• Korean Journal of Crystallography
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• v.12 no.3
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• pp.127-136
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• 2001

A stoichiometric mixture of evaporating materials for ZnGa₂Se₄single crystal thin films was prepared from horizontal furnace. To obtain the single crystal thin films, ZnGa₂Se₄mixed crystal was deposited on thoroughly etched semi-insulating GaAs(100) substrate by the Hot Wall Epitaxy (HWE) system. The source and substrate temperatures were 610℃ and 450℃, respectively. The crystalline structure of the single crystal thin films was investigated by the photoluminescence and double crystal X-ray diffraction (DCXD). The carrier density and mobility of ZnGa₂Se₄single crystal thin films measured from Hall effect by von der Pauw method are 9.63×10/sup 17/㎤ and 296 ㎠/V·s at 293 K, respectively. From the photocurrent spectrum by illumination of perpendicular light on the c-axis of the ZnGa₂Se₄single crystal thin film, we have found that the values of spin orbit splitting △so and the crystal field splitting Δcr were 251.9meV and 183.2 meV at 10 K, respectively. From the photoluminescence measurement on th ZnGa₂Se₄single crystal thin film, we observed free excition (Ex) existing only high quality crystal and neutral bound exiciton (A°, X) having very strong peak intensity. Then, the full-width-at-half-maximum (FWHM) and binding energy of neutral acceptor bound excition were 11 meV and 24.4 meV, respectivity. By Haynes rule, an activation energy of impurity was 122 meV.

• Journal of the Korean Chemical Society
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• v.37 no.6
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• pp.599-603
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• 1993

Crystal structure of bis(1,2-diaminopropane)palladium(II) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: $Pd_2C_{10}H_{10}N_{4}O_{8}$, $M_W$ = 573.09, orthorhombic, space group $P_{ccn}$ (No = 56), a = 16.178(5), b = 16.381(6), c = 6.685(2)$\{AA}$, V = 1771.6 $\{AA}^3$, $M_W$W = 573.09, $D_c$ = 2.014 g${\cdot}c\;m^{-3}$, Z = 4, T = 294K, F(000) = 1056.0 and $\mu$ = 20.466 c$m^{-1}$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$ = 0.7107 $\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-squares methods using Pivot weights. The final R and S values were R = 0.065, $R_W = 0.059, R_{all}$ = 0.065 and S = 4.315 for 605 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angle of $18(l)^{\circ}$ between thier planes. In the crystal structure, they do not have the Magnus's salt type mixed stacks; instead, the complex anions form regular stacks along the c-axis with the M-M bond length of $3.343(5)\AA$ and their stacks are surrounded by the complex cations through hydrogen bonds with the nitrogen-oxygen distances of 2.94(3) and $3.31(4)\AA.$

• Korean Journal of Crystallography
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• v.12 no.4
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• pp.197-206
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• 2001

A stoichiometric mixture of evaporating materials for AgInS₂ single crystal thin films was prepared from horizontal electric furnace. To obtain the single crystal thin films. AgInS₂ mixed crystal was deposited on thoroughly etched semi-insulating GaAs(100) substrate by the Hot Wall Epitaxy(HWE)system. The source and substrate temperatures were 680℃ and 410℃, respectively. The crystalline structure of the single crystal thin films was investigated by the photoluminescence and double crystal X-ray diffraction(DCXD). The carrier density and mobility of AgInS₂ single crystal thin film mea-sured from Hall effect by van der Pauw method are 9.35×10/sup 16/㎤ and 294㎠/V·s at 293K respectively. The temperature dependence of the energy band gap of the AgInS₂ obtained from the absorption spectra was well described by the Varshni's relation , E/sub g/(T)=2.1365eV-(9.89×10/sup-3/eV/K/)T²(T+2930K). The crystal field and the spin-orbit splitting energies for the valence band of the AgInS₂ have been estimated to be 0.1541eV and 0.0129 eV, respectively, by means of the photocur-rent spectra and the Hopfield quasicubic model. These results indicate that the splitting of the Δso definitely exists in the Γ/sub 5/ states of the valence band of the AgInS₂ /GaAs epilayer. The three photo-current peaks ovserved at 10K are ascribed to the A₁-, B-₁and C₁-exction peaks for n=1.

• Korean Journal of Crystallography
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• v.4 no.2
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• pp.54-62
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• 1993

The crystal shnture of dehydrated fully Cd2+-exchanged zeolite A evacuated at 2 × 10-6 Torr and 650℃ (a:12.189(2) A) and of its iodine sorption corrplex (a:12.168(2)A) have been netsmlmn by single uystal x-ray diffraction techliques in the cubic space group hkTn at 21(1)℃. The strutures were refined to final error indices, Ri:0.057 and R2 =0.063 with 186 reflections and Rl:0.082 and R2:0.085 with 181 reflections, respectively, for which 1>3σ(In both structure, six lie at two distinguished threefold axes of unit cell ten the crystal structure of an iodine sorption complex of Cd6-A four Cd2+ ions are recessed 0.69(1) A into the large cavity to complex each with from the (111) plane of 0(3), whereas two Cd2+ ions recessed 0.68(1) A into the sodalite unit Awximately 4.0 l3ions per nit cell are sorbed. Each bridge between a Cd2+ ion and 8-ring oxygens ((I-I-I)= 117(1) ˚ and 0(1)-I(1)-I(2)=172(1)). The near linear I-I-0 angle and its interatomic distance (I-0=3.57(3) A) are indicative of a weak charge transfer interacticn between the frarrework oxygen and iodine. The existence of In3 inside the large cavity indicates that the If ions and H ions may be produced by reaction of In vapor with water molecules which maybe associated with Cd2+ ions in partially dehydrated Cd6-A In3- ions may be produced by the combination of I- and I2.

• Korean Journal of Crystallography
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• v.2 no.1
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• pp.17-22
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• 1991

The crystal structure of an acetylene sorption complex of vacuum dehydrated fully Cda+ _exchanged zeolite A has been determined from three-dimensional X-ray diffraction data gathered by counter method. The structure was solved and refined in the cubic space group Pm3m at 294(1) K, a=12.202(3) A and Z=1. We crystal was prepared by dehydration at 723 K and 2.67×104 Pa for 2 days, followed by exposure to 1.60×104 Pa of acetylene gas at 298(1) K. All six Cd2+ions per unit cell are associated with 6-oxgen rings of the aluminosilicate framework. They are distributed over two distinguished threefold axes of unit cell; two of these Cd2+ ions are recessed 0.694 into the sodalite unit from (111) plane of three 0(3)'s and each approaches three framework oxides; the other four Cd2+ ions extend approximately 0.586A into the large cavity. The four Cd2+ ions are in a near tetrahedral environment, 2.220(9)A from·three framework oxide ions and 2.74(7) A from each carbon atom of an acetylene molecule(which is here counted as a monodentate ligand). Full matrix least squares refinement converged to the final error indices R1=0.093 and R2=0.105 using the 292 independent reflections for which I>3σ(I).

• Korean Journal of Crystallography
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• v.8 no.2
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• pp.127-131
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• 1997

The crystal structure of a bromine sorption complex of vacuum-dehydrated Ag+ and Ca2+ exchanged zeolite A(a=12,234(1) Å) has been determined by single-crystal X-ray diffraction methods in the cubic space group Pm3m. The crystal was prepared by flow method using exchange solution in which mole ratio of AgNo3 and Ca(NO3)2 was 1:150 with a total concentration of 0.05M. The crystal was dehydrated at 360℃ and 2 ×10-6 Torr for 2days, followed by exposure to 180 Torr of Br2 vapor for 20min. full-matrix least-squares refinements converged to the final error indices of R1=0.111 and R2=0.101 using 90 reflections for which I>3o(I). About 3.1 Ag+ ions and 4.45 Ca2+ ions lie on the two crystallographically nonequivalent three-fold axes associated with 6-ring oxygens. A total of six bromine molecules are sorbed per unit cell. Each bromine molecule approaches a framework oxide ions axially (Br-Br-O=171(2)', O-Br=3.25(6) Å; and Br-Br=2,61(8) Å by a charge-transfer interaction.

• 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).

• Korean Journal of Crystallography
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• v.6 no.2
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• pp.125-133
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• 1995

The crystal structure of dehydrated, partially Co(II)-exchanged zeolite X, stoichiometry Co2+Na+-X (Co41+Na10Si100Al92O384) per unit cell, has been determined from three-dimensional X-ray diffraction data gathered by counter methods. The structure was solved and refined in the cubic space group Fd3:α=24.544(1)Å at 21(1)℃. The crystal was prepared by ion exchange in a flowing stream using a solution 0.025 M each in Co(NO3)2 and Co(O2CCH3)2. The crystal was then dehydrated at 380℃ and 2×10-6 Torr for two days. The structure was refined to the final error indices, R1=0.059 and R2=0.046 with 211 reflections for which I > 3σ(I). Co2+ ions and Na+ ions are located at the four different crystallographic sites. Co2+ ions are located at two different sites of high occupancies. Sixteen Co2+ ions are located at the center of the double six-ring (site I; Co-O = 2.21(1)Å, O-Co-O = 90.0(4)°) and twenty-five Co2+ ions are located at site II in the supercage. Twenty-five Co2+ ions are recessed 0.09Å into the supercage from its three oxygen plane (Co-O = 2.05(1)Å, O-Co-O = 119.8(7)°). Na+ ions are located at two different sites of occupandies. Seven Na+ ions are located at site II in the supercage (Na-O = 2.29(1)Å, O-Na-O = 102(1)°). Three Na+ ions are statistically distribyted over site III, a 48-fold equipoint in the supercages on twofold axes (Na-O = 2.59(10)Å, O-Na-O = 69.0(3)°). Seven Na+ ions are recessed 1.02Å into the supercage from the three oxygen plane. It appears that Co2+ ions prefer sites I and II in order, and that Na+ ions occupy the remaining sites, II and III.

• Korean Journal of Crystallography
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• v.8 no.1
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• pp.6-14
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• 1997

The crystal structures of $Sr_{31}K_{30}-X\;(Sr_{31}K_{30}Si_{100}A1_{92}O_{384};\;a=25.169(5) {\AA}$) and $Sr_{8.5}Tl_{75}-X (Sr_{8.5}Tl_{75}Si_{100}A1_{92}O_{384};\;a=25.041(5) {\AA}$) have been determined by single-crystal X-ray diffraction techniques in the cubic space group $\=F{d3}\;at\;21(1)^{\circ}C$. Each crystal was prepared by ion exchange in a flowing stream of aqueous $Sr(ClO_4)_2\;and\;(K\;or\;T1)NO_3$ whose mole ratio was 1 : 5 for five days. Vacuum dehydration was done at $360^{\circ}C$ for 2d. Their structures were refined to the final error indices $R_1=0.072\;and\;R_w=0.057$ with 293 reflections, and $R_1= 0.058\;and\;R_w=0.044$ with 351 reflections, for which $I>2{\sigma}(I)$, respectively. In dehydrated $Sr_{31}K_{30}-X,\;all\;Sr^{2+}$ ions and $K^+$ ions are located at five different crystallographic sites. Six-teen $Sr^{2+}$ ions per unit cell are at the centers of the double six-rings (site I), filling that position. The remaining 15 $Sr^{2+}$ ions and 17 $K^+$ ions fill site II in the supercage. These $Sr^{2+}$ and $K^+$ ions are recessed ca $0.45{\AA}\;and\;1.06{\AA}$ into the supercage, respectively, from the plane of three oxygens to which each is bound. ($Sr-O=2.45(1){\AA}\;and\;K-O=2.64(1){\AA}$) Eight $K^+$ ons occupy site III'($K-O=3.09(7){\AA}\;and\;3.11(10){\AA}$) and the remaining five $K^+$ ions occupy another site III'($K-O=2.88(7){\AA}\;and\;2.76(7){\AA}$). In $Sr_{8.5}Tl_{75}-X,\;Sr^{2+}\;and\;Tl^+$ ions also occupy five different crystallographic sites. About 8.5 $Sr^{2+}$ ions are at site I. Fifteen $Tl^+$ ions are at site I' in the sodalite cavities on threefold axes opposite double six-rings: each is $1.68{\AA}$ from the plane of its three oxygens ($T1-O=2.70(2){\AA}$). Together these fill the double six-rings. Another 32 $Tl^+$ ions fill site II opposite single six-rings in the supercage, each being $1.48{\AA}$ from the plane of three oxygens ($T1-O=2.70(1){\AA}$). About 18 $Tl^+$ ions occupy site III in the supercage ($T1-O=2.86(2){\AA}$), and the remaining 10 are found at site III' in the supercage ($T1-O=2.96(4){\AA}$).

• Korean Journal of Crystallography
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• v.17 no.1
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• pp.24-32
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• 2006

The microwave dielectric properties of $Zn_3Nb_2O_8\;with\;V_2O_5$ addition were investigated. The addition of $V_2O_5$ enhanced the sinterability of $Zn_3Nb_2O_8$, which resulted in high density of $Zn_3Nb_2O_8$ ceramic greater than 95% of the theoretical value when sintered at $900^{\circ}C$ for 4 hours. X-ray diffraction analysis of sintered $Zn_3Nb_2O_8$ ceramic showed no second phase with $V_2O_5$ addition. Dielectric permittivity(${\varepsilon}_r$) and quality factor($Q{\times}f$) varied with both density at different sintering temperature and $V_2O_5$ addition. Dielectric permittivity, quality factor and temperature coefficient($T_{cf}$) of the two mole of $V_2O_5\;added\;Zn_3Nb_2O_8$ that was sintered at $900^{\circ}C$ were 21.4, 40,000, $-54ppm/^{\circ}C$, respectively.