16(2)-03.fm
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1 Korean J. Crystallography Vol. 16, No. 2, pp.75~80, 2005 LiK 1 x Rb x (x = 0.1, 0.2) ½ ³aÁ½ aá½w bá yc aw» w x, bw» w w, cš w yw Structure Analysis of Mixed Crystals, LiK 1 x Rb x (x = 0.1, 0.2) Jin-Gyu Kim a, Youn Joong Kim a, Hae Jin Kim b and Il-Hwan Suh c a Division of Electron Microscopic Research, Korea Basic Science Institute, 52 Yeoeun-Dong, Yusung-Ku, Daejon , Korea b Frontier Research Laboratory, Korea Basic Science Institute, 52 Yeoeun-Dong, Yusung-Ku, Daejon , Korea c Department of Material Chemistry, Korea University, 208 Seochang, Chochiwon, Chung-nam , Korea LiK 1 Rb SO x x 4 (x = 0.1, 0.2) 313 K g. X- ray z w w œ P6 3 (#173) w. w e ƒ yw ƒƒ 3z z ewš Li w 3 x wš š, 6z z ewš K Rb ƒƒ O š. K Rb (0.91 : 0.09), (0.77 : 0.23) y w ƒ k w. Abstract LiK 1 Rb SO x x 4 (x = 0.1, 0.2) crystals were grown by means of aqueous solution growth technique at 313 K. Structure analysis of them was carried out with space group P6 3 (#173) by X-ray diffraction. In these compounds, the Li and ions lying on the three-fold axes formed infinite three-dimensional network and K and Rb atoms located on the six-fold axes are coordinated by twelve and fifteen O atoms respectively. The most suitable stabilization was achieved when the occupancy factors of K and Rb atoms are (0.91 : 0.09), (0.77 : 0.23) respectively. 1. Double sulfate family LiA, A(= Li, Na, K, Rb, Cs), w ƒ y w š. family ü tetrahedral sulfate groups orientation dynamics ùkù š š. 1-3) K ƒ hexagonal axis ew 9 O š, sulfate tetrahedral group w O ƒ p 3 sixfold axis ewš š. 4) Sulfate group w w w wš, Fig. 1 ùkü hexagonal P6 3 trigonal P31c unit cell 75
2 76 ½ ³Á½ Á½w Á y w wz w single crystal X-ray z» w šwš w. 2. x 2-1. LiK 1 x Rb x w Fig. 1. Crystallographic structure of LiK. (a) Hexagonal structure with the P6 3 phase at room temperature. (b) Trigonal structure with the P31c phase. One of tetrahedral of is rotated about a basal axis (marked r and r') or any equivalent axis. ü wù sulfate group z w. wr 5), w LiK w e y w LiK 1 xrb x (x = 0.1, 0.2, 0.5) w ƒ š ƒ. 6) Raman scattering briefringence d w Rb ƒ LiK wù, ƒ w w. w LiK 0.9 Rb 0.1 w NMR m w 10% Rb ƒ w w LiK trigonal monoclinic ƒ 50 K û šw. w 7) ƒ w Rb ƒƒ e w e š K ey ù. w LiK 1 xrb x (x = 0.1, 0.2) LiK 0.9 Rb 0.1 Li 2 ÁH 2 O, K 2 (90%) Rb 2 (80%) yww w š, rp (ICP- AES) w d w LiK 0.9 Rb 0.1 Rb 9.4 mol% y w. XRD w w š, xk ƒx v xk š. LiK 0.8 Rb 0.2 w X-ray n w x Enraf-Nonius CAD4 diffractometer w š, 8) cell parameters data collection w orientation matrix w. X-ray z graphite-monochromated Mo-Kα radiation(λ = ç) w ω-2θ scan w, 4.5 < θ < 27.4 ü ƒƒ 164 o 316 w. w z ƒ w 3 z kw d w q w. k 3 z 5 d w w, z 1% ü w d. d z Lorentz polarization effects w z, psi-scan 9) ww. SHELXS v w g w w š, SHELXL- 9) 97 v w y w. p, Wycoff letter 2(a) site ew K Rb occupancy factors y w, ƒ ƒƒ 0.91K Rb 0.77K Rb w w. e y w, R » w w
3 16«2y, 2005 LiK 1 xrb x (x = 0.1, 0.2) 77 Table 1. Summary of crystal data and structure refinement for LiK 1 xrb x (x = 0.1, 0.2) LiK 0.91 (x = 0.1) (x = 0.2) Crystal data Formular weight Temperature 293(2) K 293(2) K Wavelength Mo Kα radiation, ç Mo Kα radiation, ç Crystal system Hexagonal Hexagonal Space group P6 3 P6 3 Unit cell dimensions a = (5) ç, α =90 o a = (5) ç, α =90 o b = (5) ç, β =90 o c = 8.655(5) ç, γ = 120 o b = (5) ç, β =90 o c = (15) ç, γ = 120 o Volume (5) ç (4) ç 3 Z, Calculated density 2, Mg/m 3 2, Mg/m 3 Absorption coefficient mm mm 1 Crystal size mm mm Data Collection Diffractometer Enraf-Nonius CAD4 Enraf-Nonius CAD4 θ range for data collection 4.57~27.43 o 4.56~27.44 o Index ranges 1 <= h <= 5 0 <= h <= 6 0 <= k <= 6 6 <= k <= 5 0 <= l <= <= l <= 11 Reflections collected/unique 164/158 (R int = ) 316/285 (R int = ) Completeness to θ = 100% 100% Absorption correction Psi-scan Psi-scan Max. and min. transmission and and Used standard reflections 3 3 Intensity decay 1% 1% Refinement Refinement method Full-matrix least-squares on F 2 Full-matrix least-squares on F 2 Final R indices [I > 2σ(I)] R1 a = , wr2 b = R1 a = , wr2 b = R indices (all data) R1 a = , wr2 b = R1 a = , wr2 b = Weight w = 1/[σ 2 (F o2 ) + (0.0176P) P], w = 1/[σ 2 (F o2 ) + (0.0176P) P], where P = (F o2 + 2F c2 )/3 where P = (F o2 + 2F c2 )/3 Data/restraints/parameters 164/1/35 316/1/36 Goodness-of-fit on F Extinction coefficient none none Largest diff. peak and hole and eç and eç 3 Atomic scattering factors from International Tables for Crystallography 10) a R1 = Σ F o F c /Σ F o, b wr 2 = [Σ[w(F o 2 F c2 ) 2 /Σ[w(F o2 ) 2 ] 1/2 Table 2. Atomic coordinates ( 10 4 ) and equivalent isotropic displacement parameters (Å ) LiK 0.91 x y z S.O.F U(eq) x y z S.O.F U(eq) K (7) (2) (20) (3) Rb (140) (30) (20) (4) Li (40) (7) (20) (3) S (3) (1) (0) (1) O (18) (4) (8) (2) O2 3960(20) 3440(20) 2370(20) (3) 4077(14) 3493(14) 2599(8) (2) O2' 4080(30) 640(30) 2400(30) (4) 4043(15) 573(13) 2613(8) (2) U(eq) is defined as one-third of the trace of the orthogonalized U ij tensor.
4 78 ½ ³Á½ Á½w Á y w wz Table 1 š, t Table 2 ùkü. 3. š» Li(1), K(1), Rb(1), S(1), O(2) 6 e» wš. Li, S, O1 3-z z ewš, K Rb 6-z z ewš. w O2 t w, O2' disordering w y ùkü (Table 2). Table 1 Table 2 ùkù, w LiK 11),12) LiK 1 xrb x w w, LiK Rb Fig. 2. View along the c-axis of LiK 0.91 using ORTEP diagram. Thermal ellipsoids are drawn at 30% probability. Table 3. Selected bond distances (Å) and angles ( o ) for LiK 1 xrb x LiK 0.91 K-O (2) Rb-O (15) K-O (2) Rb-O (3) K-O1 a 2.990(2) Rb-O1 a 2.991(15) K-O1 a 2.997(2) Rb-O1 a 3.004(3) K-O1 b (17) Rb-O1 b 2.991(15) K-O1 b 2.997(2) Rb-O1 b 3.004(3) K-O2 c 2.816(17) Rb-O2 c 2.808(86) K-O2 c 2.877(15) Rb-O2 c 2.833(22) K-O2 d 2.816(17) Rb-O2 d 2.808(86) K-O2 d 2.877(15) Rb-O2 d 2.833(22) K-O2 e 2.816(17) Rb-O2 e 2.808(86) K-O2 e 2.877(15) Rb-O2 e 2.833(22) K-O (19) Rb-O (89) K-O (16) Rb-O (24) K-O2 f 2.971(19) Rb-O2 f 2.979(89) K-O2 f 2.985(16) Rb-O2 f 3.031(24) K-O2 g 2.971(19) Rb-O2 g 2.979(89) K-O2 g 2.985(16) Rb-O2 g 3.031(24) K-O2' c 2.821(22) Rb-O2' c 2.814(87) K-O2' c 2.858(16) Rb-O2' c 2.814(22) K-O2' d 2.821(22) Rb-O2' d 2.814(87) K-O2' d 2.858(16) Rb-O2' d 2.814(22) K-O2' e 2.821(22) Rb-O2' e 2.814(87) K-O2' e 2.858(16) Rb-O2' e 2.814(22) K-O2' 3.014(24) Rb-O2' 3.021(91) K-O2' 2.983(16) Rb-O2' 3.030(24) K-O2' f 3.014(24) Rb-O2' f 3.021(91) K-O2' f 2.983(16) Rb-O2' f 3.030(24) K-O2' g 3.014(24) Rb-O2' g 3.021(91) K-O2' g 2.983(16) Rb-O2' g 3.030(24) S-O (16) Li-O1 j 1.859(33) S-O (7) Li-O1 j 1.911(13) S-O (12) Li-O (15) S-O (6) Li-O (7) S-O2 h 1.499(12) Li-O2 k 1.921(15) S-O2 h 1.460(6) Li-O2 k 1.923(7) S-O2 i 1.499(12) Li-O2 l 1.921(15) S-O2 i 1.460(6) Li-O2 l 1.923(7) S-O2' 1.451(15) Li-O2' f 1.952(17) S-O2' 1.475(6) Li-O2' f 1.921(7) S-O2' h 1.451(15) Li-O2' i 1.952(17) S-O2' h 1.475(6) Li-O2' i 1.921(7) S-O2' i 1.451(15) Li-O2' m 1.952(17) S-O2' i 1.475(6) Li-O2' m 1.921(7) O1-S-O (8) O1 j -Li-O (2) O1-S-O (3) O1 j -Li-O (6) O2-S-O2 h 110.2(8) O2-Li-O2 k 112.5(10) O2-S-O2 h 109.9(3) O2-Li-O2 k 113.9(4) O2 h -S-O2 i 110.2(8) O2 k -Li-O2 l 112.5(10) O2 h -S-O2 i 109.9(3) O2 k -Li-O2 l 113.9(4) O1-S-O2' 110.5(11) O1 j -Li-O2' f 105.2(13) O1-S-O2' 109.3(3) O1 j -Li-O2' f 105.2(13) O2'-S-O2' h 108.4(11) O2' f -Li-O2' h 113.4(11) O2'-S-O2' h 109.6(3) O2' f -Li-O2' h 104.2(5) O2' h -S-O2' i 108.4(11) O2' h -Li-O2' i 113.4(11) O2' h -S-O2' i 109.6(3) O2' h -Li-O2' i 104.2(5) Symmetry codes: (a) x 1, y 1, z; (b) x 1, y, z; (c) x, y, z 1/2; (d) y, x+y, z 1/2; (e) x y, x, z 1/ 2; (f) y, x y, z; (g) x+y, x, z; (h) y + 1, x y, z; (i) x+y+1, x + 1, z; (j) x + 1, y + 1, z + 1/2; (k) y + 1, x y + 1, z; (l) x+y, x + 1, z; (m) x, y + 1, z.
5 16«2y, 2005 LiK 1 xrb x (x = 0.1, 0.2) 79 e w, cell parameters w š, K e ey œ. K Rb t R w EXYZ constraint j š y ww» š. w w» w Fig. 2 13) ORTEP v w LiK 0.91 c- unit cell ùkü.» sulfate groups K r, Fig. 1 w P6 3 w e, K Rb 6 LiO 4 groups w. K 2.816(17) ç ~ 2.990(2) ç ü 12 O w š, Rb 2.808(86) ç ~ 3.021(91) ç ü 15 O w. w K 2.858(15) ç ~ 2.997(2) ç ü 15 w š, Rb w 2.833(22) ç ~ 3.031(24) ç ü 15 w š. w K O w sulfate tetrahedral group. ü w ¼ ƒ Table 3 ùkü. Fig. 3 tetrahedral LiO4 group ù kü. LiK 1 xrb x LiK ü O2 ƒ disordering. Rb ƒ unit cell y œ w w O2 anisotropic displacementƒ w. w tetrahedral ( wƒ ) o w. LiK 0.91 ü w¼ wƒ r, S-O1 = 1.449(16) ç, S-O2 = 1.499(12) o ç š, O1-S-O2 = 108.7(8) o, O2-S-O2 = 110.2(8) p tetrahedral ƒ š. ƒ LiO 4 ü w¼ wƒ r Li- O1 = 1.859(33) ç, Li-O2 = ç š o, O1-Li- O2 = 106.3(2) o, O2-Li-O2 = 112.5(10) p tetrahedral x wš. w ü w¼ wƒ r, S-O1 = 1.464(7) ç, S-O2 = 1.460(6) ç š o, O1-S-O2 = 109.0(3) o, O2-S-O2 = 109.9(3) tetrahederal x wš w¼ wƒ w tetrahedral x wš Fig. 3. ORTEP diagram of the tetrahedral group and LiO 4 group. Fig. 4. View of network of tetrahedral chain in the crystal. The O2' atoms are omitted for simplicity of the structure. The thermal ellipsoids are drawn to a scale of 50% probability.
6 80 ½ ³Á½ Á½w Á y w wz š, Li groups p tetrahedral x wš. sulfate groups K Rb coordination š w š. š Rb ƒ y k e wš š w. w yw ƒ þƒ x mw v w., Fig. 4 ü LiO 4 groups tetrahedral chain network [100] w ùkü. Tetrahedral chain š O w š. p, O1 [001] w S Li w tetrahedral group chain x w w wš, O2 O2' 3-z z e w [210], [110], [120] w tetrahedral groups w 3 network x wš. 4. LiK 1 xrb x (x = 0.1, 0.2) XRD» w ww,. 1) w LiK e w, Rb ƒ w cell parametersƒ y š. w Rb unit cell j wš K e ey w. 3) ƒ Rb ƒ O coordination y w tetrahedral sulfate groups» wš. 4) O1, O2 w LiO 4 tetrahedral groupsƒ chain 3 network x wš. š x 1) Cummins, H. Z., Phys. Rep., 185, 211 (1990). 2) Desért, A., Gibaud, A., Righi, A., Leitão, U. A. and Moreira, R. L., J. Phys.: Condens. Matter, 7, 8445 (1995). 3) Willis, F., Leisure, R. G. and Kanashiro, T., Phys. Rev. B, 54, 9077 (1996). 4) Tomaszewski, P. E. and Lukaszewicz, K., Phase Transit., 4, 37 (1983). 5) Bansal, M. L. and Roy, A. P., Phys. Rev. B, 30, 7307 (1984). 6) Moreira, R. L., Bourson, P., Leitao, U. A., Righi, A., Belo, L. C. M. and Pimenta, M. A., Phys. Rev. B, 52, (1995). 7) Kim, H. J., Jeong. D. Y., Zalar. B., Blinc, R. and Choh, S. H., Phys. Rev. B, 61, 9307 (2000). 8) Enraf-Nonius CAD4 Express software. Structure Determination Package, Enraf-Nonius, Delft The Netherlans (1994). 9) Sheldrick, G. M., SHELXS and SHELX-97, Program for the Refinement of Crystal Structures, University of Gottingen, Germany (1997). 10) International Tables for Crystallography, Vol. C, by Wilson, A. J. C., Kluwer Academic Publisher, Dordrecht, Netherlands (1995). 11) Karppinen, M., Lundgren, J. O. and Liminga, R., Acta Cryst., C39, 34 (1983). 12) Sandhya, B. T., Sequeira, A. and Chidambram, R., Acta Cryst., Sect., C40, 1648 (1984). 13) Burnett, M. N. and Johnson, C. K., ORTEP III, Oak Ridge National Lab. Tennessess, U.S.A. (1996).
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Journal of the Korean Ceramic Society Vol. 43, No. 1, pp. 859~864, 006. FE Analysis of Alumina Green Body Density for Pressure Compaction Process Jong-In Im and Young-Jin Yook Simulation Center for Fine
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Journal of the Korean Chemical Society 2007, Vol. 51, No. 4 Printed in the Republic of Korea w x - w y *Á š w w w yw (2007. 3. 28 ) Case Study on Verbal Interactions of Teacher-Small Group StudentsG in
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Journal of the Korean Ceramic Society Vol. 44, No. 1, pp. 12~17, 2007. A Study on the Preparation of Bone Ash and Celadon Bone Body Using Pig Bone Jae-Jin Jeong, Sang-Hee Lee, Yong-Seok Lee,* and Byung-Ha
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Journal of the Korean Ceramic Society Vol. 46, No. 3, pp. 295~300, 2009. DOI:10.4191/KCERS.2009.46.3.295 Analysis of Oxide Coatings Formed on Al1050 Alloy by Plasma Electrolytic Oxidation Bae-Yeon Kim,
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w CAD/CAM wz 15«3y 2010 6 pp. 189-203 œ w w *, **, x***, v ** The Conceptual Design of Semi-submersible Type Mobile Harbor Using Axiomatic Design Principles Joohee Lee*, Seongjin Yoon**, Hyun Chung***
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2007, Vol. 51, No. 2 Printed in the Republic of Korea xw yw w w» e w z Á Á y Áw # Á k * w yw w w w w w # w w w (2006. 10. 30 ) Influences of Current Education Programs for Preservice Chemistry Teachers
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w y wz 10«( 1y) 47~52, 2007 J. of the Korean Society for Environmental Analysis œ w t y ½ xá Á x Á½ Á x* Ÿ œ, * w œw Optimization of Coagulation In The Conventional Water Treatment Plant Jun-Hyun Kim,
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JOURNAL OF KOREA SOCIETY OF PACKAGING SCIENCE & TECHNOLOGY. Vol. 14, No. 1 1~8 (2008) s w Á w» w Comparative Study on the Changes and Prospects of Flexible Food Packaging Design Kyung Soo Noh and Wang
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Jurnal f the Krean Ceramic Sciety Vl. 46, N. 6, pp. 643~647, 2009. DOI:10.4191/KCERS.2009.46.6.643 Densificatin Behavir f C/C Cmpsite Derived frm Cal Tar Pitch with Small Amunt f Idine Additin Kwang Yun
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w y wz 11«1y 73~80 (2011.8.) Journal of Korean Society of Urban Environment SWMM 을이용한도시지역비점오염부하저류시설용량산정 Áw«Á *Áy **Á½ yá½ Á x w w Á* û w y œw Á** w y lœw (2011 6 13, 2011 6 27 k) Determine Capacity of
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Krean J. Crystallgraphy Vl., N. 1, pp.14~18, 006 LP-MOCVD w ZnO ù Ÿw p Á yá * w w» w» l Structural and Optical Prperties f ZnO Nanwires Synthesized by LP-MOCVD Prcess Yung-Jin Chi, Jae-Hwan Park and Jae-Gwan
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Atmosphere. Korean Meteorological Society Vol. 21, No. 1 (2011) pp. 123-130 w EUV-B p k D w w Á½ y* w»y w ( : 2010 12 1, : 2011 2 18, y : 2011 3 19 ) The Radiative Characteristics of EUV-B over the Korean
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Korean Journal of Remote Sensing, Vol.23, No.2, 2007, pp.45~52 Measurement of Backscattering Coefficients of Rice Canopy Using a Ground Polarimetric Scatterometer System Suk-Young Hong*, Jin-Young Hong**,
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w wz J. Kor. Soc. Cloth. Ind. 8«2y, 2006 Vol. 8, No. 2, pp.177-182(2006) x w e w 1) Á Ÿ 1) Á»û 2) 1) ƒm w q w 2) w w w The Effect of Media on Taking Plastic Surgery Chong-Hee Yun 1), Su-Kwang Sung 1) and
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Journal of the Korean Ceramic Society Vol. 45, No. 7, pp. 395~400, 2008. Preparation and its Characteristics of Fly Ash-based Geopolymeric Mortar using Low Grade Silica Waste Se Gu Son, Seung Yeob Hong,