scholarly journals Фазовые равновесия в системах Ag8SnS6–Cu2SnS3 и Ag2SnS3–Cu2Sn4S9

Author(s):  
Vidadi A. Rzaguliyev ◽  
Oruj S. Kerimli ◽  
Dilbar S. Ajdarova ◽  
Sharafat H. Mammadov ◽  
Ozbek M. Aliev

Комплексными методами физико-химического анализа (дифференциально-термический, рентгенофазовый, микроструктурный, измерение микротвердости и определение плотности) изучены фазовые равновесия и построены Т–х фазовые диаграммыв системах Ag8SnS6–Cu2SnS3 и Ag2SnS3–Cu2Sn4S9. Показано, что система Ag8SnS6–Cu2SnS3является квазибинарным сечением квазитройной системы Ag2S-SnS2-Cu2S и относится кпростому эвтектическому типу с ограниченными областями растворимости на основеисходных сульфидов. Координаты эвтектической точки: 50 mol % Ag2SnS3 И Т = 900 К.Растворимость на основе Ag8SnS6 и Cu2SnS3 при эвтектической температуре простираетсядо 20 и 28 mol % соответственно. С уменьшением температуры твердые растворы распадаются и при 300 К составляют 5 и 10 mol %. Установлено, что с увеличением концентрацииAg8SnS6 в твердых растворах (Cu2SnS3)1-х (Ag8SnS6)х параметр кубической решетки увеличивается от а = 0.5445 nm (для чистого Cu2SnS3) до а = 0.725 nm (для состава х = 0.1) т. е. концентрационная зависимость параметра решетки имеет линейный характер.Система Ag2SnS3–Cu2Sn4S9 из-за перитектического плавления Cu2Sn4S9 имеет сложный характер и является частично квазибинарным сечением. Квазибинарность нарушается вобласти концентрации 65-100 mol % Cu2Sn4S9 и выше температуры 900 К. Твердые растворына основе Ag2SnS3 и Cu2Sn4S9 узкие и при 300 К составляют 10; 2.5 mol % соответственно         ЛИТЕРАТУРА1. Wang N., Fan A. K. An experimental study of the Ag2S-SnS2 pseudobinary join // Neues Jahrb. Mineral.-Abh, 1989, v. 160, pp. 33–36.2. Wang N. New data for Ag8SnS6 (canfeildite) and Ag8GeS6 (argyrodite) // Neues Jahrb. Mineral. Monatsh.,1978, pp. 269–272.3. Бабанлы М. Б., Юсибов Ю. А., Абишев В. Т. Трехкомпонентные халькогениды на основе медии серебра. Баку: Изд-во БГУ, 1993, 342 с.4. Parasyuk O. V., Chykhrij S. I., Bozhko V. V., Piskach L. V., Bogdanyuk M. S., Olekseyuk I. D.,Bulatetska L. V., Pekhnyo. Phase diagramm of the Ag2S–HgS–SnS2 system and single crystal prepartion,crystal structure and properties of Ag2HgSnS4 // J. Alloys and Compounds, 2005, v. 399, pp. 32–37. DOI:            https://doi.org/10.1016/j.jallcom.2005.03.0085. Olekseyuk I. D., Dudchak I. B., Piskach L. V. Phase equilibria in the Cu2S–ZnSe–SnS2 // J. Alloys andCompounds, 2004, v. 368, pp. 135–143. https:doi.org/10.1016/j.jallcom.2003.08.0846. Ollitrault-Fitchet R., Rivet J., Flahaut J., et.al. Description du systeme ternaire Ag–Sn–Se // J. Less-Common. Met., 1988, v. 138(2), pp. 241–261. DOI:https://doi.org/10.1016/0022-5088(88)90113-07. Delgado C. E., Mora A. J., Marcano E. Crystal structure refi nement of the semiconducting compoundCu2SnSe3 from X-ray powder difraction data // Mater. Res. Bull., 2003, v. 38, pp. 1949–1955. DOI: https://doi.org/10.1016/j.materresbull.2003.09.0178. Parasyuk O. V., Olekseyuk I. D., Marchuk O. V. The Cu2Se–HgSe–SnSe2 // J. Alloys and Compounds.,1999, v. 287, pp. 197–205. DOI: https//doi.org/10.1016/S0925-8388(99)00047-X9. Parasyuk O. V., Gulay L. D., Piskach L. V., Kumanska Yu. O. The Ag2Se–HgSe–SnSe2 system and thecrystal structure of the Ag2HgSnSe4 // J. Alloys and Сompounds, 2002, v. 339, pp.1 40–143. DOI: https//doi.org/10.1016/S0925-8388(01)01985-510. Babanly M. B., Yusibov Y. A., Babanly N. B. Electromotive force and measucement in several systema.Ed. by S. Kara, Intechneb. Org., 2011, pp. 57–58.11. Gulay L. D., Olekseyuk I. D., Parasyuk O. V. Crystal structure of b-Ag8SnSe6 // J. Alloys and compounds,2002, v. 339, pp. 113–117. DOI: https//doi.org/10.1016/S0925-8388(01)01970-312. Гусейнов Г. М. Получение соединения Ag8SnS6 в среде диметилформамида // Вестн. Томского гос. ун-та. Химия, 2016, № 1(3), c. 24–34. Режим доступа: fi le:///C:/Users/Lab351/Downloads/sub_%20%20in%20dimethylformamide%20medium.pdf (дата обращения: 19.09.2019)13. Gorchov O. Les composes Ag8MX6 (M = Si, Ge, Sn et X = S, Se, Te) // Bull. Soc. Chim. Fr., 1968, № 6.pp. 2263–2275.14. Kokhan O. P. The Interactions in Ag2X–BIVX2 (BIV – Si, Ge, Sn; X – S, Se) systems and the propertiesof compounds. Doctoral Thesis, Uzhgorod, Uzhgorod State Univ., 1996.15. Onoda U., Chen X. A., Sato A., Wada H. Crystal structure and twinning of monoclinic Cu2SnS3 // Mater.Res. Bull., 2000, v. 35, № 8, pp. 1563–1570. DOI: https//doi.org/10.1016/S0025-5408(00)00347-016. Рзагулиев В. А., Керимли О. Ш., Мамедов Ш. Г. Изучение квазитройной системы Ag2S–SnS2–Cu2S по разрезу Ag8SnS6–Cu2SnS3. Труды Международ. научно–практич. конф., Россия, Белгород,2019, c. 18.17. Рзагулиев В. А., Керимли О. Ш., Маме дов Ш. Г. Исследование квазибинарного разреза Cu2SnS3–Ag2SnS3 в квазитройной системеAg2S–Cu2S–SnS2 . Труды XXI Междун. конф., Санкт-Петербург, 2019,c. 20–21.18. Цигика В. В., Переш Е. Ю., Лазарев В. В. и др. Получение и свойства мнонокристаллов соединений/TlPbJ3, Tl3PbJ5, TlSnJ3, TlSn2J5 and Tl3PbBr5 Изв. АН СССР. Неорган. материалы, 1981, т. 17(6), c. 970–974.

2003 ◽  
Vol 07 (01) ◽  
pp. 58-69 ◽  
Author(s):  
Fumiihiro Maeda ◽  
Kenjiro Uno ◽  
Kazuchika Ohta ◽  
Makiko Sugibayashi ◽  
Naotake Nakamura ◽  
...  

When long alkylthio-substituted phthalocyaninato copper(II) complexes, ( C n S )8 PcCu , were rapidly prepared in an α-diol by using our developed see-through microwave reactor and/or a conventional hot stirrer, novel purple intermediates were selectively obtained instead of the expected green complex, ( C n S )8 PcCu , for some specific combinations of the reaction solvent and metal salt. The reaction conditions to obtain the purple intermediates were established and the unique molecular structure was clarified for a buthylthio-substituted intermediate by X-ray single crystal structure analysis.


1996 ◽  
Vol 51 (12) ◽  
pp. 1732-1738 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick

[(NH2)3PNP(NH2)3]Cl has been prepared by a three step synthesis. The last step is the ammonolysis of [Cl3PNPCl3]Cl. Single crystals of 1,1,1,3,3,3-hexaamino-1λ5, 3λ5-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -100 °C [(NH2)3PNP(NH2)3]Cl is subject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P1̄, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, β = 76.36(3)°, γ = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles.


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 272
Author(s):  
Seungyeol Lee ◽  
Huifang Xu ◽  
Hongwu Xu ◽  
Joerg Neuefeind

The crystal structure of moganite from the Mogán formation on Gran Canaria has been re-investigated using high-resolution synchrotron X-ray diffraction (XRD) and X-ray/neutron pair distribution function (PDF) analyses. Our study for the first time reports the anisotropic atomic displacement parameters (ADPs) of a natural moganite. Rietveld analysis of synchrotron XRD data determined the crystal structure of moganite with the space group I2/a. The refined unit-cell parameters are a = 8.7363(8), b = 4.8688(5), c = 10.7203(9) Å, and β = 90.212(4)°. The ADPs of Si and O in moganite were obtained from X-ray and neutron PDF analyses. The shapes and orientations of the anisotropic ellipsoids determined from X-ray and neutron measurements are similar. The anisotropic ellipsoids for O extend along planes perpendicular to the Si-Si axis of corner-sharing SiO4 tetrahedra, suggesting precession-like movement. Neutron PDF result confirms the occurrence of OH over some of the tetrahedral sites. We postulate that moganite nanomineral is stable with respect to quartz in hypersaline water. The ADPs of moganite show a similar trend as those of quartz determined by single-crystal XRD. In short, the combined methods can provide high-quality structural parameters of moganite nanomineral, including its ADPs and extra OH position at the surface. This approach can be used as an alternative means for solving the structures of crystals that are not large enough for single-crystal XRD measurements, such as fine-grained and nanocrystalline minerals formed in various geological environments.


2020 ◽  
Vol 75 (8) ◽  
pp. 765-768
Author(s):  
Bohdana Belan ◽  
Dorota Kowalska ◽  
Mariya Dzevenko ◽  
Mykola Manyako ◽  
Roman Gladyshevskii

AbstractThe crystal structure of the phase Ce5AgxGe4−x (x = 0.1−1.08) has been determined using single-crystal X-ray diffraction data for Ce5Ag0.1Ge3.9. This phase is isotypic with Sm5Ge4: space group Pnma (No. 62), Pearson code oP36, Z = 4, a = 7.9632(2), b = 15.2693(5), c = 8.0803(2) Å; R1 = 0.0261, wR2 = 0.0460, 1428 F2 values and 48 variables. The two crystallographic positions 8d and 4c show Ge/Ag mixing, leading to a slight increase in the lattice parameters as compared to those of the pure binary compound Ce5Ge4.


1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.


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