $Ag^+$ ion is nearly in the [111] plane of its 3 O(3) ligands, and each $Na^+$ ion is 0.9${\AA}$ from its corresponding plane, on the large-cavity side. One reduced silver atom per unit cell was found inside the sodalite unit. It was presumably formed from the reduction of a $Ag^+$ ion by an oxide ion of a residual water molecule or of the zeolite framework. It may be present as a hexasilver cluster in 1/6 of the sodalite units, or, most attractively among several alternatives, as an isolated Ag atom coordinated to 4 Ag ions in each sodalite unit to give $(Ag_5)^{4+}$, symmetry 4mm.