UA148594U - METHOD OF GROWING SOLID SOLUTION Ag ₇ Si _0.4 Ge _0.6 S ₅ I BY METHOD OF DIRECTED CRYSTALLIZATION OF ROS - Google Patents

Abstract

The method of growing a solid solution of Ag7Si0.4Ge0.6S5I by the method of directional crystallization from a melt-solution includes stepwise heating of vacuum quartz ampoules from pre-synthesized tetralogical halogen chalcogenides Ag7SiS5I and Ag7GeS5I, taken in accordance with K. to 1273 K and exposure at this temperature for 72 hours. for homogenization of the melt of the obtained charge. The charge is heated to a maximum temperature of 1223 K and kept at this temperature for 24 hours. and further growing single crystals at a rate of 0.4-0.5 mm / h, in vacuum quartz ampoules, by the method of directional crystallization from the melt-solution at a temperature of the melt zone 1223 K and annealing zone 873 K followed by annealing for 72 hours. Then the single crystal is cooled to room temperature at a rate of 5 K / h.

Description

A useful model belongs to the field of inorganic chemistry and inorganic materials science, in particular to the technology of growing single crystals of tetrahalogen sulfides, some of which are promising superionic materials with high cationic conductivity in the solid state.

The closest analogue to the proposed useful model is the method of growing solid solutions (Sy:-xAdh)/c1ez5iI by the method of directed crystallization from melt-solution (11.

The task of a useful model is to obtain a new superionic material with high cationic conductivity in the solid state.

The problem is solved in such a way that a method of growing a solid solution of Ad7bio(160655I by the method of directional crystallization from melt-solution, which includes stepwise heating of vacuumed quartz ampoules, from pre-synthesized tetrarhalogenchalcogenides Ad75isvi and Ad7sevzv5i, taken in a stoichiometric ratio, at a speed of 100 K /hour to 1273 K and holding at this temperature for 72 hours to homogenize the melt of the resulting batch, according to a useful model, the batch is heated to the maximum temperature of 1223 K and held at this temperature for 24 hours, and further growth of single crystals is carried out at a rate of 0 ,4-0.5 mm/h., in vacuumed quartz ampoules by the method of directional melt-solution crystallization at the temperature of the melt zone of 1223 K and the annealing zone of 873 K with subsequent annealing for 72 hours, after which the single crystal is cooled to room temperature at a rate 5 K/h.

The method was carried out as follows.

The synthesis of a solid solution of the composition Ad7siol(360655I to obtain single crystals was carried out from previously synthesized tetrarhalogenides Ad75ib5I and Ad;7Sbeb5iI, taken in stoichiometric ratios in vacuumed quartz ampoules.

The synthesis mode included stepwise heating at a rate from 100 to 1273 K with exposure at this temperature for 72 hours. Cooling was carried out with the furnace turned off.

The growth of single crystals of the Adbiol (eovO5BI) solid solution by crystallization from the melt solution was carried out in a vertical two-zone tubular resistance furnace using a quartz container of a special configuration. The temperature of the melt zone was 1223 K, the annealing zone - 873 K. In order to homogenize the melt, the ampoule was kept in the zone for 24 hours

From the melt. The growth of a single crystal consists of the formation of a seed in the lower cone-shaped part of the container by the collective recrystallization method within 48 hours. and crystal growth on the formed nucleus. The optimal speed of movement of the crystallization front was 0.4-0.5 mm/h, the cooling speed to room temperature was 5

K/hour According to this method, single crystals of Adobio4(C160v55iI) of dark gray color with a metallic luster, 30-40 mm long and 12 mm in diameter, were obtained (Fig. 1).

By the method of X-ray phase analysis (Fig. 2), with the help of the BISMOI 04 |Z, 41 program, the powders of the obtained single crystal were studied |2| and it was established that the solid solution of the composition Adbiol(zeovO5I crystallizes in cubic syngonia, space group E4Zt, a-10.6508(3) A, 7-4. The density determined by the method of hydrostatic weighing is 5981

KG/m3.

A useful model can be used in the preparation of a patent-protected superionic material with high cationic conductivity at room temperature.

Sources of information: 1. Pat. 120661 Ukraine IPC SZOVv 9/00, SZOV 13/00, SZOV 13/04 (2006.01). The method of growing solid solutions of the composition (Сц1-хАдх);/езЗЖІ by the method of directed crystallization from the melt-solution / Pogodin A. I., Kokhan O. P., Solomon A. M., Izai V. Yu., Studenyak I. P. ; applicant and owner of the patent "UzhNU" DVNZ. - Meo120661; y201705597, application 06.06.17.; published 10.11.17., Bull.

Mo21. - the closest analogue. 2. Kovba L.M. Radiography in inorganic chemistry / L.M. Kovba. - M.: Moscow State University Publishing House, 1991. - 2566.

Z. Gotseg 0. Ipdehipd m/yy She vyssevzvime dispoiotu teinod, RISMOI 04. // Maiepa!v 5igisiige. 2004, 11(2), 79. 4. Her otseg O. Romaeeg racet ipaehipa apa She dispoiyutu aIdopynt. // 2. Kyiv and Poag. Zirri 2007,

Claims (1)

26, 191-196. USEFUL MODEL FORMULA The method of growing a solid solution of Adbiol(ze0ovo5I) by the method of directed crystallization from a melt-solution, which includes stepwise heating of vacuumed quartz ampoules, from 60 pre-synthesized tetrarhalochalcogenides Ad7bibbI and Ad7SbebviI, taken in a stoichiometric ratio, with a speed from 100 to 1273 K and a holding time at this temperature for 72 hours to homogenize the melt of the resulting charge, which differs in that the charge is heated to a maximum temperature of 1223 K and held at this temperature for 24 hours, and further growth of single crystals is carried out at a rate of 0.4-0.5 mm/ h., in vacuumed quartz ampoules, by the method of directed crystallization from melt-solution at a temperature of the melt zone of 1223 K and an annealing zone of 873 K with subsequent annealing for 72 h, after which the single crystal is cooled to room temperature at a rate of 5 K/h. Z i u sonya i PKT OK MON z I SHE 5 s U EE o NV Y EN KK KN she I in pf 0 F W iya S EE . with VO: n I, ,IMTSTSYATSSHI PI, III ".................................AND.. Fig. 1